CN113766683A - Semiconductor electrothermal film precursor liquid, electrothermal film structure and electrothermal structure preparation method - Google Patents
Semiconductor electrothermal film precursor liquid, electrothermal film structure and electrothermal structure preparation method Download PDFInfo
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- 239000004065 semiconductor Substances 0.000 title claims abstract description 63
- 239000002243 precursor Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000007788 liquid Substances 0.000 title description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 20
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 16
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 14
- 239000001119 stannous chloride Substances 0.000 claims abstract description 14
- 235000011150 stannous chloride Nutrition 0.000 claims abstract description 14
- 229910001887 tin oxide Inorganic materials 0.000 claims abstract description 14
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims abstract description 14
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910000416 bismuth oxide Inorganic materials 0.000 claims abstract description 10
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims abstract description 10
- GXVYSAQHWSKZFV-UHFFFAOYSA-K trichlorostibane;dihydrate Chemical compound O.O.Cl[Sb](Cl)Cl GXVYSAQHWSKZFV-UHFFFAOYSA-K 0.000 claims abstract description 10
- 239000012153 distilled water Substances 0.000 claims abstract description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 7
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052716 thallium Inorganic materials 0.000 claims abstract description 7
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000758 substrate Substances 0.000 claims description 27
- 238000005485 electric heating Methods 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 229910010293 ceramic material Inorganic materials 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 7
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000007639 printing Methods 0.000 claims description 3
- 238000007650 screen-printing Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 230000035939 shock Effects 0.000 abstract description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 230000001276 controlling effect Effects 0.000 description 8
- 229960000583 acetic acid Drugs 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000012362 glacial acetic acid Substances 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- LCTONWCANYUPML-UHFFFAOYSA-N Pyruvic acid Chemical compound CC(=O)C(O)=O LCTONWCANYUPML-UHFFFAOYSA-N 0.000 description 4
- 239000003571 electronic cigarette Substances 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 description 2
- 229940005991 chloric acid Drugs 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 229960000443 hydrochloric acid Drugs 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 229940074355 nitric acid Drugs 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000003002 pH adjusting agent Substances 0.000 description 2
- 229960004838 phosphoric acid Drugs 0.000 description 2
- 229940107700 pyruvic acid Drugs 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- QHGNHLZPVBIIPX-UHFFFAOYSA-N tin(ii) oxide Chemical compound [Sn]=O QHGNHLZPVBIIPX-UHFFFAOYSA-N 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000009658 destructive testing Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- KHMOASUYFVRATF-UHFFFAOYSA-J tin(4+);tetrachloride;pentahydrate Chemical compound O.O.O.O.O.Cl[Sn](Cl)(Cl)Cl KHMOASUYFVRATF-UHFFFAOYSA-J 0.000 description 1
Images
Classifications
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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
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
- H05B3/34—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater flexible, e.g. heating nets or webs
-
- 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
- H05B3/02—Details
- H05B3/03—Electrodes
-
- 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—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heating 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
- H05B3/14—Heating 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 the material being non-metallic
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- Non-Adjustable Resistors (AREA)
Abstract
The invention provides a precursor solution of a semiconductor electrothermal film, which comprises a component A, a component B and a component C, wherein the component A comprises the following components in parts by weight: 2-10 parts of stannic chloride pentahydrate, 3-6 parts of stannous chloride and 0.3-1 part of glycerol, and further comprises a pH regulator, wherein the pH of the component A is 4.7-6.2; the component B comprises the following components in parts by weight: 5-10 parts of a conductivity regulator, wherein the conductivity regulator is one or a combination of more of antimony trichloride dihydrate, bismuth trioxide, aluminum trioxide and thallium dioxide, 0.6-1 part of aluminum chloride and a pH regulator, and the pH of the component B is 4.7-5.0; the component C comprises the following components in parts by weight: 0.5-0.7 part of tin oxide, 0.8-1.5 parts of bismuth oxide and 15-25 parts of ethanol; 15-30 parts of distilled water, and a preparation method of the electrothermal film and the electrothermal structure, wherein the obtained semiconductor electrothermal film has the properties of temperature shock resistance, good temperature stability, attenuation resistance, high temperature rise speed and good high temperature resistance.
