CN106998596B - It is used to prepare the saturated solution of Electric radiant Heating Film - Google Patents
It is used to prepare the saturated solution of Electric radiant Heating Film Download PDFInfo
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- CN106998596B CN106998596B CN201710121200.6A CN201710121200A CN106998596B CN 106998596 B CN106998596 B CN 106998596B CN 201710121200 A CN201710121200 A CN 201710121200A CN 106998596 B CN106998596 B CN 106998596B
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
- H05B2203/017—Manufacturing methods or apparatus for heaters
Abstract
The invention discloses a kind of saturated solutions for being used to prepare Electric radiant Heating Film, including soluble tin class chloride, titanium tetrachloride, four nickel chlorides, zinc class dopant, gallium trichloride, catalyst, isopropanol, dehydrated alcohol.The saturated solution of the present invention for being used to prepare Electric radiant Heating Film, preparation process is simple, is easy to quantitative doping, the Electric radiant Heating Film the operation is stable being prepared using the solution, long service life, and the adhesion property of Electric radiant Heating Film and matrix is good, and the thermal efficiency is high.
Description
Technical field
The invention belongs to electrothermal semiconductor technology field of membrane materials more particularly to a kind of saturation for being used to prepare Electric radiant Heating Film are molten
Liquid.
Background technique
Electric radiant Heating Film is widely used in various different occasions, is a kind of film heating material.So-called film heating material be
Insulating materials surface forms layer of conductive film after certain technique processing, on insulating materials surface.Conducting particles is exhausted
The surface of edge layer forms netted lattice structure, the adjustable Electric radiant Heating Film power of the various auxiliary agents being added in film.After energization, this layer
Film can realize conversion, and then people are also known as Electric radiant Heating Film.
The present invention prepares film using spray pyrolysis, and the basic principle that spray pyrolysis prepares film is: by metal alcohol
Salt or inorganic salts are dissolved in solvent (water or organic solvent) as presoma and form uniform solution, and solute and solvent generate water
Solution or alcoholysis reaction, reaction product is gathered into the particle of several rans and forms solution, then the taking in carrier gas by solution
Leukorrhagia is atomized into tiny droplet, is subsequently deposited upon heating substrate surface, and pyrolytic reaction occurs, and solvent volatilizees to form amorphous state
Film, finally sintering obtains required film at a certain temperature.Therefore, it is used to prepare the precursor solution of Electric radiant Heating Film
Quality has a great impact to the property of film.
Existing Electric radiant Heating Film is primarily present following problems: stability is insufficient；Temperature tolerance is poor；The thermal efficiency is low；Poor adhesive force, electricity
Hotting mask coating is easy to fall off from matrix.The present invention starts with from the saturated solution for being used to prepare Electric radiant Heating Film, is dedicated to improving electric heating
The performance of film.
Summary of the invention
Aiming at the above shortcomings existing in the prior art, technical problem to be solved by the invention is to provide one kind for making
The saturated solution of standby Electric radiant Heating Film, good using the Electric radiant Heating Film of solution preparation and the adhesion property of matrix, the thermal efficiency is high.
Object of the present invention is to what is be achieved through the following technical solutions:
A kind of saturated solution being used to prepare Electric radiant Heating Film, which is characterized in that including soluble tin class chloride, four chlorinations
Titanium, four nickel chlorides, zinc class dopant, gallium trichloride, catalyst, isopropanol, dehydrated alcohol.
A kind of saturated solution being used to prepare Electric radiant Heating Film, which is characterized in that be prepared by the raw material of following weight parts: can
45-55 parts of dissolubility tin class chloride, 3-8 parts of titanium tetrachloride, 2-6 parts of four nickel chloride, 1-5 parts of zinc class dopant, gallium trichloride 2-5
Part, 3-8 parts of catalyst, 1-5 parts of isopropanol, 20-35 parts of dehydrated alcohol.
