CN112654105A - Environment-friendly green semiconductor electrothermal film and preparation method thereof - Google Patents
Environment-friendly green semiconductor electrothermal film and preparation method thereof Download PDFInfo
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- CN112654105A CN112654105A CN202011492164.2A CN202011492164A CN112654105A CN 112654105 A CN112654105 A CN 112654105A CN 202011492164 A CN202011492164 A CN 202011492164A CN 112654105 A CN112654105 A CN 112654105A
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- 239000004065 semiconductor Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title abstract description 11
- XXLJGBGJDROPKW-UHFFFAOYSA-N antimony;oxotin Chemical compound [Sb].[Sn]=O XXLJGBGJDROPKW-UHFFFAOYSA-N 0.000 claims abstract description 105
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 63
- 229910052751 metal Inorganic materials 0.000 claims abstract description 38
- 239000002184 metal Substances 0.000 claims abstract description 38
- 239000000463 material Substances 0.000 claims abstract description 36
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 30
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 30
- 239000000758 substrate Substances 0.000 claims abstract description 30
- 238000000151 deposition Methods 0.000 claims description 61
- 238000001704 evaporation Methods 0.000 claims description 58
- 230000008020 evaporation Effects 0.000 claims description 53
- 230000008021 deposition Effects 0.000 claims description 23
- 238000001771 vacuum deposition Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- 239000011248 coating agent Substances 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims description 10
- 239000010935 stainless steel Substances 0.000 claims description 10
- 238000010894 electron beam technology Methods 0.000 claims description 8
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 claims 2
- 239000012528 membrane Substances 0.000 claims 2
- 238000005485 electric heating Methods 0.000 abstract description 18
- 239000000853 adhesive Substances 0.000 abstract description 7
- 230000001070 adhesive effect Effects 0.000 abstract description 7
- 230000002035 prolonged effect Effects 0.000 abstract description 3
- 239000002585 base Substances 0.000 description 25
- 238000010438 heat treatment Methods 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 229910000838 Al alloy Inorganic materials 0.000 description 5
- 229910001069 Ti alloy Inorganic materials 0.000 description 5
- 238000007740 vapor deposition Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000005670 electromagnetic radiation Effects 0.000 description 3
- 230000007774 longterm Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 229920003319 Araldite® Polymers 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000007718 adhesive strength test Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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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—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
- H05B3/141—Conductive ceramics, e.g. metal oxides, metal carbides, barium titanate, ferrites, zirconia, vitrous compounds
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/10—Glass or silica
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/50—Substrate holders
- C23C14/505—Substrate holders for rotation of the substrates
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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
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Abstract
The invention relates to an environment-friendly green semiconductor electrothermal film and a preparation method thereof, in particular to the environment-friendly green semiconductor electrothermal film which comprises the following components: the tin antimony oxide electrothermal film comprises a metal base material, a tin antimony oxide electrothermal film and a silicon dioxide dielectric film layer between the metal base material and the tin antimony oxide electrothermal film; the tin antimony oxide electrothermal film comprises a tin antimony oxide layer and a tin antimony oxide spiral structure layer, wherein the tin antimony oxide layer is positioned on the dielectric layer, and the tin antimony oxide spiral structure layer is positioned on the tin antimony oxide layer. The adhesive force between the electrothermal film and the substrate is greatly improved, the electrothermal film is not easy to peel even if the temperature is changed continuously, and the service life is greatly prolonged; in addition, the electric heating energy efficiency ratio is greatly improved by combining the semi-spherical bulges with the surface spiral structure, and the high-temperature attenuation resistance is excellent.
Description
Technical Field
The invention relates to the technical field of electric heating materials, in particular to an environment-friendly green semiconductor electric heating film and a preparation method thereof.
