CN105744661A - Preparation method of semiconductor electrothermal film - Google Patents

Preparation method of semiconductor electrothermal film Download PDF

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Publication number
CN105744661A
CN105744661A CN201610087088.4A CN201610087088A CN105744661A CN 105744661 A CN105744661 A CN 105744661A CN 201610087088 A CN201610087088 A CN 201610087088A CN 105744661 A CN105744661 A CN 105744661A
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substrate
semiconductor thermoelectric
preparation
thermoelectric film
film
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顾伟
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    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • H05B3/20Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
    • H05B3/34Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater flexible, e.g. heating nets or webs
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • H05B3/10Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/12Heating 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
    • H05B3/14Heating 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
    • H05B3/141Conductive ceramics, e.g. metal oxides, metal carbides, barium titanate, ferrites, zirconia, vitrous compounds
    • H05B3/143Conductive ceramics, e.g. metal oxides, metal carbides, barium titanate, ferrites, zirconia, vitrous compounds applied to semiconductors, e.g. wafers heating
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2203/00Aspects relating to Ohmic resistive heating covered by group H05B3/00
    • H05B2203/013Heaters using resistive films or coatings
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2203/00Aspects relating to Ohmic resistive heating covered by group H05B3/00
    • H05B2203/017Manufacturing methods or apparatus for heaters

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)

Abstract

The invention relates to a preparation method of a semiconductor electrothermal film. The method mainly comprises the following steps: cleaning a substrate; preparing a source solution, wherein the source solution is prepared from the following components in parts by weight: 20-30 parts of stannic chloride, 10-30 parts of graphite, 10-20 parts of antimony trichloride and the like; spraying the substrate; carrying out first thermal treatment; carrying out dipping for film formation; and carrying out second thermal treatment. The semiconductor electrothermal film prepared according to the preparation method has relatively high adhesive force on the substrate and is over 190N; the leakage current is smaller than 0.10mA; the electrothermal conversion efficiency is greater than or equal to 99%; the square resistance is 45-400ohm/square; and the lifetime is over 5,000 hours.