A kind of saturated solution being used to prepare Electric radiant Heating Film, which is characterized in that be prepared by the raw material of following weight parts: can
45-55 parts of dissolubility tin class chloride, 3-8 parts of titanium tetrachloride, 2-6 parts of four nickel chloride, 1-5 parts of zinc class dopant, gallium trichloride 2-5
Part, 3-8 parts of catalyst, 1-5 parts of isopropanol, 4-6 parts of hydrogen peroxide, 20-35 parts of dehydrated alcohol.
A kind of saturated solution being used to prepare Electric radiant Heating Film, which is characterized in that be prepared by the raw material of following weight parts: can
45-55 parts of dissolubility tin class chloride, 3-8 parts of titanium tetrachloride, 2-6 parts of four nickel chloride, 1-5 parts of zinc class dopant, gallium trichloride 2-5
Part, 3-8 parts of catalyst, 1-5 parts of isopropanol, 2-6 parts of complexing agent, 4-6 parts of hydrogen peroxide, 20-35 parts of dehydrated alcohol.
Preferably, the soluble tin class chloride in tin tetrachloride, stannous chloride, dioctyl stannous chloride one
Kind is several.
Preferably, the catalyst is selected from one or more of hydrochloric acid, glacial acetic acid, stearic acid, succinic acid.More preferably
Ground, the catalyst are stearic acid.
Preferably, the complexing agent is ethylenediamine and/or triethanolamine.
Preferably, the zinc class dopant is selected from one of zinc chloride, zinc acetate, pentaerythrite zinc, zinc sulfate or several
Kind.It is highly preferred that the zinc class dopant is pentaerythrite zinc.
The invention also discloses a kind of methods for preparing and being used to prepare the saturated solution of Electric radiant Heating Film, weigh each original by weight
Material, places it in mixed at high speed heater, and heating temperature is small with 600-800 revs/min of revolving speed stirring 4-6 to 45-60 DEG C
When, be mixed evenly, make solid all dissolve, after being cooled to room temperature, using 100-200 mesh filter-cloth filtering to get.
Part metals ion is uniformly dispersed poor in ethanol solution, and stearic acid is a kind of amphiphilic organic acid,
The carboxylic acid group of end group almost has stronger coordination with all metal ions, and therefore, addition is hard in the solution
Resin acid, each metal ion species can achieve the stable mixing of high uniformity in liquid phase.
The saturated solution of the present invention for being used to prepare Electric radiant Heating Film, preparation process is simple, is easy to quantitative doping, molten using this
Electric radiant Heating Film the operation is stable that liquid is prepared, long service life, the thermal efficiency are high.
Specific embodiment
The present invention will be further explained with reference to the examples below, as described below, is only to preferable implementation of the invention
Example, not limits the present invention, any person skilled in the art is possibly also with the disclosure above
Technology contents be changed to the equivalent embodiment changed on an equal basis.Without departing from the concept of the present invention, according to the present invention
Technical spirit any simple modification or equivalent variations that following embodiment is made, fall within the scope of protection of the present invention.
Adhesion performance test: according to national machinery industry standard JB/T 8554-1997 " vapor deposition film and matrix
The scratch method for test of adhesive force " it carries out, test equipment uses the automatic scratching instrument of WS-2005 type coating adhesion, and test method is
The test of sound emission measurement method, loading speed 5N/min, scratch rate 2mm/min.
Thermal efficiency performance test: the patent that specific test method application reference number is 02139432.6 carries out.
Each raw material introduction in embodiment:
Stearic acid, No. CAS: 57-11-4, the product number provided using Shanghai Aladdin biochemical technology limited liability company
For the stearic acid of S108287.
Succinic acid, No. CAS: 110-15-6, use Shanghai Mike woods biochemical technology Co., Ltd provide product number for
The succinic acid of S817845.
Dioctyl stannous chloride, No. CAS: 3542-36-7, the production provided using Shanghai Mai Ruier chemical technology Co., Ltd
The dioctyl stannous chloride that product number is GEL-SND4410.
Pentaerythrite zinc, preparation method (are made with reference to " synthesis of pentaerythrite zinc and its application in profile stabilizer "
Person: Chen Zhaohan, " Guangdong chemical industry " the 15th phase of volume 40 in 2013) 1.3 section pentaerythrite zinc preparation.
