CN105651012A - Vacuum drying oven based on vapor detection function - Google Patents
Vacuum drying oven based on vapor detection function Download PDFInfo
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- CN105651012A CN105651012A CN201610064960.3A CN201610064960A CN105651012A CN 105651012 A CN105651012 A CN 105651012A CN 201610064960 A CN201610064960 A CN 201610064960A CN 105651012 A CN105651012 A CN 105651012A
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- vacuum drying
- drying oven
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- zinc oxide
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Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B9/00—Machines or apparatus for drying solid materials or objects at rest or with only local agitation; Domestic airing cupboards
- F26B9/06—Machines or apparatus for drying solid materials or objects at rest or with only local agitation; Domestic airing cupboards in stationary drums or chambers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0011—Casting solutions therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/08—Hollow fibre membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/38—Polyalkenylalcohols; Polyalkenylesters; Polyalkenylethers; Polyalkenylaldehydes; Polyalkenylketones; Polyalkenylacetals; Polyalkenylketals
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/22—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance
- G01N27/223—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance for determining moisture content, e.g. humidity
- G01N27/225—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance for determining moisture content, e.g. humidity by using hygroscopic materials
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/22—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance
- G01N27/227—Sensors changing capacitance upon adsorption or absorption of fluid components, e.g. electrolyte-insulator-semiconductor sensors, MOS capacitors
Abstract
The invention discloses a vacuum drying oven based on a vapor detection function. A ZnO-based humidity sensor module is mounted in the vacuum drying oven; the humidity sensitive element part of the ZnO-basedhumidity sensor module adopts a silicon nanoporous pillar material as a substrate; ZnO nanowires combined with a graphene material serve as a sensitive material; and humidity sensitive elements of the ZnO-based humidity sensor module are of the type of interdigital electrodes. The vacuum drying oven adopting the structure has a very large specific surface area and a favorable gas diffusion passage; and moreover, a dehumidifying hollow fiber composite membrane component adopting a polyvinyl alcohol-EDTMPA-polysulfone-based membrane is arranged on the inner surface of the vacuum drying oven, so that the functions of humidity induction, moisture absorption and corrosion resistance of the vacuum drying oven are greatly improved.
Description
Technical field
The present invention relates to drying baker field, be specifically related to a kind of vacuum drying oven based on steam detection function.
Background technology
Vacuum drying oven is usually and aims at dry thermal sensitivity, easily decomposition and readily oxidizable substance and design, can make to keep in operating room certain vacuum during work, and can internally be filled with noble gas, particularly the article of some complicated components also can carry out rapid draing, adopts Intelligent Digital humidostat carry out the setting of temperature, display and control.
Owing to vacuum drying oven is higher to humidity requirement, and in existing vacuum drying oven, Humidity Detection sensitivity is not high, and repeatability is poor.
Summary of the invention
It is an object of the invention to avoid above-mentioned weak point of the prior art to provide a kind of vacuum drying oven based on steam detection function.
The purpose of the present invention is achieved through the following technical solutions:
The invention provides a kind of vacuum drying oven based on steam detection function, it is characterised in that: the internally installed of described vacuum drying oven (1) has zno-based moisture sensor module (2); Described zno-based moisture sensor module (2) is mainly made up of wet sensitive sensing element and data read element, described wet sensitive sensing element is interdigital electrode type, including silicon chip substrate (10), Si NPA (20), zinc oxide nanowire (30) and graphene layer (40); Described vacuum drying oven (1) is additionally provided with microprocessor, LED display lamp bar and wireless communication module; The input of described microprocessor is connected with the outfan of described ZnO moisture sensor module (2), described ZnO moisture sensor module (2) detected value reaches preset value, described microprocessor controls LED display lamp bar and flashes, described LED display lamp bar is connected to a buzzer, touches buzzer and send alarm while the flicker of LED display lamp bar; Described wireless communication module is CC2420 wireless communication module, described ZnO moisture sensor module (2) can by described CC2420 wireless communication module transmission detection data to data basestation, by the Internet, mobile subscriber terminal can check that detection data are maybe uploaded to cloud storage center by testing result, form detection and monitoring network; The inside of described vacuum drying oven (1) is additionally provided with a polyvinyl alcohol ethylenediamine tetraacetic methene phosphoric acid polysulfones basement membrane hollow fiber composite membrane assembly for dehumidification, polyvinyl alcohol ethylenediamine tetraacetic methene phosphoric acid polysulfones basement membrane hollow fiber composite membrane is fixed in glass electrode by this membrane module, and glass electrode is connected with moisture sensor;Described zinc oxide nanowire (30) length about 3 ��m.
Preferably, the preparation method of described wet sensitive sensing element is as follows:
Step one, prepares Si-NPA substrate: the silicon chip substrate (10) of 3cm �� 3cm is included clean dirt, hydro-thermal method corrosion preparation Si-NPA substrate; 1. take the silicon chip of 3cm �� 3cm, silicon chip is placed in the mixed solution of sulphuric acid and hydrogen peroxide volume ratio 4:1, supersound process 20min, taking-up deionized water cleans, to remove the organic impurities of silicon chip surface; It is H that silicon chip is positioned over volume ratio2O:H2O2: NH4In the mixed solution of OH=5:2:1, ultrasonic cleaning 20min, the deionized water of taking-up subsequently cleans, to remove Organic substance and the metal complex of silicon chip surface; 2. hydro-thermal method corrosion is utilized to prepare Si-NPA: to weigh the Fe (NO of 1.0g3)��9H2O pours in politef, is added thereto to the HF solution of 20ml deionized water and 30ml40% subsequently; Putting in solution by the silicon chip that upper step is cleaned, add a cover and put in water heating kettle, put in drying baker by water heating kettle subsequently, 180 DEG C of constant temperature keep 30min, after natural cooling, take out Wafer Cleaning and namely obtain Si-NPA substrate;
Step 2, growth of zinc oxide nano line: adopt magnetron sputtering to prepare zinc oxide nanowire in conjunction with thermal oxidation method; Silicon nano hole column substrate is put in magnetic control sputtering device, when sputtering voltage 220V, sputtering current 0.8A, magnetron sputtering Zn film, thickness is 50nm, putting it into subsequently in batch-type furnace, at 400 DEG C, thermal oxidation method processes 4h, obtains diameter and is about the zinc oxide nanowire of 30nm;
Step 3, grows graphene layer: adopt process for preparing graphenes by chemical vapour deposition; First magnetron sputtering layer of metal Ni film on the substrate that upper step obtains, thickness is about 5nm; Secondly, putting in tube furnace by this substrate, be warming up to 900 DEG C, pass into hydrogen as protection reducing gas by given pace, stablize 30min, then, pass into methane 2h according to a certain percentage simultaneously, stopping starts Temperature fall after passing into methane; Under Ni catalyst action, methane molecule at high temperature can be cracked into carbon atom and hydrogen atom, at temperature-fall period and under the protection of hydrogen, and carbon atom meeting formation of deposits one layer graphene thin film;
