WO2015180080A1 - Method for preparing micropore atomization sheet, micropore atomization sheet, and micropore atomization apparatus - Google Patents

Method for preparing micropore atomization sheet, micropore atomization sheet, and micropore atomization apparatus Download PDF

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Publication number
WO2015180080A1
WO2015180080A1 PCT/CN2014/078703 CN2014078703W WO2015180080A1 WO 2015180080 A1 WO2015180080 A1 WO 2015180080A1 CN 2014078703 W CN2014078703 W CN 2014078703W WO 2015180080 A1 WO2015180080 A1 WO 2015180080A1
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WO
WIPO (PCT)
Prior art keywords
film
microporous
sheet
base material
oxide
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PCT/CN2014/078703
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French (fr)
Chinese (zh)
Inventor
王长津
Original Assignee
王长津
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Application filed by 王长津 filed Critical 王长津
Priority to PCT/CN2014/078703 priority Critical patent/WO2015180080A1/en
Publication of WO2015180080A1 publication Critical patent/WO2015180080A1/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B17/00—Apparatus for spraying or atomising liquids or other fluent materials, not covered by the preceding groups
    • B05B17/04—Apparatus for spraying or atomising liquids or other fluent materials, not covered by the preceding groups operating with special methods
    • B05B17/06—Apparatus for spraying or atomising liquids or other fluent materials, not covered by the preceding groups operating with special methods using ultrasonic or other kinds of vibrations
    • B05B17/0607—Apparatus for spraying or atomising liquids or other fluent materials, not covered by the preceding groups operating with special methods using ultrasonic or other kinds of vibrations generated by electrical means, e.g. piezoelectric transducers
    • B05B17/0638—Apparatus for spraying or atomising liquids or other fluent materials, not covered by the preceding groups operating with special methods using ultrasonic or other kinds of vibrations generated by electrical means, e.g. piezoelectric transducers spray being produced by discharging the liquid or other fluent material through a plate comprising a plurality of orifices
    • B05B17/0646—Vibrating plates, i.e. plates being directly subjected to the vibrations, e.g. having a piezoelectric transducer attached thereto

Definitions

  • the invention relates to atomization technology, in particular to a preparation method of a microporous atomization sheet, a micropore atomization sheet and a micropore atomization device. Background technique
  • the atomized sheet is widely used in air humidifiers, incense burners, beauty machines, lung drug delivery devices, sterilizers, bathtub fog machines and the like.
  • the main atomizing sheets are metal atomizing sheets, ceramic atomizing sheets, organic material atomizing sheets, etc., among which metal atomizing sheets such as stainless steel atomizing sheets, nickel-plated atomizing sheets, titanium-plated atomizing sheets, etc. It has certain advantages of fatigue resistance, easy cleaning, and not easy to break. It is widely used in aerosol generators for different purposes, and its share has an absolute market advantage. However, the long-term use of the metal atomized sheet inevitably leads to the precipitation of harmful metal ions, thereby affecting the liquid component, and if it is applied to the aerosol generator of the drug delivery device, it may even be harmful to human health.
  • Ceramic atomized sheets or organic material atomized sheets also have a certain market share, but due to the nature of the materials themselves, the atomized sheets are easily broken and require very careful cleaning. On the other hand, the energy required for atomization essentially acts on the atomizing sheet, and the life of the atomized sheet of the organic material is greatly reduced as the temperature rises.
  • the microporous pore size of the atomized sheet reported in the literature and patents is as small as 3 micrometers, and the aerosol particles of 1-5 micrometers are about 50%, but the atomized sheet is extremely easy to block. The finer the pore size of the atomizing sheet, the more easily the atomized sheet is blocked.
  • the existing aerosol generators on the market when the atomizing sheet starts to work, the aerosol particles sprayed have a large specific surface area and are easily adsorbed in the atomization zone.
  • the aerosol particles accumulated in the atomization zone hinder the subsequent aerosol atomization of the aerosol particles, affecting the amount of fog and the atomization rate.
  • embodiments of the present invention provide a method for preparing a microporous atomized sheet, a microporous atomizing sheet, and a micropore atomizing device.
  • the technical solution of the embodiment of the present invention is as follows:
  • the embodiment of the present invention provides a method for preparing a microporous atomized sheet, wherein the atomized sheet is used as a base material; the method includes: a film is deposited on the inner wall of the microporous channel and its surface;
  • the substrate material on which the film is deposited is cured.
  • the atomizing sheet is any one of a metal atomizing sheet, a ceramic atomizing sheet, and an organic material atomizing sheet.
  • the depositing a film on the inner wall of the microporous channel of the base material and the surface thereof comprises:
  • Step 1 placing the substrate material in the reaction chamber
  • Step two introducing a first precursor, reacting the first precursor with a material of the inner wall of the microporous channel of the base material and a surface thereof;
  • Step 3 After the reaction is completed, the reaction chamber is purged with a cleaning gas, or the reaction chamber is evacuated, and the free first precursor is discharged from the reaction chamber, and then Second precursor
  • Step 4 The steps 2 and 3 are performed cyclically until a film of a predetermined thickness is deposited on the inner wall of the microporous channel of the base material and the surface thereof.
  • the film is one or more layers of thickness-hooked film
  • the film is any one of the following films;
  • the film is a multilayer film formed by overlapping any one of the following films, or a multilayer film formed by alternately overlapping any of the following, or a multilayer film formed by overlapping one of the following And a combined multilayer film of a plurality of layers formed by alternately overlapping with any of the following;
  • the film comprises: an alumina (A1 2 0 3 ) film, a silicon dioxide (Si0 2 ) film, and a dioxane Titanium (Ti0 2 ) film, zinc oxide (ZnO) film, hafnium oxide (Hf0 2 ) film, magnesium oxide (MgO) film, zirconium dioxide (Zr0 2 ) film, nickel oxide (NiO) film, cobalt oxide ( CoO) thin film (FeO x ) film formed by film and iron oxide, thin film (CuO x ) film formed by copper oxide, boron oxide (B 2 0 3 ) film, indium oxide (In 2
  • the curing the substrate material deposited with the film comprises: plasma curing the substrate material deposited with the film.
  • the method before the film is deposited on the inner wall of the microporous channel of the base material and the surface thereof, the method further includes:
  • the substrate material is activated.
  • the activation comprises: chemical solution impregnation activation and ultraviolet activation.
  • the step of impregnating and activating the chemical solution comprises:
  • the base material is immersed in an acidic solution for ultrasonic cleaning for 5-30 min, and then the base material is washed with distilled water, and washed until the pH of the surface liquid attached to the base material is neutral;
  • the base material was immersed in an alkaline solution for ultrasonic cleaning for 5 to 30 minutes, and then the base material was washed with distilled water, and washed until the pH of the liquid adhering to the surface of the base material was neutral.
  • the step of ultraviolet activation comprises: The substrate material is placed under an ultraviolet lamp or in a plasma atmosphere capable of generating ultraviolet gas, and irradiated with ls-120s for activation.
  • the embodiment of the present invention further provides a microporous atomization sheet, wherein the microporous atomization sheet is provided with a micropore region, and a plurality of micropores are distributed in the micropore region; The inner wall of the pore channel and the surface thereof are coated with a film; the pore diameter of the micropores is 0.05 ⁇ -20 ⁇ .
  • the number of micropores in the microporous region is 100-1000000.
  • the microporous atomized sheet has a diameter of from 1 to 50 mm.
  • the outer diameter of the microporous region is l-50 mm.
  • the microporous atomizing sheet is any one of a metal atomizing sheet, a ceramic atomizing sheet, and an organic material atomizing sheet.
  • the inner wall of the microporous channel of the microporous atomization sheet and the coating material of the surface thereof are one or more layers of uniform thickness;
  • the coating material is any one of the following films; when the coating material is a plurality of layers, the coating material is overlapped by any one of the following films a multilayer film formed, or a multilayer film formed by alternately overlapping any of the following, or a composite film of a multilayer film formed by overlapping one of the following and a multilayer film of any of the following alternately stacked layers;
  • the shape of the microporous channel in the microporous atomization sheet is any one of a circular shape, a triangular shape, an elliptical shape, a square shape and a horn shape.
  • the cross-sectional shape of the microporous channel in the microporous atomization sheet is any one of a parabolic shape, a horn shape, a square shape and a trapezoidal shape.
  • the embodiment of the invention further provides a micropore atomization device, the micropore atomization device comprising: an atomizer housing, an aerosol generator connected to the atomizer housing, and an atomizer An electronic circuit controller connected to the cabinet; wherein the gas mist generator comprises a microporous atomizing sheet, and the microporous atomizing sheet is any of the microporous atomizing sheets described above.
  • the microporous atomized sheet prepared by using the embodiment of the invention has a pore size which can be precisely controlled between several nanometers and several tens of micrometers, that is, the size of the micropore diameter of the microporous atomized sheet can be accurately controlled,
  • the ultra-fine aerosol particles can be realized; in addition, since the atomization sheet selected in the embodiment of the invention is an atomization sheet commonly used in the market, and the atomization sheet can have the aperture of the atomization area thereof according to the embodiment of the invention Therefore, the embodiment of the present invention can lay a foundation for realizing the versatility of the atomized sheet in the aerosol generator in various fields.
  • FIG. 1 is a schematic flow chart of an implementation process of a method for preparing a microporous atomization sheet according to an embodiment of the present invention
  • FIG. 2 is a schematic flow chart 2 of a method for preparing a microporous atomization sheet according to an embodiment of the present invention
  • FIG. 4 is a cross-sectional view of a microporous orifice in a microporous atomization sheet according to an embodiment of the present invention
  • FIG. 5 is a schematic structural view of an atomizer case according to an embodiment of the present invention.
  • FIG. 6 is a schematic structural view 1 of an aerosol generator according to an embodiment of the present invention.
  • FIG. 7 is a schematic structural view 2 of an aerosol generator according to an embodiment of the present invention.
  • FIG. 8 is a schematic structural diagram of an electronic circuit controller according to an embodiment of the present invention.
  • FIG. 1 is a schematic flow chart showing the implementation of a method for preparing a microporous atomized sheet according to an embodiment of the present invention, and the atomized sheet is used as a base material; as shown in FIG. 1, the method includes:
  • Step 101 depositing a film on the inner wall of the microporous channel of the base material and the surface thereof; wherein the atomizing sheet is any one of a metal atomizing sheet, a ceramic atomizing sheet and an organic material atomizing sheet.
  • the substrate material is placed in the reaction chamber, and each precursor is alternately introduced into the reaction chamber in a pulsed gas manner, and a film is deposited on the inner wall of the microporous channel of the base material and the surface thereof;
  • the purge gas such as an inert gas or the like is purged in the gap before the introduction of the precursor and before the passage into the next precursor.
  • the reaction chamber is subjected to a vacuum treatment to isolate the two precursors before and after, so that the two precursors do not simultaneously appear in the reaction chamber.
  • the depositing a film on the inner wall of the microporous channel of the substrate material and the surface thereof comprises:
  • Step 1 placing the substrate material in the reaction chamber
  • Step two introducing a first precursor, reacting the first precursor with a material of the inner wall of the microporous channel of the base material and a surface thereof;
  • Step 3 After the reaction is completed, the reaction chamber is purged with a cleaning gas, or the reaction chamber is evacuated, and the free first precursor is discharged from the reaction chamber, and then Second precursor
  • Step 4 The steps 2 and 3 are performed cyclically until a film of a predetermined thickness is deposited on the inner wall of the microporous channel of the base material and the surface thereof.
  • the entire experimental process is carried out under vacuum, but before the first pulse precursor, the pressure of the reaction chamber is in the range of OPa to l (T 2 Pa;
  • the method of introducing a precursor into the reaction chamber, each pulse precursor 0. 015S -50S, after the pulse is completed once, a flow rate of 0sccm-120sccm of argon Ar or nitrogen is introduced into the reaction chamber.
  • each precursor may enter the reaction chamber through a carrier gas, the carrier may be nitrogen N 2 or argon Ar; Since argon gas Ar or nitrogen gas N 2 is introduced into the reaction chamber in the gap between the two precursors of the pulse, excess precursor and reaction by-products in the reaction chamber can be discharged.
  • the flow rate of the argon gas Ar or the nitrogen gas N 2 introduced into the reaction chamber is Osccm, it means that no gas is introduced into the reaction chamber, and at this time, since the reaction chamber still maintains a vacuum. State, therefore, a free portion or reaction by-product in the precursor of the last pulse can be discharged by a vacuuming process.
  • the first-passed precursor may be chemically adsorbed with the material of the inner wall of the microporous channel of the base material and the surface thereof to form a first film, and then the first film and the second-pass precursor are formed. The reaction takes place to form a second film, and so on, until a film of a predetermined thickness is formed; wherein each precursor can be arbitrarily selected according to the chemical composition of the film.
  • the film is one or more layers of thickness-hooked film
  • the film is any one of the following films;
  • the film is a multilayer film formed by overlapping any one of the following films, or a multilayer film formed by alternately overlapping any of the following, or a multilayer film formed by overlapping one of the following And a combined multilayer film of a plurality of layers formed by alternately overlapping with any of the following:
  • the film comprises: A1 2 0 3 film, SiO 2 film, Ti0 2 film, ZnO film, Hf0 2 film, MgO film, Zr0 2 film , NiO film, CoO film, FeO x film, 01 ( 3 ⁇ 4 film, B 2 0 3 film, In 2 0 3 film, Sn0 2 film, Ga 2 0 3 film, Nb 2 0 5 film, Gd 2 0 3 film, Ta 2 0 5 film, BN film, A1N film, TiN film, SiC film, ZnS film, ZrS film, HA film, W film, Pt film, Ru film, Pd film, PMDA-DAH film,
  • the base material on which the thin film is deposited is subjected to plasma curing
  • the energy of the plasma of the inert gas reaches the surface of the base material is mild, and the film of the inner wall of the microporous channel of the base material and the film of the surface thereof are not chemically oxidized.
  • the reaction, and the plasma of the inert gas can provide energy for the film of the inner wall of the microporous channel of the base material and the film of the surface thereof, and the substrate material, thereby being plasma-cured with an inert gas as compared with the conventional annealing curing.
  • the film of the inner wall of the microporous channel of the base material and the film on the surface thereof are not resistant to high temperature, causing damage to the material of the film, and on the other hand, the film on the inner wall of the microporous channel of the base material. Under the condition that the base material is not etched, the film of the inner wall of the microporous channel of the base material and the bonding property with the base material can be improved.
  • the step of curing comprises: placing a substrate material deposited with a film into a plasma generator to cure ls-200s; wherein the power of the plasma generator is 50W-500W, and the curing gas is ⁇ He, ⁇ Ne a combination of one or more of an inert gas such as argon Ar, krypton Kr and ⁇ Xe, having a gas flow rate of 10 sccm to 200 sccm;
  • an inert gas or the like is introduced into the ion generator with a certain gas flow, and the inert gas is converted into a plasma corresponding to the inert gas by the ion generator, and the substrate material deposited with the film is in a plasma atmosphere of an inert gas. Cured.
  • the method before the step 101, the method further includes:
  • the substrate material is washed.
  • the substrate material is ultrasonically cleaned.
  • the method before the step 101, the method further includes:
  • the substrate material is activated.
  • the method before the step 101, the method further includes:
  • the cleaned substrate material is activated.
  • FIG. 2 is a schematic diagram 2 of an implementation flow of a method for preparing a microporous atomization sheet according to an embodiment of the present invention. As shown in FIG. 2, the method includes:
  • Step 201 cleaning the base material by using the atomized sheet as a base material; wherein the atomized sheet is any one of a metal atomized sheet, a ceramic atomized sheet, and an organic material atomized sheet.
  • Step 202 activating the cleaned substrate material
  • the activation includes: chemical solution impregnation activation and ultraviolet activation;
  • step of impregnating and activating the chemical solution comprises:
  • Step A immersing the base material in an acidic solution for ultrasonic cleaning for 5-30 min, then washing the base material with distilled water, and washing until the pH of the surface liquid attached to the base material is neutral;
  • Step B The base material is immersed in an alkaline solution for ultrasonic cleaning for 5-30 min, and then the base material is washed with distilled water, and washed until the pH of the liquid attached to the surface of the base material is neutral.
  • the acidic solution is a weakly acidic solution in which one or several acids are diluted; and the acidic solution is one or a mixture of the following solutions; the solution includes: a concentration of 0.01- 5g / L phosphoric acid solution, concentration of 0.1-7g / L oxalic acid solution, concentration of l-10 g / L acetic acid solution, concentration of 0.01-lg / L hydrochloric acid solution, concentration of 0.1-2g / L hydrofluoric acid solution, concentration It is a 5-20 g/L ammonium hydrogen fluoride solution;
  • the acidic solution is one or a mixture of the following solutions; the solution comprises: a concentration of lg/L phosphoric acid solution, a concentration of 15 g/L hydrogen fluoride ammonia solution, a concentration of 0.1 g /L hydrofluoric acid solution.
  • the acidic solution is one or a mixture of any of the following solutions;
  • the solution comprises: a concentration of 5 g / L of oxalic acid solution, a concentration of 10 g / L of hydrogen fluoride ammonia solution; in an embodiment, the acidic solution is one or a mixture of the following solutions; the solution To include: a concentration of 6.5 g / L acetic acid solution, a concentration of 0.05 g / L hydrochloric acid solution, a concentration of 10 g / L hydrogen fluoride ammonia solution.
  • the alkaline solution is aqueous ammonia having a mass percentage of 1 to 20%; in one embodiment, the alkaline solution is aqueous ammonia having a mass percentage of 5-15%.
  • the step of ultraviolet activation comprises: activating the substrate material under an ultraviolet lamp or in a plasma atmosphere capable of generating ultraviolet gas by irradiating ls-120s.
  • Step 203 depositing a film on the inner wall of the microporous channel of the base material after activation and a surface thereof;
  • the activated substrate material is placed in the reaction chamber, and each precursor is alternately introduced into the reaction chamber in a pulsed manner, and a film is deposited on the inner wall of the microporous channel of the base material and the surface thereof. ;
  • the purge gas such as an inert gas or the like is purged in the gap before the introduction of the precursor and before the passage into the next precursor.
  • the reaction chamber is subjected to a vacuum treatment to isolate the two precursors before and after, so that the two precursors do not simultaneously appear in the reaction chamber.
  • the depositing a film on the inner wall of the microporous channel of the substrate material and the surface thereof comprises:
  • Step 1 placing the substrate material in the reaction chamber
  • Step two introducing a first precursor, reacting the first precursor with a material of the inner wall of the microporous channel of the base material and a surface thereof;
  • Step three after the reaction is completed, purging the reaction chamber with a cleaning gas, or After the reaction chamber is evacuated, the free first precursor is discharged into the reaction chamber, and then the second precursor is introduced;
  • Step 4 The steps 2 and 3 are performed cyclically until a film of a predetermined thickness is deposited on the inner wall of the microporous channel of the base material and the surface thereof.
  • the entire experimental process is carried out under vacuum, but before the first pulse precursor, the pressure of the reaction chamber is in the range of OPa to l (T 2 Pa;
  • the method of introducing a precursor into the reaction chamber, each pulse precursor 0. 015S -50S, after the pulse is completed once, a flow rate of 0sccm-120sccm of argon Ar or nitrogen is introduced into the reaction chamber.
  • each precursor may enter the reaction chamber through a carrier gas, the carrier may be nitrogen N 2 or argon Ar; Since argon gas Ar or nitrogen gas N 2 is introduced into the reaction chamber in the gap between the two precursors of the pulse, excess precursor and reaction by-products in the reaction chamber can be discharged.
  • the flow rate of the argon gas Ar or the nitrogen gas N 2 introduced into the reaction chamber is Osccm, it means that no gas is introduced into the reaction chamber, and at this time, since the reaction chamber still maintains a vacuum. State, therefore, a free portion or reaction by-product in the precursor of the last pulse can be discharged by a vacuuming process.
  • the first-passed precursor may be chemically adsorbed with the material of the inner wall of the microporous channel of the base material and the surface thereof to form a first film, and then the first film and the second-pass precursor are formed. The reaction takes place to form a second film, and so on, until a film of a predetermined thickness is formed; wherein each precursor can be arbitrarily selected according to the chemical composition of the film.
  • the film is one or more layers of thickness-hooked film
  • the film is any one of the following films;
  • the film is a multilayer film formed by overlapping any one of the following films, or a multilayer film formed by alternately overlapping any of the following, or a multilayer film formed by overlapping one of the following a combined multilayer film of a multilayer film formed by alternately overlapping any of the following;
  • the film comprises: A1 2 0 3 film, SiO 2 film, Ti 2 film, ZnO film, Hf0 2 film, MgO film, Zr0 2 film, NiO film, CoO film, FeO x film, 01 (3 ⁇ 4 film, B 2 0 3 film, In 2 0 3 film, Sn0 2 film, Ga 2 0 3 film, Nb 2 0 5 film, Gd 2 0 3 film, Ta 2 5 film, BN film, A1N film, TiN film, SiC film, ZnS film, ZrS film, HA film, W film, Pt film, Ru film, Pd film, PMDA-DAH film, PMDA-ODA film, PM
  • Step 204 Curing the substrate material on which the film is deposited.