Heated at high speed mixing machine, using the high speed for the model SHR-600A that Hai Hong Machinery Co., Ltd., Zhangjagang City provides
Heat mixing machine.
Ultrasonic cleaner, the ultrasonic wave using the model KQ-250B of Kunshan Ultrasonic Instruments Co., Ltd.'s offer are clear
Wash device.
Air dry oven, using the electric heating air blast for the model TH-007-260-B that sky experimental facilities Co., Ltd provides
Drying box.
Embodiment 1
Electric radiant Heating Film solution materials (parts by weight): 48 parts of tin tetrachloride, 5 parts of titanium tetrachloride, 4 parts of four nickel chloride, zinc acetate 3
Part, 3 parts of gallium trichloride, 5 parts of hydrochloric acid, 3 parts of isopropanol, 28 parts of dehydrated alcohol.
Specific preparation process is as follows for Electric radiant Heating Film:
(1) it configures Electric radiant Heating Film treatment fluid: weighing each raw material by weight, place it in mixed at high speed heater, heat
Temperature is stirred 4 hours with 600 revs/min of revolving speed, is mixed evenly to 60 DEG C, is dissolved solid all, is cooled to room temperature
Afterwards, using 100 mesh filter-cloth filterings to get Electric radiant Heating Film treatment fluid；
(2) it is washed with distilled water Quartz glass surfaces first, removes the dust of Quartz glass surfaces, is then placed in ultrasonic clear
It washes with EtOH Sonicate 30 minutes in device, the supersonic frequency of ultrasonic cleaning machine is 30kHz, and taking-up is placed in air dry oven in 80
DEG C dry 6 hours, the quartz glass after being dried；
(2) saturated solution for being used to prepare Electric radiant Heating Film is heated as steam, steam temperature is 230 DEG C, and steam is by nitrogen
On the surface of quartz glass, quartz glass temperature is 600 DEG C, spray distance 25cm, carrier gas flux 50L/min for gas jet,
Steam shallow lake stain (the shallow lake stain is industry generic term) forms the film with a thickness of 5 μm in Quartz glass surfaces；
(3) film is sintered, sintering temperature is 760 DEG C, and sintering time is 20 minutes, then by sintered film
Natural cooling in air obtains Electric radiant Heating Film；
(4) silver paste is uniformly smeared in Electric radiant Heating Film, is carried out at being then 800 DEG C in temperature at heating in 10 minutes
Reason.
Embodiment 2
Substantially the same manner as Example 1, difference is only that:
Electric radiant Heating Film solution materials (parts by weight): 48 parts of tin tetrachloride, 5 parts of titanium tetrachloride, 4 parts of four nickel chloride, zinc acetate 3
Part, 3 parts of gallium trichloride, 5 parts of hydrochloric acid, 3 parts of isopropanol, 4 parts of hydrogen peroxide, 28 parts of dehydrated alcohol.
Embodiment 3
Substantially the same manner as Example 1, difference is only that:
Electric radiant Heating Film solution materials (parts by weight): 48 parts of tin tetrachloride, 5 parts of titanium tetrachloride, 4 parts of four nickel chloride, zinc acetate 3
Part, 3 parts of gallium trichloride, 5 parts of glacial acetic acid, 3 parts of isopropanol, 4 parts of hydrogen peroxide, 28 parts of dehydrated alcohol.
Embodiment 4
Substantially the same manner as Example 1, difference is only that:
Electric radiant Heating Film solution materials (parts by weight): 48 parts of tin tetrachloride, 5 parts of titanium tetrachloride, 4 parts of four nickel chloride, zinc acetate 3
Part, 3 parts of gallium trichloride, 5 parts of stearic acid, 3 parts of isopropanol, 4 parts of hydrogen peroxide, 28 parts of dehydrated alcohol.