Step 4, is deposited with interdigital electrode: after obtaining growing the silicon nano hole column substrate having zinc oxide nanowire and Graphene, covers interdigital electrode mask at substrate surface, utilizes magnetron sputtering method to be deposited with Au thin film thick for one layer of 500nm on its surface as electrode;
Step 5, assembles sensing element and reads data element: the both positive and negative polarity wire reading data element is connected in interdigital electrode, two parts composition Zinc oxide-base moisture sensor device;
The preparation method of described polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly is as follows:
Step one, polysulfone hollow fibre basement membrane pretreatment: polysulfone hollow fibre basement membrane to carry out pretreatment before coating, after soaking 12h with deionized water, with the soak with hydrochloric acid 60min of 1.0mol/l, remove glycerin layer and other organic solvents on film surface; Then use in the sodium hydroxide solution of 1.0mol/l and excessive hydrochloric acid, finally repeatedly rinse with deionized water, make film surface in neutrality, dry in the shade standby;
Step 2, prepare polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane: add in deionized water by the polyvinyl alcohol that the average degree of polymerization of certain mass is 1750 �� 50, it is about 3h 50 DEG C of stirred in water bath to be completely dissolved to polyvinyl alcohol, obtains 5wt% polyvinyl alcohol homogeneous phase aqueous solution;Adding a certain amount of ethylenediamine tetraacetic methene phosphoric acid after solution is cooled to room temperature, and at room temperature stir 1.5h, namely standing and defoaming obtains casting solution; Polysulfones basement membrane (molecular cut off 30000) through pretreatment is taken out after casting solution soaks 20min, is vertically fixed on the guide frame that dries in the air and dries in the shade; After the film of primary coating soaks 20min again in casting solution, will reversely be fixed on and dry in the air on guide frame, dry at room temperature over night, prepare required PVA-EDTMPA/PS hollow fiber composite membrane.
Step 3, fixing: polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane is fixed in glass electrode.
There is advantages that
1. configuration aspects, the present invention adopts Si-NPA (silicon nano hole column) material to be substrate, ZnONWs (zinc oxide nanowire) is sensitive material in conjunction with Graphene, this structure has great specific surface area and good gas diffusion paths, substantially increases the sensitivity of this vacuum drying oven sensitive material;
2. adopting grapheme material can increase the conductivity of material greatly, hydrone primary attachment is on the surface of nano wire Yu Graphene simultaneously, it is easy to desorption, and the repeatability that interior humidity is responded by vacuum drying oven is good;
3. preparation process material consumption is few, and the controllable degree of technique is high, device small volume and less weight, it is easy to batch production.
Accompanying drawing explanation
Utilize accompanying drawing that invention is described further, but the embodiment in accompanying drawing does not constitute any limitation of the invention, for those of ordinary skill in the art, under the premise not paying creative work, it is also possible to obtain other accompanying drawing according to the following drawings.
Fig. 1 is the schematic diagram of vacuum drying oven of the present invention.
Fig. 2 is sensor sensing componentry schematic diagram.
Detailed description of the invention
Sensor technology is able to obtain main path and the means of various information in nature, production field. It is the cutting edge technology of a kind of modern science and technology, and it is one of three big pillars of modern information technologies, is the important benchmark weighing a national science and technology level of development. According to definition, sensor is: " can experience the measured of regulation and convert device or the device of usable output signal according to certain rule to, being generally made up of sensing element, conversion element and measuring circuit. " to be able to direct feeling measured and be converted into and the measured element of physical quantity having the electricity determining relation or easily becoming electricity for sensing element. Conversion element is able to the measured element being converted directly into the electricity determining relation experienced by sensing element. Measuring circuit is that the signal of telecommunication that conversion element exports is converted to the circuit of easy-to-handle capable telecommunications number.
Humidity refers to the content of water vapor in air. Along with the development of modern science and technology, the Detection & Controling of humidity in productive life being had very important meaning, the application of moisture sensor is also more and more extensive, and such as moisture sensor has a wide range of applications in the such as field such as household electrical appliance, automobile, industrial or agricultural.
Dew cell refers to that ambient humidity has response maybe can be converted to the element that can measure signal accordingly by ambient humidity, and it has a wide range of applications in fields such as industrial and agricultural production, environment measuring and Engineering Control. The core of humidity sensor is humidity-sensitive material, and it is the hydrone utilizing adsorption effect directly to adsorb in air, makes the electrology characteristic etc. of material change, thus detecting the change of humidity. Zinc oxide is a kind of semiconductor material with wide forbidden band, and it is all widely used in fields such as sensor, solaode, lithium battery, catalysis. And zinc oxide material to have preparation cost low, chemical stability, Heat stability is good, prepare the advantages such as controlled and pattern is abundant, be a kind of desirably humidity sensor material. The advantage of the aspects such as the pattern that has additionally, due to nano material itself, structure, nano zinc oxide material is very sensitive to humidity of external environment condition etc., has obvious Unordered system.
Humidity sensor refers to after utilizing humidity-sensitive material adsorbed water molecule, and the principle that measured amount changes is made.Generally accepted theory be the Water Molecular Adsorption in air when sensitive material surface and grain boundaries, reduce surface and the grain boundary resistance of material.
The problem such as not high, response recovery time length for existing moisture sensor sensitivity, this programme, based on nano zinc oxide material, is prepared for the zinc oxide nanowire with large specific surface area, and in conjunction with the high grapheme material of conductivity, makes moisture sensor.
Moisture sensor of the present invention is made up of wet sensitive sensing element part and data read element part. Wherein, wet sensitive sensing element is based on zinc oxide nanowire, make in conjunction with grapheme material, device architecture is interdigital electrode type, when moisture sensor periphery humidity changes, Water Molecular Adsorption can change in the speed of sensitive material surface and crystal boundary, causes the conductivity of sensitive material to change, and then reflects its capacitance variations from read element part; Digital independent element is with microprocessor, and it is the voltage applying characteristic frequency to sensing element, reads different numerical value according to the change of sensing element electric capacity at this voltage and carrys out the change of display environment humidity.
Illustrate that the present invention is further described below in conjunction with accompanying drawing.
Fig. 1 is the schematic diagram of vacuum drying oven of the present invention. The internally installed of vacuum drying oven (1) has zno-based moisture sensor module (2).