  • the substrate material on which the thin film is deposited is subjected to plasma curing, and the step of plasma curing comprises: placing a substrate material deposited with a thin film into a plasma generator to cure ls-200s; wherein the plasma
  • the power of the body generator is 50W-500W
  • the curing gas is a combination of one or more of He, Ne, Ar, Kr, Xe, and the gas flow rate is 10 sccm-200 sccm.
  • the pore size of the microporous atomized sheet prepared by using the embodiment of the invention can be precisely controlled between several nanometers and several tens of micrometers, that is, the size of the micropore diameter of the microporous atomized sheet can be precisely controlled, thereby enabling Ultrafine aerosol particles; moreover, due to the deposition of a film on the inner wall of the microporous channel of the microporous atomized sheet and the surface thereof, and the materials available for the film are various, and due to the different chemical properties of the films of different materials, Therefore, a film formed by a single material, or a plurality of materials alternately overlap to form a combined film having a thickness-hook, which can realize different chemical properties of the microporous atomized sheet, and expand the kind of the atomized liquid; for example, through a film.
  • the chemical formation makes the microporous atomized sheet have the properties of biocompatibility, barrier of harmful ion precipitation, self-cleaning, acid/alkali corrosion resistance, superfine atomization effect, anti-aerosol condensation, and easy cleaning;
  • Depositing a film of a certain thickness on the inner wall of the microporous orifice of the microporous atomization sheet enables the atomization zone of the microporous atomization sheet to form a hydrophobic layer. Therefore, it is possible to avoid the problem of reducing the atomization efficiency caused by the accumulation of aerosol in the atomization zone.
  • the film of the inner wall of the microporous channel of the microporous atomization sheet prepared by the embodiment of the invention and the film on the surface thereof are deposited layer by layer, and the film is microporous to the microporous atomization sheet.
  • the surface of the inner wall is completely covered.
  • the atomized sheet can be repaired by laminating the crack or the fracture which is difficult to be observed by the naked eye in the conventional atomized sheet, thereby improving the present invention.
  • the breaking strength of the microporous atomized sheet prepared by the embodiment of the invention moreover, the film is firmly bonded to the substrate material, and the film glass is not peeled off or peeled off due to vibration.
  • the atomizing sheet selected in the embodiment of the present invention is an atomizing sheet commonly used in the market, and the atomizing sheet can reduce the aperture of the atomizing area by the embodiment of the present invention, the embodiment of the present invention can realize The general basis for the atomization of the aerosol generator in various fields.
  • FIG. 3 is a schematic structural view of a microporous atomization sheet according to an embodiment of the present invention
  • ⁇ a microporous atomization sheet as shown in FIG. 3 is prepared by using the above microporous atomization sheet preparation method, as shown in FIG.
  • the pore atomizing sheet is provided with a microporous region 301, wherein the microporous region 301 is distributed with a plurality of micropores 302; the inner wall of the microporous orifice of the microporous atomizing sheet and the surface thereof are coated with a thin film;
  • the aperture is
  • the number of the micro holes 302 in the micropore region 301 is 100-1000000.
  • the hole atomizing sheet has a diameter of 1 to 50 mm.
  • the outer diameter R 2 of the micropore region is 1 to 50 mm.
  • the microporous atomized sheet is any one of a metal atomizing sheet, a ceramic atomizing sheet, and an organic material atomizing sheet.
  • the inner wall of the microporous channel of the microporous atomization sheet and the coating material of the surface thereof are one or more layers of uniform thickness;
  • the coating material is any one of the following films; when the coating material is a plurality of layers, the coating material is overlapped by any one of the following films a multilayer film formed, or a multilayer film formed by alternately overlapping any of the following, or a composite film of a multilayer film formed by overlapping one of the following and a multilayer film of any of the following alternately stacked layers;
  • the film comprises: A1 2 0 3 film, SiO 2 film, Ti 2 film, ZnO film, Hf0 2 Film, MgO film, Zr0 2 film, NiO film, CoO film, FeO x film, 01 ( 3 ⁇ 4 film, B 2 0 3 film, In 2 3 3 film, Sn0 2 film, Ga 2 0 3 film, Nb 2 0 5 Film, Gd 2 0 3 film, Ta 2 5 5 film, BN film, A1N film, TiN film, SiC film, ZnS film, ZrS film, HA film, W film, Pt film, Ru film, Pd film, PMDA-DAH Film, PMDA-ODA film, PMDA-EDA film, PMDA-PDA film.
  • the shape of the microporous channel in the microporous atomization sheet is any one of a circle, a triangle, an ellipse and a square.
  • the shape of the cross section of the microporous channel in the microporous atomization sheet is: any one of a parabola shape, a bar shape, a square shape, and a trapezoid shape; here, the shape of the cross section of the microporous channel is further Can be any symmetrical shape.
  • the shape of the microporous channel in the microporous atomization sheet of the embodiment of the present invention is only used to further explain the structure of the microporous atomization sheet, and is not used to limit the present invention.
  • the micro The shape of the microporous channel in the hole atomizing sheet may also be any other shape, which will not be described herein.
  • FIG. 4 is a cross-sectional view of a microporous orifice in a microporous atomization sheet according to an embodiment of the present invention. As shown in FIG. 4, the microporous orifice has a parabolic shape.
  • the embodiment of the invention further provides a micropore atomization device, comprising: an atomizer box, an aerosol generator connected to the atomizer box, and an electronic circuit control connected to the atomizer box
  • the gas mist generator includes a microporous atomization sheet, and the microporous atomization sheet is any one of the microporous atomization sheets described above.
  • FIG. 5 is a schematic structural view of an atomizer case according to an embodiment of the present invention
  • FIG. 5( a ) is a front view of the atomizer case according to an embodiment of the present invention
  • FIG. 5 ( b ) is an atomizer case according to an embodiment of the present invention
  • Figure 5 (c) is a cross-sectional view taken along line AA of Figure 5 (b) of the embodiment of the present invention
  • the atomizer case 10 includes: an upper casing 11, a lower casing 21, and An aerosol attachment 31; wherein the upper casing 11 is connected to the lower casing 21 via an aerosol attachment 31;
  • FIG. 6 is a schematic structural view 1 of an aerosol generator according to an embodiment of the present invention
  • Figure 6 (a) is the present invention
  • FIG. 6(b) is a schematic view showing a specific structure of an aerosol generator according to an embodiment of the present invention
  • FIG. 6(c) is a view along line BB of FIG. 6(a) according to an embodiment of the present invention.
  • the gas mist generator 40 includes: a microporous atomizing sheet 41, a ring-shaped piezoelectric ceramic sheet 42, a sealing member 43 and a circuit lead-out line 44;
  • FIG. 7 is a schematic structural view of an aerosol generator according to an embodiment of the present invention
  • FIG. 7(a) is a side view of an aerosol generator according to an embodiment of the present invention
  • FIG. 7(b) is a specific embodiment of an aerosol generator according to an embodiment of the present invention
  • Figure 7 (c) is a cross-sectional view taken along line CC of Figure 7 (a) of the embodiment of the present invention
  • the aerosol generator 40 comprises: a micro-atomized atomizing sheet 41, annular pressure An electric ceramic sheet 42, a sealing member 43, a circuit lead wire 44 and an annular gasket 45;
  • FIG. 8 is a schematic structural view of an electronic circuit controller according to an embodiment of the present invention
  • FIG. 8(a) is a front view of an electronic circuit controller according to an embodiment of the present invention
  • FIG. 8(b) is a side view of an electronic circuit controller according to an embodiment of the present invention
  • Figure 8 (c) is a cross-sectional view taken along line DD of Figure 8 (b) of the embodiment of the present invention
  • the electronic circuit controller 50 includes: a circuit board 51, and is fixed to the circuit board The switch controller 52 on the 51, the display lamp 53 and the external power input port 54; wherein the electronic circuit controller 50 can be powered by an internal battery, or can be connected to an external power source through the external power input port 54 for power supply.
  • the upper casing 11 includes: an upper cover 12, a liquid tank 13, an aerosol generator fixing device 14, and a line outlet 15; wherein the upper cover 12 is provided with a card slot
  • the upper outer surface of the liquid tank 13 is provided with a threaded slot structure, and the upper cover 12 can be rotatably fixed to the liquid tank by a slot structure of the inner portion thereof and a threaded slot structure of the upper outer surface of the liquid tank 13
  • the upper portion of 13 in this way, prevents the atomization tank from tipping over and causing the liquid to flow out;
  • the aerosol generator fixing device 14 fixes the aerosol generator 40 shown in Fig. 6 or Fig.
  • the lower casing 21 includes: an arc-shaped aerosol discharge passage 22, gas a sol discharge port 23; wherein, the upper outer surface of the lower outer casing 21 is provided a grooved structure, the lower inner surface of the upper casing 11 is provided with a convex groove structure, such that the lower casing 21 and the upper casing 11 are connected to each other by snapping; the aerosol generator 40 and the electronic circuit shown in FIG.
  • the controller 50 is connected through the line interface 15.
  • the aerosol attachment 31 can be applied to different devices; for example, the aerosol attachment 31 according to the embodiment of the present invention can act as an aerosol in any one of a mouth suction cover, a nasal suction cover, a face mask, and a diffusion cover. annex. After the aerosol attachment 31 is opened, the aerosol dissolved by the aerosol generator 40 is passed through the arc-shaped aerosol discharge passage 22 and the aerosol discharge port 23 to the atmosphere.
  • the central region of the microporous atomization sheet 41 has micropores uniformly distributed, and the region where the micropores distributed by the hooks are located is called a microporous region, and the annular piezoelectric ceramic sheet is An inner diameter of 42 is opposite to the microporous region of the microporous atomizing sheet 41 and surrounds the microporous region, and the annular piezoelectric ceramic sheet 42 is fixed to the microporous atomization by welding or gluing techniques.
  • the center of the microporous atomizing sheet 41 coincides with the center of the annular piezoelectric ceramic sheet 42; here, the annular piezoelectric ceramic sheet 42 may be fixed to the upper surface of the microporous atomizing sheet 41.
  • the sealing member 43 tightly wraps the microporous atomizing sheet 41 and the annular piezoelectric ceramic sheet 42 fixed together, and only The micropore region in the microporous atomization sheet 41, wherein the micropore region is also referred to as an atomization region, so that a portion other than the atomization region can be isolated from the atomized liquid, and further It is possible to prevent the microporous atomizing sheet 41 and the annular piezoelectric ceramic sheet 42 from coming into contact for a long time.
  • the circuit lead wire 44 is connected to any two points of the upper and lower surfaces of the annular piezoceramic piece 42; wherein the circuit lead wire 44 is connected to the annular piezoceramic piece 42 Partially sealed by the sealing member 43; the circuit lead wire 44 is connected to the electronic circuit controller 50 shown in FIG. 8 through the upper casing 11 and the line outlet 15 shown in FIG.
  • the central region of the microporous atomization sheet 41 has micropores distributed uniformly, and the region where the micropores distributed by the hooks are located is called a micropore region, and the microporous mist
  • the edge region of the chemical sheet 41 except the microporous region is fixed to the annular gasket 45 by soldering or gluing techniques.
  • the inner diameter of the annular spacer 45 surrounds the micropore region, but does not block the micropores in the micropore region; the center of the microporous atomization sheet 41 coincides with the center of the annular spacer 45.
  • the annular piezoelectric ceramic piece 42 is fixed to the annular spacer 45 by soldering or gluing, and the center of the annular piezoelectric ceramic piece 42 coincides with the center of the annular spacer 45, that is, The inner diameter of the annular piezoelectric ceramic piece 42 is opposite to the micropore area in the microporous atomizing sheet 41; here, the annular piezoelectric ceramic piece 42 may be fixed to the upper surface of the annular spacer 45, It may be fixed to the lower surface of the annular gasket 45; the sealing member 43 tightly surrounds the microporous atomizing sheet 41, the annular piezoelectric ceramic sheet 42 and the annular gasket 45 fixed together, leaving only the The microporous region in the microporous atomizing sheet 41, wherein the microporous region is also referred to as an atomizing region, so that a portion other than the atomizing region can be isolated from the atomized liquid, thereby preventing the The microporous atomizing sheet 41, the annular
  • a method for preparing a microporous atomized sheet comprising:
  • Step 1 using a metal atomized sheet as a substrate material, the substrate material is ultrasonically cleaned; wherein the metal atomized sheet has a micropore diameter of 21 ⁇ m;
  • Step 2 The substrate material is placed in the reaction chamber, and a vacuum is applied to reduce the pressure in the reaction chamber to 10 Pa. Subsequently, after first pulsing trimethylaluminum (TMA) for 50 s, a flow rate of 100 sec is introduced. 2 gas purging the reaction chamber 120s; secondly, after pulse water vapor H 2 0 30s, the reaction chamber 120s is purged with N 2 gas having a flow rate of 120 sccm, so that the pulses TMA and 3 ⁇ 40 are alternated until The inner wall of the microporous channel of the base material and the surface thereof are deposited 4200 layers A1 2 0 3 film; wherein, the A1 2 0 3 film has a thickness of about 500 nm;
  • Step 3 The substrate material deposited with the film is placed in a plasma generator and cured for 200 s; wherein the plasma generator has a power of 50 W, the curing gas is a He plasma, and the gas flow is 200 sccm.
  • the A1 2 0 3 film is tightly coated on the inner wall of the microporous channel of the metal atomizing sheet and the surface thereof, so that the pore diameter of the micropores in the metal atomizing sheet is reduced to 20 ⁇ m to obtain a micropore mist.
  • the microporous atomization sheet has a diameter of 1 mm; the micropore region of the microporous atomization sheet has an outer diameter of 1 mm; and the micropores in the microporous region have a total of 100;
  • the shape of the microporous channel in the hole atomizing sheet is circular; the shape of the cross section of the microporous channel of the microporous atomizing sheet is a bell shape.
  • a method for preparing a microporous atomized sheet comprising:
  • Step 1 using a ceramic atomized sheet as a base material, the base material is ultrasonically cleaned; wherein the ceramic atomized sheet has a micropore diameter of ⁇ ;
  • Step 2 The substrate material is placed in the reaction chamber, and a vacuum is applied to reduce the pressure in the reaction chamber to 10 ⁇ Pa; subsequently, after the trimethylaluminum (TMA) is pulsed for 10 seconds, the flow rate is 50 sccm.
  • TMA trimethylaluminum
  • the Ar gas is purged into the reaction chamber 80s; after the water vapor is pulsed for 3 ⁇ 40 5s, the reaction chamber is purged with an Ar gas having a flow rate of 50 sccm, so that the pulses TMA and 3 ⁇ 40 are alternately pulsed until the base material is
  • the inner wall of the microporous channel and the surface thereof are deposited with 1000 layers of A1 2 0 3 film, wherein the thickness of the A1 2 0 3 film is about 120 nm; finally, the pulsed tetramethylamino titanium (TDMAT)
  • flow rate of Ar gas into the reaction chamber was purged 80s 30sccm after ozone pulse 0 3 0.02s, introduced at a flow of 30 sccm of Ar gas purging the reaction chamber Is, thus alternately month Wing Punching TDMAT and 0 3 , depositing 500 layers of Ti0 2 film on the surface of the A1 2 0 3 film, the thickness of the Ti0 2 film is about 30 nm;
  • Step 3 The substrate material deposited with the film is placed in a plasma generator and cured for 90 s; wherein the plasma generator has a power of 100 W, the curing gas is a He and Ne mixed plasma, and the gas He gas flow. At 100 sccm, the gas flow of the gas Ne was 40 sccm.
  • the A1 2 0 3 film and the Ti 2 2 film are tightly coated on the inner wall of the microporous channel of the ceramic atomizing sheet and the surface thereof, so that the pore diameter of the micropores in the ceramic atomizing sheet is reduced to 9.7.
  • the microporous atomized sheet obtained by the embodiment of the invention has biocompatibility and self-cleaning property.
  • the diameter of the microporous atomization sheet is 30 mm
  • the outer diameter of the micropore region of the microporous atomization sheet is 25 mm
  • the number of micropores in the micropore region is 5000
  • the shape of the microporous channel in the microporous atomization sheet is elliptical; the cross section of the microporous channel has a parabolic shape.
  • a method for preparing a microporous atomized sheet comprising:
  • Step 1 using an organic material atomized sheet as a base material, and ultrasonically cleaning the base material;
  • microporous pore diameter of the organic material atomized sheet is 5 ⁇ ;
  • Step 2 The substrate material is placed in the reaction chamber, and a vacuum is applied to reduce the pressure in the reaction chamber to 1 (T 2 Pa; then, after the pulse of diethyl zinc (DEZ) is 0.015 s, vacuum is applied. Purging the reaction chamber for 50 s; after pulsing the oxygen plasma for 0.5 s, vacuuming the reaction chamber for 30 s, thus alternately pulse DEZ and oxygen plasma until the micropores in the base material A 5000-layer ZnO thin film is deposited on the inner wall of the track and the surface thereof, wherein the thickness of the ZnO thin film is about 100 nm; then, after pulsed pyromellitic dianhydride (PMDA) for 8 s, a N 2 gas purge having a flow rate of 30 sccm is introduced.
  • PMDA pulsed pyromellitic dianhydride
  • the reaction chamber 20s pulsed hexamethylene diamine (ODA) for 3 s, the reaction chamber was purged with N 2 gas at a flow rate of 30 sccm for 15 s, so that PMDA and ODA were alternately pulsed, and 1250 layers of PMDA were deposited on the surface of the ZnO thin film.
  • ODA hexamethylene diamine
  • the thickness of the PMDA-ODA film is about 1075 nm; finally, after pulsed tetramethylamino hydrazine (TDMAHf) for 0.1 s, the reaction chamber is purged with Ar gas having a flow rate of 20 sccm for 5 s, pulse water vapor After H 2 0 0.015 s, the reaction chamber was purged with Ar gas having a flow rate of 20 sccm for 3 s, thus alternately pulsed TDMAHf and 3 ⁇ 40, and 3334 layers of HfO 2 film deposited on the surface of the PMDA-ODA film, the Hf0 2 film The thickness is about 400 nm;
  • Step 3 The substrate material deposited with the film is placed in a plasma generator to cure Is; wherein the plasma generator has a power of 500 W, the curing gas is a plasma mixed with Ar and Xe, and the gas of the gas Ar At 10 sccm, the gas flow of the gas Xe was 50 sccm.
  • the ZnO film, the PMDA-ODA film, and the Hf0 2 film are tightly coated on the inner wall of the microporous channel of the organic material atomizing sheet and the surface thereof, so that the microporous material in the organic material atomizing sheet is The pore diameter is reduced to 0.05 ⁇ m to obtain a microporous atomized sheet; since the inner wall and surface of the microporous orifice of the microporous atomized sheet are tightly coated with a ZnO thin film, a PMDA-ODA thin film and an HfO 2 thin film, it is possible to avoid turbulence The problem of causing the film to fall off; and the microporous atomized sheet obtained by the embodiment of the invention has wear resistance due to the chemical and physical properties of the ZnO film, the PMDA-ODA film and the Hf0 2 film in the microporous atomized sheet. Sex, acid and alkali corrosion and effective barrier to the deposition of harmful ions.
  • the microporous atomization sheet has a diameter of 50 mm
  • the micropore region of the microporous atomization sheet has an outer diameter of 50 mm
  • the micropores in the micropore region have a total of 1,000,000
  • the shape of the microporous channel in the microporous atomization sheet is a triangle; the shape of the cross section of the microporous channel is trapezoidal.
  • Embodiment 4 A method for preparing a microporous atomized sheet, the specific steps comprising:
  • Step 1 using a metal atomizing sheet as a substrate material, the substrate material is cleaned; wherein the metal atomized sheet has a micropore diameter of 5 ⁇ m;
  • Step two activating the cleaned substrate material
  • the step of activating includes:
  • the base material is immersed in a phosphoric acid solution having a concentration of lg/L for ultrasonic cleaning for 5 min, and then the base material is washed with distilled water, and the pH of the surface liquid adhered to the base material is neutral. So far
  • the substrate material is immersed in a 15% by mass aqueous ammonia solution for ultrasonic cleaning for 15 minutes, and then the substrate material is washed with distilled water and washed until the pH of the liquid attached to the surface of the substrate material is neutral. ;
  • the substrate material is activated by irradiating Is under an ultraviolet lamp.
  • Step 3 placing the activated substrate material in the reaction chamber, evacuating to reduce the pressure in the reaction chamber to 1 (T 2 Pa; subsequently, first pulse 3-aminopropyltriethoxysilane After 30 s (AMEO), the reaction chamber was purged with N 2 gas with a flow rate of 20 sccm for 50 s, and after the water vapor H 2 0 0.015 s was pulsed, the reaction chamber ls was evacuated, and finally, the ozone O 3 was pulsed.
  • the reaction chamber was purged with N 2 gas with a flow rate of 5 sccm for 10 s, so that AMEO, H 2 0 and 0 3 were alternately pulsed, and a layer of Si0 was deposited on the inner wall of the microporous channel of the base material and the surface thereof. 2 film, wherein the SiO 2 film has a thickness of about 0.1 nm.
  • Step 4 The substrate material deposited with the film is placed in a plasma generator to cure Is; wherein the plasma generator has a power of 500 W, and the curing gas is a plasma of He and Kr mixed, and the gas He The gas flow was 10 sccm, and the gas flow of the gas Kr was 30 sccm.
