CN104091882A - Double-layer high-radiation electrothermal film structure and manufacturing method - Google Patents
Double-layer high-radiation electrothermal film structure and manufacturing method Download PDFInfo
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- CN104091882A CN104091882A CN201410313179.6A CN201410313179A CN104091882A CN 104091882 A CN104091882 A CN 104091882A CN 201410313179 A CN201410313179 A CN 201410313179A CN 104091882 A CN104091882 A CN 104091882A
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- film
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- doping
- tin ash
- membrane structure
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Abstract
The invention discloses a manufacturing method for a double-layer high-radiation electrothermal film structure. The manufacturing method includes the steps of (1) using a ceramic plate and quartz glass as substrate materials, (2) etching the surface of the substrate materials to enable the surface of the substrate materials to be a flocked surface in a convex-table shape or a concave-pit shape, (3) depositing stannic oxide doped electrothermal film on the flocked surface of the substrate materials, (4) depositing silicon carbide thin film on the stannic oxide doped electrothermal film, and (5) removing the portion, where an electrode needs to be welded, of the silicon carbide thin film to form an electrode welding window, and welding an electrothermal film electrode to the window. According to the manufacturing method, after surface treatment is carried out on different substrates, the electrothermal film with different doping concentrations has different heating radiation ranges, and the intensity selection capacity is achieved on different infrared radiation wave bands. Due to silicon carbide provided with the designed performance and deposited on the surface of the stannic oxide electrothermal film, radiation of a middle-infrared band and use safety are improved while the performance of the electrothermal film is stabilized, and further application of the product is expanded.
Description
Technical field
The present invention relates to utilize transparent membrane oxide material characteristic of semiconductor and feature to design, prepare the method for high radiation electric heating film.Belong to the transparent membrane field of different film resistor application.
Background technology
In recent years, along with the continuous propelling of energy-conserving and environment-protective process, high-efficiency electric-heating mode also enters the people visual field, as heating buildings, industry heating, life electric heating etc.Semiconductor tin dioxide thin film has very high conductivity and light transmission, can be combined securely with glass or pottery, can be made into not only electro-conductive glass and the various heating element of transparent but also conduction, and the resistor of applying in electronic equipment and electronic instrument.Tin dioxide thin film is deposited on glass or ceramic bases surface, utilize its conduction property as heater, heat utilization rate can reach 96%, again because its light transmission is good, can be applicable on the outer window glass of the transport facilitys such as automobile, aircraft, steamer, form layer of conductive film as heater, prevent mist, frost, steam condensation and freezing and fuzzy.Tin dioxide thin film has the physicochemical characteristics that high rigidity, high transmission rate, high conductivity, high temperature heat-resistant stability etc. are excellent, is widely used in household electrical appliance, building and heating, photovoltaic cell, large scale integrated circuit substrate, film resistor heating element, optical instrument, sensor aviation, national defence, medical science, electronics industry.
The electric property of pure tin ash semiconductive thin film is comparatively unstable, is difficult to temperature coefficient of resistance to be controlled in very narrow scope.Add a small amount of impurity as oxides such as antimony, indium, boron, can improve its electric stability and thermal endurance, obtain certain resistivity and very little temperature coefficient of resistance, for manufacturing all size thin film resistor and electric heater.In recent years, the application of electric heating tin dioxide thin film was more and more wide, and the solution not satisfactory and security and stability problem of its electric radiation seems particularly urgent.
Summary of the invention
The present invention is directed to the on the low side and security and stability problem of tin ash doping electric-heating thin film electric radiation, a kind of electric-heating thin film structure of special design and film surface structure, compound another kind of semiconductive thin film.The designed structure of this invention and product, significantly improve the thermal radiation of tin ash electrothermal film electric, improved safety, infrared radiation stability and the safety issue of Electric radiant Heating Film simultaneously.
It is as follows that the present invention solves the problems of the technologies described above taked technical scheme:
A preparation method for the high radiate electric heating membrane structure of bilayer, comprising:
1) adopt potsherd or quartz glass as base material;
2) substrate material surface is carried out to etching processing, make substrate material surface present the suede surface of boss-shaped or pit shape;
3) on the suede surface of base material, deposit tin ash doping Electric radiant Heating Film;
4) depositing silicon carbide film on tin ash doping Electric radiant Heating Film;
5) remove the carborundum films layer of required welding electrode part, form electrode welding window, at this window welding electrothermal electrode.