Fig. 2 is sensor sensing componentry schematic diagram. Wherein: 10-silicon chip substrate, 20-Si-NPA, 30-zinc oxide nanowire, 40-graphene layer.
The invention will be further described with the following Examples.
Embodiment 1:
A kind of vacuum drying oven detecting function based on steam as shown in Figure 1, the internally installed of described vacuum drying oven 1 has zno-based moisture sensor module 2; Described zno-based moisture sensor module 2 is mainly made up of wet sensitive sensing element and data read element. As in figure 2 it is shown, described wet sensitive sensing element is interdigital electrode type, it includes silicon chip substrate 10, Si-NPA20, zinc oxide nanowire 30 and graphene layer 40; Described vacuum drying oven 1 is additionally provided with microprocessor, LED display lamp bar and wireless communication module; The input of described microprocessor is connected with the outfan of described ZnO moisture sensor module, described ZnO moisture sensor module detected value reaches preset value, described microprocessor controls LED display lamp bar and flashes, described LED display lamp bar is connected to a buzzer, touches buzzer and send alarm while the flicker of LED display lamp bar; Described wireless communication module is CC2420 wireless communication module, described ZnO moisture sensor module can by described CC2420 wireless communication module transmission detection data to data basestation, by the Internet, mobile subscriber terminal can check that detection data are maybe uploaded to cloud storage center by testing result, form detection and monitoring network; The inside of described vacuum drying oven is additionally provided with a polyvinyl alcohol for dehumidification-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly, polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane is fixed in glass electrode by this membrane module, and glass electrode is connected with moisture sensor; Described zinc oxide nanowire 30 length about 3 ��m.
Preferably, the preparation method of described wet sensitive sensing element is as follows:
Step one, prepares Si-NPA substrate: the silicon chip substrate of 3cm �� 3cm is included clean dirt, hydro-thermal method corrosion preparation Si-NPA substrate; 1. take the silicon chip of 3cm �� 3cm, silicon chip is placed in the mixed solution of sulphuric acid and hydrogen peroxide volume ratio 4:1, supersound process 20min, taking-up deionized water cleans, to remove the organic impurities of silicon chip surface;It is H that silicon chip is positioned over volume ratio2O:H2O2: NH4In the mixed solution of OH=5:2:1, ultrasonic cleaning 20min, the deionized water of taking-up subsequently cleans, to remove Organic substance and the metal complex of silicon chip surface; 2. hydro-thermal method corrosion is utilized to prepare Si-NPA: to weigh the Fe (NO of 1.0g3)��9H2O pours in politef, is added thereto to the HF solution of 20ml deionized water and 30ml40% subsequently; Putting in solution by the silicon chip that upper step is cleaned, add a cover and put in water heating kettle, put in drying baker by water heating kettle subsequently, 180 DEG C of constant temperature keep 30min, after natural cooling, take out Wafer Cleaning and namely obtain Si-NPA substrate;
Step 2, growth of zinc oxide nano line: adopt magnetron sputtering to prepare zinc oxide nanowire in conjunction with thermal oxidation method; Silicon nano hole column substrate is put in magnetic control sputtering device, when sputtering voltage 220V, sputtering current 0.8A, magnetron sputtering Zn film, thickness is 50nm, putting it into subsequently in batch-type furnace, at 400 DEG C, thermal oxidation method processes 4h, obtains diameter and is about the zinc oxide nanowire of 30nm;
Step 3, grows graphene layer: adopt process for preparing graphenes by chemical vapour deposition; First magnetron sputtering layer of metal Ni film on the substrate that upper step obtains, thickness is about 5nm; Secondly, putting in tube furnace by this substrate, be warming up to 900 DEG C, pass into hydrogen as protection reducing gas by given pace, stablize 30min, then, pass into methane 2h according to a certain percentage simultaneously, stopping starts Temperature fall after passing into methane; Under Ni catalyst action, methane molecule at high temperature can be cracked into carbon atom and hydrogen atom, at temperature-fall period and under the protection of hydrogen, and carbon atom meeting formation of deposits one layer graphene thin film;
Step 4, is deposited with interdigital electrode: after obtaining growing the silicon nano hole column substrate having zinc oxide nanowire and Graphene, covers interdigital electrode mask at substrate surface, utilizes magnetron sputtering method to be deposited with Au thin film thick for one layer of 500nm on its surface as electrode;
Step 5, assembles sensing element and reads data element: the both positive and negative polarity wire reading data element is connected in interdigital electrode, two parts composition Zinc oxide-base moisture sensor device;
Wherein, the preparation method of described polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly is as follows:
Step one, polysulfone hollow fibre basement membrane pretreatment: polysulfone hollow fibre basement membrane to carry out pretreatment before coating, after soaking 12h with deionized water, with the soak with hydrochloric acid 60min of 1.0mol/l, remove glycerin layer and other organic solvents on film surface; Then use in the sodium hydroxide solution of 1.0mol/l and excessive hydrochloric acid, finally repeatedly rinse with deionized water, make film surface in neutrality, dry in the shade standby;
Step 2, prepare polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane: add in deionized water by the polyvinyl alcohol that the average degree of polymerization of certain mass is 1750 �� 50, it is about 3h 50 DEG C of stirred in water bath to be completely dissolved to polyvinyl alcohol, obtains 5wt% polyvinyl alcohol homogeneous phase aqueous solution; Adding a certain amount of ethylenediamine tetraacetic methene phosphoric acid after solution is cooled to room temperature, and at room temperature stir 1.5h, namely standing and defoaming obtains casting solution; Polysulfones basement membrane (molecular cut off 30000) through pretreatment is taken out after casting solution soaks 20min, is vertically fixed on the guide frame that dries in the air and dries in the shade; After the film of primary coating soaks 20min again in casting solution, will reversely be fixed on and dry in the air on guide frame, dry at room temperature over night, prepare required PVA-EDTMPA/PS hollow fiber composite membrane.
Step 3, fixing: polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane is fixed in glass electrode.
Wet sensitive is tested:
Zinc oxide-base moisture sensor is put in control appliance of temperature and humidity. Test temperature is set as 20 DEG C, then controls relative humidity variations and ranges for 10%��95%, reads the electric capacity of sensing element with humidity situation of change;
The sensitivity definition of dew cell is: CRH-C11/ C11�� 100%, wherein CRHFor the component capacitance value obtained under test environment humidity, C11Capacitance for 11% time element of relative humidity. Are defined as the response of dew cell or recovery time testing capacitor value and reach the time used by total variation 80% at the variable quantity of 11%RH to 75%RH;
When testing frequency and being 100Hz, under the relative humidity of 15%, 35%, 55%, 75%, 95%, the sensitivity of sensing element respectively 4,39,154,543 and 2371, response and respectively 8s and 11s recovery time, test result shows that this vacuum drying oven has good wet sensitive performance, the interior humidity environment of vacuum drying oven can be detected whether in admissible scope, ensure the normal use of this drying baker.