Description

A kind of preparation method of semiconductor thermoelectric film
Technical field
The invention belongs to Electric radiant Heating Film field, particularly relate to the preparation method of a kind of semiconductor thermoelectric film.
Background technology
In recent years, tradition thermo electric material because consumable quantity is big, service life is short, shape difficulty, operating mode is unstable etc., and shortcoming is gradually replaced by new electrically heating material.Wherein, semiconductor thermoelectric film, owing to can closely combine on dielectric surfaces, the film like semi-conductive heating substance of planar thermal source is become after energising, there is the features such as fusing point is high, hardness is big, resistance is low, the thermal efficiency is high, chemical stability is good, the most resistance to bronsted lowry acids and bases bronsted lowry, the characteristic of the flames of anger in heating process, it is subject to people's attention in electric heating field, becomes the important materials replacing tradition thermo electric material.
Chinese patent CN201210250016.9 discloses a kind of method for manufacturing semiconductor electric heating membrane, and it mainly uses butter of tin, titanium tetrachloride, titanous chloride., Butter of antimony., ethanol to be that raw material passes through spraying plating, annealing, electrode sintering prepare semiconductor thermoelectric film.Being similar to, patent CN201310099190.2 also discloses a kind of method for manufacturing semiconductor electric heating membrane, its mainly by configure Electric radiant Heating Film treatment fluid, base mask, spray, anneal, electrode sintering preparation Electric radiant Heating Film.
Patent CN201510683050.9 discloses a kind of precursor solution for preparing semiconductor thermoelectric film, include by weight: butter of tin 25 ~ 45, nano-stannic oxide 5 ~ 25, Butter of antimony. 1 ~ 6, Fluohydric acid. 0.5 ~ 4, boric acid 0.1 ~ 1.5, potassium chloride 0.3 ~ 0.5, triethanolamine 0.2 ~ 0.8, solvent 20 ~ 60.And obtain, by spraying process, dipping film formation step, heat treatment step, the Electric radiant Heating Film that a kind of square resistance adjustable extent is bigger, although improve the adhesion of Electric radiant Heating Film and substrate, and the stability of operating resistance to a certain extent, but still need to be improved further.Additionally, patent CN201510638248.5 also discloses a kind of preparation method for preparing semiconductor thermoelectric film, selecting Pyrex, quartz glass, devitrified glass is base material, with butter of tin, titanium tetrachloride, Butter of antimony., titanous chloride., surplus dehydrated alcohol is stock;Being placed in heating cavity, temperature controls at 600-620 DEG C, by nozzle by source solution atomization the substrate surface that is sprayed onto in heating cavity, the base material being coated with Electric radiant Heating Film is carried out resistance test;The two ends of base material coated surface are uniformly coated with silver electrode paste;Then heating prepares semiconductor thermoelectric film.
The electrothermal semiconductor membrane preparation method of prior art still suffers from techniques below problem: the Electric radiant Heating Film stability of preparation is not enough, and Electric radiant Heating Film is combined defective tightness with substrate, easily ftractures or come off under external force or thermal stress effect;Square resistance controls difficulty;The defects such as leakage current is bigger.
Summary of the invention
It is desirable to provide a kind of method that can prepare high stability Electric radiant Heating Film, meanwhile, the semiconductor thermoelectric film leakage current obtained by the method is low, and electric conversion efficiency is high;Further, the semiconductor thermoelectric film square resistance adjustable extent being prepared by the method for the present invention is big and easily controllable, thus, the method for the present invention is particularly suitable for preparing the semiconductor thermoelectric film of different square resistance.
The present invention solves the problems referred to above by following electrothermal semiconductor membrane preparation method:
(1) substrate is cleaned: cleaned up by substrate distilled water, dry stand-by;
(2) preparation source solution: weigh following parts by weight of component, after mixing, be heated to 40-80 DEG C, stirring 1-2h, obtains semiconductor thermoelectric film source solution: butter of tin 20-30 part, graphite 10-30 part, Butter of antimony. 10-20 part, titanium tetrachloride 2-8 part, fluoboric acid 0.6-1.5 part, fuller olefinic carbon 60 .1-0.8 part, sodium chloride 0.3-0.5 part, water 1-3 part, toluene 2-4 part, ethanol 30-50 part;
(3) spraying substrate: the substrate of step (1) is placed in heating cavity, control heating cavity temperature in the range of 400-600 DEG C, treat that substrate surface temperatures reaches 300-500 DEG C, the semiconductor thermoelectric film source solution atomization of gained in step (2) is sprayed into substrate surface;