Preferably, in step 1), prepare tin ash doping film based on aumospheric pressure cvd (APCVD) mode, its thickness is at 1.5mm ~ 7mm.
Preferably, in step 4), adopt CVD method at depositing silicon carbide film on tin ash doping Electric radiant Heating Film to prepare carborundum films.
Preferably, in step 4), before depositing silicon carbide film, oxygen gas plasma processing is carried out in the surface of tin ash doping Electric radiant Heating Film.
Preferably, step 2) in, use hydrofluoric acid to carry out etching processing to substrate material surface, make substrate surface present the suede surface of boss-shaped or pit shape;
Wherein, hydrofluoric acid concentration 1.5% ~ 10%, process treatment time 35s ~ 500s, the roughness of prepared substrate is controlled at 500nm ~ 50 μ m, the raised or sunken aspect ratio 1.5 ~ 8 of etching.
Preferably, in step 3), base material is through carrying out the deposition preparation of doping stannic oxide Electric radiant Heating Film after cleaning;
Base material cleaning process adopts ultrasonic clean cleaning, after deionized water ultrasonic cleaning, carries out substrate and is heated to 300 DEG C ~ 900 DEG C, carries out subsequently surperficial oxygen plasma cleaning;
After plasma cleaning, carry out the preparation of tin ash doping film, film thickness 300nm ~ 2000nm, doping weight ratio 1.8% ~ 9%.
Preferably, comprising: aumospheric pressure cvd legal system is for tin ash doping Electric radiant Heating Film and carborundum films layer.
Preferably, specifically comprise:
SnCl
2and SbCl
3n is all used in source
2do carrier gas, gasify at 90 DEG C ~ 130 DEG C and 70 DEG C ~ 100 DEG C respectively, 0
2as oxidant, N
2as diluent gas, be used for diluting reaction gaseous mixture, prepare thickness 300nm ~ 2000nm, doping weight ratio 1.8% ~ 9% tin ash doping Electric radiant Heating Film.
Preferably, adopt SiH
4-C3H
8-H
2gas reaction system is prepared carborundum films on tin dioxide thin film, and THICKNESS CONTROL is between 50nm ~ 300nm.
The high radiating electrothermal membrane of a kind of bilayer being prepared from based on above method.
The present invention carries out after surface treatment different base, prepares different levels of doping Electric radiant Heating Film and has different heating radiation scope, and Different Red external radiation wave band is possessed to intensity selective power.The carborundum of the designed performance of tin ash Electric radiant Heating Film surface deposition plays stable electrical hotting mask performance simultaneously, has strengthened the radiation of middle-infrared band and has used safety, the further application of having expanded product.
Other features and advantages of the present invention will be set forth in the following description, and, partly from specification, become apparent, or understand by implementing the present invention.Object of the present invention and other advantages can be realized and be obtained by specifically noted structure in write specification, claims and accompanying drawing.
Brief description of the drawings
Below in conjunction with accompanying drawing, the present invention is described in detail, to make above-mentioned advantage of the present invention clearer and more definite.Wherein,
Fig. 1 is Electric radiant Heating Film structural representation in the preparation method of the double-deck high radiate electric heating membrane structure of the present invention;
Fig. 2 is that in the preparation method of the double-deck high radiate electric heating membrane structure of the present invention, Electric radiant Heating Film substrate surface is processed pattern schematic diagram;
Fig. 3 is that in the preparation method of the double-deck high radiate electric heating membrane structure of the present invention, Electric radiant Heating Film substrate surface is processed pattern schematic diagram;
Fig. 4 is that in the present invention, tin dioxide thin film is prepared APCVD equipment schematic diagram.
In diagram, 11 is Electric radiant Heating Film substrate, and 12 is tin ash doping film, and 13 is carborundum films, and 14 is wire; 21 is pyramid-like type surface, 22 substrates, and 23 is protruding umbilicate type surface, 24 is substrate; 1: flowmeter 2: electromagnetically operated valve 3: nitrogen 4: oxygen 5: tin Sn source 6: antimony Sb source 7: reaction hood 8: heating module 9: Electric radiant Heating Film substrate 10: delivery module 11: thermocouple 12: response controller.