Embodiment 2
A kind of vacuum drying oven detecting function based on steam as shown in Figure 1, the internally installed of described vacuum drying oven 1 has zno-based moisture sensor module 2; Described zno-based moisture sensor module 2 is mainly made up of wet sensitive sensing element and data read element. As in figure 2 it is shown, described wet sensitive sensing element is interdigital electrode type, it includes silicon chip substrate 10, Si-NPA20, zinc oxide nanowire 30 and graphene layer 40; Described vacuum drying oven 1 is additionally provided with microprocessor, LED display lamp bar and wireless communication module; The input of described microprocessor is connected with the outfan of described ZnO moisture sensor module, described ZnO moisture sensor module detected value reaches preset value, described microprocessor controls LED display lamp bar and flashes, described LED display lamp bar is connected to a buzzer, touches buzzer and send alarm while the flicker of LED display lamp bar; Described wireless communication module is CC2420 wireless communication module, described ZnO moisture sensor module can by described CC2420 wireless communication module transmission detection data to data basestation, by the Internet, mobile subscriber terminal can check that detection data are maybe uploaded to cloud storage center by testing result, form detection and monitoring network; The inside of described vacuum drying oven is additionally provided with a polyvinyl alcohol for dehumidification-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly, polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane is fixed in glass electrode by this membrane module, and glass electrode is connected with moisture sensor; Described zinc oxide nanowire 30 length about 6 ��m.
Preferably, the preparation method of described wet sensitive sensing element is as follows:
Step one, prepares Si-NPA substrate: the silicon chip substrate of 3cm �� 3cm is included clean dirt, hydro-thermal method corrosion preparation Si-NPA substrate; 1. take the silicon chip of 3cm �� 3cm, silicon chip is placed in the mixed solution of sulphuric acid and hydrogen peroxide volume ratio 4:1, supersound process 20min, taking-up deionized water cleans, to remove the organic impurities of silicon chip surface; It is H that silicon chip is positioned over volume ratio2O:H2O2: NH4In the mixed solution of OH=5:2:1, ultrasonic cleaning 20min, the deionized water of taking-up subsequently cleans, to remove Organic substance and the metal complex of silicon chip surface;2. hydro-thermal method corrosion is utilized to prepare Si-NPA: to weigh the Fe (NO of 1.0g3)��9H2O pours in politef, is added thereto to the HF solution of 20ml deionized water and 30ml40% subsequently; Putting in solution by the silicon chip that upper step is cleaned, add a cover and put in water heating kettle, put in drying baker by water heating kettle subsequently, 180 DEG C of constant temperature keep 30min, after natural cooling, take out Wafer Cleaning and namely obtain Si-NPA substrate;
Step 2, growth of zinc oxide nano line: adopt magnetron sputtering to prepare zinc oxide nanowire in conjunction with thermal oxidation method; Silicon nano hole column substrate is put in magnetic control sputtering device, when sputtering voltage 250V, sputtering current 0.3A, magnetron sputtering Zn film, thickness is 30nm, putting it into subsequently in batch-type furnace, at 400 DEG C, thermal oxidation method processes 2h, obtains diameter and is about the zinc oxide nanowire of 30nm;
Step 3, grows graphene layer: adopt process for preparing graphenes by chemical vapour deposition; First magnetron sputtering layer of metal Ni film on the substrate that upper step obtains, thickness is about 5nm; Secondly, putting in tube furnace by this substrate, be warming up to 900 DEG C, pass into hydrogen as protection reducing gas by given pace, stablize 30min, then, pass into methane 2h according to a certain percentage simultaneously, stopping starts Temperature fall after passing into methane; Under Ni catalyst action, methane molecule at high temperature can be cracked into carbon atom and hydrogen atom, at temperature-fall period and under the protection of hydrogen, and carbon atom meeting formation of deposits one layer graphene thin film;
Step 4, is deposited with interdigital electrode: after obtaining growing the silicon nano hole column substrate having zinc oxide nanowire and Graphene, covers interdigital electrode mask at substrate surface, utilizes magnetron sputtering method to be deposited with Au thin film thick for one layer of 500nm on its surface as electrode;
Step 5, assembles sensing element and reads data element: the both positive and negative polarity wire reading data element is connected in interdigital electrode, two parts composition Zinc oxide-base moisture sensor device;
Wherein, the preparation method of described polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly is as follows:
Step one, polysulfone hollow fibre basement membrane pretreatment: polysulfone hollow fibre basement membrane to carry out pretreatment before coating, after soaking 12h with deionized water, with the soak with hydrochloric acid 60min of 1.0mol/l, remove glycerin layer and other organic solvents on film surface; Then use in the sodium hydroxide solution of 1.0mol/l and excessive hydrochloric acid, finally repeatedly rinse with deionized water, make film surface in neutrality, dry in the shade standby;
Step 2, prepare polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane: add in deionized water by the polyvinyl alcohol that the average degree of polymerization of certain mass is 1750 �� 50, it is about 3h 50 DEG C of stirred in water bath to be completely dissolved to polyvinyl alcohol, obtains 5wt% polyvinyl alcohol homogeneous phase aqueous solution; Adding a certain amount of ethylenediamine tetraacetic methene phosphoric acid after solution is cooled to room temperature, and at room temperature stir 1.5h, namely standing and defoaming obtains casting solution; Polysulfones basement membrane (molecular cut off 30000) through pretreatment is taken out after casting solution soaks 20min, is vertically fixed on the guide frame that dries in the air and dries in the shade; After the film of primary coating soaks 20min again in casting solution, will reversely be fixed on and dry in the air on guide frame, dry at room temperature over night, prepare required PVA-EDTMPA/PS hollow fiber composite membrane.
Step 3, fixing: polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane is fixed in glass electrode.
Wet sensitive is tested:
Zinc oxide-base moisture sensor is put in control appliance of temperature and humidity.Test temperature is set as 20 DEG C, then controls relative humidity variations and ranges for 10%��95%, reads the electric capacity of sensing element with humidity situation of change;
The sensitivity definition of dew cell is: CRH-C11/ C11�� 100%, wherein CRHFor the component capacitance value obtained under test environment humidity, C11Capacitance for 11% time element of relative humidity. Are defined as the response of dew cell or recovery time testing capacitor value and reach the time used by total variation 80% at the variable quantity of 11%RH to 75%RH;
When testing frequency and being 100Hz, under the relative humidity of 15%, 35%, 55%, 75%, 95%, the sensitivity of sensing element respectively 4,35,212,943 and 2171, response and respectively 10s and 12s recovery time, test result shows that this vacuum drying oven has good wet sensitive performance, the interior humidity environment of vacuum drying oven can be detected whether in admissible scope, ensure the normal use of this drying baker.