Background
At present, on occasions needing heating, modes such as resistance wire heating, electromagnetic radiation heating and the like are common. Generally, resistance wire heating is a heating mode for adjusting heating power by changing a resistance value, the heating mode has the defects of low thermal efficiency, low safety coefficient, high later maintenance cost, short service life and the like, and the conversion rate of converting electric energy into heat energy is not more than 56%. Electromagnetic radiation heating utilizes radiant energy for heating, and the problems of electromagnetic radiation damage and high cost exist.
The electrothermal film has high electrothermal conversion efficiency and obvious energy-saving effect, which is determined by the characteristics of large heating area and tight combination with a heated body. Among them, the semiconductor electric heating film (abbreviated as SEHF) is a film-like semiconductor electric heating material which can be tightly combined on the surface of a base material and becomes a surface-shaped heat source after being electrified, and has the characteristics of high melting point, high hardness, low resistance, high heat efficiency, good chemical stability and the like, particularly the characteristics of acid and alkali resistance and no open fire in the heating process, and is valued by people in the electric heating field.
At present, researchers make a lot of researches on the electrothermal film, in the prior art CN 1074579A, the tin dioxide semiconductor electrothermal film can be made into the semiconductor electrothermal film with various resistance ranges by doping trace components such as bismuth, antimony, iron, titanium or fluorine, and the like, although the electrothermal film with stable working performance is obtained, the actual electrothermal conversion rate is not high. CN102925880A discloses a tin antimony oxide semiconductor transparent electrothermal film, wherein an ultrasonic spraying method is used for depositing a tin antimony oxide film on the surface of a glass or ceramic tube, although the preparation process is simple and the industrialized production is facilitated, the obtained tin antimony oxide semiconductor transparent electrothermal film has low electrothermal conversion rate, poor high-temperature thermal stability and performance attenuation phenomenon after long-term use. CN 105992408A discloses that a mixture containing indium tin oxide is formed into an electric heating film layer on the surface of an insulating substrate at a high temperature of 450-600 ℃ by an evaporation method, which can convert radiant heat energy into far infrared heat energy, realize rapid temperature increase, reduce the temperature of moisture discharge loss, enhance the speed of being absorbed by heating energy, reduce the heat energy loss, and achieve an energy efficiency utilization rate of more than 90 percent, but the electric heating conversion is unstable along with the change of the temperature, and the performance is attenuated.
Therefore, how to improve the electric-to-heat conversion energy efficiency ratio of the semiconductor current film to improve the utilization rate of energy and improve the stability of the temperature change of the semiconductor current film to better meet the national energy-saving and environment-friendly requirements is a technical problem that needs to be solved by technical personnel in the field at present.
Disclosure of Invention
The invention aims to provide an environment-friendly green semiconductor electrothermal film and a preparation method thereof, which aim to solve the problems in the background technology.
In order to achieve the above object, an object of the present invention is to provide an environment-friendly green semiconductor electrothermal film, which includes: the tin antimony oxide electrothermal film comprises a metal base material, a tin antimony oxide electrothermal film and a silicon dioxide dielectric layer between the metal base material and the tin antimony oxide electrothermal film; the tin antimony oxide electrothermal film comprises a tin antimony oxide layer and a spiral structure layer, wherein the tin antimony oxide layer is positioned on the dielectric layer, and the spiral structure layer is positioned on the tin antimony oxide layer.
Further, the spiral structure layer is located on the plurality of hemispherical protrusions on the tin antimony oxide layer.
Further, the metal substrate is selected from any one of stainless steel, aluminum, copper, titanium and alloys thereof.
Furthermore, the silicon dioxide dielectric layer and the tin antimony oxide layer are sequentially and uniformly paved on the metal base material with the semi-spherical bulges in a horizontal mode.
Further, the spiral structure layer is a triangle-like spiral structure layer.
Furthermore, the silicon dioxide dielectric layer and the tin antimony oxide electrothermal film are prepared by a vacuum evaporation method.
Furthermore, the mass ratio of tin dioxide to antimony trioxide in the tin antimony oxide electrothermal film is 1:1 to 1: 1.5.