  • the SiO 2 film is tightly coated on the inner wall of the microporous channel of the metal atomizing sheet and the surface thereof, so that the inner wall of the microporous channel of the metal atomizing sheet and the surface thereof are coated with a layer of SiO 2 film.
  • microporous atomizing sheet although the pore diameter of the micropore in the microporous atomizing sheet hardly changes, but Since the inner wall of the microporous orifice of the microporous atomized sheet and the surface thereof are coated with a SiO 2 film, the breaking strength of the atomized sheet is enhanced, and the SiO 2 film is resistant to acid/alkali corrosion, thereby The microporous atomized sheet has good resistance to alkali/corrosion and can effectively block harmful ion precipitation.
  • the microporous atomization sheet has a diameter of 50 mm
  • the micropore region of the microporous atomization sheet has an outer diameter of 50 mm
  • the micropores in the micropore region have a total of 1,000,000
  • the shape of the microporous channels in the microporous atomization sheet is square; the shape of the cross section of the microporous channels is square.
  • a method for preparing a microporous atomized sheet comprising:
  • Step 1 The organic material atomized sheet is used as a base material, and the base material is washed; wherein, the microporous pore diameter of the organic material atomized sheet is 21 ⁇ ;
  • Step two activating the cleaned substrate material
  • the step of activating includes:
  • the base material is immersed in a mixed solution of a concentration of 0.05 g/L hydrochloric acid and a concentration of 10 g / L of hydrogen fluoride ammonia solution for ultrasonic cleaning for 30 min, and then the base material is washed with distilled water, and washed until attached thereto.
  • the pH of the surface liquid of the base material is neutral;
  • the substrate material is immersed in ammonia water having a mass percentage of 1% for ultrasonic cleaning for 5 minutes, and then the substrate material is washed with distilled water, and the pH of the liquid attached to the surface of the substrate material is cleaned until the pH is neutral. ;
  • the substrate material is activated by irradiation in a plasma atmosphere capable of generating ultraviolet gas for 120 s.
  • Step 3 The activated substrate material is placed in the reaction chamber, and a vacuum is applied to reduce the pressure in the reaction chamber to 10 Pa. Subsequently, the tetramethylaminozirconium (TDMAZ) is pulsed for 0.1 s.
  • TDMAZ tetramethylaminozirconium
  • the reaction chamber was purged with an Ar gas having a flow rate of 30 sccm for 5 s; after a pulsed oxygen plasma for 0.8 s, the reaction chamber was purged with an Ar gas having a flow rate of 50 sccm for 100 s, thus alternately pulsed TDMAZ and oxygen plasma.
  • the reaction chamber is purged with Ar gas having a flow rate of 120 sccm. 120s, after pulsed NH 3 0.02s, the reaction chamber is purged with Ar gas having a flow rate of 8sccm for 10s, so that BBr 3 and NH 3 are alternately pulsed, and 45000 layers of BN film are deposited on the surface of the Zr0 2 film.
  • the thickness of the BN film is about 3600 nm.
  • the reaction chamber is purged with an Ar gas having a flow rate of 120 sccm for 120 s, and after pulsed diaminodiphenyl ether (DAH) for 8 s, The reaction chamber was purged with Ar gas having a flow rate of 8 sccm for 50 s, so that PMDA and DAH were alternately pulsed, and 300 layers of PMDA-DAH film were deposited on the surface of the BN film, wherein the PMDA-DAH film had a thickness of about 399.95. Nm.
  • PMDA pulsed pyromellitic dianhydride
  • Step 4 The substrate material deposited with the film is placed in a plasma generator and cured for 200 s; wherein, the power of the plasma generator is 50 W, the plasma of the curing gas is Ne, and the gas flow of the gas Ne is 200 sccm. .
  • the Zr0 2 film, the BN film, and the PMDA-DAH film are tightly coated on the inner wall of the microporous channel of the organic material atomizing sheet and the surface thereof, so that the microporous material in the organic material atomizing sheet is The pore size is reduced to 0.05 ⁇ m; since the inner wall and the surface of the microporous channel are tightly adhered to the Zr0 2 film, the BN film and the PMDA-DAH film, the ceramic atomized sheet of the embodiment has good barrier properties.
  • the diameter of the atomized sheet of the organic material is 45 mm; the outer diameter of the microporous region of the organic material atomized sheet is 40 mm; and the micropores in the microporous region are 5000;
  • the shape of the microporous channel in the atomizing sheet is circular; the shape of the cross section of the microporous channel is parabolic.
  • a method for preparing a microporous atomized sheet comprising:
  • Step 1 using a ceramic atomized sheet as a substrate material, the substrate material is cleaned; wherein the ceramic atomized sheet has a micropore diameter of 21 ⁇ m;
  • Step two activating the cleaned substrate material; Specifically, the step of activating includes:
  • the base material is immersed in a mixed solution having a concentration of 6.5 g/L acetic acid solution, a concentration of 0.05 g/L hydrochloric acid solution, and a concentration of 10 g/L of hydrogen fluoride ammonia solution for 15 minutes, and then washed with distilled water.
  • the base material is cleaned until the pH of the surface liquid attached to the base material is neutral;
  • the substrate material is immersed in ammonia water having a mass percentage of 20% for ultrasonic cleaning for 30 minutes, and then the substrate material is washed with distilled water, and the pH of the liquid attached to the surface of the substrate material is cleaned until neutral. ;
  • the substrate material is activated by irradiation in a plasma atmosphere capable of generating ultraviolet gas for 90 s.
  • Step 3 The activated substrate material is placed in the reaction chamber, and a vacuum is applied to reduce the pressure in the reaction chamber to 1 OPa. Subsequently, the pyromellitic dianhydride (PMDA) is pulsed for 5 seconds.
  • the reaction chamber was purged with N 2 gas at a flow rate of 20 sccm for 15 s.
  • the reaction chamber was purged with N 2 gas at a flow rate of 20 sccm for 20 s, thus alternately pulsed PMDA and
  • the PDA deposits 1250 layers of PMDA-PDA film on the surface of the substrate material, wherein the PMDA-PDA film has a thickness of about 1000 nm.
  • Step 4 The substrate material deposited with the thin film is placed in a plasma generator and cured for 90 s; wherein the plasma generator has a power of 250 W, and the curing gas is a mixed plasma of Ar and Xe, and the gas is Ar The gas flow was 160 sccm, and the gas flow of the gas Xe was 40 sccm.
  • the PMDA-PDA film is tightly coated on the inner wall of the microporous channel of the ceramic atomizing sheet and the surface thereof, so that the pore diameter of the micropores in the ceramic atomizing sheet is reduced to 20 ⁇ m;
  • the inner wall and the surface are tightly adhered to the PMDA-PDA film, and therefore, the ceramic atomized sheet of the embodiment has extremely strong breaking strength and good barrier property.
  • the ceramic atomizing sheet has a diameter of 1 mm; the outer diameter of the microporous region of the organic material atomizing sheet is 1 mm; and the micropores in the microporous region have a total of 100; Chemical film The shape of the pore channel is square; the shape of the cross section of the microporous channel is square.
  • reaction chamber is evacuated before the pulse precursor, and the entire reaction process is performed under vacuum.

Abstract

A method for preparing a micropore atomization sheet (41), wherein the atomization sheet is used as a substrate material. The method comprises: depositing a film on the inner wall and the surface of a micropore channel of the substrate material; and solidifying the substrate material on which the film is deposited. Also disclosed are a micropore atomization sheet and a micropore atomization apparatus.

Description

一种微孔雾化片的制备方法、 微孔雾化片及微孔雾化装置 技术领域  Preparation method of microporous atomized sheet, microporous atomizing sheet and micropore atomizing device
本发明涉及雾化技术， 尤其涉及一种微孔雾化片的制备方法、 微孔雾 化片及微孔雾化装置。 背景技术  The invention relates to atomization technology, in particular to a preparation method of a microporous atomization sheet, a micropore atomization sheet and a micropore atomization device. Background technique
雾化片广泛地应用于空气加湿器、 熏香器、 美容机、 肺部给药装置、 消毒机、 浴缸造雾机等仪器设备上面。  The atomized sheet is widely used in air humidifiers, incense burners, beauty machines, lung drug delivery devices, sterilizers, bathtub fog machines and the like.
目前主要的雾化片有金属雾化片、 陶瓷雾化片、 有机材质雾化片等种 类， 其中由于金属雾化片如不锈钢雾化片、 镀镍雾化片、 镀钛雾化片等， 具有一定的耐疲劳， 易清洗， 不易断裂等优势， 被广泛应用于不同用途的 气雾发生器中， 份额占据绝对的市场优势。 但是金属雾化片长期使用不可 避免地会导致有害金属离子析出， 从而影响液体成分， 如果应用于给药装 置气雾发生器， 甚至会对人体健康有害。 陶瓷雾化片或有机材质雾化片也 有一定的市场份额， 但是由于其材料本身的性质决定了雾化片易断裂， 需 要非常小心清洗。 另一方面， 雾化所需的能量基本上作用于雾化片上， 随 着温度的升高大大减少有机材质雾化片的使用寿命。 文献和专利报导的雾 化片微孔孔径最小的做到了 3微米， 1-5微米喷出气雾颗粒在 50%左右， 但 是雾化片极易堵塞。 雾化片微孔孔径越细小， 雾化片即越易堵塞。  At present, the main atomizing sheets are metal atomizing sheets, ceramic atomizing sheets, organic material atomizing sheets, etc., among which metal atomizing sheets such as stainless steel atomizing sheets, nickel-plated atomizing sheets, titanium-plated atomizing sheets, etc. It has certain advantages of fatigue resistance, easy cleaning, and not easy to break. It is widely used in aerosol generators for different purposes, and its share has an absolute market advantage. However, the long-term use of the metal atomized sheet inevitably leads to the precipitation of harmful metal ions, thereby affecting the liquid component, and if it is applied to the aerosol generator of the drug delivery device, it may even be harmful to human health. Ceramic atomized sheets or organic material atomized sheets also have a certain market share, but due to the nature of the materials themselves, the atomized sheets are easily broken and require very careful cleaning. On the other hand, the energy required for atomization essentially acts on the atomizing sheet, and the life of the atomized sheet of the organic material is greatly reduced as the temperature rises. The microporous pore size of the atomized sheet reported in the literature and patents is as small as 3 micrometers, and the aerosol particles of 1-5 micrometers are about 50%, but the atomized sheet is extremely easy to block. The finer the pore size of the atomizing sheet, the more easily the atomized sheet is blocked.
另外， 市场上现有的气雾发生器， 雾化片开始工作时， 喷出的气溶胶 颗粒比表面积很大， 极易吸附在雾化区。 而聚集在雾化区的气溶胶颗粒就 阻碍了后续的气溶胶颗粒雾化喷出， 影响出雾量及雾化速率。 发明内容 In addition, the existing aerosol generators on the market, when the atomizing sheet starts to work, the aerosol particles sprayed have a large specific surface area and are easily adsorbed in the atomization zone. The aerosol particles accumulated in the atomization zone hinder the subsequent aerosol atomization of the aerosol particles, affecting the amount of fog and the atomization rate. Summary of the invention
为解决现有存在的技术问题， 本发明实施例提供一种微孔雾化片的制 备方法、 微孔雾化片及微孔雾化装置。  In order to solve the existing technical problems, embodiments of the present invention provide a method for preparing a microporous atomized sheet, a microporous atomizing sheet, and a micropore atomizing device.
本发明实施例的技术方案是这样实现的： 本发明实施例提供了一种微 孔雾化片的制备方法， 其中， 将雾化片作为基底材料； 所述方法包括： 在所述基底材料的微孔孔道内壁及其表面沉积薄膜；  The technical solution of the embodiment of the present invention is as follows: The embodiment of the present invention provides a method for preparing a microporous atomized sheet, wherein the atomized sheet is used as a base material; the method includes: a film is deposited on the inner wall of the microporous channel and its surface;
将沉积有薄膜的所述基底材料固化。  The substrate material on which the film is deposited is cured.
上述方案中， 所述雾化片为金属雾化片、 陶瓷雾化片及有机材质雾化 片中的任意一种。  In the above aspect, the atomizing sheet is any one of a metal atomizing sheet, a ceramic atomizing sheet, and an organic material atomizing sheet.
上述方案中， 所述在所述基底材料的微孔孔道内壁及其表面沉积薄膜， 包括：  In the above solution, the depositing a film on the inner wall of the microporous channel of the base material and the surface thereof comprises:
步骤一： 将所述基底材料放置于反应腔体内；  Step 1: placing the substrate material in the reaction chamber;
步骤二： 通入第一前驱体， 使所述第一前驱体与所述基底材料的微孔 孔道内壁及其表面的材料发生反应；  Step two: introducing a first precursor, reacting the first precursor with a material of the inner wall of the microporous channel of the base material and a surface thereof;
步骤三： 在反应完成后， 釆用清洗气体吹扫所述反应腔体、 或对所述 反应腔体进行抽真空将游离的所述第一前驱体排出所述反应腔体后， 通入 第二前驱体；  Step 3: After the reaction is completed, the reaction chamber is purged with a cleaning gas, or the reaction chamber is evacuated, and the free first precursor is discharged from the reaction chamber, and then Second precursor
步骤四： 循环执行所述步骤二和步骤三， 直至在所述基底材料的微孔 孔道内壁及其表面沉积预设厚度的薄膜为止。  Step 4: The steps 2 and 3 are performed cyclically until a film of a predetermined thickness is deposited on the inner wall of the microporous channel of the base material and the surface thereof.
上述方案中， 所述薄膜为一层或多层厚度均勾的薄膜；  In the above solution, the film is one or more layers of thickness-hooked film;
当所述薄膜为一层时， 所述薄膜为以下薄膜中的任意一种；  When the film is a layer, the film is any one of the following films;
当所述薄膜为多层时， 所述薄膜为以下薄膜中的任意一种重叠形成的 多层薄膜， 或以下任意几种交替重叠形成的多层薄膜， 或以下一种重叠形 成的多层薄膜和以下任意几种交替重叠形成的多层薄膜的组合多层薄膜； 所述薄膜包括： 氧化铝 （A1203 ) 薄膜、 二氧化硅（Si02 )薄膜、 二氧 化钛（Ti02 )薄膜、 氧化锌（ZnO )薄膜、 二氧化铪（Hf02 )薄膜、 氧化镁 ( MgO )薄膜、二氧化锆 ( Zr02 )薄膜、氧化镍 ( NiO )薄膜、氧化钴 ( CoO ) 薄膜、铁的氧化物形成的薄膜 ( FeOx )薄膜、铜的氧化物形成的薄膜 ( CuOx ) 薄膜、 氧化硼（B203 )薄膜、 氧化铟（In203 )薄膜、 氧化锡（Sn02 )薄膜、 氧化镓（Ga203 ) 薄膜、 五氧化二铌（Nb205 )薄膜、 三氧化二钆（Gd203 ) 薄膜、 五氧化二钽（Ta205 )薄膜、 氮化硼 （BN )薄膜、 氮化铝 （A1N )薄 膜、 氮化钛（TiN )薄膜、 碳化硅（SiC )薄膜、 硫化锌（ZnS )薄膜、 硫化 锆（ZrS )薄膜、 透明质酸（HA )薄膜、 钨（W )薄膜、 铂（Pt )薄膜、 钌 ( Ru )薄膜、钯（ Pd )薄膜、 均苯四甲酸二酐-二氨基二苯醚（ PMDA-DAH ) 薄膜、 均苯四甲酸二酐-己二胺（PMDA-ODA ) 薄膜、 均苯四甲酸二酐-乙 二胺（ PMDA-EDA )薄膜及均苯四甲酸二酐-对苯二胺（ PMDA-PDA )薄膜。 When the film is a plurality of layers, the film is a multilayer film formed by overlapping any one of the following films, or a multilayer film formed by alternately overlapping any of the following, or a multilayer film formed by overlapping one of the following And a combined multilayer film of a plurality of layers formed by alternately overlapping with any of the following; the film comprises: an alumina (A1 2 0 3 ) film, a silicon dioxide (Si0 2 ) film, and a dioxane Titanium (Ti0 2 ) film, zinc oxide (ZnO) film, hafnium oxide (Hf0 2 ) film, magnesium oxide (MgO) film, zirconium dioxide (Zr0 2 ) film, nickel oxide (NiO) film, cobalt oxide ( CoO) thin film (FeO x ) film formed by film and iron oxide, thin film (CuO x ) film formed by copper oxide, boron oxide (B 2 0 3 ) film, indium oxide (In 2 0 3 ) film, Tin oxide (Sn0 2 ) film, gallium oxide (Ga 2 0 3 ) film, bismuth pentoxide (Nb 2 0 5 ) film, antimony trioxide (Gd 2 0 3 ) film, tantalum pentoxide (Ta 2 0 5 ) film, boron nitride (BN) film, aluminum nitride (A1N) film, titanium nitride (TiN) film, silicon carbide (SiC) film, zinc sulfide (ZnS) film, zirconium sulfide (ZrS) film, transparent Acid (HA) film, tungsten (W) film, platinum (Pt) film, ruthenium (Ru) film, palladium (Pd) film, pyromellitic dianhydride-diaminodiphenyl ether (PMDA-DAH) film, Pyromellitic dianhydride-hexanediamine (PMDA-ODA) film, pyromellitic dianhydride-ethylenediamine (PMDA-EDA) film and pyromellitic dianhydride-p-benzene Diamine (PMDA-PDA) film.
上述方案中， 所述将沉积有薄膜的所述基底材料固化， 包括： 将沉积有薄膜的所述基底材料进行等离子体固化。  In the above solution, the curing the substrate material deposited with the film comprises: plasma curing the substrate material deposited with the film.
上述方案中， 所述在所述基底材料的微孔孔道内壁及其表面沉积薄膜 之前， 所述方法还包括：  In the above solution, before the film is deposited on the inner wall of the microporous channel of the base material and the surface thereof, the method further includes:
将所述基底材料进行活化。  The substrate material is activated.
上述方案中， 所述活化包括： 化学溶液浸渍活化和紫外活化。  In the above scheme, the activation comprises: chemical solution impregnation activation and ultraviolet activation.
上述方案中， 所述化学溶液浸渍活化的步骤包括：  In the above solution, the step of impregnating and activating the chemical solution comprises:
将所述基底材料浸渍于酸性溶液中超声清洗 5-30min，然后釆用蒸馏水 清洗所述基底材料，清洗至附着于所述基底材料的表面液体的 pH值为中性 为止；  The base material is immersed in an acidic solution for ultrasonic cleaning for 5-30 min, and then the base material is washed with distilled water, and washed until the pH of the surface liquid attached to the base material is neutral;
将所述基底材料浸渍于碱性溶液中超声清洗 5-30min，然后釆用蒸馏水 清洗所述基底材料，清洗至附着于所述基底材料表面的液体的 pH值为中性 为止。  The base material was immersed in an alkaline solution for ultrasonic cleaning for 5 to 30 minutes, and then the base material was washed with distilled water, and washed until the pH of the liquid adhering to the surface of the base material was neutral.
上述方案中， 所述紫外活化的步骤包括： 将所述基底材料放置在紫外线灯下或者在能产生紫外气体的等离子体 气氛中， 照射 ls-120s进行活化。 In the above solution, the step of ultraviolet activation comprises: The substrate material is placed under an ultraviolet lamp or in a plasma atmosphere capable of generating ultraviolet gas, and irradiated with ls-120s for activation.
本发明实施例还提供了一种微孔雾化片， 所述微孔雾化片设置有微孔 区， 所述微孔区内分布有多个微孔； 所述微孔雾化片的微孔孔道内壁及其 表面包覆有薄膜； 所述微孔的孔径为 0.05μπι-20μπι。  The embodiment of the present invention further provides a microporous atomization sheet, wherein the microporous atomization sheet is provided with a micropore region, and a plurality of micropores are distributed in the micropore region; The inner wall of the pore channel and the surface thereof are coated with a film; the pore diameter of the micropores is 0.05 μπι-20 μπι.
上述方案中， 所述微孔区中微孔的数量为 100-1000000个。  In the above solution, the number of micropores in the microporous region is 100-1000000.
上述方案中， 所述微孔雾化片的直径为 l-50mm。  In the above solution, the microporous atomized sheet has a diameter of from 1 to 50 mm.
上述方案中， 所述微孔区的外径为 l-50mm。  In the above solution, the outer diameter of the microporous region is l-50 mm.
上述方案中， 所述微孔雾化片为金属雾化片、 陶瓷雾化片及有机材质 雾化片中的任意一种。  In the above aspect, the microporous atomizing sheet is any one of a metal atomizing sheet, a ceramic atomizing sheet, and an organic material atomizing sheet.