Embodiment 3:
A kind of vacuum drying oven detecting function based on steam as shown in Figure 1, the internally installed of described vacuum drying oven 1 has zno-based moisture sensor module 2; Described zno-based moisture sensor module 2 is mainly made up of wet sensitive sensing element and data read element. As in figure 2 it is shown, described wet sensitive sensing element is interdigital electrode type, it includes silicon chip substrate 10, Si-NPA20, zinc oxide nanowire 30 and graphene layer 40; Described vacuum drying oven 1 is additionally provided with microprocessor, LED display lamp bar and wireless communication module; The input of described microprocessor is connected with the outfan of described ZnO moisture sensor module, described ZnO moisture sensor module detected value reaches preset value, described microprocessor controls LED display lamp bar and flashes, described LED display lamp bar is connected to a buzzer, touches buzzer and send alarm while the flicker of LED display lamp bar; Described wireless communication module is CC2420 wireless communication module, described ZnO moisture sensor module can by described CC2420 wireless communication module transmission detection data to data basestation, by the Internet, mobile subscriber terminal can check that detection data are maybe uploaded to cloud storage center by testing result, form detection and monitoring network; The inside of described vacuum drying oven is additionally provided with a polyvinyl alcohol for dehumidification-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly, polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane is fixed in glass electrode by this membrane module, and glass electrode is connected with moisture sensor; Described zinc oxide nanowire 30 length about 5 ��m.
Preferably, the preparation method of described wet sensitive sensing element is as follows:
Step one, prepares Si-NPA substrate: the silicon chip substrate of 3cm �� 3cm is included clean dirt, hydro-thermal method corrosion preparation Si-NPA substrate; 1. take the silicon chip of 3cm �� 3cm, silicon chip is placed in the mixed solution of sulphuric acid and hydrogen peroxide volume ratio 4:3, supersound process 20min, taking-up deionized water cleans, to remove the organic impurities of silicon chip surface; It is H that silicon chip is positioned over volume ratio2O:H2O2: NH4In the mixed solution of OH=5:7:1, ultrasonic cleaning 20min, the deionized water of taking-up subsequently cleans, to remove Organic substance and the metal complex of silicon chip surface; 2. hydro-thermal method corrosion is utilized to prepare Si-NPA: to weigh the Fe (NO of 1.0g3)��9H2O pours in politef, is added thereto to the HF solution of 20ml deionized water and 60ml40% subsequently;Putting in solution by the silicon chip that upper step is cleaned, add a cover and put in water heating kettle, put in drying baker by water heating kettle subsequently, 180 DEG C of constant temperature keep 30min, after natural cooling, take out Wafer Cleaning and namely obtain Si-NPA substrate;
Step 2, growth of zinc oxide nano line: adopt magnetron sputtering to prepare zinc oxide nanowire in conjunction with thermal oxidation method; Silicon nano hole column substrate is put in magnetic control sputtering device, when sputtering voltage 180V, sputtering current 0.8A, magnetron sputtering Zn film, thickness is 50nm, putting it into subsequently in batch-type furnace, at 400 DEG C, thermal oxidation method processes 2h, obtains diameter and is about the zinc oxide nanowire of 60nm;
Step 3, grows graphene layer: adopt process for preparing graphenes by chemical vapour deposition; First magnetron sputtering layer of metal Ni film on the substrate that upper step obtains, thickness is about 5nm; Secondly, putting in tube furnace by this substrate, be warming up to 900 DEG C, pass into hydrogen as protection reducing gas by given pace, stablize 30min, then, pass into methane 2h according to a certain percentage simultaneously, stopping starts Temperature fall after passing into methane; Under Ni catalyst action, methane molecule at high temperature can be cracked into carbon atom and hydrogen atom, at temperature-fall period and under the protection of hydrogen, and carbon atom meeting formation of deposits one layer graphene thin film;
Step 4, is deposited with interdigital electrode: after obtaining growing the silicon nano hole column substrate having zinc oxide nanowire and Graphene, covers interdigital electrode mask at substrate surface, utilizes magnetron sputtering method to be deposited with Au thin film thick for one layer of 500nm on its surface as electrode;
Step 5, assembles sensing element and reads data element: the both positive and negative polarity wire reading data element is connected in interdigital electrode, two parts composition Zinc oxide-base moisture sensor device;
Wherein, the preparation method of described polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly is as follows:
Step one, polysulfone hollow fibre basement membrane pretreatment: polysulfone hollow fibre basement membrane to carry out pretreatment before coating, after soaking 12h with deionized water, with the soak with hydrochloric acid 60min of 1.0mol/l, remove glycerin layer and other organic solvents on film surface; Then use in the sodium hydroxide solution of 1.0mol/l and excessive hydrochloric acid, finally repeatedly rinse with deionized water, make film surface in neutrality, dry in the shade standby;
Step 2, prepare polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane: add in deionized water by the polyvinyl alcohol that the average degree of polymerization of certain mass is 1750 �� 50, it is about 3h 50 DEG C of stirred in water bath to be completely dissolved to polyvinyl alcohol, obtains 5wt% polyvinyl alcohol homogeneous phase aqueous solution; Adding a certain amount of ethylenediamine tetraacetic methene phosphoric acid after solution is cooled to room temperature, and at room temperature stir 1.5h, namely standing and defoaming obtains casting solution; Polysulfones basement membrane (molecular cut off 30000) through pretreatment is taken out after casting solution soaks 20min, is vertically fixed on the guide frame that dries in the air and dries in the shade; After the film of primary coating soaks 20min again in casting solution, will reversely be fixed on and dry in the air on guide frame, dry at room temperature over night, prepare required PVA-EDTMPA/PS hollow fiber composite membrane.
Step 3, fixing: polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane is fixed in glass electrode.
Wet sensitive is tested:
Zinc oxide-base moisture sensor is put in control appliance of temperature and humidity. Test temperature is set as 20 DEG C, then controls relative humidity variations and ranges for 10%��95%, reads the electric capacity of sensing element with humidity situation of change;
The sensitivity definition of dew cell is: CRH-C11/ C11�� 100%, wherein CRHFor the component capacitance value obtained under test environment humidity, C11Capacitance for 11% time element of relative humidity. Are defined as the response of dew cell or recovery time testing capacitor value and reach the time used by total variation 80% at the variable quantity of 11%RH to 75%RH;
When testing frequency and being 100Hz, under the relative humidity of 15%, 35%, 55%, 75%, 95%, the sensitivity of sensing element respectively 4,31,138,1023 and 2052, response and respectively 12s and 13s recovery time, test result shows that this vacuum drying oven has good wet sensitive performance, the interior humidity environment of vacuum drying oven can be detected whether in admissible scope, ensure the normal use of this drying baker.