The invention also aims to provide a preparation method of the environment-friendly green semiconductor electrothermal film, which specifically comprises the following steps:
(1) the method comprises the following steps of metal substrate pretreatment, wherein the metal substrate is subjected to punch forming treatment to obtain a metal substrate with the hemispherical bulges, and then the metal substrate with the hemispherical bulges is subjected to ultrasonic cleaning to remove surface dirt.
(2) And (2) depositing a silicon dioxide medium layer, putting the metal base material obtained in the step (1) on a sample platform of a vacuum coating machine, taking silicon dioxide as an evaporation source, closing the evaporation coating device, vacuumizing, then opening the evaporation coating device, and evaporating a silicon dioxide medium layer on the surface of the metal base material with the hemispherical bulge.
(3) And (3) depositing a tin antimony oxide layer, taking tin antimony oxide as an evaporation source, adjusting the evaporation angle to be 90 degrees, adjusting the corresponding evaporation process, and depositing a tin antimony oxide layer on the surface of the silicon dioxide dielectric layer obtained in the step (2).
(4) Depositing a spiral structure layer, rotating a sample table of a vacuum coating machine, setting an evaporation angle to be 10 degrees, and continuously depositing a tin antimony oxide layer on the surface of the tin antimony oxide layer for T1; then, the sample table is rotated anticlockwise by 120 degrees in a plane parallel to the sample table, and a tin antimony oxide layer is deposited for the second time, wherein the deposition time is T2; and (3) rotating the sample table 120 degrees counterclockwise again in the plane parallel to the sample table, and depositing the tin antimony oxide layer again for T3, wherein the deposition time is T3> T2> T1, so that the triangular-like spiral structure layer is deposited on the surface of the tin antimony oxide layer obtained in the step (3).
Further, the specific evaporation process in the step (3) and the step (4) is as follows: vacuumizing the vacuum coating machine until the vacuum degree reaches 4 multiplied by 10-3When Pa is below, start to fill O2The working air pressure is 0.5Pa, tin antimony oxide is used as an evaporation source, the evaporation voltage is 2.5kV, the electron beam current is 15mA, the substrate temperature is 450 ℃, and the deposition rate is controlled at
By adopting the structural form of the metal base material with the semi-spherical bulges, the dielectric film and the tin antimony oxide layer, on one hand, the adhesive force of the electrothermal film and the base body is greatly improved, the electrothermal film is not easy to peel off even if the temperature is changed continuously, and the service life is greatly prolonged; in addition, the semi-spherical bulges are combined with the surface spiral structure, the electric heating energy efficiency ratio of the prepared semiconductor electric heating film is greatly improved and can reach more than 95 percent at most, the high-temperature thermal stability is good, and the performance attenuation is not easy to occur in long-term use.
Drawings
Fig. 1 is a schematic structural diagram of a semiconductor electrothermal film of the present invention.
FIG. 2 is a schematic view showing the process of preparing the electrothermal semiconductor film of the present invention.
FIG. 3 is a schematic view of a process for preparing a spiral structure layer according to the present invention.
FIG. 4 is an expanded view of the spiral structure layer of the present invention.
FIG. 5 is a schematic structural view of a vacuum deposition apparatus according to the present invention.
Fig. 6 is a graph of power factor versus temperature for the semiconductor electrothermal films of examples 1-3 and comparative examples 1-2.
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.
Referring to the attached drawing 1, the environment-friendly green semiconductor electrothermal film comprises a four-layer structure, namely a metal substrate layer 1, a silicon dioxide dielectric layer 2, a tin antimony oxide layer 3 and a spiral structure layer 4 in sequence. The metal substrate layer 1 can play a good supporting role for the semiconductor electric heating film, is easier to process and form compared with the traditional base materials such as ceramic glass and the like, and is not limited by the shape of the base materials, and on the other hand, the electric heating film provided by the invention has a semi-spherical convex structure, so that local heat distribution is possibly uneven, and the good heat conductivity of the metal substrate can improve the uniformity of the overall heat distribution of the electric heating film.