Embodiment
Describe embodiments of the present invention in detail below with reference to drawings and Examples, to the present invention, how application technology means solve technical problem whereby, and the implementation procedure of reaching technique effect can fully understand and implement according to this.It should be noted that, only otherwise form conflict, each feature in each embodiment and each embodiment in the present invention can mutually combine, and the technical scheme forming is all within protection scope of the present invention.
embodiment mono-:
Specifically, method of the present invention mainly comprises the following steps:
A preparation method for the high radiate electric heating membrane structure of bilayer, comprising:
1) adopt potsherd or quartz glass as base material;
2) substrate material surface is carried out to etching processing, make substrate material surface present the suede surface of boss-shaped or pit shape;
3) on the suede surface of base material, deposit tin ash doping Electric radiant Heating Film;
4) depositing silicon carbide film on tin ash doping Electric radiant Heating Film;
5) remove the carborundum films layer of required welding electrode part, form electrode welding window, at this window welding electrothermal electrode.
Preferably, in step 1), prepare tin ash doping film based on aumospheric pressure cvd (APCVD) mode, its thickness is at 1.5mm ~ 7mm.
Preferably, in step 4), adopt CVD method at depositing silicon carbide film on tin ash doping Electric radiant Heating Film to prepare carborundum films.
Preferably, in step 4), before depositing silicon carbide film, oxygen gas plasma processing is carried out in the surface of tin ash doping Electric radiant Heating Film.
Preferably, step 2) in, use hydrofluoric acid to carry out etching processing to substrate material surface, make substrate surface present the suede surface of boss-shaped or pit shape;
Wherein, hydrofluoric acid concentration 1.5% ~ 10%, process treatment time 35s ~ 500s, the roughness of prepared substrate is controlled at 500nm ~ 50 μ m, the raised or sunken aspect ratio 1.5 ~ 8 of etching.
Preferably, in step 3), base material is through carrying out the deposition preparation of doping stannic oxide Electric radiant Heating Film after cleaning;
Base material cleaning process adopts ultrasonic clean cleaning, after deionized water ultrasonic cleaning, carries out substrate and is heated to 300 DEG C ~ 900 DEG C, carries out subsequently surperficial oxygen plasma cleaning;
After plasma cleaning, carry out the preparation of tin ash doping film, film thickness 300nm ~ 2000nm, doping weight ratio 1.8% ~ 9%.
Preferably, comprising: aumospheric pressure cvd legal system is for tin ash doping Electric radiant Heating Film and carborundum films layer.
Preferably, specifically comprise:
SnCl
2and SbCl
3n is all used in source
2do carrier gas, gasify at 90 DEG C ~ 130 DEG C and 70 DEG C ~ 100 DEG C respectively, 0
2as oxidant, N
2as diluent gas, be used for diluting reaction gaseous mixture, prepare thickness 300nm ~ 2000nm, doping weight ratio 1.8% ~ 9% tin ash doping Electric radiant Heating Film.
Preferably, adopt SiH
4-C3H
8-H
2gas reaction system is prepared carborundum films on tin dioxide thin film, and THICKNESS CONTROL is between 50nm ~ 300nm.
The present invention carries out after surface treatment different base, prepares different levels of doping Electric radiant Heating Film and has different heating radiation scope, and Different Red external radiation wave band is possessed to intensity selective power.The carborundum of the designed performance of tin ash Electric radiant Heating Film surface deposition plays stable electrical hotting mask performance simultaneously, has strengthened the radiation of middle-infrared band and has used safety, the further application of having expanded product.
embodiment bis-:
Specifically, in one embodiment, the present invention adopts substrate surface to present similar surfaces pattern in Fig. 2 and 3.
It mainly adopts hydrofluoric acid to carry out substrate material surface suede etch processes, hydrofluoric acid concentration 1.5% ~ 10%, process treatment time 35s ~ 500s.Roughness is controlled at 500nm ~ 50 μ m, the raised or sunken aspect ratio 1.5 ~ 8 of etching.
Suedeization substrate after treatment in surface is put into the deionized water for ultrasonic of 55 DEG C ~ 70 DEG C of temperature and is cleaned 1 ~ 2min, adopts 70 DEG C ~ 85 DEG C of air knives to dry up, and is then placed in 100 DEG C ~ 160 DEG C drying boxes dry.
And clean dry substrate is fixed on fixture, sends into film deposition equipment-aumospheric pressure cvd equipment (APCVD) and carries out the preparation of Electric radiant Heating Film.
Wherein, substrate, through device heating chamber chamber, makes base reservoir temperature rise to 300 DEG C ~ 900 DEG C, carries out oxygen plasma surface cleaning process under heating state, and substrate subsequently enters tin ash Electric radiant Heating Film preparation technology chamber, carries out the preparation of tin ash doping Electric radiant Heating Film.Preparation equipment schematic diagram as shown in Figure 4.