上述方案中， 所述微孔雾化片的微孔孔道内壁及其表面的包覆材料为 一层或多层厚度均匀的薄膜；  In the above solution, the inner wall of the microporous channel of the microporous atomization sheet and the coating material of the surface thereof are one or more layers of uniform thickness;
当所述包覆材料为一层时， 所述包覆材料为以下薄膜中的任意一种； 当所述包覆材料为多层时， 所述包覆材料为以下薄膜中的任意一种重 叠形成的多层薄膜， 或以下任意几种交替重叠形成的多层薄膜， 或以下一 种重叠形成的多层薄膜和以下任意几种交替重叠形成的多层薄膜的组合多 层薄膜；  When the coating material is a layer, the coating material is any one of the following films; when the coating material is a plurality of layers, the coating material is overlapped by any one of the following films a multilayer film formed, or a multilayer film formed by alternately overlapping any of the following, or a composite film of a multilayer film formed by overlapping one of the following and a multilayer film of any of the following alternately stacked layers;
上述方案中， 所述微孔雾化片中微孔孔道的形状为： 圓形、 三角形、 椭圓形、 方形及喇叭形中的任意一种。  In the above solution, the shape of the microporous channel in the microporous atomization sheet is any one of a circular shape, a triangular shape, an elliptical shape, a square shape and a horn shape.
上述方案中， 所述微孔雾化片中微孔孔道的横截面的形状为： 抛物线 形、 喇叭形、 方形及梯形中的任意一种。  In the above solution, the cross-sectional shape of the microporous channel in the microporous atomization sheet is any one of a parabolic shape, a horn shape, a square shape and a trapezoidal shape.
本发明实施例又提供了一种微孔雾化装置， 所述微孔雾化装置包括： 雾化器箱体、 与所述雾化器箱体连接的气雾发生器、 以及与雾化器箱体连 接的电子电路控制器； 其中， 所述气雾发生器中包括微孔雾化片， 所述微 孔雾化片为以上所述的任一微孔雾化片。 釆用本发明实施例制备出的微孔雾化片， 其微孔孔径尺寸能够在几纳 米到几十微米间精确可控， 即能精确控制微孔雾化片的微孔孔径的尺寸， 因此， 能够实现超微细气雾颗粒； 另外， 由于本发明实施例选用的雾化片 为市场中常用的雾化片， 又由于所述雾化片能够通过本发明实施例将其雾 化区的孔径缩小， 因此， 本发明实施例能够为实现各领域的气雾发生器中 雾化片的通用奠定基础。 附图说明 The embodiment of the invention further provides a micropore atomization device, the micropore atomization device comprising: an atomizer housing, an aerosol generator connected to the atomizer housing, and an atomizer An electronic circuit controller connected to the cabinet; wherein the gas mist generator comprises a microporous atomizing sheet, and the microporous atomizing sheet is any of the microporous atomizing sheets described above. The microporous atomized sheet prepared by using the embodiment of the invention has a pore size which can be precisely controlled between several nanometers and several tens of micrometers, that is, the size of the micropore diameter of the microporous atomized sheet can be accurately controlled, The ultra-fine aerosol particles can be realized; in addition, since the atomization sheet selected in the embodiment of the invention is an atomization sheet commonly used in the market, and the atomization sheet can have the aperture of the atomization area thereof according to the embodiment of the invention Therefore, the embodiment of the present invention can lay a foundation for realizing the versatility of the atomized sheet in the aerosol generator in various fields. DRAWINGS
图 1为本发明实施例微孔雾化片的制备方法的实现流程示意图一； 图 2为本发明实施例微孔雾化片的制备方法的实现流程示意图二； 图 3为本发明实施例微孔雾化片的结构示意图；  1 is a schematic flow chart of an implementation process of a method for preparing a microporous atomization sheet according to an embodiment of the present invention; FIG. 2 is a schematic flow chart 2 of a method for preparing a microporous atomization sheet according to an embodiment of the present invention; Schematic diagram of the pore atomizing sheet;
图 4为本发明实施例微孔雾化片中微孔孔道的横截面图；  4 is a cross-sectional view of a microporous orifice in a microporous atomization sheet according to an embodiment of the present invention;
图 5为本发明实施例雾化器箱体的结构示意图；  FIG. 5 is a schematic structural view of an atomizer case according to an embodiment of the present invention; FIG.
图 6为本发明实施例气雾发生器的结构示意图一；  6 is a schematic structural view 1 of an aerosol generator according to an embodiment of the present invention;
图 7为本发明实施例气雾发生器的结构示意图二；  7 is a schematic structural view 2 of an aerosol generator according to an embodiment of the present invention;
图 8为本发明实施例电子电路控制器的结构示意图。  FIG. 8 is a schematic structural diagram of an electronic circuit controller according to an embodiment of the present invention.
附图标记说明  Description of the reference numerals
11、 上外壳， 12、 上盖板， 13、 液体槽， 14、 气雾发生器固定装置， 15、 线路出口， 21、 下外壳， 22、 弧形气溶胶排出通道， 23、 气溶胶排出 口， 31、 气雾附件， 40、 气雾发生器， 41、 微孔雾化片， 42、 环形压电陶 瓷片， 43、 密封件， 44、 电路引出线， 45、 环形垫片， 50、 电子电路控制 器， 51、 电路板， 52、 开关控制器， 53、 显示灯， 54、 外接电源输入口。 具体实施方式  11. Upper casing, 12, upper cover, 13, liquid tank, 14, aerosol generator fixing device, 15, line outlet, 21, lower casing, 22, arc aerosol discharge passage, 23, aerosol discharge port 31, aerosol attachment, 40, aerosol generator, 41, microporous atomization sheet, 42, annular piezoelectric ceramic sheet, 43, seal, 44, circuit lead, 45, ring gasket, 50, electronic Circuit controller, 51, circuit board, 52, switch controller, 53, display light, 54, external power input. detailed description
为了能够更加详尽地了解本发明的特点与技术内容， 下面结合附图对 本发明的实现进行详细阐述， 所附附图仅供参考说明之用， 并非用来限定 本发明。 In order to be able to understand the features and technical details of the present invention in detail, the embodiments of the present invention are described in detail below with reference to the accompanying drawings. this invention.
图 1 为本发明实施例微孔雾化片的制备方法的实现流程示意图一， 将 雾化片作为基底材料； 如图 1所示， 所述方法包括：  1 is a schematic flow chart showing the implementation of a method for preparing a microporous atomized sheet according to an embodiment of the present invention, and the atomized sheet is used as a base material; as shown in FIG. 1, the method includes:
步骤 101 : 在所述基底材料的微孔孔道内壁及其表面沉积薄膜； 其中， 所述雾化片为金属雾化片、 陶瓷雾化片及有机材质雾化片中的 任意一种。  Step 101: depositing a film on the inner wall of the microporous channel of the base material and the surface thereof; wherein the atomizing sheet is any one of a metal atomizing sheet, a ceramic atomizing sheet and an organic material atomizing sheet.
具体地， 将所述基底材料放置于反应腔体内， 将各前驱体以脉冲气体 的方式交替通入所述反应腔体内， 在所述基底材料的微孔孔道内壁及其表 面沉积薄膜；  Specifically, the substrate material is placed in the reaction chamber, and each precursor is alternately introduced into the reaction chamber in a pulsed gas manner, and a film is deposited on the inner wall of the microporous channel of the base material and the surface thereof;
这里， 为使前后两种前驱体在反应腔体内不同时出现， 在通入一种前 驱体后、 与通入下一种前驱体前的间隙中， 使用清洗气体例如惰性气体等 吹扫所述反应腔体、 或对所述反应腔体进行抽真空处理， 以隔离前后两种 前驱体， 使前后两种前驱体不同时出现于所述反应腔体内。  Here, in order to prevent the two precursors from appearing differently in the reaction chamber, the purge gas such as an inert gas or the like is purged in the gap before the introduction of the precursor and before the passage into the next precursor. The reaction chamber is subjected to a vacuum treatment to isolate the two precursors before and after, so that the two precursors do not simultaneously appear in the reaction chamber.
在一实施例中， 所述在所述基底材料的微孔孔道内壁及其表面沉积薄 膜， 包括：  In one embodiment, the depositing a film on the inner wall of the microporous channel of the substrate material and the surface thereof comprises:
步骤一： 将所述基底材料放置于反应腔体内；  Step 1: placing the substrate material in the reaction chamber;
步骤二： 通入第一前驱体， 使所述第一前驱体与所述基底材料的微孔 孔道内壁及其表面的材料发生反应；  Step two: introducing a first precursor, reacting the first precursor with a material of the inner wall of the microporous channel of the base material and a surface thereof;
步骤三： 在反应完成后， 釆用清洗气体吹扫所述反应腔体、 或对所述 反应腔体进行抽真空将游离的所述第一前驱体排出所述反应腔体后， 通入 第二前驱体；  Step 3: After the reaction is completed, the reaction chamber is purged with a cleaning gas, or the reaction chamber is evacuated, and the free first precursor is discharged from the reaction chamber, and then Second precursor
步骤四： 循环执行所述步骤二和步骤三， 直至在所述基底材料的微孔 孔道内壁及其表面沉积预设厚度的薄膜为止。  Step 4: The steps 2 and 3 are performed cyclically until a film of a predetermined thickness is deposited on the inner wall of the microporous channel of the base material and the surface thereof.
在本实施例整个实验过程均是在抽真空下进行的， 但是， 在第一次脉 冲前驱体前， 所述反应腔体的压强处于 l OPa至 l (T2 Pa; 每次釆用脉冲气体 的方式向所述反应腔体内通入前驱体， 每次脉冲前驱体 0. 015S -50S, 脉冲 完一次前驱体后， 向所述反应腔体内通入流量为 0sccm-120sccm的氩气 Ar 或氮气 N2吹扫所述反应腔体 ls-120s， 随后脉冲另一前驱体； 这里， 各前驱 体可以通过载气进入所述反应腔体内， 所述载体可以为氮气 N2或氩气 Ar; 这里， 由于在脉冲两种前驱体的间隙中， 向所述反应腔体中通入氩气 Ar或 氮气 N2， 因此， 能将所述反应腔体内多余的前驱体及反应副产物排出。 In the present embodiment, the entire experimental process is carried out under vacuum, but before the first pulse precursor, the pressure of the reaction chamber is in the range of OPa to l (T 2 Pa; The method of introducing a precursor into the reaction chamber, each pulse precursor 0. 015S -50S, after the pulse is completed once, a flow rate of 0sccm-120sccm of argon Ar or nitrogen is introduced into the reaction chamber. N 2 purging the reaction chamber ls-120s, and then pulse another precursor; here, each precursor may enter the reaction chamber through a carrier gas, the carrier may be nitrogen N 2 or argon Ar; Since argon gas Ar or nitrogen gas N 2 is introduced into the reaction chamber in the gap between the two precursors of the pulse, excess precursor and reaction by-products in the reaction chamber can be discharged.
这里，当向所述反应腔体内通入的氩气 Ar或氮气 N2的流量为 Osccm时， 表示未向反应腔体中通入气体， 此时， 由于反应腔体中依然保持着抽真空 的状态， 因此， 通过抽真空的过程可以使上一次脉冲的前驱体中游离的部 分或反应副产物排出。 Here, when the flow rate of the argon gas Ar or the nitrogen gas N 2 introduced into the reaction chamber is Osccm, it means that no gas is introduced into the reaction chamber, and at this time, since the reaction chamber still maintains a vacuum. State, therefore, a free portion or reaction by-product in the precursor of the last pulse can be discharged by a vacuuming process.
这里， 第一次通入的前驱体可以和基底材料的微孔孔道内壁及其表面 的材料发生化学吸附反应， 形成第一薄膜， 随后， 所述第一薄膜与第二次 通入的前驱体发生反应形成第二薄膜， 依此类推， 直至形成预设厚度的薄 膜为止； 其中， 各前驱体可以根据薄膜的化学组成任意选择。  Here, the first-passed precursor may be chemically adsorbed with the material of the inner wall of the microporous channel of the base material and the surface thereof to form a first film, and then the first film and the second-pass precursor are formed. The reaction takes place to form a second film, and so on, until a film of a predetermined thickness is formed; wherein each precursor can be arbitrarily selected according to the chemical composition of the film.
在一实施例中， 所述薄膜为一层或多层厚度均勾的薄膜；  In one embodiment, the film is one or more layers of thickness-hooked film;
当所述薄膜为一层时， 所述薄膜为以下薄膜中的任意一种；  When the film is a layer, the film is any one of the following films;
当所述薄膜为多层时， 所述薄膜为以下薄膜中的任意一种重叠形成的 多层薄膜， 或以下任意几种交替重叠形成的多层薄膜， 或以下一种重叠形 成的多层薄膜和以下任意几种交替重叠形成的多层薄膜的组合多层薄膜； 所述薄膜包括： A1203薄膜、 Si02薄膜、 Ti02薄膜、 ZnO薄膜、 Hf02 薄膜、 MgO薄膜、 Zr02薄膜、 NiO薄膜、 CoO薄膜、 FeOx薄膜、 01(¾薄 膜、 B203薄膜、 In203薄膜、 Sn02薄膜、 Ga203薄膜、 Nb205薄膜、 Gd203 薄膜、 Ta205薄膜、 BN薄膜、 A1N薄膜、 TiN薄膜、 SiC薄膜、 ZnS薄膜、 ZrS薄膜、 HA薄膜、 W薄膜、 Pt薄膜、 Ru薄膜、 Pd薄膜、 PMDA-DAH 薄膜、 PMDA-ODA薄膜、 PMDA-EDA薄膜、 PMDA-PDA薄膜。 步骤 102: 将沉积有薄膜的所述基底材料固化。 When the film is a plurality of layers, the film is a multilayer film formed by overlapping any one of the following films, or a multilayer film formed by alternately overlapping any of the following, or a multilayer film formed by overlapping one of the following And a combined multilayer film of a plurality of layers formed by alternately overlapping with any of the following: the film comprises: A1 2 0 3 film, SiO 2 film, Ti0 2 film, ZnO film, Hf0 2 film, MgO film, Zr0 2 film , NiO film, CoO film, FeO x film, 01 ( 3⁄4 film, B 2 0 3 film, In 2 0 3 film, Sn0 2 film, Ga 2 0 3 film, Nb 2 0 5 film, Gd 2 0 3 film, Ta 2 0 5 film, BN film, A1N film, TiN film, SiC film, ZnS film, ZrS film, HA film, W film, Pt film, Ru film, Pd film, PMDA-DAH film, PMDA-ODA film, PMDA - EDA film, PMDA-PDA film. Step 102: Curing the substrate material deposited with a film.
具体地， 将沉积有薄膜的所述基底材料进行等离子体固化；  Specifically, the base material on which the thin film is deposited is subjected to plasma curing;
这里， 釆用惰性气体的等离子对沉积于基底材料的薄膜进行固化时， 由于惰性气体的等离子体到达基底材料表面能量温和， 不与基底材料的微 孔孔道内壁的薄膜及其表面的薄膜发生化学反应， 而且所述惰性气体的等 离子体能为基底材料的微孔孔道内壁的薄膜及其表面的薄膜、 以及基底材 料提供能量， 因此， 与传统的退火固化相比， 釆用惰性气体的等离子体固 化， 一方面能避免由于基底材料的微孔孔道内壁的薄膜及其表面的薄膜不 耐高温而导致对所述薄膜的材料造成损害的问题， 另一方面在对基底材料 的微孔孔道内壁的薄膜、 与基底材料不进行刻蚀的条件下， 能提高基底材 料的微孔孔道内壁的薄膜、 与基底材料的结合性。  Here, when the film deposited on the base material is cured by the plasma of the inert gas, the energy of the plasma of the inert gas reaches the surface of the base material is mild, and the film of the inner wall of the microporous channel of the base material and the film of the surface thereof are not chemically oxidized. The reaction, and the plasma of the inert gas can provide energy for the film of the inner wall of the microporous channel of the base material and the film of the surface thereof, and the substrate material, thereby being plasma-cured with an inert gas as compared with the conventional annealing curing. On the one hand, it can avoid the problem that the film of the inner wall of the microporous channel of the base material and the film on the surface thereof are not resistant to high temperature, causing damage to the material of the film, and on the other hand, the film on the inner wall of the microporous channel of the base material. Under the condition that the base material is not etched, the film of the inner wall of the microporous channel of the base material and the bonding property with the base material can be improved.
所述固化的步骤包括： 将沉积有薄膜的基底材料放入等离子体发生器 中， 固化 ls-200s; 其中， 所述等离子体发生器的功率为 50W-500W, 固化 气体为氦 He、 氖 Ne、 氩 Ar、 氪 Kr及氙 Xe等惰性气体中的一种或多种的 组合， 气体流量为 10sccm-200sccm;  The step of curing comprises: placing a substrate material deposited with a film into a plasma generator to cure ls-200s; wherein the power of the plasma generator is 50W-500W, and the curing gas is 氦He, 氖Ne a combination of one or more of an inert gas such as argon Ar, krypton Kr and 氙Xe, having a gas flow rate of 10 sccm to 200 sccm;
具体地， 将惰性气体等以一定的气流通入离子发生器中， 通过离子发 生器将惰性气体转化为与惰性气体对应的等离子体， 将沉积有薄膜的基底 材料在惰性气体的等离子体氛围下固化。  Specifically, an inert gas or the like is introduced into the ion generator with a certain gas flow, and the inert gas is converted into a plasma corresponding to the inert gas by the ion generator, and the substrate material deposited with the film is in a plasma atmosphere of an inert gas. Cured.
在一实施例中， 所述步骤 101之前， 所述方法还包括：  In an embodiment, before the step 101, the method further includes:
将所述基底材料进行清洗。  The substrate material is washed.
具体地， 将所述基底材料进行超声清洗。  Specifically, the substrate material is ultrasonically cleaned.
在一实施例中， 所述步骤 101之前， 所述方法还包括：  In an embodiment, before the step 101, the method further includes:
将所述基底材料进行活化。  The substrate material is activated.
在一实施例中， 所述步骤 101之前， 所述方法还包括：  In an embodiment, before the step 101, the method further includes:
将所述基底材料进行清洗； 将清洗后的所述基底材料进行活化。 Cleaning the substrate material; The cleaned substrate material is activated.
图 2 为本发明实施例微孔雾化片的制备方法的实现流程示意图二， 如 图 2所示， 所述方法包括：  FIG. 2 is a schematic diagram 2 of an implementation flow of a method for preparing a microporous atomization sheet according to an embodiment of the present invention. As shown in FIG. 2, the method includes:
步骤 201 : 将雾化片作为基底材料， 将所述基底材料进行清洗； 其中， 所述雾化片为金属雾化片、 陶瓷雾化片及有机材质雾化片中的 任——种。  Step 201: cleaning the base material by using the atomized sheet as a base material; wherein the atomized sheet is any one of a metal atomized sheet, a ceramic atomized sheet, and an organic material atomized sheet.
步骤 202: 将清洗后的所述基底材料进行活化；  Step 202: activating the cleaned substrate material;
这里， 所述活化包括： 化学溶液浸渍活化和紫外活化；  Here, the activation includes: chemical solution impregnation activation and ultraviolet activation;
其中， 所述化学溶液浸渍活化的步骤包括：  Wherein the step of impregnating and activating the chemical solution comprises:
步骤 A: 将所述基底材料浸渍于酸性溶液中超声清洗 5-30min， 然后釆 用蒸馏水清洗所述基底材料， 清洗至附着于所述基底材料的表面液体的 pH 值为中性为止；  Step A: immersing the base material in an acidic solution for ultrasonic cleaning for 5-30 min, then washing the base material with distilled water, and washing until the pH of the surface liquid attached to the base material is neutral;
步骤 B: 将所述基底材料浸渍于碱性溶液中超声清洗 5-30min， 然后釆 用蒸馏水清洗所述基底材料， 清洗至附着于所述基底材料表面的液体的 pH 值为中性为止。  Step B: The base material is immersed in an alkaline solution for ultrasonic cleaning for 5-30 min, and then the base material is washed with distilled water, and washed until the pH of the liquid attached to the surface of the base material is neutral.
这里， 所述步骤 A和步骤 B的执行顺序可以调换。  Here, the execution order of the steps A and B can be reversed.
其中， 所述酸性溶液为一种或几种酸经稀释后配置的弱酸性溶液； 且 所述酸性溶液为以下溶液中的一种或任意几种的混合； 所述溶液包括： 浓 度为 0.01-5g/L磷酸溶液， 浓度为 0.1-7g/L草酸溶液， 浓度为 l-10g/L醋酸 溶液， 浓度为 0.01-lg/L 盐酸溶液， 浓度为 0.1-2g/L 氢氟酸溶液， 浓度为 5-20g/L氟化氢铵溶液； Wherein, the acidic solution is a weakly acidic solution in which one or several acids are diluted; and the acidic solution is one or a mixture of the following solutions; the solution includes: a concentration of 0.01- 5g / L phosphoric acid solution, concentration of 0.1-7g / L oxalic acid solution, concentration of l-10 g / L acetic acid solution, concentration of 0.01-lg / L hydrochloric acid solution, concentration of 0.1-2g / L hydrofluoric acid solution, concentration It is a 5-20 g/L ammonium hydrogen fluoride solution;
在一实施例中， 所述酸性溶液为以下溶液中的一种或任意几种的混合； 所述溶液包括： 浓度为 lg/L磷酸溶液， 浓度为 15g/L氟化氢氨溶液， 浓度 为 0.1g/L氢氟酸溶液。  In one embodiment, the acidic solution is one or a mixture of the following solutions; the solution comprises: a concentration of lg/L phosphoric acid solution, a concentration of 15 g/L hydrogen fluoride ammonia solution, a concentration of 0.1 g /L hydrofluoric acid solution.