The metal substrate of the present invention is preferably formed by stamping and forming as shown in fig. 1-2 with a semi-spherical convex structure, and the finally formed electrothermal film also has a semi-spherical convex structure. Compared with the traditional planar electrothermal film, the radiating surface of the electrothermal film finally formed by the invention is larger, and the electrothermal energy efficiency ratio is greatly improved. And because of adopting the structural style of the metal substrate with the semi-spherical bulge, the dielectric film and the tin antimony oxide layer, the adhesive force of the electrothermal film and the substrate is greatly improved, the electrothermal film is not easy to peel off even the temperature is changed continuously, and the service life is greatly prolonged.
For the shape of the metal substrate formed by stamping, the invention is not limited to the hemispherical convex structure, and the convex structure can be a pyramid, a semi-ellipsoid, a square and the like. However, the hemispherical convex structure is preferable in terms of easier and more uniform angle of the spiral structure layer. Referring to fig. 3-4, the spiral structure layer of the present invention is a triangle-like structure, the spiral structure layer is composed of a tin antimony oxide layer at position No. 1, a tin antimony oxide layer at position No. 2 and a tin antimony oxide layer at position No. 3, and since the deposition time T3 at position No. 3> the deposition time T2 at position No. 2> the deposition time at position No. 1 during the deposition process, as shown in expanded fig. 4, the thicknesses of the tin antimony oxides at position No. 1, position No. 2 and position No. 3 are sequentially increased, and thus the spiral structure layer of the triangle-like structure is finally formed on the surface of the tin antimony oxide layer, the spiral structure layer of the present invention can further improve the electric heating energy efficiency ratio, and is advantageous to the high-temperature thermal stability of the electric heating film.
Referring to fig. 2-4, the process for preparing the semiconductor electrothermal film of the present invention is further described, and fig. 2 is a schematic flow chart of the preparation process of the semiconductor electrothermal film of the present invention, wherein, first, the planar plate-shaped metal substrate is subjected to punch forming in the steps (1) - (2), and convex structures such as a hemispherical shape, a pyramidal shape, a semi-ellipsoidal shape, a square shape, etc. can be formed on the surface of the metal substrate according to different mold shape structures. And (4) depositing a silicon dioxide dielectric layer on the surface of the metal base material with the convex structure in the step (3) to play a role in insulation and heat insulation between the electrothermal film and the metal base body. And (4) further depositing a tin antimony oxide layer on the surface of the silicon dioxide dielectric layer to serve as a main heating part of the electrothermal film. And (5) further depositing a spiral structure layer on the tin antimony oxide layer.
Referring to fig. 5, the vacuum coater of the present invention comprises an evaporation source 5, a sample stage support 7, a sample stage 8 and a sample 9, wherein during the deposition of the tin antimony oxide layer in step (4), the evaporation angle is set to 90 °, and a layer of tin antimony oxide layer is uniformly spread on the surface of the substrate as in step (4) of fig. 2. When the spiral structure layer is deposited, as shown in fig. 5, the evaporation angle is set to 10 °, and the tin antimony oxide layer is evaporated continuously for T1. Because the semispherical protruding structure exists on the tin antimony oxide layer, as shown in fig. 3, a strip-shaped tin antimony oxide layer is formed at the position 1 of the semispherical protruding structure, then the sample table is rotated anticlockwise in the plane parallel to the sample table by 120 degrees, the tin antimony oxide layer is deposited for the second time, the deposition time is T2, so that a strip-shaped tin antimony oxide layer is formed at the position 2 of the semispherical protruding structure, the tin antimony oxide layer is deposited again by rotating the sample table anticlockwise by 120 degrees, the deposition time is T3, a strip-shaped tin antimony oxide layer is formed at the position 3 of the semispherical protruding structure, and a structure similar to a triangular shape is formed. The thicknesses of the positions 1, 2 and 3 are regulated by regulating the deposition time of the positions 1, 2 and 3 respectively, and when T3 is more than T2 is more than T1, a triangle-like spiral structure is formed on the surface of the tin antimony oxide layer, and the development of the triangle-like spiral structure is shown in FIG. 4. Of course, the present invention is not limited to this, and additional layers of other structures can be obtained by adjusting the rotation angle and the evaporation time. The excellent effects of the semiconductor electrothermal film of the present invention will be described with reference to specific embodiments.