Embodiment 4
A kind of vacuum drying oven detecting function based on steam as shown in Figure 1, the internally installed of described vacuum drying oven 1 has zno-based moisture sensor module 2; Described zno-based moisture sensor module 2 is mainly made up of wet sensitive sensing element and data read element. As in figure 2 it is shown, described wet sensitive sensing element is interdigital electrode type, it includes silicon chip substrate 10, Si-NPA20, zinc oxide nanowire 30 and graphene layer 40; Described vacuum drying oven 1 is additionally provided with microprocessor, LED display lamp bar and wireless communication module; The input of described microprocessor is connected with the outfan of described ZnO moisture sensor module, described ZnO moisture sensor module detected value reaches preset value, described microprocessor controls LED display lamp bar and flashes, described LED display lamp bar is connected to a buzzer, touches buzzer and send alarm while the flicker of LED display lamp bar; Described wireless communication module is CC2420 wireless communication module, described ZnO moisture sensor module can by described CC2420 wireless communication module transmission detection data to data basestation, by the Internet, mobile subscriber terminal can check that detection data are maybe uploaded to cloud storage center by testing result, form detection and monitoring network; The inside of described vacuum drying oven is additionally provided with a polyvinyl alcohol for dehumidification-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly, polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane is fixed in glass electrode by this membrane module, and glass electrode is connected with moisture sensor; Described zinc oxide nanowire 30 length about 8 ��m.
Preferably, the preparation method of described wet sensitive sensing element is as follows:
Step one, prepares Si-NPA substrate: the silicon chip substrate of 3cm �� 3cm is included clean dirt, hydro-thermal method corrosion preparation Si-NPA substrate; 1. take the silicon chip of 3cm �� 3cm, silicon chip is placed in the mixed solution of sulphuric acid and hydrogen peroxide volume ratio 4:1, supersound process 20min, taking-up deionized water cleans, to remove the organic impurities of silicon chip surface; It is H that silicon chip is positioned over volume ratio2O:H2O2: NH4In the mixed solution of OH=1:2:1, ultrasonic cleaning 20min, the deionized water of taking-up subsequently cleans, to remove Organic substance and the metal complex of silicon chip surface; 2. hydro-thermal method corrosion is utilized to prepare Si-NPA: to weigh the Fe (NO of 1.0g3)��9H2O pours in politef, is added thereto to the HF solution of 20ml deionized water and 30ml40% subsequently; Putting in solution by the silicon chip that upper step is cleaned, add a cover and put in water heating kettle, put in drying baker by water heating kettle subsequently, 180 DEG C of constant temperature keep 30min, after natural cooling, take out Wafer Cleaning and namely obtain Si-NPA substrate;
Step 2, growth of zinc oxide nano line: adopt magnetron sputtering to prepare zinc oxide nanowire in conjunction with thermal oxidation method; Silicon nano hole column substrate is put in magnetic control sputtering device, when sputtering voltage 220V, sputtering current 0.9A, magnetron sputtering Zn film, thickness is 50nm, putting it into subsequently in batch-type furnace, at 400 DEG C, thermal oxidation method processes 4h, obtains diameter and is about the zinc oxide nanowire of 30nm;
Step 3, grows graphene layer: adopt process for preparing graphenes by chemical vapour deposition; First magnetron sputtering layer of metal Ni film on the substrate that upper step obtains, thickness is about 9nm; Secondly, putting in tube furnace by this substrate, be warming up to 900 DEG C, pass into hydrogen as protection reducing gas by given pace, stablize 30min, then, pass into methane 2h according to a certain percentage simultaneously, stopping starts Temperature fall after passing into methane; Under Ni catalyst action, methane molecule at high temperature can be cracked into carbon atom and hydrogen atom, at temperature-fall period and under the protection of hydrogen, and carbon atom meeting formation of deposits one layer graphene thin film;
Step 4, is deposited with interdigital electrode: after obtaining growing the silicon nano hole column substrate having zinc oxide nanowire and Graphene, covers interdigital electrode mask at substrate surface, utilizes magnetron sputtering method to be deposited with Au thin film thick for one layer of 500nm on its surface as electrode;
Step 5, assembles sensing element and reads data element: the both positive and negative polarity wire reading data element is connected in interdigital electrode, two parts composition Zinc oxide-base moisture sensor device;
Wherein, the preparation method of described polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly is as follows:
Step one, polysulfone hollow fibre basement membrane pretreatment: polysulfone hollow fibre basement membrane to carry out pretreatment before coating, after soaking 12h with deionized water, with the soak with hydrochloric acid 60min of 1.0mol/l, remove glycerin layer and other organic solvents on film surface; Then use in the sodium hydroxide solution of 1.0mol/l and excessive hydrochloric acid, finally repeatedly rinse with deionized water, make film surface in neutrality, dry in the shade standby;
Step 2, prepare polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane: add in deionized water by the polyvinyl alcohol that the average degree of polymerization of certain mass is 1750 �� 50, it is about 3h 50 DEG C of stirred in water bath to be completely dissolved to polyvinyl alcohol, obtains 5wt% polyvinyl alcohol homogeneous phase aqueous solution; Adding a certain amount of ethylenediamine tetraacetic methene phosphoric acid after solution is cooled to room temperature, and at room temperature stir 1.5h, namely standing and defoaming obtains casting solution; Polysulfones basement membrane (molecular cut off 30000) through pretreatment is taken out after casting solution soaks 20min, is vertically fixed on the guide frame that dries in the air and dries in the shade; After the film of primary coating soaks 20min again in casting solution, will reversely be fixed on and dry in the air on guide frame, dry at room temperature over night, prepare required PVA-EDTMPA/PS hollow fiber composite membrane.
Step 3, fixing: polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane is fixed in glass electrode.
Wet sensitive is tested:
Zinc oxide-base moisture sensor is put in control appliance of temperature and humidity. Test temperature is set as 20 DEG C, then controls relative humidity variations and ranges for 10%��95%, reads the electric capacity of sensing element with humidity situation of change;
The sensitivity definition of dew cell is: CRH-C11/ C11�� 100%, wherein CRHFor the component capacitance value obtained under test environment humidity, C11Capacitance for 11% time element of relative humidity.Are defined as the response of dew cell or recovery time testing capacitor value and reach the time used by total variation 80% at the variable quantity of 11%RH to 75%RH;
When testing frequency and being 100Hz, under the relative humidity of 15%, 35%, 55%, 75%, 95%, the sensitivity of sensing element respectively 4,28,128,778 and 3232, response and respectively 12s and 13s recovery time, test result shows that this vacuum drying oven has good wet sensitive performance, the interior humidity environment of vacuum drying oven can be detected whether in admissible scope, ensure the normal use of this drying baker.