在一实施例中， 所述酸性溶液为以下溶液中的一种或任意几种的混合； 所述溶液包括： 浓度为 5g/L草酸溶液， 浓度为 10g/L氟化氢氨溶液； 在一实施例中， 所述酸性溶液为以下溶液中的一种或任意几种的混合； 所述溶液为包括； 浓度为 6.5g/L醋酸溶液， 浓度为 0.05g/L盐酸溶液， 浓度 为 10g/L氟化氢氨溶液。 In one embodiment, the acidic solution is one or a mixture of any of the following solutions; The solution comprises: a concentration of 5 g / L of oxalic acid solution, a concentration of 10 g / L of hydrogen fluoride ammonia solution; in an embodiment, the acidic solution is one or a mixture of the following solutions; the solution To include: a concentration of 6.5 g / L acetic acid solution, a concentration of 0.05 g / L hydrochloric acid solution, a concentration of 10 g / L hydrogen fluoride ammonia solution.
所述碱性溶液为质量百分数为 1-20%的氨水； 在一实施例中， 所述碱 性溶液为质量百分数为 5-15%的氨水。  The alkaline solution is aqueous ammonia having a mass percentage of 1 to 20%; in one embodiment, the alkaline solution is aqueous ammonia having a mass percentage of 5-15%.
所述紫外活化的步骤包括： 将所述基底材料在紫外线灯下或者在能产 生紫外气体的等离子体气氛中， 照射 ls-120s进行活化。  The step of ultraviolet activation comprises: activating the substrate material under an ultraviolet lamp or in a plasma atmosphere capable of generating ultraviolet gas by irradiating ls-120s.
在具体实验过程中， 所述化学溶液浸渍活化和紫外活化的执行顺序能 够任意调换。  The order of execution of the chemical solution impregnation activation and ultraviolet activation can be arbitrarily exchanged during a specific experiment.
步骤 203: 在活化后的所述基底材料的微孔孔道内壁及其表面沉积薄 膜；  Step 203: depositing a film on the inner wall of the microporous channel of the base material after activation and a surface thereof;
具体地， 将活化后的所述基底材料放置于反应腔体内， 将各前驱体以 脉冲气体的方式交替通入所述反应腔体内， 在所述基底材料的微孔孔道内 壁及其表面沉积薄膜；  Specifically, the activated substrate material is placed in the reaction chamber, and each precursor is alternately introduced into the reaction chamber in a pulsed manner, and a film is deposited on the inner wall of the microporous channel of the base material and the surface thereof. ;
这里， 为使前后两种前驱体在反应腔体内不同时出现， 在通入一种前 驱体后、 与通入下一种前驱体前的间隙中， 使用清洗气体例如惰性气体等 吹扫所述反应腔体、 或对所述反应腔体进行抽真空处理， 以隔离前后两种 前驱体， 使前后两种前驱体不同时出现于所述反应腔体内。  Here, in order to prevent the two precursors from appearing differently in the reaction chamber, the purge gas such as an inert gas or the like is purged in the gap before the introduction of the precursor and before the passage into the next precursor. The reaction chamber is subjected to a vacuum treatment to isolate the two precursors before and after, so that the two precursors do not simultaneously appear in the reaction chamber.
在一实施例中， 所述在所述基底材料的微孔孔道内壁及其表面沉积薄 膜， 包括：  In one embodiment, the depositing a film on the inner wall of the microporous channel of the substrate material and the surface thereof comprises:
步骤一： 将所述基底材料放置于反应腔体内；  Step 1: placing the substrate material in the reaction chamber;
步骤二： 通入第一前驱体， 使所述第一前驱体与所述基底材料的微孔 孔道内壁及其表面的材料发生反应；  Step two: introducing a first precursor, reacting the first precursor with a material of the inner wall of the microporous channel of the base material and a surface thereof;
步骤三： 在反应完成后， 釆用清洗气体吹扫所述反应腔体、 或对所述 反应腔体进行抽真空将游离的所述第一前驱体排出所述反应腔体后， 通入 第二前驱体； Step three: after the reaction is completed, purging the reaction chamber with a cleaning gas, or After the reaction chamber is evacuated, the free first precursor is discharged into the reaction chamber, and then the second precursor is introduced;
步骤四： 循环执行所述步骤二和步骤三， 直至在所述基底材料的微孔 孔道内壁及其表面沉积预设厚度的薄膜为止。  Step 4: The steps 2 and 3 are performed cyclically until a film of a predetermined thickness is deposited on the inner wall of the microporous channel of the base material and the surface thereof.
在本实施例整个实验过程均是在抽真空下进行的， 但是， 在第一次脉 冲前驱体前， 所述反应腔体的压强处于 l OPa至 l (T2 Pa; 每次釆用脉冲气体 的方式向所述反应腔体内通入前驱体， 每次脉冲前驱体 0. 015S -50S , 脉冲 完一次前驱体后， 向所述反应腔体内通入流量为 0sccm-120sccm的氩气 Ar 或氮气 N2吹扫所述反应腔体 ls-120s， 随后脉冲另一前驱体； 这里， 各前驱 体可以通过载气进入所述反应腔体内， 所述载体可以为氮气 N2或氩气 Ar; 这里， 由于在脉冲两种前驱体的间隙中， 向所述反应腔体中通入氩气 Ar或 氮气 N2， 因此， 能将所述反应腔体内多余的前驱体及反应副产物排出。 In the present embodiment, the entire experimental process is carried out under vacuum, but before the first pulse precursor, the pressure of the reaction chamber is in the range of OPa to l (T 2 Pa; The method of introducing a precursor into the reaction chamber, each pulse precursor 0. 015S -50S, after the pulse is completed once, a flow rate of 0sccm-120sccm of argon Ar or nitrogen is introduced into the reaction chamber. N 2 purging the reaction chamber ls-120s, and then pulse another precursor; here, each precursor may enter the reaction chamber through a carrier gas, the carrier may be nitrogen N 2 or argon Ar; Since argon gas Ar or nitrogen gas N 2 is introduced into the reaction chamber in the gap between the two precursors of the pulse, excess precursor and reaction by-products in the reaction chamber can be discharged.
这里，当向所述反应腔体内通入的氩气 Ar或氮气 N2的流量为 Osccm时， 表示未向反应腔体中通入气体， 此时， 由于反应腔体中依然保持着抽真空 的状态， 因此， 通过抽真空的过程可以使上一次脉冲的前驱体中游离的部 分或反应副产物排出。 Here, when the flow rate of the argon gas Ar or the nitrogen gas N 2 introduced into the reaction chamber is Osccm, it means that no gas is introduced into the reaction chamber, and at this time, since the reaction chamber still maintains a vacuum. State, therefore, a free portion or reaction by-product in the precursor of the last pulse can be discharged by a vacuuming process.
这里， 第一次通入的前驱体可以与基底材料的微孔孔道内壁及其表面 的材料发生化学吸附反应， 形成第一薄膜， 随后， 所述第一薄膜与第二次 通入的前驱体发生反应形成第二薄膜， 依此类推， 直至形成预设厚度的薄 膜为止； 其中， 各前驱体可以根据薄膜的化学组成任意选择。  Here, the first-passed precursor may be chemically adsorbed with the material of the inner wall of the microporous channel of the base material and the surface thereof to form a first film, and then the first film and the second-pass precursor are formed. The reaction takes place to form a second film, and so on, until a film of a predetermined thickness is formed; wherein each precursor can be arbitrarily selected according to the chemical composition of the film.
较佳地， 所述薄膜为一层或多层厚度均勾的薄膜；  Preferably, the film is one or more layers of thickness-hooked film;
当所述薄膜为一层时， 所述薄膜为以下薄膜中的任意一种；  When the film is a layer, the film is any one of the following films;
当所述薄膜为多层时， 所述薄膜为以下薄膜中的任意一种重叠形成的 多层薄膜， 或以下任意几种交替重叠形成的多层薄膜， 或以下一种重叠形 成的多层薄膜和以下任意几种交替重叠形成的多层薄膜的组合多层薄膜； 所述薄膜包括： A1203薄膜、 Si02薄膜、 Ti02薄膜、 ZnO薄膜、 Hf02 薄膜、 MgO薄膜、 Zr02薄膜、 NiO薄膜、 CoO薄膜、 FeOx薄膜、 01(¾薄 膜、 B203薄膜、 In203薄膜、 Sn02薄膜、 Ga203薄膜、 Nb205薄膜、 Gd203 薄膜、 Ta205薄膜、 BN薄膜、 A1N薄膜、 TiN薄膜、 SiC薄膜、 ZnS薄膜、 ZrS薄膜、 HA薄膜、 W薄膜、 Pt薄膜、 Ru薄膜、 Pd薄膜、 PMDA-DAH 薄膜、 PMDA-ODA薄膜、 PMDA-EDA薄膜及 PMDA-PDA薄膜。 When the film is a plurality of layers, the film is a multilayer film formed by overlapping any one of the following films, or a multilayer film formed by alternately overlapping any of the following, or a multilayer film formed by overlapping one of the following a combined multilayer film of a multilayer film formed by alternately overlapping any of the following; The film comprises: A1 2 0 3 film, SiO 2 film, Ti 2 film, ZnO film, Hf0 2 film, MgO film, Zr0 2 film, NiO film, CoO film, FeO x film, 01 (3⁄4 film, B 2 0 3 film, In 2 0 3 film, Sn0 2 film, Ga 2 0 3 film, Nb 2 0 5 film, Gd 2 0 3 film, Ta 2 5 film, BN film, A1N film, TiN film, SiC film, ZnS film, ZrS film, HA film, W film, Pt film, Ru film, Pd film, PMDA-DAH film, PMDA-ODA film, PMDA-EDA film and PMDA-PDA film.
步骤 204: 将沉积有薄膜的所述基底材料固化。  Step 204: Curing the substrate material on which the film is deposited.
具体地， 将沉积有薄膜的所述基底材料进行等离子体固化， 所述等离 子固化的步骤包括： 将沉积有薄膜的基底材料放入等离子体发生器中， 固 化 ls-200s; 其中， 所述等离子体发生器的功率为 50W-500W, 固化气体为 He、 Ne、 Ar、 Kr、 Xe中的一种或多种的组合， 气体流量为 10sccm-200sccm。  Specifically, the substrate material on which the thin film is deposited is subjected to plasma curing, and the step of plasma curing comprises: placing a substrate material deposited with a thin film into a plasma generator to cure ls-200s; wherein the plasma The power of the body generator is 50W-500W, and the curing gas is a combination of one or more of He, Ne, Ar, Kr, Xe, and the gas flow rate is 10 sccm-200 sccm.
釆用本发明实施例制备出的微孔雾化片的孔径尺寸能够在几纳米到几 十微米间精确可控， 即能精确控制微孔雾化片的微孔孔径的尺寸， 因此， 能够实现超微细气雾颗粒； 而且， 由于所述微孔雾化片的微孔孔道内壁及 其表面沉积薄膜， 且所述薄膜能够选用的材料多种多样， 又由于不同材料 的薄膜的化学性能不同， 因此， 通过单一材料形成的薄膜、 或多种材料交 替重叠形成厚度均勾的组合薄膜， 能够实现所述微孔雾化片的不同化学性 能， 扩充了被雾化液体的种类； 如通过薄膜的化学形成使所述微孔雾化片 具有生物相容性、 阻隔有害离子析出、 自清洁、 耐酸 /耐碱腐蚀、 超微细雾 化效果好、 防气溶胶凝聚疏水、 易于清洗等性能； 而且， 在微孔雾化片的 微孔孔道内壁沉积一定厚度的薄膜， 能够使所述微孔雾化片的雾化区形成 疏水层， 因此， 能够避免气溶胶聚集在所述雾化区而导致的降低雾化效率 的问题。  The pore size of the microporous atomized sheet prepared by using the embodiment of the invention can be precisely controlled between several nanometers and several tens of micrometers, that is, the size of the micropore diameter of the microporous atomized sheet can be precisely controlled, thereby enabling Ultrafine aerosol particles; moreover, due to the deposition of a film on the inner wall of the microporous channel of the microporous atomized sheet and the surface thereof, and the materials available for the film are various, and due to the different chemical properties of the films of different materials, Therefore, a film formed by a single material, or a plurality of materials alternately overlap to form a combined film having a thickness-hook, which can realize different chemical properties of the microporous atomized sheet, and expand the kind of the atomized liquid; for example, through a film. The chemical formation makes the microporous atomized sheet have the properties of biocompatibility, barrier of harmful ion precipitation, self-cleaning, acid/alkali corrosion resistance, superfine atomization effect, anti-aerosol condensation, and easy cleaning; Depositing a film of a certain thickness on the inner wall of the microporous orifice of the microporous atomization sheet enables the atomization zone of the microporous atomization sheet to form a hydrophobic layer. Therefore, it is possible to avoid the problem of reducing the atomization efficiency caused by the accumulation of aerosol in the atomization zone.
另外， 由于本发明实施例制备的微孔雾化片的微孔孔道内壁的薄膜及 其表面的薄膜为逐层沉积的， 而且所述薄膜对所述微孔雾化片的微孔孔道 内壁其表面进行了全包覆， 例如， 本发明实施例能够将常用雾化片中肉眼 难以观测出的裂痕或断裂通过逐层包覆的方式， 修复所述雾化片， 如此， 能够提高本发明实施例制备出的微孔雾化片的断裂强度； 而且， 所述薄膜 与基底材料结合牢固紧密， 不会因为震动而导致薄膜玻璃剥离或脱落。 In addition, the film of the inner wall of the microporous channel of the microporous atomization sheet prepared by the embodiment of the invention and the film on the surface thereof are deposited layer by layer, and the film is microporous to the microporous atomization sheet. The surface of the inner wall is completely covered. For example, in the embodiment of the present invention, the atomized sheet can be repaired by laminating the crack or the fracture which is difficult to be observed by the naked eye in the conventional atomized sheet, thereby improving the present invention. The breaking strength of the microporous atomized sheet prepared by the embodiment of the invention; moreover, the film is firmly bonded to the substrate material, and the film glass is not peeled off or peeled off due to vibration.
由于本发明实施例选用的雾化片为市场中常用的雾化片， 又由于所述 雾化片能够通过本发明实施例将其雾化区的孔径缩小， 因此， 本发明实施 例能够为实现各领域的气雾发生器中雾化片的通用奠定基础。  Since the atomizing sheet selected in the embodiment of the present invention is an atomizing sheet commonly used in the market, and the atomizing sheet can reduce the aperture of the atomizing area by the embodiment of the present invention, the embodiment of the present invention can realize The general basis for the atomization of the aerosol generator in various fields.
图 3 为本发明实施例微孔雾化片的结构示意图； 釆用上述微孔雾化片 的制备方法制备出如图 3所示的微孔雾化片， 如图 3所示， 所述微孔雾化 片设置有微孔区 301， 所述微孔区内 301分布有多个微孔 302; 所述微孔雾 化片的微孔孔道内壁及其表面包覆有薄膜； 所述微孔的孔径为
Figure imgf000014_0001
3 is a schematic structural view of a microporous atomization sheet according to an embodiment of the present invention; 微 a microporous atomization sheet as shown in FIG. 3 is prepared by using the above microporous atomization sheet preparation method, as shown in FIG. The pore atomizing sheet is provided with a microporous region 301, wherein the microporous region 301 is distributed with a plurality of micropores 302; the inner wall of the microporous orifice of the microporous atomizing sheet and the surface thereof are coated with a thin film; The aperture is
Figure imgf000014_0001
上述方案中， 所述微孔区 301中微孔 302的数量为 100-1000000个。 上述方案中， 如图 3所示， 所述 孔雾化片的直径 为 l-50mm。 上述方案中， 如图 3所示， 所述微孔区的外径 R2为 l-50mm。 In the above solution, the number of the micro holes 302 in the micropore region 301 is 100-1000000. In the above solution, as shown in FIG. 3, the hole atomizing sheet has a diameter of 1 to 50 mm. In the above solution, as shown in FIG. 3, the outer diameter R 2 of the micropore region is 1 to 50 mm.
上述方案中， 所述微孔雾化片： 为金属雾化片、 陶瓷雾化片及有机材 质雾化片中的任意一种。  In the above aspect, the microporous atomized sheet is any one of a metal atomizing sheet, a ceramic atomizing sheet, and an organic material atomizing sheet.
上述方案中， 所述微孔雾化片的微孔孔道内壁及其表面的包覆材料为 一层或多层厚度均匀的薄膜；  In the above solution, the inner wall of the microporous channel of the microporous atomization sheet and the coating material of the surface thereof are one or more layers of uniform thickness;
当所述包覆材料为一层时， 所述包覆材料为以下薄膜中的任意一种； 当所述包覆材料为多层时， 所述包覆材料为以下薄膜中的任意一种重 叠形成的多层薄膜， 或以下任意几种交替重叠形成的多层薄膜， 或以下一 种重叠形成的多层薄膜和以下任意几种交替重叠形成的多层薄膜的组合多 层薄膜；  When the coating material is a layer, the coating material is any one of the following films; when the coating material is a plurality of layers, the coating material is overlapped by any one of the following films a multilayer film formed, or a multilayer film formed by alternately overlapping any of the following, or a composite film of a multilayer film formed by overlapping one of the following and a multilayer film of any of the following alternately stacked layers;
所述薄膜包括： A1203薄膜、 Si02薄膜、 Ti02薄膜、 ZnO薄膜、 Hf02 薄膜、 MgO薄膜、 Zr02薄膜、 NiO薄膜、 CoO薄膜、 FeOx薄膜、 01(¾薄 膜、 B203薄膜、 In203薄膜、 Sn02薄膜、 Ga203薄膜、 Nb205薄膜、 Gd203 薄膜、 Ta205薄膜、 BN薄膜、 A1N薄膜、 TiN薄膜、 SiC薄膜、 ZnS薄膜、 ZrS薄膜、 HA薄膜、 W薄膜、 Pt薄膜、 Ru薄膜、 Pd薄膜、 PMDA-DAH 薄膜、 PMDA-ODA薄膜、 PMDA-EDA薄膜、 PMDA-PDA薄膜。 The film comprises: A1 2 0 3 film, SiO 2 film, Ti 2 film, ZnO film, Hf0 2 Film, MgO film, Zr0 2 film, NiO film, CoO film, FeO x film, 01 ( 3⁄4 film, B 2 0 3 film, In 2 3 3 film, Sn0 2 film, Ga 2 0 3 film, Nb 2 0 5 Film, Gd 2 0 3 film, Ta 2 5 5 film, BN film, A1N film, TiN film, SiC film, ZnS film, ZrS film, HA film, W film, Pt film, Ru film, Pd film, PMDA-DAH Film, PMDA-ODA film, PMDA-EDA film, PMDA-PDA film.
上述方案中， 所述微孔雾化片中微孔孔道的形状为： 圓形、 三角形、 椭圓形及方形中的任意一种。  In the above solution, the shape of the microporous channel in the microporous atomization sheet is any one of a circle, a triangle, an ellipse and a square.
上述方案中， 所述微孔雾化片中微孔孔道的横截面的形状为： 抛物线 形、 喇 形、 方形及梯形中的任意一种； 这里， 所述微孔孔道的横截面的 形状还可以为任意对称型图形。  In the above solution, the shape of the cross section of the microporous channel in the microporous atomization sheet is: any one of a parabola shape, a bar shape, a square shape, and a trapezoid shape; here, the shape of the cross section of the microporous channel is further Can be any symmetrical shape.
这里， 本发明实施例给出的微孔雾化片中微孔孔道的形状仅用于进一 步详细说明微孔雾化片结构， 并未用于限制本发明， 在实际应用过程中， 所述微孔雾化片中微孔孔道的形状还可以为其他任意形状， 此处不再赘述。  Here, the shape of the microporous channel in the microporous atomization sheet of the embodiment of the present invention is only used to further explain the structure of the microporous atomization sheet, and is not used to limit the present invention. In practical application, the micro The shape of the microporous channel in the hole atomizing sheet may also be any other shape, which will not be described herein.
图 4为本发明实施例微孔雾化片中微孔孔道的横截面图， 如图 4所示， 所述微孔孔道形状为抛物线形。  4 is a cross-sectional view of a microporous orifice in a microporous atomization sheet according to an embodiment of the present invention. As shown in FIG. 4, the microporous orifice has a parabolic shape.
本发明实施例还提供了一种微孔雾化装置， 包括： 雾化器箱体、 与所 述雾化器箱体连接的气雾发生器、 以及与雾化器箱体连接的电子电路控制 器； 其中， 所述气雾发生器中包括微孔雾化片， 所述微孔雾化片为以上所 述的任意一种微孔雾化片。  The embodiment of the invention further provides a micropore atomization device, comprising: an atomizer box, an aerosol generator connected to the atomizer box, and an electronic circuit control connected to the atomizer box The gas mist generator includes a microporous atomization sheet, and the microporous atomization sheet is any one of the microporous atomization sheets described above.