Example 1
The embodiment provides a preparation method of an environment-friendly green semiconductor electrothermal film, which specifically comprises the following steps:
(1) a stainless steel plate with the thickness of 100cm multiplied by 50cm multiplied by 1cm is selected as a metal base material, and the stainless steel plate is subjected to punch forming treatment to obtain the stainless steel base material with the hemispherical bulges. And then, carrying out ultrasonic cleaning on the stainless steel substrate by using acetone, alcohol and deionized water to remove surface dirt.
(2) Sink with a metal plateAnd (2) depositing a silicon dioxide medium layer, putting the stainless steel base material obtained in the step (1) on a sample platform of a vacuum coating machine, adopting high-purity quartz glass as a vapor deposition source, closing an evaporation coating device, vacuumizing, then starting the evaporation coating device, and vapor depositing a silicon dioxide medium layer on the surface of the stainless steel base material with the hemispherical bulges, wherein the thickness of the silicon dioxide medium layer is 50 nm. The evaporation process conditions are as follows: vapor deposition angle of 90 DEG, vacuum degree of 5.0X 10 or more-3Pa, evaporation voltage of 3kV, electron beam current of 20mA, substrate temperature of 350 deg.C, deposition rate controlled at
(3) And (3) depositing a tin antimony oxide layer, taking high-purity tin antimony oxide as an evaporation source, wherein the evaporation angle is 90 degrees, and depositing a tin antimony oxide layer on the surface of the silicon dioxide dielectric layer obtained in the step (2), wherein the thickness of the tin antimony oxide layer is 100 nm. The evaporation process conditions are as follows: vacuumizing the vacuum coating machine until the vacuum degree reaches 4 multiplied by 10-3When Pa is below, start to fill O2The working pressure is 0.5Pa, the evaporation voltage is 2.5kV, the electron beam current is 15mA, the substrate temperature is 450 ℃, and the deposition rate is controlled
(4) Depositing a spiral structure layer, rotating a sample table of a vacuum coating machine, setting an evaporation angle to be 10 degrees, and continuously depositing a tin antimony oxide layer on the surface of the tin antimony oxide layer for 10 min; then, the sample table is rotated anticlockwise by 120 degrees in a plane parallel to the sample table, a tin antimony oxide layer is deposited for the second time, and the deposition time is 20 min; and (4) rotating the sample table 120 degrees anticlockwise again in the plane parallel to the sample table, and depositing the tin antimony oxide layer again for 30min, so that the triangular-like spiral structure layer is obtained by depositing on the surface of the tin antimony oxide layer obtained in the step (3).
Example 2
The embodiment provides a preparation method of an environment-friendly green semiconductor electrothermal film, which specifically comprises the following steps:
(1) selecting an aluminum alloy plate with the thickness of 100cm multiplied by 50cm multiplied by 1cm as a metal base material, and carrying out punch forming treatment on the aluminum alloy plate to obtain the aluminum alloy plate base material with the semi-spherical bulge. And then, carrying out ultrasonic cleaning on the aluminum alloy plate substrate by using acetone, alcohol and deionized water to remove surface dirt.