Description
Technical Field
The invention relates to the field of semiconductor electrothermal films, in particular to a precursor liquid of a semiconductor electrothermal film, a semiconductor electrothermal film structure and a preparation method of the electrothermal structure.
Background
Compared with the traditional electric heating material, such as a resistance wire, the semiconductor electric heating film has great advantages, such as high electric heating conversion efficiency, capability of realizing full surface coverage, increased heat transfer area, improved heat transfer rate and long service life, and can be applied to a heating atomizer of an electronic cigarette, but the working temperature of the semiconductor electric heating film is usually 300 ℃ plus 100 ℃ compared with the working temperature of the resistance wire being 1000 ℃ plus 100 ℃, and the working temperature is relatively low.
In addition, the current tin oxide electrothermal film has more obvious resistance change at the temperature of more than 500 ℃, so the attenuation is more severe, and the application range of the tin oxide electrothermal film is limited.
In addition, the heating speed of the electric heating film is relatively slow, the electrifying temperature is unstable in a short time, and carcinogenic substances are easily generated when the electric heating film is applied to the electronic cigarette.
At present, an inorganic electrothermal film usually adopts tin chloride pentahydrate or tin chloride or stannous chloride as a main component, the weight part is usually 10-60 parts according to different formulas, the tin oxide electrothermal film is formed by hydrolysis, and the performance of the electrothermal film is improved by a doping mode, but the technical problem cannot be solved by doping of the component.
Therefore, it is necessary to provide a new precursor solution of a semiconductor electrothermal film, and as a further step, it is necessary to provide a method for preparing a semiconductor electrothermal film structure, and as a further step, it is also necessary to provide a method for preparing an electrothermal structure.
Disclosure of Invention
The first objective of the present invention is to provide a precursor solution for a semiconductor electrothermal film, so as to solve the problems in the background art.
In order to achieve the purpose, the invention provides a precursor solution of a semiconductor electrothermal film, which is characterized by comprising a component A, a component B and a component C, wherein,
the component A comprises the following components in parts by weight: 2-10 parts of stannic chloride pentahydrate, 3-6 parts of stannous chloride and 0.3-1 part of glycerol, and also comprises a pH regulator, wherein the pH of the component A is 4.7-6.2;
the component B comprises the following components in parts by weight: 5-10 parts of a conductivity regulator, wherein the conductivity regulator is one or a combination of more of antimony trichloride dihydrate, bismuth trioxide, aluminum trioxide and thallium dioxide, 0.6-1 part of aluminum chloride and a pH regulator, and the pH of the component B is 4.7-5.0;
the component C comprises the following components in parts by weight: 0.5-0.7 part of tin oxide, 0.8-1.5 parts of bismuth oxide and 15-25 parts of ethanol;
also comprises 15-30 parts of distilled water.
The second purpose of the invention is to provide a preparation method of a semiconductor electrothermal film structure, which comprises the precursor solution of the semiconductor electrothermal film, and is characterized by comprising the following steps:
preparing a precursor solution of the semiconductor electrothermal film:
the method comprises the following steps:
according to the proportion, taking stannic chloride pentahydrate and stannous chloride, fully mixing, adding into a pH regulator, controlling the pH value to be 4.7-6.2, controlling the temperature to be 8-12 ℃, stirring until the stannic chloride pentahydrate and the stannous chloride are completely dissolved, adding glycerol according to the proportion, and continuously stirring for 5-10min to obtain a component A;
adding a conductivity regulator and aluminum chloride in a ratio into a pH regulator, wherein the conductivity regulator is one or a combination of more of antimony trichloride dihydrate, bismuth trioxide, aluminum trioxide and thallium dioxide, controlling the pH value to be 4.7-5.0, controlling the temperature to be 15-20 ℃, and uniformly stirring to obtain a component B;
taking ethanol according to the proportion, adding tin oxide and bismuth oxide into the ethanol according to the proportion, and uniformly mixing to obtain a component C;
step two:
adding the component A and the component B into the component C, adding distilled water according to the proportion, fully reacting, and filtering out solid particles to obtain a precursor solution of the semiconductor electrothermal film;
preparing a semiconductor electrothermal film structure:
heating the substrate to 380-860 ℃, fully mixing the precursor solution of the semiconductor electrothermal film with 3-7kg of air, spraying the mixture on one side surface of the substrate by a spray gun, and cooling to room temperature to obtain the semiconductor electrothermal film structure.