Embodiment 5
A kind of vacuum drying oven detecting function based on steam as shown in Figure 1, the internally installed of described vacuum drying oven 1 has zno-based moisture sensor module 2; Described zno-based moisture sensor module 2 is mainly made up of wet sensitive sensing element and data read element. As in figure 2 it is shown, described wet sensitive sensing element is interdigital electrode type, it includes silicon chip substrate 10, Si-NPA20, zinc oxide nanowire 30 and graphene layer 40; Described vacuum drying oven 1 is additionally provided with microprocessor, LED display lamp bar and wireless communication module; The input of described microprocessor is connected with the outfan of described ZnO moisture sensor module, described ZnO moisture sensor module detected value reaches preset value, described microprocessor controls LED display lamp bar and flashes, described LED display lamp bar is connected to a buzzer, touches buzzer and send alarm while the flicker of LED display lamp bar; Described wireless communication module is CC2420 wireless communication module, described ZnO moisture sensor module can by described CC2420 wireless communication module transmission detection data to data basestation, by the Internet, mobile subscriber terminal can check that detection data are maybe uploaded to cloud storage center by testing result, form detection and monitoring network; The inside of described vacuum drying oven is additionally provided with a polyvinyl alcohol for dehumidification-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly, polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane is fixed in glass electrode by this membrane module, and glass electrode is connected with moisture sensor; Described zinc oxide nanowire 30 length about 10 ��m.
Preferably, the preparation method of described wet sensitive sensing element is as follows:
Step one, prepares Si-NPA substrate: the silicon chip substrate of 3cm �� 3cm is included clean dirt, hydro-thermal method corrosion preparation Si-NPA substrate; 1. take the silicon chip of 3cm �� 3cm, silicon chip is placed in the mixed solution of sulphuric acid and hydrogen peroxide volume ratio 4:1, supersound process 20min, taking-up deionized water cleans, to remove the organic impurities of silicon chip surface; It is H that silicon chip is positioned over volume ratio2O:H2O2: NH4In the mixed solution of OH=5:2:1, ultrasonic cleaning 20min, the deionized water of taking-up subsequently cleans, to remove Organic substance and the metal complex of silicon chip surface; 2. hydro-thermal method corrosion is utilized to prepare Si-NPA: to weigh the Fe (NO of 1.0g3)��9H2O pours in politef, is added thereto to the HF solution of 20ml deionized water and 30ml60% subsequently; Putting in solution by the silicon chip that upper step is cleaned, add a cover and put in water heating kettle, put in drying baker by water heating kettle subsequently, 180 DEG C of constant temperature keep 30min, after natural cooling, take out Wafer Cleaning and namely obtain Si-NPA substrate;
Step 2, growth of zinc oxide nano line: adopt magnetron sputtering to prepare zinc oxide nanowire in conjunction with thermal oxidation method; Silicon nano hole column substrate is put in magnetic control sputtering device, when sputtering voltage 220V, sputtering current 0.8A, magnetron sputtering Zn film, thickness is 50nm, putting it into subsequently in batch-type furnace, at 400 DEG C, thermal oxidation method processes 4h, obtains diameter and is about the zinc oxide nanowire of 30nm;
Step 3, grows graphene layer: adopt process for preparing graphenes by chemical vapour deposition; First magnetron sputtering layer of metal Ni film on the substrate that upper step obtains, thickness is about 5nm; Secondly, putting in tube furnace by this substrate, be warming up to 700 DEG C, pass into hydrogen as protection reducing gas by given pace, stablize 30min, then, pass into methane 2h according to a certain percentage simultaneously, stopping starts Temperature fall after passing into methane; Under Ni catalyst action, methane molecule at high temperature can be cracked into carbon atom and hydrogen atom, at temperature-fall period and under the protection of hydrogen, and carbon atom meeting formation of deposits one layer graphene thin film;
Step 4, is deposited with interdigital electrode: after obtaining growing the silicon nano hole column substrate having zinc oxide nanowire and Graphene, covers interdigital electrode mask at substrate surface, utilizes magnetron sputtering method to be deposited with Au thin film thick for one layer of 500nm on its surface as electrode;
Step 5, assembles sensing element and reads data element: the both positive and negative polarity wire reading data element is connected in interdigital electrode, two parts composition Zinc oxide-base moisture sensor device;
Wherein, the preparation method of described polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly is as follows:
Step one, polysulfone hollow fibre basement membrane pretreatment: polysulfone hollow fibre basement membrane to carry out pretreatment before coating, after soaking 12h with deionized water, with the soak with hydrochloric acid 60min of 1.5mol/l, remove glycerin layer and other organic solvents on film surface; Then use in the sodium hydroxide solution of 1.0mol/l and excessive hydrochloric acid, finally repeatedly rinse with deionized water, make film surface in neutrality, dry in the shade standby;
Step 2, prepare polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane: add in deionized water by the polyvinyl alcohol that the average degree of polymerization of certain mass is 1750 �� 50, it is about 3h 50 DEG C of stirred in water bath to be completely dissolved to polyvinyl alcohol, obtains 5wt% polyvinyl alcohol homogeneous phase aqueous solution; Adding a certain amount of ethylenediamine tetraacetic methene phosphoric acid after solution is cooled to room temperature, and at room temperature stir 1.5h, namely standing and defoaming obtains casting solution; Polysulfones basement membrane (molecular cut off 30000) through pretreatment is taken out after casting solution soaks 20min, is vertically fixed on the guide frame that dries in the air and dries in the shade; After the film of primary coating soaks 20min again in casting solution, will reversely be fixed on and dry in the air on guide frame, dry at room temperature over night, prepare required PVA-EDTMPA/PS hollow fiber composite membrane.
Step 3, fixing: polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane is fixed in glass electrode.
Wet sensitive is tested:
Zinc oxide-base moisture sensor is put in control appliance of temperature and humidity. Test temperature is set as 20 DEG C, then controls relative humidity variations and ranges for 10%��95%, reads the electric capacity of sensing element with humidity situation of change;
The sensitivity definition of dew cell is: CRH-C11/ C11�� 100%, wherein CRHFor the component capacitance value obtained under test environment humidity, C11Capacitance for 11% time element of relative humidity. Are defined as the response of dew cell or recovery time testing capacitor value and reach the time used by total variation 80% at the variable quantity of 11%RH to 75%RH;
When testing frequency and being 100Hz, under the relative humidity of 15%, 35%, 55%, 75%, 95%, the sensitivity of sensing element respectively 4,21,373,588 and 1932, response and respectively 15s and 17s recovery time, test result shows that this vacuum drying oven has good wet sensitive performance, the interior humidity environment of vacuum drying oven can be detected whether in admissible scope, ensure the normal use of this drying baker.