(2) And (2) depositing a silicon dioxide medium layer, putting the aluminum alloy base material obtained in the step (1) on a sample platform of a vacuum coating machine, closing the evaporation coating device by taking high-purity quartz glass as an evaporation source, vacuumizing, then opening the evaporation coating device, and evaporating a silicon dioxide medium layer on the surface of the stainless steel base material with the hemispherical bulges, wherein the thickness of the silicon dioxide medium layer is 30 nm. The evaporation process conditions are as follows: vapor deposition angle of 90 DEG, vacuum degree of 5.0X 10 or more-3Pa, evaporation voltage of 3kV, electron beam current of 20mA, substrate temperature of 350 deg.C, deposition rate controlled at
(3) And (3) depositing a tin antimony oxide layer, taking high-purity tin antimony oxide as an evaporation source, wherein the evaporation angle is 90 degrees, and depositing a tin antimony oxide layer on the surface of the silicon dioxide dielectric layer obtained in the step (2), wherein the thickness of the tin antimony oxide layer is 80 nm. The evaporation process conditions are as follows: vacuumizing the vacuum coating machine until the vacuum degree reaches 4 multiplied by 10-3When Pa is below, start to fill O2The working pressure is 0.5Pa, the evaporation voltage is 2.5kV, the electron beam current is 15mA, the substrate temperature is 450 ℃, and the deposition rate is controlled
(4) Depositing a spiral structure layer, rotating a sample table of a vacuum coating machine, setting an evaporation angle to be 10 degrees, and continuously depositing a tin antimony oxide layer on the surface of the tin antimony oxide layer for 15 min; then, the sample table is rotated anticlockwise by 120 degrees in a plane parallel to the sample table, a tin antimony oxide layer is deposited for the second time, and the deposition time is 25 min; and (4) rotating the sample table 120 degrees anticlockwise again in the plane parallel to the sample table, and depositing the tin antimony oxide layer again for 35min, so that the triangular-like spiral structure layer is obtained by depositing on the surface of the tin antimony oxide layer obtained in the step (3).
Example 3
The embodiment provides a preparation method of an environment-friendly green semiconductor electrothermal film, which specifically comprises the following steps:
(1) selecting a titanium alloy plate with the thickness of 100cm multiplied by 50cm multiplied by 1cm as a metal base material, and carrying out punch forming treatment on the titanium alloy plate to obtain the titanium alloy plate base material with the semi-spherical bulge. And then, carrying out ultrasonic cleaning on the titanium alloy plate substrate by using acetone, alcohol and deionized water to remove surface dirt.
(2) And (2) depositing a silicon dioxide medium layer, putting the titanium alloy base material obtained in the step (1) on a sample platform of a vacuum coating machine, adopting high-purity quartz glass as an evaporation source, closing the evaporation coating device, vacuumizing, then starting the evaporation coating device, and evaporating a silicon dioxide medium layer on the surface of the stainless steel base material with the hemispherical bulges, wherein the thickness of the silicon dioxide medium layer is 60 nm. The evaporation process conditions are as follows: vapor deposition angle of 90 DEG, vacuum degree of 5.0X 10 or more-3Pa, evaporation voltage of 3kV, electron beam current of 20mA, substrate temperature of 350 deg.C, deposition rate controlled at
(3) And (3) depositing a tin antimony oxide layer, taking high-purity tin antimony oxide as an evaporation source, wherein the evaporation angle is 90 degrees, and depositing a tin antimony oxide layer on the surface of the silicon dioxide dielectric layer obtained in the step (2), wherein the thickness of the tin antimony oxide layer is 120 nm. The evaporation process conditions are as follows: vacuumizing the vacuum coating machine until the vacuum degree reaches 4 multiplied by 10-3When Pa is below, start to fill O2The working pressure is 0.5Pa, the evaporation voltage is 2.5kV, the electron beam current is 15mA, the substrate temperature is 450 ℃, and the deposition rate is controlled
(4) Depositing a spiral structure layer, rotating a sample table of a vacuum coating machine, setting an evaporation angle to be 10 degrees, and continuously depositing a tin antimony oxide layer on the surface of the tin antimony oxide layer for 12 min; then, the sample table is rotated anticlockwise by 120 degrees in a plane parallel to the sample table, a tin antimony oxide layer is deposited for the second time, and the deposition time is 24 min; and (4) rotating the sample table 120 degrees anticlockwise again in the plane parallel to the sample table, and depositing the tin antimony oxide layer again for 36min, so that the triangular-like spiral structure layer is obtained by depositing on the surface of the tin antimony oxide layer obtained in the step (3).