Preferably, the substrate is a ceramic material and/or a glass material.
The third purpose of the present invention is to provide a method for preparing an electrothermal structure, which is characterized in that the method comprises the steps of:
preparing an electrode:
printing conductive paste on one side surface, far away from the substrate, of the semiconductor electrothermal film through screen printing to form a first electrode and a second electrode, wherein the first electrode and the second electrode are oppositely arranged, and the mesh number of the silk screen is 80-200 meshes;
preparing an electrothermal structure:
and heating the substrate coated with the semiconductor electric heating film, the first electrode and the second electrode to 180-.
Preferably, the conductive paste is a conductive silver paste.
Preferably, the substrate is a ceramic material and/or a glass material.
The PH adjusting agent is used for adjusting PH to prevent chloride from being hydrolyzed in advance to cause deterioration, and includes, but is not limited to, hydrochloric acid, glacial acetic acid, nitric acid, chloric acid, phosphoric acid, pyruvic acid, nitrous acid, and formic acid.
Compared with the prior art, the invention has the beneficial technical effects that:
(1) the semiconductor electrothermal film obtained by crystallizing the precursor solution of the semiconductor electrothermal film has the properties of temperature shock resistance, good temperature stability, attenuation resistance, high temperature rise speed and good high temperature resistance;
(2) the preparation method of the semiconductor electrothermal film structure is provided, and the method can realize stable large-scale automatic industrial production;
(3) the preparation method of the electric heating structure is provided, and the obtained electric heating structure has the properties of temperature shock resistance, breakdown resistance, adaptability to large-range voltage change, high electric heating conversion efficiency and good high temperature resistance.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is a schematic structural diagram of an electrothermal structure according to an embodiment of the present invention;
fig. 2 is a second schematic structural diagram of an electrothermal structure according to an embodiment of the present invention.
The reference numbers illustrate: 1-a substrate; 2-semiconductor electrothermal film; 3-a first electrode, 4-a second electrode, 5-a conductive member.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, the descriptions related to "first", "second", etc. in the present invention are for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature.
In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
Example 1:
a precursor solution of a semiconductor electrothermal film comprises a component A, a component B and a component C, wherein the component A comprises the following components in parts by weight: 2 parts of stannic chloride pentahydrate, 3 parts of stannous chloride, 0.3 part of glycerol and a pH regulator, wherein the pH of the component A is regulated to 4.7-6.2, and the pH regulator of the component A is glacial acetic acid;
the component B comprises the following components in parts by weight: 5 parts of a conductivity regulator, wherein the conductivity regulator is antimony trichloride dihydrate and 0.6 part of aluminum chloride, and the conductivity regulator further comprises a pH regulator, the pH of the component B is 4.7-5.0, and the pH regulator of the component B is hydrochloric acid;
the component C comprises the following components in parts by weight: 0.5 parts of tin oxide, 0.8 parts of bismuth oxide and 15 parts of ethanol;
also comprises 15 parts of distilled water.