(4) heat treatment for the first time: the substrate of heating intracavity is heated to 600-800 DEG C, keeps 1-2h;Then, take out substrate, naturally cool to 300-450 DEG C;
(5) dipping film forming: will be in the semiconductor thermoelectric film source solution of step (2) gained is immersed in the substrate that step (4) process, pulling film forming;
(6) heat treatment for the second time: the substrate heat treatment 30-60min at 900-1000 DEG C after step (5) being processed, naturally cools to room temperature, it is thus achieved that semiconductor thermoelectric film.
As preferred scheme, the component of step (2) preparation source solution is made up of following: butter of tin 20-25 part, graphite 12-25 part, Butter of antimony. 10-15 part, titanium tetrachloride 4-6 part, fluoboric acid 0.8-1.2 part, fuller olefinic carbon 60 .2-0.6 part, sodium chloride 0.3-0.5 part, water 1-3 part, toluene 2-4 part, ethanol 30-50 part.
It is further preferred that substrate is heated to surface temperature by step (3) reaches 350-450 DEG C, then spray.
Further, it is preferable to the expulsion pressure that step (3) sprays is 8 ~ 15kpa, injection flow is 3 ~ 8ml/s.
Preferentially, step (4) heat treatment for the first time, the substrate of heating intracavity is heated to 600-700 DEG C, keeps 1-2h, be subsequently cooled to 350-400 DEG C.
Further, the pulling film forming condition of the inventive method is: 50-100mm/min.
Titanium tetrachloride in film-forming components of the present invention is conducive to improving the electric property of thin film, and fluoboric acid can strengthen the electrothermal semiconductor membrane coat permeability to insulating matrix material, improves the adhesion of electrothermal semiconductor membrane coat and base material so that it is be not easy breakage or come off.
Wherein, graphite usually makes the electric conversion of coating keep stable, prevent the rapid decay of its electric thermal power, and make coating surface can reach certain hardness, and in the present invention, inventor finds the consumption by regulating graphite, achieve the regulation to square resistance unexpectedly, can adjust by adjusting the consumption of graphite according to the reality needs to square resistance sizes.
Wherein, Butter of antimony. can improve the stability of electrothermal semiconductor membrane coat, improves its aging-resistant ability further, reaches the purpose increased the service life.
The present invention uses secondary heat treatment, can be effectively improved the adhesive force of Electric radiant Heating Film and substrate, improve the stability of Electric radiant Heating Film simultaneously, significantly reduce the rate of change of Electric radiant Heating Film in use resistance.
Prepared according to the methods of the invention semiconductor thermoelectric film adhesive force on base material is less than 0.10mA at more than 190N, leakage current, and electric conversion efficiency is more than or equal to 99%, and square resistance is 45-400 Ω/, and the life-span is more than 5000 hours.
Compared to prior art, the method for the present invention possesses following beneficial effect:
(1) the electrothermal semiconductor membrane preparation method of the present invention, have employed secondary heat treatment, is found to the adhesive force significantly improving Electric radiant Heating Film with substrate, can reach more than 190N, improve its stability simultaneously, resistance change rate is little, work has no inefficacy in more than 5000 hours continuously, is hardly damaged.
(2) present invention is by adding graphite and appropriate Graphene in the composition of semiconductor thermoelectric film so that the semiconductor thermoelectric film leakage current of the application is minimum, and makes its electric conversion keep stable, prevents the rapid decay of its electric thermal power;And can adjust by adjusting the consumption of graphite according to the reality needs to square resistance sizes.
Detailed description of the invention
For making technical scheme and technique effect thereof clearer, clear and definite, enumerate example below and the specific embodiment of the invention is further described by comparative example, but be not intended to limit the present invention.
The substrate that the present invention uses is quartz and prepares semiconductor thermoelectric film:
Embodiment 1
(1) substrate is cleaned: cleaned up by substrate distilled water, dry stand-by;
(2) preparation source solution: weigh following parts by weight of component, after mixing, be heated to 50 DEG C, stirring 1-2h, obtains semiconductor thermoelectric film source solution: butter of tin 22 parts, 15 parts of graphite, Butter of antimony. 10 parts, titanium tetrachloride 6 parts, fluoboric acid 1.0 parts, fuller olefinic carbon 60 .4 part, 0.5 part of sodium chloride, 1 part of water, toluene 4 parts, ethanol 45 parts;
(3) spraying substrate: the substrate of step (1) is placed in heating cavity, control heating cavity temperature in the range of 450-500 DEG C, treat that substrate surface temperatures reaches about 350 DEG C, start the semiconductor thermoelectric film source solution atomization of gained in step (2) is sprayed into substrate surface;