图 5为本发明实施例雾化器箱体的结构示意图； 图 5 ( a ) 为本发明实 施例雾化器箱体的主视图； 图 5 ( b )为本发明实施例雾化器箱体的侧视图； 图 5 ( c )为本发明实施例沿图 5 ( b ) 中 A-A线的剖视图； 如图 5所示， 所 述雾化器箱体 10包括： 上外壳 11、 下外壳 21及气雾附件 31 ; 其中， 所述 上外壳 11通过气雾附件 31与下外壳 21连接；  5 is a schematic structural view of an atomizer case according to an embodiment of the present invention; FIG. 5( a ) is a front view of the atomizer case according to an embodiment of the present invention; FIG. 5 ( b ) is an atomizer case according to an embodiment of the present invention; Figure 5 (c) is a cross-sectional view taken along line AA of Figure 5 (b) of the embodiment of the present invention; as shown in Figure 5, the atomizer case 10 includes: an upper casing 11, a lower casing 21, and An aerosol attachment 31; wherein the upper casing 11 is connected to the lower casing 21 via an aerosol attachment 31;
图 6为本发明实施例气雾发生器的结构示意图一； 图 6 ( a ) 为本发明 实施例气雾发生器的侧视图； 图 6 (b) 为本发明实施例气雾发生器的具体 结构示意图； 图 6 (c) 为本发明实施例沿图 6 (a) 中的 B-B线的剖视图； 如图 6所示， 所述气雾发生器 40 包括： 微孔雾化片 41、 环形压电陶瓷片 42、 密封件 43及电路引出线 44; Figure 6 is a schematic structural view 1 of an aerosol generator according to an embodiment of the present invention; Figure 6 (a) is the present invention FIG. 6(b) is a schematic view showing a specific structure of an aerosol generator according to an embodiment of the present invention; FIG. 6(c) is a view along line BB of FIG. 6(a) according to an embodiment of the present invention. The gas mist generator 40 includes: a microporous atomizing sheet 41, a ring-shaped piezoelectric ceramic sheet 42, a sealing member 43 and a circuit lead-out line 44;
图 7为本发明实施例气雾发生器的结构示意图二； 图 7 (a) 为本发明 实施例气雾发生器的侧视图； 图 7 (b) 为本发明实施例气雾发生器的具体 结构示意图； 图 7 (c) 为本发明实施例沿图 7 (a) 中的 C-C线的剖视图； 如图 7所示， 所述气雾发生器 40 包括： 微孔雾化片 41、 环形压电陶瓷片 42、 密封件 43、 电路引出线 44及环形垫片 45;  7 is a schematic structural view of an aerosol generator according to an embodiment of the present invention; FIG. 7(a) is a side view of an aerosol generator according to an embodiment of the present invention; and FIG. 7(b) is a specific embodiment of an aerosol generator according to an embodiment of the present invention; Figure 7 (c) is a cross-sectional view taken along line CC of Figure 7 (a) of the embodiment of the present invention; as shown in Figure 7, the aerosol generator 40 comprises: a micro-atomized atomizing sheet 41, annular pressure An electric ceramic sheet 42, a sealing member 43, a circuit lead wire 44 and an annular gasket 45;
图 8为本发明实施例电子电路控制器的结构示意图； 图 8 (a) 为本发 明实施例电子电路控制器的主视图； 图 8 (b) 为本发明实施例电子电路控 制器的侧视图； 图 8(c)为本发明实施例沿图 8(b)中的 D-D线的剖视图； 如图 8所示， 所述电子电路控制器 50包括： 电路板 51、 及固定于所述电路 板 51上的开关控制器 52、 显示灯 53和外接电源输入口 54; 其中， 所述电 子电路控制器 50可以由内部电池供电， 也可以通过外接电源输入口 54与 外接电源连接进行供电。  8 is a schematic structural view of an electronic circuit controller according to an embodiment of the present invention; FIG. 8(a) is a front view of an electronic circuit controller according to an embodiment of the present invention; and FIG. 8(b) is a side view of an electronic circuit controller according to an embodiment of the present invention; Figure 8 (c) is a cross-sectional view taken along line DD of Figure 8 (b) of the embodiment of the present invention; as shown in Figure 8, the electronic circuit controller 50 includes: a circuit board 51, and is fixed to the circuit board The switch controller 52 on the 51, the display lamp 53 and the external power input port 54; wherein the electronic circuit controller 50 can be powered by an internal battery, or can be connected to an external power source through the external power input port 54 for power supply.
具体地， 如图 5所示， 所述上外壳 11 包括： 上盖板 12、 液体槽 13、 气雾发生器固定装置 14及线路出口 15; 其中， 所述上盖板 12内部设有卡 槽结构， 所述液体槽 13上部外表面设有螺紋卡槽结构， 且上盖板 12可以 通过自身内部的卡槽结构、 及液体槽 13上部外表面的螺紋卡槽结构旋转固 定于所述液体槽 13的上部， 如此， 能防止雾化箱体翻倒导致液体流出； 所 述气雾发生器固定装置 14将图 6或图 7所示的气雾发生器 40固定于所述 液体槽 13的下部， 且所述液体槽 13底部是通孔或者栅板结构， 如此， 能 使被雾化的液体与气雾发生器 40充分接触； 所述下外壳 21 包括： 弧形气 溶胶排出通道 22、 气溶胶排出口 23; 其中， 所述下外壳 21上部外表面设 有凹槽结构， 所述上外壳 11下部内表面设有凸槽结构， 如此， 所述下外壳 21与上外壳 11通过咬合相互连接； 所述气雾发生器 40与图 8所示的电子 电路控制器 50通过所述线路接口 15连接。 Specifically, as shown in FIG. 5, the upper casing 11 includes: an upper cover 12, a liquid tank 13, an aerosol generator fixing device 14, and a line outlet 15; wherein the upper cover 12 is provided with a card slot The upper outer surface of the liquid tank 13 is provided with a threaded slot structure, and the upper cover 12 can be rotatably fixed to the liquid tank by a slot structure of the inner portion thereof and a threaded slot structure of the upper outer surface of the liquid tank 13 The upper portion of 13, in this way, prevents the atomization tank from tipping over and causing the liquid to flow out; the aerosol generator fixing device 14 fixes the aerosol generator 40 shown in Fig. 6 or Fig. 7 to the lower portion of the liquid tank 13 And the bottom of the liquid tank 13 is a through hole or a grid structure, so that the atomized liquid can be in sufficient contact with the aerosol generator 40; the lower casing 21 includes: an arc-shaped aerosol discharge passage 22, gas a sol discharge port 23; wherein, the upper outer surface of the lower outer casing 21 is provided a grooved structure, the lower inner surface of the upper casing 11 is provided with a convex groove structure, such that the lower casing 21 and the upper casing 11 are connected to each other by snapping; the aerosol generator 40 and the electronic circuit shown in FIG. The controller 50 is connected through the line interface 15.
这里， 所述气雾附件 31能够适用于不同装置中； 例如本发明实施例所 述的气雾附件 31能够在口吸入罩、 鼻吸入罩、 面罩及扩散罩等中任意一个 装置中充当气雾附件。 待气雾附件 31开启后， 气雾发生器 40产生的气溶 胶通过弧形气溶胶排出通道 22及气溶胶排出口 23与大气相通。  Here, the aerosol attachment 31 can be applied to different devices; for example, the aerosol attachment 31 according to the embodiment of the present invention can act as an aerosol in any one of a mouth suction cover, a nasal suction cover, a face mask, and a diffusion cover. annex. After the aerosol attachment 31 is opened, the aerosol dissolved by the aerosol generator 40 is passed through the arc-shaped aerosol discharge passage 22 and the aerosol discharge port 23 to the atmosphere.
具体地， 如图 6所示， 所述微孔雾化片 41中心区域具有均勾分布的微 孔， 所述均勾分布的微孔所处的区域称为微孔区， 环形压电陶瓷片 42内径 与所述微孔雾化片 41中所述微孔区相对且包围所述微孔区， 并通过焊接或 者胶粘技术将所述环形压电陶瓷片 42 固定于所述微孔雾化片 41上， 所述 微孔雾化片 41的中心与所述环形压电陶瓷片 42的中心重合； 这里， 所述 环形压电陶瓷片 42可以固定于所述微孔雾化片 41上表面， 也可以固定于 所述微孔雾化片 41 的下表面； 所述密封件 43将固定于一起的所述微孔雾 化片 41和所述环形压电陶瓷片 42紧紧包裹， 仅剩下所述微孔雾化片 41中 的所述微孔区， 这里， 所述微孔区又称为雾化区， 如此， 能够将除雾化区 以外的部分与被雾化液体隔离， 进而能防止所述微孔雾化片 41和环形压电 陶瓷片 42由于长时间接触被雾化液体而被腐蚀； 所述电路引出线 44与所 述环形压电陶瓷片 42的上下表面的任意两点连接； 其中， 所述电路引出线 44与所述环形压电陶瓷片 42连接的部分由密封件 43均勾包裹密封； 所述 电路引出线 44穿过图 5所示的所述上外壳 11及线路出口 15与图 8所示的 所述电子电路控制器 50相连接。  Specifically, as shown in FIG. 6 , the central region of the microporous atomization sheet 41 has micropores uniformly distributed, and the region where the micropores distributed by the hooks are located is called a microporous region, and the annular piezoelectric ceramic sheet is An inner diameter of 42 is opposite to the microporous region of the microporous atomizing sheet 41 and surrounds the microporous region, and the annular piezoelectric ceramic sheet 42 is fixed to the microporous atomization by welding or gluing techniques. On the sheet 41, the center of the microporous atomizing sheet 41 coincides with the center of the annular piezoelectric ceramic sheet 42; here, the annular piezoelectric ceramic sheet 42 may be fixed to the upper surface of the microporous atomizing sheet 41. And may be fixed to the lower surface of the microporous atomizing sheet 41; the sealing member 43 tightly wraps the microporous atomizing sheet 41 and the annular piezoelectric ceramic sheet 42 fixed together, and only The micropore region in the microporous atomization sheet 41, wherein the micropore region is also referred to as an atomization region, so that a portion other than the atomization region can be isolated from the atomized liquid, and further It is possible to prevent the microporous atomizing sheet 41 and the annular piezoelectric ceramic sheet 42 from coming into contact for a long time. The circuit lead wire 44 is connected to any two points of the upper and lower surfaces of the annular piezoceramic piece 42; wherein the circuit lead wire 44 is connected to the annular piezoceramic piece 42 Partially sealed by the sealing member 43; the circuit lead wire 44 is connected to the electronic circuit controller 50 shown in FIG. 8 through the upper casing 11 and the line outlet 15 shown in FIG.
或者，如图 7所示，所述微孔雾化片 41中心区域具有分布均勾的微孔， 所述均勾分布的微孔所处的区域称为微孔区， 且所述微孔雾化片 41除所述 微孔区以外的边缘区域通过焊接或者胶粘技术固定于所述环形垫片 45上， 同时， 所述环形垫片 45的内径包围所述微孔区， 但不堵塞所述微孔区中的 微孔； 所述微孔雾化片 41 的中心与所述环形垫片 45的中心重合； 所述环 形压电陶瓷片 42通过焊接或者胶粘技术固定于所述环形垫片 45上， 且所 述环形压电陶瓷片 42的中心与所述环形垫片 45的中心重合， 即所述环形 压电陶瓷片 42的内径与所述微孔雾化片 41 中的所述微孔区相对； 这里， 所述环形压电陶瓷片 42可以固定于所述环形垫片 45的上表面， 也可以固 定于所述环形垫片 45的下表面； 所述密封件 43将固定于一起的微孔雾化 片 41、 环形压电陶瓷片 42及环形垫片 45紧紧包围， 仅剩下所述微孔雾化 片 41中的所述微孔区， 这里， 所述微孔区又称为雾化区， 如此， 能够将除 雾化区以外的部分与被雾化液体隔离， 进而能防止所述微孔雾化片 41、 环 形压电陶瓷片 42和环形垫片 45由于长时间接触被雾化液体而被腐蚀； 所 述环形压电陶瓷片 42与所述环形垫片 45相连通， 所述环形压电陶瓷片 42 与所述环形垫片 45的未连通的棵露的上下表面两点与电路引出线 44相连 接； 其中， 所述电路引出线 44与所述环形压电陶瓷片 42连接的部分由密 封件 43均匀包裹密封； 所述电路引出线 44穿过图 5所示的所述上外壳 11 及线路出口 15与图 8所示的所述电子电路控制器 50相连接。 Or, as shown in FIG. 7, the central region of the microporous atomization sheet 41 has micropores distributed uniformly, and the region where the micropores distributed by the hooks are located is called a micropore region, and the microporous mist The edge region of the chemical sheet 41 except the microporous region is fixed to the annular gasket 45 by soldering or gluing techniques. Meanwhile, the inner diameter of the annular spacer 45 surrounds the micropore region, but does not block the micropores in the micropore region; the center of the microporous atomization sheet 41 coincides with the center of the annular spacer 45. The annular piezoelectric ceramic piece 42 is fixed to the annular spacer 45 by soldering or gluing, and the center of the annular piezoelectric ceramic piece 42 coincides with the center of the annular spacer 45, that is, The inner diameter of the annular piezoelectric ceramic piece 42 is opposite to the micropore area in the microporous atomizing sheet 41; here, the annular piezoelectric ceramic piece 42 may be fixed to the upper surface of the annular spacer 45, It may be fixed to the lower surface of the annular gasket 45; the sealing member 43 tightly surrounds the microporous atomizing sheet 41, the annular piezoelectric ceramic sheet 42 and the annular gasket 45 fixed together, leaving only the The microporous region in the microporous atomizing sheet 41, wherein the microporous region is also referred to as an atomizing region, so that a portion other than the atomizing region can be isolated from the atomized liquid, thereby preventing the The microporous atomizing sheet 41, the annular piezoelectric ceramic sheet 42 and the annular spacer 45 are in contact for a long time The annular piezoelectric ceramic piece 42 is in communication with the annular gasket 45, and the annular piezoelectric ceramic piece 42 and the unconnected upper and lower surfaces of the annular spacer 45 are The point is connected to the circuit lead wire 44; wherein the portion of the circuit lead wire 44 connected to the annular piezoceramic piece 42 is uniformly wrapped and sealed by the sealing member 43; the circuit lead wire 44 passes through the circuit shown in FIG. The upper casing 11 and the line outlet 15 are connected to the electronic circuit controller 50 shown in FIG.
实施例一  Embodiment 1
一种微孔雾化片的制备方法， 具体步骤包括：  A method for preparing a microporous atomized sheet, the specific steps comprising:
步骤一： 将金属雾化片作为基底材料， 将所述基底材料进行超声清洗； 其中， 所述金属雾化片的微孔孔径为 21μπι;  Step 1: using a metal atomized sheet as a substrate material, the substrate material is ultrasonically cleaned; wherein the metal atomized sheet has a micropore diameter of 21 μm;
步骤二： 将所述基底材料放置于反应腔体内， 抽真空以使所述反应腔 体内的压强降至 10Pa; 随后， 首先脉冲三甲基铝 （TMA ) 50s后， 通入流 量为 lOOsccm的 N2气吹扫所述反应腔体 120s; 其次， 脉冲水蒸气 H20 30s 后， 通入流量为 120 sccm的 N2气吹扫所述反应腔体 120s， 如此交替脉冲 TMA和 ¾0， 直至在所述基底材料的微孔孔道内壁及其表面沉积 4200层 A1203薄膜为止； 其中， 所述 A1203薄膜厚度约为 500nm; Step 2: The substrate material is placed in the reaction chamber, and a vacuum is applied to reduce the pressure in the reaction chamber to 10 Pa. Subsequently, after first pulsing trimethylaluminum (TMA) for 50 s, a flow rate of 100 sec is introduced. 2 gas purging the reaction chamber 120s; secondly, after pulse water vapor H 2 0 30s, the reaction chamber 120s is purged with N 2 gas having a flow rate of 120 sccm, so that the pulses TMA and 3⁄40 are alternated until The inner wall of the microporous channel of the base material and the surface thereof are deposited 4200 layers A1 2 0 3 film; wherein, the A1 2 0 3 film has a thickness of about 500 nm;
步骤三： 将沉积有薄膜的所述基底材料放入等离子体发生器中， 固化 200s; 其中， 所述等离子体发生器的功率为 50W， 固化气体为 He的等离子 体， 气体气流为 200sccm。  Step 3: The substrate material deposited with the film is placed in a plasma generator and cured for 200 s; wherein the plasma generator has a power of 50 W, the curing gas is a He plasma, and the gas flow is 200 sccm.
这里，所述 A1203薄膜紧紧包覆于所述金属雾化片的微孔孔道内壁及其 表面，如此，将所述金属雾化片中微孔的孔径缩小至 20μπι得到微孔雾化片； 由于所述微孔雾化片的微孔孔道内壁及表面紧紧包覆有 Α1203薄膜， 因此， 能够避免因震荡而导致薄膜脱落的问题； 又由于所述微孔雾化片中 Α1203 薄膜的疏水性， 使得所述微孔雾化片具有良好的疏水性， 因此， 能够避免 气溶胶聚集在所述微孔雾化片的雾化区 （微孔区） 而导致降低雾化效率的 问题； 还由于所述 Α1203薄膜的耐腐蚀性， 因此， 使得本实施例所述微孔雾 化片具有良好的耐腐蚀性， 能够有效阻隔有害离子析出。 Here, the A1 2 0 3 film is tightly coated on the inner wall of the microporous channel of the metal atomizing sheet and the surface thereof, so that the pore diameter of the micropores in the metal atomizing sheet is reduced to 20 μm to obtain a micropore mist. of the sheet; pore wall and since the porous surface of the microporous sheet is tightly covered with atomized Α1 2 0 3 film, it is possible to avoid problems caused by the shock of the falling film; and because the microporous atomizer Α1 2 0 3 film hydrophobic film, such that the atomizing microporous sheet having good hydrophobicity, it is possible to prevent the aerosol spray gathering in the region of the microporous film atomization (micropore region) and fogging problems lead to reduced efficiency; also because the Α1 2 0 3 film corrosion resistance, therefore, that the present embodiment has good corrosion resistance of the microporous sheet atomizing embodiment, can effectively block harmful ion elution.
本实施例中， 所述微孔雾化片的直径为 1mm; 所述微孔雾化片的微孔 区的外径为 1mm; 且所述微孔区中的微孔共 100; 所述微孔雾化片中微孔 孔道的形状为圓形； 所述微孔雾化片的微孔孔道的横截面的形状为喇 形。  In this embodiment, the microporous atomization sheet has a diameter of 1 mm; the micropore region of the microporous atomization sheet has an outer diameter of 1 mm; and the micropores in the microporous region have a total of 100; The shape of the microporous channel in the hole atomizing sheet is circular; the shape of the cross section of the microporous channel of the microporous atomizing sheet is a bell shape.
实施例二  Embodiment 2
一种微孔雾化片的制备方法， 具体步骤包括：  A method for preparing a microporous atomized sheet, the specific steps comprising:
步骤一： 将陶瓷雾化片作为基底材料， 将所述基底材料进行超声清洗； 其中， 所述陶瓷雾化片的微孔孔径为 ΙΟμπι;  Step 1: using a ceramic atomized sheet as a base material, the base material is ultrasonically cleaned; wherein the ceramic atomized sheet has a micropore diameter of ΙΟμπι;
步骤二： 将所述基底材料放置于反应腔体内， 抽真空以使所述反应腔 体内的压强降至 lO^Pa; 随后， 先脉冲三甲基铝（TMA ) 10s后， 通入流量 为 50sccm的 Ar气吹扫所述反应腔体 80s; 再脉冲水蒸气 ¾0 5s后， 通入 流量为 50sccm的 Ar气吹扫所述反应腔体 100s，如此交替脉冲 TMA和 ¾0， 直至在所述基底材料的微孔孔道内壁及其表面沉积 1000层 A1203薄膜， 其 中，所述 A1203薄膜的厚度约为 120nm;最后，脉冲四二甲氨基钛（ TDMAT ) Is后，通入流量为 30sccm的 Ar气吹扫所述反应腔体 80s，脉冲臭氧 03 0.02s 后， 通入流量为 30 sccm 的 Ar 气吹扫所述反应腔体 Is, 如此交替月永冲 TDMAT和 03， 在所述 A1203薄膜表面沉积 500层 Ti02薄膜， 所述 Ti02薄 膜厚度约为 30nm; Step 2: The substrate material is placed in the reaction chamber, and a vacuum is applied to reduce the pressure in the reaction chamber to 10^Pa; subsequently, after the trimethylaluminum (TMA) is pulsed for 10 seconds, the flow rate is 50 sccm. The Ar gas is purged into the reaction chamber 80s; after the water vapor is pulsed for 3⁄40 5s, the reaction chamber is purged with an Ar gas having a flow rate of 50 sccm, so that the pulses TMA and 3⁄40 are alternately pulsed until the base material is The inner wall of the microporous channel and the surface thereof are deposited with 1000 layers of A1 2 0 3 film, wherein the thickness of the A1 2 0 3 film is about 120 nm; finally, the pulsed tetramethylamino titanium (TDMAT) After Is, flow rate of Ar gas into the reaction chamber was purged 80s 30sccm after ozone pulse 0 3 0.02s, introduced at a flow of 30 sccm of Ar gas purging the reaction chamber Is, thus alternately month Wing Punching TDMAT and 0 3 , depositing 500 layers of Ti0 2 film on the surface of the A1 2 0 3 film, the thickness of the Ti0 2 film is about 30 nm;
步骤三： 将沉积有薄膜的所述基底材料放入等离子体发生器中， 固化 90s; 其中， 所述等离子体发生器的功率 100W， 固化气体为 He和 Ne混合 的等离子体， 气体 He的气流为 100sccm， 气体 Ne的气体气流为 40sccm。  Step 3: The substrate material deposited with the film is placed in a plasma generator and cured for 90 s; wherein the plasma generator has a power of 100 W, the curing gas is a He and Ne mixed plasma, and the gas He gas flow. At 100 sccm, the gas flow of the gas Ne was 40 sccm.