Example 2:
a precursor solution of a semiconductor electrothermal film comprises a component A, a component B and a component C, wherein the component A comprises the following components in parts by weight: 10 parts of stannic chloride pentahydrate, 6 parts of stannous chloride, 1 part of glycerol and a pH regulator, wherein the pH of the component A is regulated to 4.7-6.2, and the pH regulator of the component A is glacial acetic acid;
the component B comprises the following components in parts by weight: 10 parts of a conductivity regulator, wherein the conductivity regulator is antimony trichloride dihydrate and 1 part of aluminum chloride, and the conductivity regulator further comprises a pH regulator, the pH of the component B is 4.7-5.0, and the pH regulator of the component B is hydrochloric acid;
the component C comprises the following components in parts by weight: 0.7 part of tin oxide, 1.5 parts of bismuth oxide and 25 parts of ethanol;
and also includes 25 parts of distilled water.
Example 3:
a precursor solution of a semiconductor electrothermal film comprises a component A, a component B and a component C, wherein the component A comprises the following components in parts by weight: 6 parts of stannic chloride pentahydrate, 4.5 parts of stannous chloride, 0.65 part of glycerol and a pH regulator, wherein the pH of the component A is regulated to 4.7-6.2, and the pH regulator of the component A is glacial acetic acid;
the component B comprises the following components in parts by weight: 7.5 parts of a conductivity regulator, wherein the conductivity regulator is antimony trichloride dihydrate, 0.8 part of aluminum chloride, and the conductivity regulator further comprises a pH regulator, the pH of the component B is 4.7-5.0, and the pH regulator of the component B is hydrochloric acid;
the component C comprises the following components in parts by weight: 0.6 part of tin oxide, 1.15 parts of bismuth oxide and 20 parts of ethanol;
also includes 22.5 portions of distilled water.
In other embodiments of the present invention, the conductivity modifier is one or a combination of more of antimony trichloride dihydrate, bismuth trioxide, aluminum trioxide and thallium dioxide.
The PH adjusting agent in the a component and the B component, for example, hydrochloric acid, glacial acetic acid, nitric acid, chloric acid, phosphoric acid, pyruvic acid, nitrous acid, and formic acid, plays a role in adjusting PH, and prevents premature hydrolysis of chloride and deterioration.
The semiconductor electrothermal film obtained in the above embodiment was measured by the following method:
resistance value: GB/T7278-2008;
electric-heat conversion efficiency: GB/T7287-;
normal total emissivity: B/T7287-;
increasing the electric heating conversion rate: GB/T7287-;
duration of operation: GB/T7287-;
the heating time is as follows: GB/T7287-;
acetic acid 24h lead dissolution: GBT 3534-;
acetic acid 24h cadmium dissolution: GBT 3534-;
destructive testing: GBT 3534-;
leakage current: GB/T7287-;
and (3) attenuation resistance test: GB/T7287-;
and (3) testing the heating speed: GB/T7287-
And (3) testing results:
the analysis of the test results shows that:
the electrothermal film has the following properties: the resistance value is as low as 0.7 omega; the heating is rapid, and the temperature can be raised to 200-310 ℃ within about 0.4s at the moment of electrifying; breakdown resistance, working voltage and leakage current accord with standards, and short circuit breakdown phenomenon cannot be generated; high temperature resistance is good, and the damage temperature reaches 680 ℃; the continuous working time is longer and is more than 2000 s; the electric heating conversion rate is higher and reaches more than 95 percent; the temperature shock resistance is good.
In addition, the glass has a higher heating speed, the highest temperature can reach 90% within 5 minutes, and the transparency is better and reaches 75% -88%.
And according to component analysis, the electrothermal film has the advantages of oxidation resistance, corrosion resistance, insulation, flame retardance, moisture resistance, high hardness, no toxicity, no harmful radiation, no discharge of harmful substances, 1 power factor during heating, and capability of detecting a heated water sample as small molecular group water and having far infrared rays which are most properly absorbed by a human body.