Finally should be noted that; above example is only in order to illustrate technical scheme; but not limiting the scope of the invention; although having made to explain to the present invention with reference to preferred embodiment; it will be understood by those within the art that; technical scheme can be modified or equivalent replacement, without deviating from the spirit and scope of technical solution of the present invention.
Claims (2)
1. the vacuum drying oven detecting function based on steam, it is characterised in that: the internally installed of described vacuum drying oven (1) has zno-based moisture sensor module (2); Described zno-based moisture sensor module (2) is mainly made up of wet sensitive sensing element and data read element, described wet sensitive sensing element is interdigital electrode type, including silicon chip substrate (10), Si NPA (20), zinc oxide nanowire (30) and graphene layer (40); Described vacuum drying oven (1) is additionally provided with microprocessor, LED display lamp bar and wireless communication module; The input of described microprocessor is connected with the outfan of described ZnO moisture sensor module (2), described ZnO moisture sensor module (2) detected value reaches preset value, described microprocessor controls LED display lamp bar and flashes, described LED display lamp bar is connected to a buzzer, touches buzzer and send alarm while the flicker of LED display lamp bar; Described wireless communication module is CC2420 wireless communication module, described ZnO moisture sensor module (2) can by described CC2420 wireless communication module transmission detection data to data basestation, by the Internet, mobile subscriber terminal can check that detection data are maybe uploaded to cloud storage center by testing result, form detection and monitoring network; The inside of described vacuum drying oven (1) is additionally provided with a polyvinyl alcohol ethylenediamine tetraacetic methene phosphoric acid polysulfones basement membrane hollow fiber composite membrane assembly for dehumidification, polyvinyl alcohol ethylenediamine tetraacetic methene phosphoric acid polysulfones basement membrane hollow fiber composite membrane is fixed in glass electrode by this membrane module, and glass electrode is connected with moisture sensor; Described zinc oxide nanowire (30) length about 3 ��m.
2. vacuum drying oven according to claim 1, it is characterised in that the preparation method of described wet sensitive sensing element is as follows:
Step one, prepares Si NPA substrate: the silicon chip substrate (10) of 3cm �� 3cm is included clean dirt, hydro-thermal method corrosion preparation Si NPA substrate; 1. take the silicon chip of 3cm �� 3cm, silicon chip is placed in the mixed solution of sulphuric acid and hydrogen peroxide volume ratio 4:1, supersound process 20min, taking-up deionized water cleans, to remove the organic impurities of silicon chip surface; It is H that silicon chip is positioned over volume ratio2O:H2O2: NH4In the mixed solution of OH=5:2:1, ultrasonic cleaning 20min, the deionized water of taking-up subsequently cleans, to remove Organic substance and the metal complex of silicon chip surface; 2. hydro-thermal method corrosion is utilized to prepare Si NPA: to weigh the Fe (NO of 1.0g3)��9H2O pours in politef, is added thereto to the HF solution of 20ml deionized water and 30ml40% subsequently; Putting in solution by the silicon chip that upper step is cleaned, add a cover and put in water heating kettle, put in drying baker by water heating kettle subsequently, 180 DEG C of constant temperature keep 30min, after natural cooling, take out Wafer Cleaning and namely obtain Si NPA substrate;
Step 2, growth of zinc oxide nano line: adopt magnetron sputtering to prepare zinc oxide nanowire in conjunction with thermal oxidation method; Silicon nano hole column substrate is put in magnetic control sputtering device, when sputtering voltage 220V, sputtering current 0.8A, magnetron sputtering Zn film, thickness is 50nm, putting it into subsequently in batch-type furnace, at 400 DEG C, thermal oxidation method processes 4h, obtains diameter and is about the zinc oxide nanowire of 30nm;
Step 3, grows graphene layer: adopt process for preparing graphenes by chemical vapour deposition; First magnetron sputtering layer of metal Ni film on the substrate that upper step obtains, thickness is about 5nm; Secondly, putting in tube furnace by this substrate, be warming up to 900 DEG C, pass into hydrogen as protection reducing gas by given pace, stablize 30min, then, pass into methane 2h according to a certain percentage simultaneously, stopping starts Temperature fall after passing into methane; Under Ni catalyst action, methane molecule at high temperature can be cracked into carbon atom and hydrogen atom, at temperature-fall period and under the protection of hydrogen, and carbon atom meeting formation of deposits one layer graphene thin film;
Step 4, is deposited with interdigital electrode: after obtaining growing the silicon nano hole column substrate having zinc oxide nanowire and Graphene, covers interdigital electrode mask at substrate surface, utilizes magnetron sputtering method to be deposited with Au thin film thick for one layer of 500nm on its surface as electrode;
Step 5, assembles sensing element and reads data element: the both positive and negative polarity wire reading data element is connected in interdigital electrode, two parts composition Zinc oxide-base moisture sensor device;
The preparation method of described polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly is as follows:
Step one, polysulfone hollow fibre basement membrane pretreatment: polysulfone hollow fibre basement membrane to carry out pretreatment before coating, after soaking 12h with deionized water, with the soak with hydrochloric acid 60min of 1.0mol/l, remove glycerin layer and other organic solvents on film surface; Then use in the sodium hydroxide solution of 1.0mol/l and excessive hydrochloric acid, finally repeatedly rinse with deionized water, make film surface in neutrality, dry in the shade standby;
Step 2, prepare polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane: add in deionized water by the polyvinyl alcohol that the average degree of polymerization of certain mass is 1750 �� 50, it is about 3h 50 DEG C of stirred in water bath to be completely dissolved to polyvinyl alcohol, obtains 5wt% polyvinyl alcohol homogeneous phase aqueous solution; Adding a certain amount of ethylenediamine tetraacetic methene phosphoric acid after solution is cooled to room temperature, and at room temperature stir 1.5h, namely standing and defoaming obtains casting solution; Polysulfones basement membrane (molecular cut off 30000) through pretreatment is taken out after casting solution soaks 20min, is vertically fixed on the guide frame that dries in the air and dries in the shade; After the film of primary coating soaks 20min again in casting solution, will reversely be fixed on and dry in the air on guide frame, dry at room temperature over night, prepare required PVA-EDTMPA/PS hollow fiber composite membrane.
Step 3, fixing: polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane is fixed in glass electrode.
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