Embodiment 5
Substantially the same manner as Example 1, difference is only that:
Electric radiant Heating Film solution materials (parts by weight): 48 parts of tin tetrachloride, 5 parts of titanium tetrachloride, 4 parts of four nickel chloride, zinc acetate 3
Part, 3 parts of gallium trichloride, 5 parts of succinic acid, 3 parts of isopropanol, 4 parts of hydrogen peroxide, 28 parts of dehydrated alcohol.
Embodiment 6
Substantially the same manner as Example 1, difference is only that:
Electric radiant Heating Film solution materials (parts by weight): 48 parts of tin tetrachloride, 5 parts of titanium tetrachloride, 4 parts of four nickel chloride, zinc acetate 3
Part, 3 parts of gallium trichloride, 5 parts of stearic acid, 3 parts of isopropanol, 4 parts of ethylenediamine, 4 parts of hydrogen peroxide, 28 parts of dehydrated alcohol.
Table 1: Electric radiant Heating Film adhesion property and the thermal efficiency test table
As it can be seen from table 1 embodiment 2 increases compared to embodiment 1, adhesive force and the thermal efficiency, this may be
Because hydrogen peroxide decomposes oxygen during spray pyrolysis, be conducive to the raising of electric heating film properties；It is right in embodiment 2-5
Catalyst further screens, and embodiment 4 uses stearic acid, and adhesive force and the thermal efficiency are substantially better than embodiment 2,3 and of embodiment
Embodiment 5 illustrates that stearic acid as amphiphilic organic acid, is more advantageous to the stabilization of Electric radiant Heating Film saturated solution；And 6 phase of embodiment
Compared with embodiment 4, it is added to complexing agent ethylenediamine, amino and metal ion, which are formed, to be coordinated, and Electric radiant Heating Film saturation is further increased
The stability of solution.
Embodiment 7
Substantially the same manner as Example 1, difference is only that:
Electric radiant Heating Film solution materials (parts by weight): 48 parts of tin tetrachloride, 5 parts of titanium tetrachloride, 4 parts of four nickel chloride, zinc chloride 3
Part, 3 parts of gallium trichloride, 5 parts of stearic acid, 3 parts of isopropanol, 4 parts of ethylenediamine, 4 parts of hydrogen peroxide, 28 parts of dehydrated alcohol.
Embodiment 8
Substantially the same manner as Example 1, difference is only that:
Electric radiant Heating Film solution materials (parts by weight): 48 parts of tin tetrachloride, 5 parts of titanium tetrachloride, 4 parts of four nickel chloride, zinc sulfate 3
Part, 3 parts of gallium trichloride, 5 parts of stearic acid, 3 parts of isopropanol, 4 parts of ethylenediamine, 4 parts of hydrogen peroxide, 28 parts of dehydrated alcohol.
Embodiment 9
Substantially the same manner as Example 1, difference is only that:
Electric radiant Heating Film solution materials (parts by weight): 48 parts of tin tetrachloride, 5 parts of titanium tetrachloride, 4 parts of four nickel chloride, pentaerythrite
3 parts of zinc, 3 parts of gallium trichloride, 5 parts of stearic acid, 3 parts of isopropanol, 4 parts of ethylenediamine, 4 parts of hydrogen peroxide, 28 parts of dehydrated alcohol.
Table 2: Electric radiant Heating Film adhesion property and the thermal efficiency test table
From table 2 it can be seen that embodiment 9 uses pentaerythrite zinc, and adhesive force and the thermal efficiency obtain in embodiment 6-9
Further improvement.
Acid resistance test to Electric radiant Heating Film: Electric radiant Heating Film is put into the hydrochloric acid dope that concentration is 1mol/L soaks at room temperature
Stain 24 hours, in 80 DEG C dry 2 hour Electric radiant Heating Film impregnate before and after was placed in air dry oven after taking-up wash with distilled water
There is no significant changes on surface.
Acid resistance test to Electric radiant Heating Film: Electric radiant Heating Film is put into the NaOH dope that concentration is 1mol/L soaks at room temperature
Stain 24 hours, in 80 DEG C dry 2 hour Electric radiant Heating Film impregnate before and after was placed in air dry oven after taking-up wash with distilled water
There is slight erosion on surface, but does not fall off.