Compared with the prior art, the invention has the beneficial technical effects that the proportion of the stannic chloride pentahydrate and the stannous chloride is adjusted, the multi-lattice stannic oxide and a certain proportion of stannous oxide are formed after high-temperature hydrolysis to form the n-type conductive electrothermal film, and the conductivity of the electrothermal film formed after high-temperature hydrolysis is 8-20 omega/cm through the adjustment of the proportion2And the lattice parameter of tin oxide is changed by adjusting the type and proportion of the conductivity regulator, the increase of conductivity and the reduction of resistance can be simultaneously realized in a selected proportion range, and the short-time rapid heating is realized, wherein the components and the selected proportion of aluminum chloride (hydrolyzed into aluminum oxide at high temperature)) The tin oxide and the bismuth oxide are synergistic, so that the temperature coefficient of the semiconductor electrothermal film is reduced, and the temperature shock resistance and attenuation resistance of the semiconductor electrothermal film are increased.
The invention also provides a preparation method of the semiconductor electrothermal film structure, which comprises the precursor solution of the semiconductor electrothermal film.
Example 4:
a preparation method of precursor solution of semiconductor electrothermal film comprises the following steps:
the method comprises the following steps:
according to the proportion, taking stannic chloride pentahydrate and stannous chloride, fully mixing, adding into a pH regulator, controlling the pH value to be 4.7-6.2, controlling the temperature to be 8-12 ℃, stirring until the stannic chloride pentahydrate and the stannous chloride are completely dissolved, adding glycerol according to the proportion, and continuously stirring for 5-10min to obtain a component A;
adding a conductivity regulator and aluminum chloride in a ratio into a pH regulator, wherein the conductivity regulator is one or a combination of more of antimony trichloride dihydrate, bismuth trioxide, aluminum trioxide and thallium dioxide, controlling the pH value to be 4.7-5.0, controlling the temperature to be 15-20 ℃, and uniformly stirring to obtain a component B;
taking ethanol according to the proportion, and adding tin oxide and bismuth oxide into the ethanol according to the proportion to obtain a component C;
step two:
adding the component A and the component B into the component C, adding distilled water according to the proportion, fully reacting, and filtering out solid particles to obtain semiconductor electrothermal film precursor liquid;
preparing a semiconductor electrothermal film structure:
heating the substrate to 380-860 ℃, fully mixing the precursor solution of the semiconductor electrothermal film with 3-7kg of air, spraying the mixture on one side surface of the substrate by a spray gun, and cooling to room temperature to obtain the semiconductor electrothermal film structure.
The specific mixture ratio is the same as that of the embodiment 1, and the substrate is made of a ceramic material and/or a glass material.
Example 5:
the steps of the preparation method of the semiconductor electrothermal film structure are the same as those of the embodiment 4, and the specific proportion is the same as that of the embodiment 2.
Example 6:
the steps of the preparation method of the semiconductor electrothermal film structure are the same as those of the embodiment 4, and the specific proportion is the same as that of the embodiment 3.
It should be noted that, in the above embodiment, the substrate is heated to 380-.
The invention also provides a preparation method of the electrothermal structure, which comprises the preparation method of the semiconductor electrothermal film structure.
Example 7:
a preparation method of an electrothermal structure comprises the preparation method of the semiconductor electrothermal film structure of the embodiment, and further comprises the following steps:
preparing an electrode:
printing the conductive paste on one side surface of the semiconductor electrothermal film far away from the substrate by screen printing to form a first electrode and a second electrode, wherein the first electrode and the second electrode are oppositely arranged, and the mesh number of the screen is 80-200 meshes;
preparing an electrothermal structure:
heating the substrate coated with the semiconductor electrothermal film, the first electrode and the second electrode to 180-.
In example 7, the mesh number of the silk screen is 80-200 meshes, the thickness of the electrode can be controlled, the thickness of the electrode influences the magnitude of the voltage and the current carried by the electrode, and the proportion of the components is the same as that in example 1.
Example 8:
the difference from the embodiment 7 is the proportion of the components of the precursor solution of the semiconductor electrothermal film, and the proportion of the embodiment is the same as that of the embodiment 2.
Example 9:
the difference from the embodiment 7 is the proportion of the components of the precursor solution of the semiconductor electrothermal film, and the proportion of the embodiment is the same as that of the embodiment 3.