这里， 所述 A1203薄膜和 Ti02薄膜紧紧包覆于所述陶瓷雾化片的微孔 孔道内壁及其表面， 如此， 将所述陶瓷雾化片中微孔的孔径缩小至 9.7μπι 得到微孔雾化片； 由于所述微孔雾化片的微孔孔道内壁及表面紧紧包覆有 Α1203薄膜和 Ti02薄膜， 因此， 能够避免因震荡而导致薄膜脱落的问题； 又 由于所述微孔雾化片中 A1203薄膜和 Ti02薄膜的性能， 使得本发明实施例 得到的所述微孔雾化片具有生物相容性、 及自清洁性。 Here, the A1 2 0 3 film and the Ti 2 2 film are tightly coated on the inner wall of the microporous channel of the ceramic atomizing sheet and the surface thereof, so that the pore diameter of the micropores in the ceramic atomizing sheet is reduced to 9.7. μπι to obtain a microporous film atomization; pore wall and due to the porous surface of the microporous sheet is tightly covered with atomized Α1 2 0 3 and Ti0 2 thin film, it is possible to avoid problems caused by the shock of falling film Moreover, due to the properties of the A1 2 0 3 film and the Ti 2 2 film in the microporous atomized sheet, the microporous atomized sheet obtained by the embodiment of the invention has biocompatibility and self-cleaning property.
本实施例中， 所述微孔雾化片的直径为 30mm， 所述微孔雾化片的微孔 区的外径为 25mm; 且所述微孔区中的微孔共 5000个； 所述微孔雾化片中 微孔孔道的形状为椭圓形； 所述微孔孔道的横截面的形状为抛物线形。  In this embodiment, the diameter of the microporous atomization sheet is 30 mm, the outer diameter of the micropore region of the microporous atomization sheet is 25 mm; and the number of micropores in the micropore region is 5000; The shape of the microporous channel in the microporous atomization sheet is elliptical; the cross section of the microporous channel has a parabolic shape.
实施例三  Embodiment 3
一种微孔雾化片的制备方法， 具体步骤包括：  A method for preparing a microporous atomized sheet, the specific steps comprising:
步骤一： 将有机材质雾化片作为基底材料， 将所述基底材料进行超声 清洗；  Step 1: using an organic material atomized sheet as a base material, and ultrasonically cleaning the base material;
其中， 所述有机材质雾化片的微孔孔径为 5μπι;  Wherein the microporous pore diameter of the organic material atomized sheet is 5 μπι;
步骤二： 将所述基底材料放置于反应腔体内， 抽真空以使所述反应腔 体内的压强降至 l(T2Pa; 随后， 先脉冲二乙基锌（DEZ ) 0.015s后， 抽真空 吹扫所述反应腔体 50s; 再脉冲氧等离子体 0.5s后，抽真空吹扫所述反应腔 体 30s， 如此交替脉冲 DEZ和氧等离子体， 直至在所述基底材料的微孔孔 道内壁及其表面沉积 5000层 ZnO薄膜， 其中， 所述 ZnO薄膜的厚度约为 lOOOnm; 然后， 脉冲均苯四甲酸二酐（ PMDA ) 8s后， 通入流量为 30sccm 的 N2气吹扫所述反应腔体 20s， 脉冲己二胺（ODA ) 3s后， 通入流量为 30sccm的 N2气吹扫所述反应腔 15s, 如此交替脉冲 PMDA和 ODA， 在所 述 ZnO薄膜表面沉积 1250层 PMDA-ODA薄膜， 所述 PMDA-ODA薄膜厚 度约为 1075nm; 最后， 脉冲四二甲氨基铪（ TDMAHf ) 0.1s后， 通入流量 为 20sccm的 Ar气吹扫所述反应腔体 5s, 脉冲水蒸气 H20 0.015s后， 通入 流量为 20sccm的 Ar气吹扫所述反应腔 3s，如此交替脉冲 TDMAHf和 ¾0， 在所述 PMDA-ODA薄膜表面沉积 3334层 Hf02薄膜， 所述 Hf02薄膜厚度 约为 400nm; Step 2: The substrate material is placed in the reaction chamber, and a vacuum is applied to reduce the pressure in the reaction chamber to 1 (T 2 Pa; then, after the pulse of diethyl zinc (DEZ) is 0.015 s, vacuum is applied. Purging the reaction chamber for 50 s; after pulsing the oxygen plasma for 0.5 s, vacuuming the reaction chamber for 30 s, thus alternately pulse DEZ and oxygen plasma until the micropores in the base material A 5000-layer ZnO thin film is deposited on the inner wall of the track and the surface thereof, wherein the thickness of the ZnO thin film is about 100 nm; then, after pulsed pyromellitic dianhydride (PMDA) for 8 s, a N 2 gas purge having a flow rate of 30 sccm is introduced. After the reaction chamber 20s, pulsed hexamethylene diamine (ODA) for 3 s, the reaction chamber was purged with N 2 gas at a flow rate of 30 sccm for 15 s, so that PMDA and ODA were alternately pulsed, and 1250 layers of PMDA were deposited on the surface of the ZnO thin film. -ODA film, the thickness of the PMDA-ODA film is about 1075 nm; finally, after pulsed tetramethylamino hydrazine (TDMAHf) for 0.1 s, the reaction chamber is purged with Ar gas having a flow rate of 20 sccm for 5 s, pulse water vapor After H 2 0 0.015 s, the reaction chamber was purged with Ar gas having a flow rate of 20 sccm for 3 s, thus alternately pulsed TDMAHf and 3⁄40, and 3334 layers of HfO 2 film deposited on the surface of the PMDA-ODA film, the Hf0 2 film The thickness is about 400 nm;
步骤三： 将沉积有薄膜的所述基底材料放入等离子体发生器中， 固化 Is; 其中， 所述等离子体发生器的功率 500W， 固化气体为 Ar和 Xe混合的 等离子体， 气体 Ar的气流为 10sccm， 气体 Xe的气体气流为 50sccm。  Step 3: The substrate material deposited with the film is placed in a plasma generator to cure Is; wherein the plasma generator has a power of 500 W, the curing gas is a plasma mixed with Ar and Xe, and the gas of the gas Ar At 10 sccm, the gas flow of the gas Xe was 50 sccm.
这里， 所述 ZnO薄膜、 PMDA-ODA薄膜和 Hf02薄膜紧紧包覆于所述 有机材质雾化片的微孔孔道内壁及其表面， 如此， 将所述有机材质雾化片 中微孔的孔径缩小至 0.05μπι得到微孔雾化片； 由于所述微孔雾化片的微孔 孔道内壁及表面紧紧包覆有 ZnO薄膜、 PMDA-ODA薄膜和 Hf02薄膜， 因 此，能够避免因震荡而导致薄膜脱落的问题；又由于所述微孔雾化片中 ZnO 薄膜、 PMDA-ODA薄膜和 Hf02薄膜的化学及物理性能， 使得本发明实施 例得到的所述微孔雾化片具有耐磨性、 耐酸碱腐蚀及有效阻隔有害离子析 出。 Here, the ZnO film, the PMDA-ODA film, and the Hf0 2 film are tightly coated on the inner wall of the microporous channel of the organic material atomizing sheet and the surface thereof, so that the microporous material in the organic material atomizing sheet is The pore diameter is reduced to 0.05 μm to obtain a microporous atomized sheet; since the inner wall and surface of the microporous orifice of the microporous atomized sheet are tightly coated with a ZnO thin film, a PMDA-ODA thin film and an HfO 2 thin film, it is possible to avoid turbulence The problem of causing the film to fall off; and the microporous atomized sheet obtained by the embodiment of the invention has wear resistance due to the chemical and physical properties of the ZnO film, the PMDA-ODA film and the Hf0 2 film in the microporous atomized sheet. Sex, acid and alkali corrosion and effective barrier to the deposition of harmful ions.
本实施例中， 所述微孔雾化片的直径为 50mm， 所述微孔雾化片的微孔 区的外径为 50mm; 且所述微孔区中的微孔共 1000000个； 所述微孔雾化片 中微孔孔道的形状为三角形； 所述微孔孔道的横截面的形状为梯形。  In this embodiment, the microporous atomization sheet has a diameter of 50 mm, the micropore region of the microporous atomization sheet has an outer diameter of 50 mm; and the micropores in the micropore region have a total of 1,000,000; The shape of the microporous channel in the microporous atomization sheet is a triangle; the shape of the cross section of the microporous channel is trapezoidal.
实施例四 一种微孔雾化片的制备方法， 具体步骤包括： Embodiment 4 A method for preparing a microporous atomized sheet, the specific steps comprising:
步骤一： 将金属雾化片作为基底材料， 将所述基底材料进行清洗； 其中， 所述金属雾化片的微孔孔径为 5μπι;  Step 1: using a metal atomizing sheet as a substrate material, the substrate material is cleaned; wherein the metal atomized sheet has a micropore diameter of 5 μm;
步骤二： 将清洗后的所述基底材料进行活化；  Step two: activating the cleaned substrate material;
具体地， 所述活化的步骤包括：  Specifically, the step of activating includes:
首先， 将所述基底材料浸渍于浓度为 lg/L 的磷酸溶液中超声清洗 5 min, 然后釆用蒸馏水清洗所述基底材料， 清洗至附着于所述基底材料的表 面液体的 pH值为中性为止；  First, the base material is immersed in a phosphoric acid solution having a concentration of lg/L for ultrasonic cleaning for 5 min, and then the base material is washed with distilled water, and the pH of the surface liquid adhered to the base material is neutral. So far
再次， 将所述基底材料浸渍于质量百分数为 15%的氨水中超声清洗 15 min, 然后釆用蒸馏水清洗所述基底材料， 清洗至附着于所述基底材料表面 的液体的 pH值为中性为止；  Again, the substrate material is immersed in a 15% by mass aqueous ammonia solution for ultrasonic cleaning for 15 minutes, and then the substrate material is washed with distilled water and washed until the pH of the liquid attached to the surface of the substrate material is neutral. ;
最后， 将所述基底材料在紫外线灯下照射 Is进行活化。  Finally, the substrate material is activated by irradiating Is under an ultraviolet lamp.
步骤三： 将活化后的所述基底材料放置于反应腔体内， 抽真空以使所 述反应腔体内的压强降至 l(T2Pa; 随后， 先脉冲 3-氨基丙基三乙氧基硅烷 ( AMEO ) 30s后， 通入流量为 20sccm的 N2气吹扫所述反应腔体 50s， 再 脉冲水蒸气 H20 0.015s后，抽真空所述反应腔体 ls，最后，脉冲臭氧 O320s 后，通入流量为 5sccm的 N2气吹扫所述反应腔体 10s,如此交替脉冲 AMEO、 H20和 03， 在所述基底材料的微孔孔道内壁及其表面沉积一层 Si02薄膜， 其中， 所述 Si02薄膜的厚度约为 0.1nm。 Step 3: placing the activated substrate material in the reaction chamber, evacuating to reduce the pressure in the reaction chamber to 1 (T 2 Pa; subsequently, first pulse 3-aminopropyltriethoxysilane After 30 s (AMEO), the reaction chamber was purged with N 2 gas with a flow rate of 20 sccm for 50 s, and after the water vapor H 2 0 0.015 s was pulsed, the reaction chamber ls was evacuated, and finally, the ozone O 3 was pulsed. After 20 s, the reaction chamber was purged with N 2 gas with a flow rate of 5 sccm for 10 s, so that AMEO, H 2 0 and 0 3 were alternately pulsed, and a layer of Si0 was deposited on the inner wall of the microporous channel of the base material and the surface thereof. 2 film, wherein the SiO 2 film has a thickness of about 0.1 nm.
步骤四： 将沉积有薄膜的所述基底材料放入等离子体发生器中， 固化 Is; 其中， 所述等离子体发生器的功率为 500W， 固化气体为 He和 Kr混合 的等离子体， 气体 He的气流为 10sccm， 气体 Kr的气体气流为 30sccm。  Step 4: The substrate material deposited with the film is placed in a plasma generator to cure Is; wherein the plasma generator has a power of 500 W, and the curing gas is a plasma of He and Kr mixed, and the gas He The gas flow was 10 sccm, and the gas flow of the gas Kr was 30 sccm.
这里， 所述 Si02薄膜紧紧包覆于所述金属雾化片的微孔孔道内壁及其 表面， 如此， 得到金属雾化片的微孔孔道内壁及其表面包覆有一层 Si02薄 膜的微孔雾化片， 虽然所述微孔雾化片中微孔的孔径几乎没有变化， 但是 由于所述微孔雾化片的微孔孔道内壁及其表面包覆有一层 Si02薄膜， 增强 了雾化片的断裂强度， 且所述 Si02薄膜具有耐酸 /碱腐蚀性， 因此， 使得所 述微孔雾化片具有良好的耐^/碱腐蚀性， 能有效阻隔有害离子析出。 Here, the SiO 2 film is tightly coated on the inner wall of the microporous channel of the metal atomizing sheet and the surface thereof, so that the inner wall of the microporous channel of the metal atomizing sheet and the surface thereof are coated with a layer of SiO 2 film. a microporous atomizing sheet, although the pore diameter of the micropore in the microporous atomizing sheet hardly changes, but Since the inner wall of the microporous orifice of the microporous atomized sheet and the surface thereof are coated with a SiO 2 film, the breaking strength of the atomized sheet is enhanced, and the SiO 2 film is resistant to acid/alkali corrosion, thereby The microporous atomized sheet has good resistance to alkali/corrosion and can effectively block harmful ion precipitation.
本实施例中， 所述微孔雾化片的直径为 50mm， 所述微孔雾化片的微孔 区的外径为 50mm; 且所述微孔区中的微孔共 1000000个； 所述微孔雾化片 中微孔孔道的形状为方形； 所述微孔孔道的横截面的形状为方形。  In this embodiment, the microporous atomization sheet has a diameter of 50 mm, the micropore region of the microporous atomization sheet has an outer diameter of 50 mm; and the micropores in the micropore region have a total of 1,000,000; The shape of the microporous channels in the microporous atomization sheet is square; the shape of the cross section of the microporous channels is square.
实施例五  Embodiment 5
一种微孔雾化片的制备方法， 具体步骤包括：  A method for preparing a microporous atomized sheet, the specific steps comprising:
步骤一： 将有机材质雾化片作为基底材料， 将所述基底材料进行清洗； 其中， 所述有机材质雾化片的微孔孔径为 21μπι;  Step 1: The organic material atomized sheet is used as a base material, and the base material is washed; wherein, the microporous pore diameter of the organic material atomized sheet is 21 μπι;
步骤二： 将清洗后的所述基底材料进行活化；  Step two: activating the cleaned substrate material;
具体地， 所述活化的步骤包括：  Specifically, the step of activating includes:
首先， 将所述基底材料浸渍于浓度为 0.05g/L盐酸与浓度为 10g/L氟化 氢氨溶液的混合溶液中超声清洗 30 min, 然后釆用蒸馏水清洗所述基底材 料， 清洗至附着于所述基底材料的表面液体的 pH值为中性为止； First, the base material is immersed in a mixed solution of a concentration of 0.05 g/L hydrochloric acid and a concentration of 10 g / L of hydrogen fluoride ammonia solution for ultrasonic cleaning for 30 min, and then the base material is washed with distilled water, and washed until attached thereto. The pH of the surface liquid of the base material is neutral;
再次， 将所述基底材料浸渍于质量百分数为 1%的氨水中超声清洗 5 min, 然后釆用蒸馏水清洗所述基底材料， 清洗至附着于所述基底材料表面 的液体的 pH值为中性为止；  Again, the substrate material is immersed in ammonia water having a mass percentage of 1% for ultrasonic cleaning for 5 minutes, and then the substrate material is washed with distilled water, and the pH of the liquid attached to the surface of the substrate material is cleaned until the pH is neutral. ;
最后， 将所述基底材料在可产生紫外气体的等离子体气氛中照射 120s 进行活化。  Finally, the substrate material is activated by irradiation in a plasma atmosphere capable of generating ultraviolet gas for 120 s.
步骤三： 将活化后的所述基底材料放置于反应腔体内， 抽真空以使所 述反应腔体内的压强降至 10 Pa; 随后， 先脉冲四二甲氨基锆（TDMAZ ) 0.1s后， 通入流量为 30sccm的 Ar气吹扫所述反应腔体 5s; 再脉冲氧等离 子体 0.8s后，通入流量为 50 sccm的 Ar气吹扫所述反应腔体 100s,如此交 替脉冲 TDMAZ和氧等离子体， 直至在所述基底材料的微孔孔道内壁及其 表面沉积 10000层 Zr02薄膜， 其中， 所述 Zr02薄膜的厚度约为 lOOOnm; 其次， 中三溴化硼（ BBr3 ) 5s后， 通入流量为 120sccm的 Ar气吹扫所述 反应腔体 120s， 脉冲 NH3 0.02s后， 通入流量为 8sccm的 Ar气吹扫所述反 应腔体 10s， 如此交替脉冲 BBr3和 NH3， 在所述 Zr02薄膜表面沉积 45000 层 BN薄膜， 所述 BN薄膜厚度约为 3600nm; 最后， 脉冲苯四甲酸二酐 ( PMDA ) 50s后， 通入流量为 120sccm的 Ar气吹扫所述反应腔体 120s, 脉冲二氨基二苯醚（DAH ) 8s后， 通入流量为 8sccm的 Ar气吹扫所述反 应腔体 50s， 如此交替脉冲 PMDA和 DAH， 在所述 BN薄膜表面沉积 300 层 PMDA-DAH薄膜， 其中， 所述 PMDA-DAH薄膜厚度约为 399.95nm。 Step 3: The activated substrate material is placed in the reaction chamber, and a vacuum is applied to reduce the pressure in the reaction chamber to 10 Pa. Subsequently, the tetramethylaminozirconium (TDMAZ) is pulsed for 0.1 s. The reaction chamber was purged with an Ar gas having a flow rate of 30 sccm for 5 s; after a pulsed oxygen plasma for 0.8 s, the reaction chamber was purged with an Ar gas having a flow rate of 50 sccm for 100 s, thus alternately pulsed TDMAZ and oxygen plasma. Body up to the inner wall of the microporous channel of the substrate material and 10,000 layers of Zr0 2 film are deposited on the surface, wherein the thickness of the Zr0 2 film is about 100 nm; secondly, after 5 s of boron tribromide (BBr 3 ), the reaction chamber is purged with Ar gas having a flow rate of 120 sccm. 120s, after pulsed NH 3 0.02s, the reaction chamber is purged with Ar gas having a flow rate of 8sccm for 10s, so that BBr 3 and NH 3 are alternately pulsed, and 45000 layers of BN film are deposited on the surface of the Zr0 2 film. The thickness of the BN film is about 3600 nm. Finally, after the pulsed pyromellitic dianhydride (PMDA) is used for 50 s, the reaction chamber is purged with an Ar gas having a flow rate of 120 sccm for 120 s, and after pulsed diaminodiphenyl ether (DAH) for 8 s, The reaction chamber was purged with Ar gas having a flow rate of 8 sccm for 50 s, so that PMDA and DAH were alternately pulsed, and 300 layers of PMDA-DAH film were deposited on the surface of the BN film, wherein the PMDA-DAH film had a thickness of about 399.95. Nm.
步骤四： 将沉积有薄膜的所述基底材料放入等离子体发生器中， 固化 200s; 其中， 所述等离子体发生器的功率为 50W， 固化气体为 Ne的等离子 体， 气体 Ne的气流为 200sccm。  Step 4: The substrate material deposited with the film is placed in a plasma generator and cured for 200 s; wherein, the power of the plasma generator is 50 W, the plasma of the curing gas is Ne, and the gas flow of the gas Ne is 200 sccm. .
这里， 所述 Zr02薄膜、 BN薄膜及 PMDA-DAH薄膜紧紧包覆于所述 有机材质雾化片的微孔孔道内壁及其表面， 如此， 将所述有机材质雾化片 中微孔的孔径缩小至 0.05μπι; 由于微孔孔道内壁及表面紧紧粘附有 Zr02 薄膜、 BN薄膜及 PMDA-DAH薄膜， 因此， 本实施例所述陶瓷雾化片具有 良好的阻隔性。 Here, the Zr0 2 film, the BN film, and the PMDA-DAH film are tightly coated on the inner wall of the microporous channel of the organic material atomizing sheet and the surface thereof, so that the microporous material in the organic material atomizing sheet is The pore size is reduced to 0.05 μm; since the inner wall and the surface of the microporous channel are tightly adhered to the Zr0 2 film, the BN film and the PMDA-DAH film, the ceramic atomized sheet of the embodiment has good barrier properties.