Embodiment 10
Substantially the same manner as Example 1, difference is only that:
Electric radiant Heating Film solution materials (parts by weight): 48 parts of dioctyl stannous chloride, 5 parts of titanium tetrachloride, 4 parts of four nickel chloride, season
Penta 3 parts of tetrol zinc, 3 parts of gallium trichloride, 5 parts of stearic acid, 3 parts of isopropanol, 4 parts of ethylenediamine, 4 parts of hydrogen peroxide, dehydrated alcohol 28
Part.
The adhesive force and the thermal efficiency of Electric radiant Heating Film are tested, after tested, adhesive force 179N, the thermal efficiency is
92.6%.
Acid resistance test to Electric radiant Heating Film: Electric radiant Heating Film is put into the hydrochloric acid dope that concentration is 1mol/L soaks at room temperature
Stain 24 hours, in 80 DEG C dry 2 hour Electric radiant Heating Film impregnate before and after was placed in air dry oven after taking-up wash with distilled water
Surface, which has, slightly to fall off.
Acid resistance test to Electric radiant Heating Film: Electric radiant Heating Film is put into the NaOH dope that concentration is 1mol/L soaks at room temperature
Stain 24 hours, in 80 DEG C dry 2 hour Electric radiant Heating Film impregnate before and after was placed in air dry oven after taking-up wash with distilled water
Surface, which has, slightly to fall off.
Embodiment 11
It is highly preferred that the solubility tin class chloride is made of tin tetrachloride and dioctyl stannous chloride, tin tetrachloride
Mass ratio with dioctyl stannous chloride is (4-6): 1.
Substantially the same manner as Example 1, difference is only that:
Electric radiant Heating Film solution materials (parts by weight): 40 parts of tin tetrachloride, 8 parts of dioctyl stannous chloride, 5 parts of titanium tetrachloride, four
4 parts of nickel chloride, 3 parts of pentaerythrite zinc, 3 parts of gallium trichloride, 5 parts of stearic acid, 3 parts of isopropanol, 4 parts of ethylenediamine, hydrogen peroxide 4
Part, 28 parts of dehydrated alcohol.
The adhesive force and the thermal efficiency of Electric radiant Heating Film are tested, after tested, adhesive force 194N, the thermal efficiency is
98.5%.
Acid resistance test to Electric radiant Heating Film: Electric radiant Heating Film is put into the hydrochloric acid dope that concentration is 1mol/L soaks at room temperature
Stain 24 hours, in 80 DEG C dry 2 hour Electric radiant Heating Film impregnate before and after was placed in air dry oven after taking-up wash with distilled water
There is no significant changes on surface.
Acid resistance test to Electric radiant Heating Film: Electric radiant Heating Film is put into the NaOH dope that concentration is 1mol/L soaks at room temperature
Stain 24 hours, in 80 DEG C dry 2 hour Electric radiant Heating Film impregnate before and after was placed in air dry oven after taking-up wash with distilled water
There is no significant changes on surface.
Claims (10)
1. a kind of saturated solution for being used to prepare Electric radiant Heating Film, which is characterized in that including soluble tin class chloride, titanium tetrachloride,
Four nickel chlorides, zinc class dopant, gallium trichloride, catalyst, isopropanol, dehydrated alcohol.
2. a kind of saturated solution for being used to prepare Electric radiant Heating Film, which is characterized in that be prepared by the raw material of following weight parts: solvable
45-55 parts of property tin class chloride, 3-8 parts of titanium tetrachloride, 2-6 parts of four nickel chloride, 1-5 parts of zinc class dopant, gallium trichloride 2-5
Part, 3-8 parts of catalyst, 1-5 parts of isopropanol, 20-35 parts of dehydrated alcohol.
3. a kind of saturated solution for being used to prepare Electric radiant Heating Film, which is characterized in that be prepared by the raw material of following weight parts: solvable
45-55 parts of property tin class chloride, 3-8 parts of titanium tetrachloride, 2-6 parts of four nickel chloride, 1-5 parts of zinc class dopant, gallium trichloride 2-5
Part, 3-8 parts of catalyst, 1-5 parts of isopropanol, 4-6 parts of hydrogen peroxide, 20-35 parts of dehydrated alcohol.