Comparative example 1
Different from the embodiment 1, the deposition of the spiral structure layer in the step (4) is eliminated so as to prepare the semiconductor electrothermal film without the spiral structure layer.
Comparative example 2
Different from the embodiment 1, the step (1) does not carry out punch forming treatment, and a planar metal substrate material is adopted to directly deposit a dielectric film and a tin antimony oxide layer on the surface.
Next, the existing detection methods known to those skilled in the art are used to detect the electric heating performance of the embodiments 1-4 and the comparative examples 1-2, and the relationship between the power factor and the temperature of the semiconductor electric heating film is calculated, and the specific result is shown in fig. 6. The adhesive strength of the semiconductor electrothermal film is tested by adopting a vertical traction measurement method, the adhesive used for bonding is Araldite resin, and the test is carried out under the conditions that the temperature is lower than 20 ℃ and the humidity is lower than 60%.
As can be seen from FIG. 6, the power factor of the semiconductor electrothermal film of the embodiment of the invention can reach 11.225 μ W/cmK at most2While the optimum power factor value of comparative example 1 without the spiral structure layer was 7.5. mu.W/cmK2Comparative example 2 has a power factor of only 2.5. mu.W/cmK2. Therefore, the electrothermal energy efficiency ratio of the semiconductor electrothermal film is greatly improved, and the conversion rate of converting electric energy into heat energy can reach more than 95 percent at most. In addition, the power factor of the semiconductor electrothermal film of the embodiment of the invention is only slightly reduced along with the temperature rise, while the power factor of the comparative example 1 and the comparative example 2 is obviously reduced along with the temperature rise, which shows that the semiconductor electrothermal film of the invention has good high-temperature thermal stability and does not have performance attenuation along with the temperature change. The adhesive strength of the invention is more than 250kg/cm through an adhesive strength test2The adhesive force of the electric heating film base body is good, and the problem of falling off in long-term use can not occur.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the preferred embodiments of the present invention are described in the above embodiments and the description, and are not intended to limit the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. The utility model provides an environmental protection green semiconductor electric heat membrane, environmental protection green semiconductor electric heat membrane includes: the tin antimony oxide electrothermal film comprises a metal base material, a tin antimony oxide electrothermal film and a silicon dioxide dielectric film layer between the metal base material and the tin antimony oxide electrothermal film; the tin antimony oxide electrothermal film comprises a tin antimony oxide layer and a tin antimony oxide spiral structure layer, wherein the tin antimony oxide layer is positioned on the dielectric layer, and the tin antimony oxide spiral structure layer is positioned on the tin antimony oxide layer.
2. The environment-friendly green semiconductor electrothermal film according to claim 1, wherein: the tin antimony oxide spiral structure layer is positioned on the hemispherical bulges of the tin antimony oxide layer.
3. The environment-friendly green semiconductor electrothermal film according to claim 1, wherein: the metal substrate is selected from any one of stainless steel, aluminum, copper, titanium and alloys thereof.
4. The environment-friendly green semiconductor electrothermal film according to claim 1, wherein: the silicon dioxide dielectric layer and the tin antimony oxide layer are sequentially and uniformly paved on the metal base material with the semi-spherical bulges in a horizontal mode.
5. The environment-friendly green semiconductor electrothermal film according to claim 1, wherein: the tin antimony oxide spiral structure layer is a triangular-like spiral structure layer.
6. The environment-friendly green semiconductor electrothermal film according to claim 1, wherein: the silicon dioxide dielectric layer, the tin antimony oxide layer and the tin antimony oxide spiral structure layer are prepared by a vacuum evaporation method.