(4) heat treatment for the first time: the substrate of heating intracavity is heated to 650-700 DEG C, keeps 1.5h;Then, take out substrate, naturally cool to 380 DEG C
(5) dipping film forming: will be in the semiconductor thermoelectric film source solution of step (2) gained is immersed in the substrate that step (4) process, pulling film forming, pulling film forming condition is: 50mm/min;
(6) heat treatment for the second time: the substrate heat treatment 60min at 900-950 DEG C after step (5) being processed, naturally cools to room temperature, it is thus achieved that semiconductor thermoelectric film.
Embodiment 2
(1) substrate is cleaned: cleaned up by substrate distilled water, dry stand-by;
(2) preparation source solution: weigh following parts by weight of component, after mixing, be heated to 75 DEG C, stirring 2h, obtains semiconductor thermoelectric film source solution: butter of tin 25 parts, 20 parts of graphite, Butter of antimony. 13 parts, titanium tetrachloride 4 parts, fluoboric acid 0.9 part, fuller olefinic carbon 60 .6 part, 0.3 part of sodium chloride, 3 parts of water, toluene 2 parts, ethanol 35 parts;
(3) spraying substrate: the substrate of step (1) is placed in heating cavity, control heating cavity temperature in the range of 500-550 DEG C, treat that substrate surface temperatures reaches about 400 DEG C, start the semiconductor thermoelectric film source solution atomization of gained in step (2) is sprayed into substrate surface;
(4) heat treatment for the first time: the substrate of heating intracavity is heated to 650-700 DEG C, keeps 1.5h;Then, take out substrate, naturally cool to 350 DEG C
(5) dipping film forming: will be in the semiconductor thermoelectric film source solution of step (2) gained is immersed in the substrate that step (4) process, pulling film forming, pulling film forming condition is: 100mm/min;
(6) heat treatment for the second time: the substrate heat treatment 30min at 950-1000 DEG C after step (5) being processed, naturally cools to room temperature, it is thus achieved that semiconductor thermoelectric film.
After comparative example 1: omitting step (4), remaining operation is same as in Example 1, i.e. step (3) spraying, do not carry out heat treatment for the first time, be directly entered step (5).
After comparative example 2: omitting step (4), remaining operation is same as in Example 2, i.e. step (3) spraying, do not carry out heat treatment for the first time, be directly entered step (5).
The performance test of semiconductor thermoelectric film:
(1) adhesive force test is carried out according to the related request of country machinery industry standard JB/T 8,554 1997 " vapor deposition film and the scratch method for test of matrix adhesive force ".Using the WS-2005 automatic scratching instrument of type coating adhesion to test, method of testing is: acoustic emission metering system is tested.Loading speed 5N/min, cut speed 2mm/min, result sees table 1
(2) other tests: the performance tests such as film thickness, square resistance, leakage current all use traditional test methods.Wherein square resistance: Rs=ρ/t (wherein ρ is the resistivity of bulk, and t is bulk thickness) or write as the expression formula of electrical conductivity: Rs=1/ (σ t), result sees table 1
(3) resistance change rate: operating temperature is resistance change rate A% at room temperature to 1500 DEG C;Resistance change rate B% after working 5000 hours, result sees table 1
(4) the examination graphite levels impact on Electric radiant Heating Film square resistance, with embodiment 1 for examination object, is changed the graphite levels in embodiment 1, other components unchanged, preparing different semiconductor thermoelectric films by identical preparation method, test its square resistance, result sees table 2.
Table 1. embodiment 1-2 and comparative example 1-2 Specifeca tion speeification test result
The impact on Electric radiant Heating Film square resistance of table 2 graphite levels
As can be seen from Table 1, this invention takes method unlike the prior art, pass through secondary heat treatment, before pulling film forming, i.e. carry out a heat treatment, the adhesion of electric-heating thin film and base material can be effectively improved, in the case of thickness about 0.6 μm, adhesive force all at more than 190N, considerably improves the ability of anti-thermal shock;And the resistance change rate that heats up, long-term work resistance change rate the most effectively decline.From table 2 it can be seen that the square resistance of the semiconductor thermoelectric film of the present invention has large range of square resistance, and can be adjusted by regulation graphite levels so that it is can be adjusted easily according to actual needs.
Although present invention has been a certain degree of description, it will be apparent that, without departing from the spirit and scope of the present invention, can carry out the suitable change of each condition.Being appreciated that and the invention is not restricted to described embodiment, and be attributed to the scope of claim, it includes the equivalent of described each factor.