4. a kind of saturated solution for being used to prepare Electric radiant Heating Film, which is characterized in that be prepared by the raw material of following weight parts: solvable
45-55 parts of property tin class chloride, 3-8 parts of titanium tetrachloride, 2-6 parts of four nickel chloride, 1-5 parts of zinc class dopant, gallium trichloride 2-5
Part, 3-8 parts of catalyst, 1-5 parts of isopropanol, 2-6 parts of complexing agent, 4-6 parts of hydrogen peroxide, 20-35 parts of dehydrated alcohol.
5. being used to prepare the saturated solution of Electric radiant Heating Film as claimed in claim 4, which is characterized in that the solubility tin class chlorination
Object is selected from one or more of tin tetrachloride, stannous chloride, dioctyl stannous chloride.
6. being used to prepare the saturated solution of Electric radiant Heating Film as claimed in claim 5, which is characterized in that the catalyst is selected from salt
One or more of acid, glacial acetic acid, stearic acid, succinic acid.
7. being used to prepare the saturated solution of Electric radiant Heating Film as claimed in claim 6, which is characterized in that the catalyst is tristearin
Acid.
8. being used to prepare the saturated solution of Electric radiant Heating Film as claimed in claim 7, which is characterized in that the complexing agent is ethylenediamine
And/or triethanolamine.
9. being used to prepare the saturated solution of Electric radiant Heating Film as claimed in claim 8, which is characterized in that the zinc class dopant is selected from
One or more of zinc chloride, zinc acetate, pentaerythrite zinc, zinc sulfate.
10. the method for preparing the saturated solution of any of claims 1-9 for being used to prepare Electric radiant Heating Film, feature exist
In, weigh each raw material by weight, place it in mixed at high speed heater, heating temperature to 45-60 DEG C, with 600-800 turn/
The revolving speed of minute stirs 4-6 hours, is mixed evenly, and dissolves solid all, after being cooled to room temperature, using 100-200 mesh
Filter-cloth filtering to get.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108156675B (en) * | 2017-12-20 | 2021-04-20 | 广东暖丰电热科技有限公司 | Electrothermal film sol and preparation method thereof |
| CN108337746A (en) * | 2018-01-25 | 2018-07-27 | 陈昭 | High stable heating element and preparation method thereof |
| CN110139406A (en) * | 2019-06-10 | 2019-08-16 | 上海中孚特种油品有限公司 | A kind of saturated solution and preparation method thereof being used to prepare Electric radiant Heating Film |
| CN114587022B (en) * | 2022-03-09 | 2022-10-21 | 东莞市中科智恒新材料有限公司 | Lattice electrothermal film for electronic cigarette atomizer and manufacturing method thereof |
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| CN101668359A (en) * | 2009-08-11 | 2010-03-10 | 罗日良 | Electrothermal film and manufacturing method thereof |
| CN103428910A (en) * | 2013-07-12 | 2013-12-04 | 罗日良 | Heating pipe |
| CN103796346A (en) * | 2014-02-27 | 2014-05-14 | 上海理工大学 | High-temperature nano-electrothermal film of double-film structure and preparation method thereof |
| CN104486849A (en) * | 2014-12-10 | 2015-04-01 | 罗敏 | Saturated solution for preparing semiconductor electrothermal films |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101668359A (en) * | 2009-08-11 | 2010-03-10 | 罗日良 | Electrothermal film and manufacturing method thereof |
| CN103428910A (en) * | 2013-07-12 | 2013-12-04 | 罗日良 | Heating pipe |
| CN103796346A (en) * | 2014-02-27 | 2014-05-14 | 上海理工大学 | High-temperature nano-electrothermal film of double-film structure and preparation method thereof |
| CN104486849A (en) * | 2014-12-10 | 2015-04-01 | 罗敏 | Saturated solution for preparing semiconductor electrothermal films |
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