Wherein, precursor SnCl
2and SbCl
3all use N
2do carrier gas, gasify at 90 DEG C ~ 130 DEG C and 70 DEG C ~ 100 DEG C respectively.0
2as oxidant, N
2as diluent gas, be used for diluting reaction gaseous mixture.As the follow-up prioritization scheme of the present invention, adopt air to replace oxygen and nitrogen to reach the effect of oxidation and dilution.Bubbler and gas pipeline all have heating and heat-insulating device, and reaction gas temperature before entering reactor needs insulation.By regulating the flow velocity of carrier gas throughput and the temperature of bubbler, reach the object of controlling precursor consumption, substrate temperature is monitored by thermocouple, regulates the motor power (output) of conveyer belt to change substrate feed speed.Control technological parameter, carry out the preparation of tin ash doping film, thickness 300nm ~ 2000nm, doping weight ratio 1.8% ~ 9%.According to power designs, complete the preparation of different-thickness and doping ratio tin ash Electric radiant Heating Film.
In the present invention, silicon carbide semiconductor film adopts and is same as tin dioxide thin film Preparation equipment CVD and deposits.
Oxygen gas plasma processing is carried out on tin dioxide thin film surface, subsequently at tin dioxide thin film surface deposition one deck silicon carbide semiconductor film SiC.
SiH
4-C3H
8-H
2as gas reaction system, on tin dioxide thin film, prepare layer of semiconductor film SiC, thickness 50nm ~ 300nm by Films Prepared by APCVD (APCVD) technique.Flow process parameter control is SiH
4: 0.2L/min ~ 0.8L/min, C3H
8: 0.05L/min ~ 0.2L/min, H
2: 2L/min ~ 10L/min, flow control is carried out technological parameter adjustment according to different qualities Electric radiant Heating Film demand.
As the follow-up prioritization scheme of the present invention, adopt PECVD to carry out carborundum films preparation.
Adopt diamond dust polishing mode to remove the silicon carbide film layer of required welding electrode part, form electrode welding window, at this window welding electrothermal electrode.
It should be noted that, for said method embodiment, for simple description, therefore it is all expressed as to a series of combination of actions, but those skilled in the art should know, the application is not subject to the restriction of described sequence of movement, because according to the application, some step can adopt other orders or carry out simultaneously.Secondly, those skilled in the art also should know, the embodiment described in specification all belongs to preferred embodiment, and related action and module might not be that the application is necessary.
Finally it should be noted that: the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although the present invention is had been described in detail with reference to previous embodiment, for a person skilled in the art, its technical scheme that still can record aforementioned each embodiment is modified, or part technical characterictic is wherein equal to replacement.Within the spirit and principles in the present invention all, any amendment of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a preparation method for the high radiate electric heating membrane structure of bilayer, is characterized in that, comprising:
1) adopt potsherd or quartz glass as base material;
2) substrate material surface is carried out to etching processing, make substrate material surface present the suede surface of boss-shaped or pit shape;
3) on the suede surface of base material, deposit tin ash doping Electric radiant Heating Film;
4) depositing silicon carbide film on tin ash doping Electric radiant Heating Film;
5) remove the carborundum films layer of required welding electrode part, form electrode welding window, at this window welding electrothermal electrode.
2. the preparation method of the high radiate electric heating membrane structure of bilayer according to claim 1, is characterized in that, in step 1), prepares tin ash doping film based on aumospheric pressure cvd (APCVD) mode, and its thickness is at 1.5mm ~ 7mm.
3. the preparation method of the high radiate electric heating membrane structure of bilayer according to claim 1 and 2, is characterized in that, in step 4), adopt CVD method at depositing silicon carbide film on tin ash doping Electric radiant Heating Film to prepare carborundum films.
4. the preparation method of the high radiate electric heating membrane structure of bilayer according to claim 3, is characterized in that, in step 4), before depositing silicon carbide film, oxygen gas plasma processing is carried out in the surface of tin ash doping Electric radiant Heating Film.
5. the preparation method of the high radiate electric heating membrane structure of bilayer according to claim 1 and 2, is characterized in that step 2) in, use hydrofluoric acid to carry out etching processing to substrate material surface, make substrate surface present the suede surface of boss-shaped or pit shape;
Wherein, hydrofluoric acid concentration 1.5% ~ 10%, process treatment time 35s ~ 500s, the roughness of prepared substrate is controlled at 500nm ~ 50 μ m, the raised or sunken aspect ratio 1.5 ~ 8 of etching.