7. The environment-friendly green semiconductor electrothermal film according to claim 1, wherein: the mass ratio of tin dioxide to antimony trioxide in the tin antimony oxide electrothermal film is 1: 1-1: 1.5.
8. A method for preparing the environment-friendly green semiconductor electrothermal film as claimed in any one of claims 1 to 7, which comprises the following steps:
(1) the method comprises the following steps of (1) pretreating a metal base material, namely performing punch forming treatment on the metal base material to obtain the metal base material with the hemispherical bulges, and then performing ultrasonic cleaning on the metal base material with the hemispherical bulges to remove surface dirt;
(2) depositing a silicon dioxide medium layer, putting the metal base material obtained in the step (1) on a sample table of a vacuum coating machine, taking silicon dioxide as an evaporation source, closing an evaporation coating device, vacuumizing, then starting the evaporation coating device, and evaporating a silicon dioxide medium layer on the surface of the metal base material with the hemispherical bulge;
(3) depositing a tin antimony oxide layer, taking tin antimony oxide as an evaporation source, adjusting an evaporation angle to be 90 degrees, adjusting a corresponding evaporation process, and depositing a tin antimony oxide layer on the surface of the silicon dioxide dielectric layer obtained in the step (2);
(4) depositing a spiral structure layer, rotating a sample table of a vacuum coating machine, setting an evaporation angle to be 10 degrees, and continuously depositing a tin antimony oxide layer on the surface of the tin antimony oxide layer for T1; then, the sample table is rotated anticlockwise by 120 degrees in a plane parallel to the sample table, and a tin antimony oxide layer is deposited for the second time, wherein the deposition time is T2; and (3) rotating the sample table 120 degrees counterclockwise again in the plane parallel to the sample table, and depositing the tin antimony oxide layer again for T3, wherein the deposition time is T3> T2> T1, so that the triangular-like spiral structure layer is deposited on the surface of the tin antimony oxide layer obtained in the step (3).
9. The method of claim 9, wherein: the specific evaporation process in the step (3) and the step (4) comprises the following steps: vacuumizing a vacuum coating machine, when the vacuum degree reaches below 4 multiplied by 10 < -3 > Pa, starting to charge O2 to the working air pressure of 0.5Pa, taking tin antimony oxide as an evaporation source, the evaporation voltage of 2.5kV, the electron beam current of 15mA, the substrate temperature of 450 ℃, and controlling the deposition rate at the temperature of 450 DEG C
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| JP2007220636A (en) * | 2006-02-20 | 2007-08-30 | Nissei Electric Co Ltd | Transparent conductive film heater |
| US20090126903A1 (en) * | 2006-04-24 | 2009-05-21 | Sumitomo Electric Industries, Ltd. | Heat transfer member, convex structural member, electronic apparatus, and electric product |
| CN102066109A (en) * | 2008-06-20 | 2011-05-18 | 阿尔卡特朗讯美国公司 | Heat-transfer structure |
| CN105992409A (en) * | 2015-02-11 | 2016-10-05 | 佛山市顺德区美的电热电器制造有限公司 | Electrothermal film layer manufacturing method, electrothermal film layer, electric heating disc and cooking utensil |
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| JP2001326060A (en) * | 2000-05-16 | 2001-11-22 | Miyao Company Limited:Kk | Flat heater |
| CN1883229A (en) * | 2003-11-20 | 2006-12-20 | 皇家飞利浦电子股份有限公司 | Thin- film heating element |
| JP2007220636A (en) * | 2006-02-20 | 2007-08-30 | Nissei Electric Co Ltd | Transparent conductive film heater |
| US20090126903A1 (en) * | 2006-04-24 | 2009-05-21 | Sumitomo Electric Industries, Ltd. | Heat transfer member, convex structural member, electronic apparatus, and electric product |
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Application publication date: 20210413 |