The electric heating structure obtained by the embodiment is shown in the figures 1 and 2 and comprises a substrate 1, a first electrode 3, a second motor 4 and a semiconductor electric heating film 2, wherein the semiconductor electric heating film 2 is coated on one side surface of the substrate 1, and the electric heating structure is characterized in that the semiconductor electric heating film 1 is obtained by the preparation method of the embodiment, the first electrode 3 and the second electrode 4 are arranged on one side surface of the semiconductor electric heating film 2 far away from the substrate 1, the first electrode 3 and the second electrode 4 are oppositely arranged, and the electric heating structure further comprises a conductive piece 5 arranged on the first electrode 3 and the second electrode 4 and used for transmitting electric energy of an external power supply to the first electrode 3 and the second electrode 4.
The substrate 1 is made of a ceramic material and/or a glass material, the material of the substrate 1 can be changed according to actual application, and the substrate 1 is arranged into the electrothermal structure made of the ceramic material and can be used as an atomizer of an electronic cigarette.
The first electrode 3 and the second electrode 4 are made of silver materials, mainly because the silver has the properties of high temperature resistance, temperature shock resistance, moisture resistance and oxidation resistance.
As an electronic cigarette atomizer, in order to facilitate the placement of the atomized substance, an accommodating chamber is provided in the substrate 1.
It should be noted that, according to practical applications, the thickness and shape of the substrate 1 may be adjusted, the shape and position of the first electrode 3 and the second electrode 4 may be adjusted, referring to fig. 1, the first electrode 3 and the second electrode 4 are in a square structure, and the first electrode 3 and the second electrode 4 are oppositely disposed in parallel, and the first electrode 3 and the second electrode 4 may also be in other shapes and in other forms of opposite disposition, referring to fig. 2, for example, the first electrode 3 is in a ring structure, e.g., a circular ring, the second electrode 4 is in a circular structure, and the second electrode 4 is disposed in the ring of the first electrode 3.
It should be noted that the conductive element 5 includes, but is not limited to, a conductive wire and a conductive sheet, and the installation manner of the conductive element 5 includes, but is not limited to, magnetic attraction, thimble, snap and soldering.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the contents of the present specification and the accompanying drawings, or directly/indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (6)
1. A precursor solution of a semiconductor electrothermal film is characterized by comprising a component A, a component B and a component C, wherein,
the component A comprises the following components in parts by weight: 2-10 parts of stannic chloride pentahydrate, 3-6 parts of stannous chloride and 0.3-1 part of glycerol, and also comprises a pH regulator, wherein the pH of the component A is 4.7-6.2;
the component B comprises the following components in parts by weight: 5-10 parts of a conductivity regulator, wherein the conductivity regulator is one or a combination of more of antimony trichloride dihydrate, bismuth trioxide, aluminum trioxide and thallium dioxide, 0.6-1 part of aluminum chloride and a pH regulator, and the pH of the component B is 4.7-5.0;
the component C comprises the following components in parts by weight: 0.5-0.7 part of tin oxide, 0.8-1.5 parts of bismuth oxide and 15-25 parts of ethanol;
also comprises 15-30 parts of distilled water.