本实施例中， 所述有机材质雾化片直径为 45mm; 所述有机材质雾化片 的微孔区的外径为 40mm; 且所述微孔区中的微孔共 5000; 所述微孔雾化 片中微孔孔道的形状为圓形； 所述微孔孔道的横截面的形状为抛物线形。  In this embodiment, the diameter of the atomized sheet of the organic material is 45 mm; the outer diameter of the microporous region of the organic material atomized sheet is 40 mm; and the micropores in the microporous region are 5000; The shape of the microporous channel in the atomizing sheet is circular; the shape of the cross section of the microporous channel is parabolic.
实施例六  Embodiment 6
一种微孔雾化片的制备方法， 具体步骤包括：  A method for preparing a microporous atomized sheet, the specific steps comprising:
步骤一： 将陶瓷雾化片作为基底材料， 将所述基底材料进行清洗； 其中， 所述陶瓷雾化片的微孔孔径为 21μπι;  Step 1: using a ceramic atomized sheet as a substrate material, the substrate material is cleaned; wherein the ceramic atomized sheet has a micropore diameter of 21 μm;
步骤二： 将清洗后的所述基底材料进行活化； 具体地， 所述活化的步骤包括： Step two: activating the cleaned substrate material; Specifically, the step of activating includes:
首先， 将所述基底材料浸渍于浓度为 6.5g/L醋酸溶液， 浓度为 0.05g/L 盐酸溶液， 浓度为 10g/L氟化氢氨溶液的混合溶液中超声清洗 15 min, 然 后釆用蒸馏水清洗所述基底材料， 清洗至附着于所述基底材料的表面液体 的 pH值为中性为止；  First, the base material is immersed in a mixed solution having a concentration of 6.5 g/L acetic acid solution, a concentration of 0.05 g/L hydrochloric acid solution, and a concentration of 10 g/L of hydrogen fluoride ammonia solution for 15 minutes, and then washed with distilled water. The base material is cleaned until the pH of the surface liquid attached to the base material is neutral;
再次， 将所述基底材料浸渍于质量百分数为 20%的氨水中超声清洗 30 min, 然后釆用蒸馏水清洗所述基底材料， 清洗至附着于所述基底材料表面 的液体的 pH值为中性为止；  Again, the substrate material is immersed in ammonia water having a mass percentage of 20% for ultrasonic cleaning for 30 minutes, and then the substrate material is washed with distilled water, and the pH of the liquid attached to the surface of the substrate material is cleaned until neutral. ;
最后， 将所述基底材料在可产生紫外气体的等离子体气氛中照射 90s 进行活化。  Finally, the substrate material is activated by irradiation in a plasma atmosphere capable of generating ultraviolet gas for 90 s.
步骤三： 将活化后的所述基底材料放置于反应腔体内， 抽真空以使所 述反应腔体内的压强降至 1 OPa; 随后， 先脉冲苯四甲酸二酐（ PMDA ) 5s 后，通入流量为 20sccm的 N2气吹扫所述反应腔体 15s，脉冲对苯二胺（ PDA ) Is后， 通入流量为 20sccm的 N2气吹扫所述反应腔体 20s， 如此交替脉冲 PMDA和 PDA,在所述基底材料表面沉积 1250层 PMDA-PDA薄膜，其中， 所述 PMDA-PDA薄膜厚度约为 1000nm。 Step 3: The activated substrate material is placed in the reaction chamber, and a vacuum is applied to reduce the pressure in the reaction chamber to 1 OPa. Subsequently, the pyromellitic dianhydride (PMDA) is pulsed for 5 seconds. The reaction chamber was purged with N 2 gas at a flow rate of 20 sccm for 15 s. After pulsed with p-phenylenediamine (PDA ) Is, the reaction chamber was purged with N 2 gas at a flow rate of 20 sccm for 20 s, thus alternately pulsed PMDA and The PDA deposits 1250 layers of PMDA-PDA film on the surface of the substrate material, wherein the PMDA-PDA film has a thickness of about 1000 nm.
步骤四： 将沉积有薄膜的所述基底材料放入等离子体发生器中， 固化 90s; 其中， 所述等离子体发生器的功率为 250W， 固化气体为 Ar和 Xe的 混合等离子体， 气体 Ar的气流为 160sccm， 气体 Xe的气流为 40sccm。  Step 4: The substrate material deposited with the thin film is placed in a plasma generator and cured for 90 s; wherein the plasma generator has a power of 250 W, and the curing gas is a mixed plasma of Ar and Xe, and the gas is Ar The gas flow was 160 sccm, and the gas flow of the gas Xe was 40 sccm.
这里，所述 PMDA-PDA薄膜紧紧包覆于所述陶瓷雾化片的微孔孔道内 壁及其表面， 如此， 将所述陶瓷雾化片中微孔的孔径缩小至 20μπι; 由于微 孔孔道内壁及表面紧紧粘附有 PMDA-PDA薄膜， 因此， 本实施例所述陶瓷 雾化片具有极强的断裂强度和良好的阻隔性。  Here, the PMDA-PDA film is tightly coated on the inner wall of the microporous channel of the ceramic atomizing sheet and the surface thereof, so that the pore diameter of the micropores in the ceramic atomizing sheet is reduced to 20 μm; The inner wall and the surface are tightly adhered to the PMDA-PDA film, and therefore, the ceramic atomized sheet of the embodiment has extremely strong breaking strength and good barrier property.
本实施例中， 所述陶瓷雾化片直径为 1mm; 所述有机材质雾化片的微 孔区的外径为 1mm; 且所述微孔区中的微孔共 100; 所述微孔雾化片中微 孔孔道的形状为方形； 所述微孔孔道的横截面的形状为方形。 In this embodiment, the ceramic atomizing sheet has a diameter of 1 mm; the outer diameter of the microporous region of the organic material atomizing sheet is 1 mm; and the micropores in the microporous region have a total of 100; Chemical film The shape of the pore channel is square; the shape of the cross section of the microporous channel is square.
值得注意的是， 实施例中在脉冲前驱体前对反应腔体进行抽真空处理， 且整个反应过程均是在抽真空状态下进行的。  It should be noted that in the embodiment, the reaction chamber is evacuated before the pulse precursor, and the entire reaction process is performed under vacuum.
以上所述， 仅为本发明的较佳实施例而已， 并非用于限定本发明的保 护范围。  The above is only the preferred embodiment of the present invention and is not intended to limit the scope of the present invention.

Claims

权利要求书 Claim
1、 一种微孔雾化片的制备方法， 将雾化片作为基底材料； 所述方法包 括：  A method for preparing a microporous atomized sheet, wherein the atomized sheet is used as a base material; and the method comprises:
在所述基底材料的微孔孔道内壁及其表面沉积薄膜；  Depositing a film on the inner wall of the microporous channel of the base material and its surface;
将沉积有薄膜的所述基底材料固化。  The substrate material on which the film is deposited is cured.
2、 根据权利要求 1所述的方法， 其中， 所述雾化片为金属雾化片、 陶 瓷雾化片及有机材质雾化片中的任意一种。  The method according to claim 1, wherein the atomizing sheet is any one of a metal atomizing sheet, a ceramic atomizing sheet, and an organic material atomizing sheet.
3、 根据权利要求 1所述的方法， 其中， 所述在所述基底材料的微孔孔 道内壁及其表面沉积薄膜， 包括：  3. The method according to claim 1, wherein the depositing a film on the inner wall of the microporous channel of the base material and the surface thereof comprises:
步骤一： 将所述基底材料放置于反应腔体内；  Step 1: placing the substrate material in the reaction chamber;
步骤二： 通入第一前驱体， 使所述第一前驱体与所述基底材料的微孔 孔道内壁及其表面的材料发生反应；  Step two: introducing a first precursor, reacting the first precursor with a material of the inner wall of the microporous channel of the base material and a surface thereof;
步骤三： 在反应完成后， 釆用清洗气体吹扫所述反应腔体、 或对所述 反应腔体进行抽真空将游离的所述第一前驱体排出所述反应腔体后， 通入 第二前驱体；  Step 3: After the reaction is completed, the reaction chamber is purged with a cleaning gas, or the reaction chamber is evacuated, and the free first precursor is discharged from the reaction chamber, and then Second precursor
步骤四： 循环执行所述步骤二和步骤三， 直至在所述基底材料的微孔 孔道内壁及其表面沉积预设厚度的薄膜为止。  Step 4: The steps 2 and 3 are performed cyclically until a film of a predetermined thickness is deposited on the inner wall of the microporous channel of the base material and the surface thereof.
4、 根据权利要求 1或 3所述的方法， 其中， 所述薄膜为一层或多层厚 度均勾的薄膜；  4. The method according to claim 1 or 3, wherein the film is one or more layers of thickness-hooked film;
当所述薄膜为一层时， 所述薄膜为以下薄膜中的任意一种；  When the film is a layer, the film is any one of the following films;
当所述薄膜为多层时， 所述薄膜为以下薄膜中的任意一种重叠形成的 多层薄膜， 或以下任意几种交替重叠形成的多层薄膜， 或以下一种重叠形 成的多层薄膜和以下任意几种交替重叠形成的多层薄膜的组合多层薄膜； 所述薄膜包括： 氧化铝 A1203薄膜、二氧化硅 Si02薄膜、二氧化钛 Ti02 薄膜、 氧化锌 ZnO薄膜、 二氧化铪 Hf02薄膜、 氧化镁 MgO薄膜、 二氧化 锆 Zr02薄膜、 氧化镍 NiO薄膜、 氧化钴 CoO薄膜、 铁的氧化物形成的薄 膜 FeOx薄膜、 铜的氧化物形成的薄膜 CuOx薄膜、 氧化硼 B203薄膜、 氧化 铟 In203薄膜、 氧化锡 Sn02薄膜、 氧化镓 Ga203薄膜、 五氧化二铌 Nb205 薄膜、 三氧化二钆 Gd203薄膜、 五氧化二钽 Ta205薄膜、 氮化硼 BN薄膜、 氮化铝 A1N薄膜、 氮化钛 TiN薄膜、 碳化硅 SiC薄膜、 硫化锌 ZnS薄膜、 硫化锆 ZrS薄膜、 透明质酸 HA薄膜、 钨 W薄膜、 铂 Pt薄膜、 钌 Ru薄膜、 钯 Pd薄膜、 均苯四甲酸二酐-二氨基二苯醚 PMDA-DAH薄膜、 均苯四甲酸 二酐-己二胺 PMDA-ODA薄膜、 均苯四甲酸二酐-乙二胺 PMDA-EDA薄膜 及均苯四甲酸二酐-对苯二胺 PMDA-PDA薄膜。 When the film is a plurality of layers, the film is a multilayer film formed by overlapping any one of the following films, or a multilayer film formed by alternately overlapping any of the following, or a multilayer film formed by overlapping one of the following And a combined multilayer film of a plurality of layers formed by alternately overlapping any of the following; the film comprises: an alumina A1 2 0 3 film, a silica SiO 2 film, a titanium dioxide Ti0 2 film, a zinc oxide ZnO film, and a dioxide铪Hf0 2 film, magnesium oxide MgO film, dioxide Zirconium Zr0 2 film, nickel oxide NiO film, cobalt oxide CoO film, thin film FeO x film formed by iron oxide, thin film CuO x film formed by copper oxide, boron oxide B 2 0 3 film, indium oxide In 2 0 3 film, tin oxide Sn0 2 film, gallium oxide Ga 2 0 3 film, antimony pentoxide Nb 2 0 5 film, antimony trioxide Gd 2 0 3 film, tantalum pentoxide Ta 2 0 5 film, boron nitride BN film, aluminum nitride A1N film, titanium nitride TiN film, silicon carbide SiC film, zinc sulfide ZnS film, zirconium sulfide ZrS film, hyaluronic acid HA film, tungsten W film, platinum Pt film, ruthenium Ru film, palladium Pd Film, pyromellitic dianhydride-diaminodiphenyl ether PMDA-DAH film, pyromellitic dianhydride-hexanediamine PMDA-ODA film, pyromellitic dianhydride-ethylenediamine PMDA-EDA film and both Pyromellitic dianhydride-p-phenylenediamine PMDA-PDA film.
5、 根据权利要求 1所述的方法， 其中， 所述将沉积有薄膜的所述基底 材料固化， 包括：  5. The method according to claim 1, wherein the curing the substrate material on which the thin film is deposited comprises:
将沉积有薄膜的所述基底材料进行等离子体固化。  The substrate material on which the thin film is deposited is subjected to plasma curing.
6、 根据权利要求 1所述的方法， 其中， 所述在所述基底材料的微孔孔 道内壁及其表面沉积薄膜之前， 所述方法还包括：  6. The method according to claim 1, wherein the method further comprises: before depositing a film on the inner wall of the microporous channel of the base material and the surface thereof;
将所述基底材料进行活化。  The substrate material is activated.
7、 根据权利要求 6所述的方法， 其中， 所述活化包括： 化学溶液浸渍 活化和紫外活化。  7. The method of claim 6, wherein the activating comprises: chemical solution impregnation activation and ultraviolet activation.
8、 根据权利要求 7所述的方法， 其中， 所述化学溶液浸渍活化的步骤 包括：  8. The method according to claim 7, wherein the step of chemically immersing activation comprises:
将所述基底材料浸渍于酸性溶液中超声清洗 5-30min，然后釆用蒸馏水 清洗所述基底材料，清洗至附着于所述基底材料的表面液体的 pH值为中性 为止；  The base material is immersed in an acidic solution for ultrasonic cleaning for 5-30 min, and then the base material is washed with distilled water, and washed until the pH of the surface liquid attached to the base material is neutral;
将所述基底材料浸渍于碱性溶液中超声清洗 5-30min，然后釆用蒸馏水 清洗所述基底材料，清洗至附着于所述基底材料表面的液体的 pH值为中性 为止。 The base material is immersed in an alkaline solution for ultrasonic cleaning for 5-30 min, and then the base material is washed with distilled water and washed until the pH of the liquid adhering to the surface of the base material is neutral.
9、 根据权利要求 7所述的方法， 其中， 所述紫外活化的步骤包括： 将所述基底材料放置在紫外线灯下或者在能产生紫外气体的等离子体 气氛中， 照射 ls-120s进行活化。 9. The method according to claim 7, wherein the step of ultraviolet activation comprises: placing the substrate material under an ultraviolet lamp or irradiating ls-120s for activation in a plasma atmosphere capable of generating ultraviolet gas.
10、 一种微孔雾化片， 所述微孔雾化片设置有微孔区， 所述微孔区内 分布有多个微孔； 所述微孔雾化片的微孔孔道内壁及其表面包覆有薄膜； 所述微孔的孔径为 0.05μπι-20μπι。  10. A microporous atomization sheet, wherein the microporous atomization sheet is provided with a micropore region, wherein the micropore region is provided with a plurality of micropores; the micropore orifice inner wall of the microporous atomization sheet and The surface is coated with a film; the pore size of the micropores is 0.05 μπι-20 μπι.
11、 根据权利要求 10所述的微孔雾化片， 其中， 所述微孔区中微孔的 数量为 100-1000000个。  The microporous atomization sheet according to claim 10, wherein the number of the micropores in the micropore region is from 100 to 1,000,000.
12、 根据权利要求 10所述的微孔雾化片， 其中， 所述微孔雾化片的直 径为 l-50mm。  The microporous atomization sheet according to claim 10, wherein the microporous atomized sheet has a diameter of from 1 to 50 mm.
13、 根据权利要求 10所述的微孔雾化片， 其中， 所述微孔区的外径为 l-50mm。  The microporous atomization sheet according to claim 10, wherein the micropore region has an outer diameter of from 1 to 50 mm.
14、 根据权利要求 10所述的微孔雾化片， 其中， 所述微孔雾化片为金 属雾化片、 陶瓷雾化片及有机材质雾化片中的任意一种。  The microporous atomizing sheet according to claim 10, wherein the microporous atomizing sheet is any one of a metal atomizing sheet, a ceramic atomizing sheet, and an organic material atomizing sheet.
15、 根据权利要求 10所述的微孔雾化片， 其中， 所述微孔雾化片的微 孔孔道内壁及其表面的包覆材料为一层或多层厚度均勾的薄膜；  The microporous atomization sheet according to claim 10, wherein the inner wall of the microporous channel of the microporous atomization sheet and the coating material of the surface thereof are one or more layers of thickness-hooked film;
当所述包覆材料为一层时， 所述包覆材料为以下薄膜中的任意一种； 当所述包覆材料为多层时， 所述包覆材料为以下薄膜中的任意一种重 叠形成的多层薄膜， 或以下任意几种交替重叠形成的多层薄膜， 或以下一 种重叠形成的多层薄膜和以下任意几种交替重叠形成的多层薄膜的组合多 层薄膜；  When the coating material is a layer, the coating material is any one of the following films; when the coating material is a plurality of layers, the coating material is overlapped by any one of the following films a multilayer film formed, or a multilayer film formed by alternately overlapping any of the following, or a composite film of a multilayer film formed by overlapping one of the following and a multilayer film of any of the following alternately stacked layers;
所述薄膜包括： 氧化铝 A1203薄膜、二氧化硅 Si02薄膜、二氧化钛 Ti02 薄膜、 氧化锌 ZnO薄膜、 二氧化铪 Hf02薄膜、 氧化镁 MgO薄膜、 二氧化 锆 Zr02薄膜、 氧化镍 NiO薄膜、 氧化钴 CoO薄膜、 铁的氧化物形成的薄 膜 FeOx薄膜、 铜的氧化物形成的薄膜 CuOx薄膜、 氧化硼 B203薄膜、 氧化 铟 ln203薄膜、 氧化锡 Sn02薄膜、 氧化镓 Ga203薄膜、 五氧化二铌 Nb205 薄膜、 三氧化二钆 Gd203薄膜、 五氧化二钽 Ta205薄膜、 氮化硼 BN薄膜、 氮化铝 A1N薄膜、 氮化钛 TiN薄膜、 碳化硅 SiC薄膜、 硫化锌 ZnS薄膜、 硫化锆 ZrS薄膜、 透明质酸 HA薄膜、 钨 W薄膜、 铂 Pt薄膜、 钌 Ru薄膜、 钯 Pd薄膜、 均苯四甲酸二酐-二氨基二苯醚 PMDA-DAH薄膜、 均苯四甲酸 二酐-己二胺 PMDA-ODA薄膜、 均苯四甲酸二酐-乙二胺 PMDA-EDA薄膜 及均苯四甲酸二酐-对苯二胺 PMDA-PDA薄膜。 The film comprises: an aluminum oxide A1 2 0 3 film, a silicon dioxide SiO 2 film, a titanium dioxide Ti0 2 film, a zinc oxide ZnO film, a hafnium oxide HfO 2 film, a magnesium oxide MgO film, a zirconium dioxide Zr0 2 film, and oxidation. Nickel NiO film, cobalt oxide CoO film, thin film FeO x film formed by iron oxide, thin film CuO x film formed by copper oxide, boron oxide B 2 0 3 film, oxidation Indium ln 2 0 3 film, tin oxide Sn0 2 film, gallium oxide Ga 2 0 3 film, antimony pentoxide Nb 2 0 5 film, antimony trioxide Gd 2 0 3 film, tantalum pentoxide Ta 2 0 5 film Boron nitride BN film, aluminum nitride A1N film, titanium nitride TiN film, silicon carbide SiC film, zinc sulfide ZnS film, zirconium sulfide ZrS film, hyaluronic acid HA film, tungsten W film, platinum Pt film, 钌Ru Film, palladium Pd film, pyromellitic dianhydride-diaminodiphenyl ether PMDA-DAH film, pyromellitic dianhydride-hexanediamine PMDA-ODA film, pyromellitic dianhydride-ethylenediamine PMDA- EDA film and pyromellitic dianhydride-p-phenylenediamine PMDA-PDA film.
16、 根据权利要求 10所述的微孔雾化片， 其中， 所述微孔雾化片中微 孔孔道的形状为： 圓形、 三角形、 椭圓形、 方形及喇 形中的任意一种。  The microporous atomization sheet according to claim 10, wherein the microporous orifice has a shape of a circular orifice, a triangular shape, an elliptical shape, a square shape, and a circular shape. .
17、 根据权利要求 10所述的微孔雾化片， 其中， 所述微孔雾化片中微 孔孔道的横截面的形状为： 抛物线形、 喇 形、 方形及梯形中的任意一种。  The microporous atomization sheet according to claim 10, wherein a shape of a cross section of the microporous channel in the microporous atomization sheet is any one of a parabolic shape, a circular shape, a square shape, and a trapezoidal shape.
18、 一种微孔雾化装置， 所述微孔雾化装置包括： 雾化器箱体、 与所 述雾化器箱体连接的气雾发生器、 以及与雾化器箱体连接的电子电路控制 器； 其中， 所述气雾发生器中包括微孔雾化片， 所述微孔雾化片为权利要 求 10至 17中任一项所述的微孔雾化片。  18. A micropore atomization device, the micropore atomization device comprising: an atomizer housing, an aerosol generator connected to the nebulizer housing, and an electron connected to the nebulizer housing The circuit controller; wherein the gas mist generator comprises a microporous atomizing sheet, and the microporous atomizing sheet is the microporous atomizing sheet according to any one of claims 10 to 17.
PCT/CN2014/078703 2014-05-28 2014-05-28 Method for preparing micropore atomization sheet, micropore atomization sheet, and micropore atomization apparatus WO2015180080A1 (en)

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