6. the preparation method of the high radiate electric heating membrane structure of bilayer according to claim 1 and 2, is characterized in that, in step 3), base material is through carrying out the deposition preparation of doping stannic oxide Electric radiant Heating Film after cleaning;
Base material cleaning process adopts ultrasonic clean cleaning, after deionized water ultrasonic cleaning, carries out substrate and is heated to 300 DEG C ~ 900 DEG C, carries out subsequently surperficial oxygen plasma cleaning;
After plasma cleaning, carry out the preparation of tin ash doping film, film thickness 300nm ~ 2000nm, doping weight ratio 1.8% ~ 9%.
7. the preparation method of the high radiate electric heating membrane structure of bilayer according to claim 6, is characterized in that, comprising: aumospheric pressure cvd legal system is for tin ash doping Electric radiant Heating Film and carborundum films layer.
8. the preparation method of the high radiate electric heating membrane structure of bilayer according to claim 7, is characterized in that, specifically comprises:
SnCl
2and SbCl
3n is all used in source
2do carrier gas, gasify at 90 DEG C ~ 130 DEG C and 70 DEG C ~ 100 DEG C respectively, O
2as oxidant, N
2as diluent gas, be used for diluting reaction gaseous mixture, prepare thickness 300nm ~ 2000nm, doping weight ratio 1.8% ~ 9% tin ash doping Electric radiant Heating Film.
9. the preparation method of the high radiate electric heating membrane structure of bilayer according to claim 7, is characterized in that, adopts SiH
4-C
3h
8-H
2gas reaction system is prepared carborundum films on tin dioxide thin film, and THICKNESS CONTROL is between 50nm ~ 300nm.
10. the high radiating electrothermal membrane of bilayer being prepared from based on claim 1 ~ 9 either method.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106684235A (en) * | 2015-11-09 | 2017-05-17 | 北京卫星环境工程研究所 | Porous structure of solar radiation power generation material used in space, device and manufacturing method |
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| CN1074579A (en) * | 1992-12-11 | 1993-07-21 | 戴金利 | A kind of semiconductor electric-heating thin film and processing method thereof |
| CN1174487A (en) * | 1996-08-21 | 1998-02-25 | 无锡市现代技术发展公司 | Production process of transparent electrothermic film element |
| CN1220570A (en) * | 1998-11-12 | 1999-06-23 | 马秀芝 | Method for making surface electric heating element with modified insulating base material surface |
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| CN101668359A (en) * | 2009-08-11 | 2010-03-10 | 罗日良 | Electrothermal film and manufacturing method thereof |
| CN102291860A (en) * | 2011-04-25 | 2011-12-21 | 马秀芝 | Method for manufacturing automatic temperature-limiting oxide electric-heating film |
| CN202425073U (en) * | 2011-11-14 | 2012-09-05 | 美亚奈米科技股份有限公司 | Heating assembly |
| 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 |
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2014
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Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS59213629A (en) * | 1983-05-19 | 1984-12-03 | Nippon Sheet Glass Co Ltd | Heating furnace |
| CN1033225A (en) * | 1988-11-26 | 1989-05-31 | 上海大华化轻工业公司 | Doped-semiconductor electrothermal film |
| CN1074579A (en) * | 1992-12-11 | 1993-07-21 | 戴金利 | A kind of semiconductor electric-heating thin film and processing method thereof |
| CN1174487A (en) * | 1996-08-21 | 1998-02-25 | 无锡市现代技术发展公司 | Production process of transparent electrothermic film element |
| CN1220570A (en) * | 1998-11-12 | 1999-06-23 | 马秀芝 | Method for making surface electric heating element with modified insulating base material surface |
| DE19852366A1 (en) * | 1998-11-13 | 2000-05-18 | Schott Glas | Low cost ceramic heat-conductive body for ceramic hobs or hot-plates has a surface layer with a specified planarity giving good aesthetic and cleaning properties |
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| CN102291860A (en) * | 2011-04-25 | 2011-12-21 | 马秀芝 | Method for manufacturing automatic temperature-limiting oxide electric-heating film |
| CN202425073U (en) * | 2011-11-14 | 2012-09-05 | 美亚奈米科技股份有限公司 | Heating assembly |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106684235A (en) * | 2015-11-09 | 2017-05-17 | 北京卫星环境工程研究所 | Porous structure of solar radiation power generation material used in space, device and manufacturing method |
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Application publication date: 20141008 |