2. A preparation method of a semiconductor electrothermal film structure comprises the precursor solution of the semiconductor electrothermal film as claimed in claim 1, and is characterized by comprising the following steps:
preparing a precursor solution of the semiconductor electrothermal film:
the method comprises the following steps:
according to the proportion, taking stannic chloride pentahydrate and stannous chloride, fully mixing, adding into a pH regulator, controlling the pH value to be 4.7-6.2, controlling the temperature to be 8-12 ℃, stirring until the stannic chloride pentahydrate and the stannous chloride are completely dissolved, adding glycerol according to the proportion, and continuously stirring for 5-10min to obtain a component A;
adding a conductivity regulator and aluminum chloride in a ratio into a pH regulator, wherein the conductivity regulator is one or a combination of more of antimony trichloride dihydrate, bismuth trioxide, aluminum trioxide and thallium dioxide, controlling the pH value to be 4.7-5.0, controlling the temperature to be 15-20 ℃, and uniformly stirring to obtain a component B;
taking ethanol according to the proportion, adding tin oxide and bismuth oxide into the ethanol according to the proportion, and uniformly mixing to obtain a component C;
step two:
adding the component A and the component B into the component C, adding distilled water according to the proportion, fully reacting, and filtering out solid particles to obtain a precursor solution of the semiconductor electrothermal film;
preparing a semiconductor electrothermal film structure:
heating the substrate to 380-860 ℃, fully mixing the precursor solution of the semiconductor electrothermal film with 3-7kg of air, spraying the mixture on one side surface of the substrate by a spray gun, and cooling to room temperature to obtain the semiconductor electrothermal film structure.
3. The method for preparing a semiconductor electrothermal film structure according to claim 2, wherein the substrate is a ceramic material and/or a glass material.
4. A method for preparing an electrothermal structure, comprising the method for preparing a semiconductor electrothermal film structure of claim 2, further comprising the steps of:
preparing an electrode:
printing the conductive paste on one side surface of the semiconductor electrothermal film far away from the substrate by screen printing to form a first electrode and a second electrode, wherein the first electrode and the second electrode are oppositely arranged, and the mesh number of the screen is 80-200 meshes;
preparing an electrothermal structure:
and heating the substrate coated with the semiconductor electric heating film, the first electrode and the second electrode to 180-.
5. The method of claim 4, wherein the conductive paste is a conductive silver paste.
6. A method of forming an electrothermal structure according to claim 4, wherein the substrate is a ceramic material and/or a glass material.
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| CN202110772226.3A CN113766683A (en) | 2021-07-08 | 2021-07-08 | Semiconductor electrothermal film precursor liquid, electrothermal film structure and electrothermal structure preparation method |
| JP2021116138A JP7162164B1 (en) | 2021-05-07 | 2021-07-14 | Semiconductor electrothermal film precursor solution, semiconductor electrothermal film structure, and method for manufacturing electrothermal structure |
| US17/383,418 US11834346B2 (en) | 2021-05-07 | 2021-07-22 | Semiconductor electrothermal film precursor solution and preparation method of semiconductor electrothermal film structure and electrothermal structure |
| KR1020210098989A KR102565781B1 (en) | 2021-05-07 | 2021-07-28 | Semiconductor electrothermal film precursor solution and preparation method of semiconductor electrothermal film structure and electrothermal structure |
| EP21188835.9A EP4087371A1 (en) | 2021-05-07 | 2021-07-30 | Semiconductor electrothermal film precursor solution and preparation method of semiconductor electrothermal film structure and electrothermal structure |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20060083080A (en) * | 2005-01-15 | 2006-07-20 | 쳉-핑 린 | Method of fabricating semiconductor electric heating film |
| CN109246871A (en) * | 2018-09-07 | 2019-01-18 | 南京运膜科技有限公司 | A kind of preparation method of Electric radiant Heating Film spraying filming liquid and Electric radiant Heating Film |
| CN113017158A (en) * | 2021-05-07 | 2021-06-25 | 福建晶烯新材料科技有限公司 | Heating and atomizing structure of miniature semiconductor heating atomizer and manufacturing method thereof |
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2021
- 2021-07-08 CN CN202110772226.3A patent/CN113766683A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20060083080A (en) * | 2005-01-15 | 2006-07-20 | 쳉-핑 린 | Method of fabricating semiconductor electric heating film |
| CN109246871A (en) * | 2018-09-07 | 2019-01-18 | 南京运膜科技有限公司 | A kind of preparation method of Electric radiant Heating Film spraying filming liquid and Electric radiant Heating Film |
| CN113017158A (en) * | 2021-05-07 | 2021-06-25 | 福建晶烯新材料科技有限公司 | Heating and atomizing structure of miniature semiconductor heating atomizer and manufacturing method thereof |
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