Claims (6)

1. the preparation method of a semiconductor thermoelectric film, it is characterised in that comprise the following steps:
(1) substrate is cleaned: cleaned up by substrate distilled water, dry stand-by;
(2) preparation source solution: weigh following parts by weight of component, after mixing, be heated to 40-80 DEG C, stirring 1-2h, obtains semiconductor thermoelectric film source solution: butter of tin 20-30 part, graphite 10-30 part, Butter of antimony. 10-20 part, titanium tetrachloride 2-8 part, fluoboric acid 0.6-1.5 part, fuller olefinic carbon 60 .1-0.8 part, sodium chloride 0.3-0.5 part, water 1-3 part, toluene 2-4 part, ethanol 30-50 part;
(3) spraying substrate: the substrate of step (1) is placed in heating cavity, control heating cavity temperature in the range of 400-600 DEG C, treat that substrate surface temperatures reaches 300-500 DEG C, the semiconductor thermoelectric film source solution atomization of gained in step (2) is sprayed into substrate surface;
(4) heat treatment for the first time: the substrate of heating intracavity is heated to 600-800 DEG C, it is preferable that be heated to 600-700 DEG C, keeps 1-2h;Then, take out substrate, naturally cool to 300-450 DEG C, it is preferable that be cooled to 350-400 DEG C
(5) dipping film forming: will be in the semiconductor thermoelectric film source solution of step (2) gained is immersed in the substrate that step (4) process, pulling film forming, pulling film forming condition is: 50-100mm/min;
(6) heat treatment for the second time: the substrate heat treatment 30-60min at 900-1000 DEG C after step (5) being processed, naturally cools to room temperature, it is thus achieved that semiconductor thermoelectric film.
The preparation method of semiconductor thermoelectric film the most according to claim 1, it is characterized in that, the component of described step (2) preparation source solution is made up of following: butter of tin 20-25 part, graphite 12-25 part, Butter of antimony. 10-15 part, titanium tetrachloride 4-6 part, fluoboric acid 0.8-1.2 part, fuller olefinic carbon 60 .2-0.6 part, sodium chloride 0.3-0.5 part, water 1-3 part, toluene 2-4 part, ethanol 30-50 part.
The preparation method of semiconductor thermoelectric film the most according to claim 1 or claim 2, it is characterised in that in step (3), substrate is heated to surface temperature and reaches 350-450 DEG C, then spray.
4., according to the preparation method of semiconductor thermoelectric film described in claim 1-3, it is characterised in that the expulsion pressure that step (3) sprays is 8 ~ 15kpa, injection flow is 3 ~ 8ml/s.
5., according to the preparation method of semiconductor thermoelectric film described in claim 1-4, it is characterised in that the substrate of heating intracavity is heated to 600-700 DEG C by step (4) heat treatment for the first time, keep 1-2h, be subsequently cooled to 350-400 DEG C.
6., according to the preparation method of semiconductor thermoelectric film described in claim 1-5, it is characterised in that the square resistance of described semiconductor thermoelectric film is 45-400 Ω/, leakage current is less than 0.1mA, and semiconductor thermoelectric film adhesive force on base material is at more than 190N.
CN201610087088.4A 2016-02-16 2016-02-16 Preparation method of semiconductor electrothermal film Pending CN105744661A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107172727A (en) * 2017-05-31 2017-09-15 广西泰亿诺新能源有限公司 Nano electroheating film film liquid is formulated and preparation method and the preparation method of electrothermal tube
CN107682944A (en) * 2017-10-24 2018-02-09 张东升 A kind of semiconductor thermoelectric film and preparation method thereof
CN110028895A (en) * 2019-04-30 2019-07-19 蔡国宇 A kind of preparation method of high conversion efficiency Electric radiant Heating Film

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1671254A (en) * 2005-02-07 2005-09-21 杨葆华 A formulation of semiconductor surface electrothermal coat and making method thereof
CN101668359A (en) * 2009-08-11 2010-03-10 罗日良 Electrothermal film and manufacturing method thereof
CN105142250A (en) * 2015-10-07 2015-12-09 江苏江汉电热设备科技有限公司 Preparation method for semiconductor thermoelectric film
CN105228273A (en) * 2015-10-21 2016-01-06 江苏江汉电热设备科技有限公司 For the preparation of the precursor solution of semiconductor thermoelectric film, Electric radiant Heating Film and preparation method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1671254A (en) * 2005-02-07 2005-09-21 杨葆华 A formulation of semiconductor surface electrothermal coat and making method thereof
CN101668359A (en) * 2009-08-11 2010-03-10 罗日良 Electrothermal film and manufacturing method thereof
CN105142250A (en) * 2015-10-07 2015-12-09 江苏江汉电热设备科技有限公司 Preparation method for semiconductor thermoelectric film
CN105228273A (en) * 2015-10-21 2016-01-06 江苏江汉电热设备科技有限公司 For the preparation of the precursor solution of semiconductor thermoelectric film, Electric radiant Heating Film and preparation method

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107172727A (en) * 2017-05-31 2017-09-15 广西泰亿诺新能源有限公司 Nano electroheating film film liquid is formulated and preparation method and the preparation method of electrothermal tube
CN107682944A (en) * 2017-10-24 2018-02-09 张东升 A kind of semiconductor thermoelectric film and preparation method thereof
CN110028895A (en) * 2019-04-30 2019-07-19 蔡国宇 A kind of preparation method of high conversion efficiency Electric radiant Heating Film

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Application publication date: 20160706