WO2005055662A1 - Film chauffant electrique inorganique multifonction, a haute efficacite, resistant aux temperatures elevees, et son procede de production - Google Patents

Film chauffant electrique inorganique multifonction, a haute efficacite, resistant aux temperatures elevees, et son procede de production Download PDF

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Publication number
WO2005055662A1
WO2005055662A1 PCT/CN2004/001381 CN2004001381W WO2005055662A1 WO 2005055662 A1 WO2005055662 A1 WO 2005055662A1 CN 2004001381 W CN2004001381 W CN 2004001381W WO 2005055662 A1 WO2005055662 A1 WO 2005055662A1
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WO
WIPO (PCT)
Prior art keywords
carrier
film
temperature
electrothermal film
water
Prior art date
Application number
PCT/CN2004/001381
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English (en)
Chinese (zh)
Inventor
Jian Chen
Qingfa Hu
Original Assignee
Jian Chen
Qingfa Hu
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jian Chen, Qingfa Hu filed Critical Jian Chen
Publication of WO2005055662A1 publication Critical patent/WO2005055662A1/fr

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Classifications

    • 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01CRESISTORS
    • H01C17/00Apparatus or processes specially adapted for manufacturing resistors
    • H01C17/06Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base
    • H01C17/065Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base by thick film techniques, e.g. serigraphy
    • H01C17/06506Precursor compositions therefor, e.g. pastes, inks, glass frits
    • H01C17/06513Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the resistive component

Definitions

  • the present invention relates to an electric heating film, in particular to a high-temperature and high-efficiency multifunctional inorganic electric heating film and a manufacturing method thereof.
  • BACKGROUND As early as the 1950s, there were reports of Sn0 2 -Sb semiconductor electrothermal coatings abroad. In the 1970s and 1980s, China strengthened its research in this area. For example, Chinese patent applications Nos. 88108194, 89107751, 92106609, and other public documents recorded relevant discussions.
  • the components of the aforementioned electrothermal coatings mainly include an aqueous solution of stannous chloride (SnCl 2 * 2H 2 0) containing crystal water or tin tetrachloride (SnCl 4 * 5H 2 0) containing crystal water.
  • the raw material uses antimony trichloride (SbCl 3 ) as a doping substance, is hydrolyzed at high temperature, and is oxidized by water to obtain a Sn0 2 * Sb semiconductor electric heating film.
  • the semiconductor electrothermal film is provided with conductive properties. Due to the existence of a large number of unsaturated valence metal ions and oxygen vacancies in the fabricated semiconductor electrothermal film, their chemical structures are unstable and there is a tendency and possibility to continue to be oxidized, so When the fabricated semiconductor electrothermal film is used, these large amounts of unsaturated valence ions will gradually continue to be oxidized under high temperature conditions, which will cause the chemical structure of the semiconductor electrothermal film to change and cause thermal shock due to the high temperature. As a result, the electrothermal film is discarded; or these unsaturated valence ions are gradually oxidized, which gradually reduces the electrical conductivity of the electrothermal film and reduces the power density greatly, thereby losing the heating function.
  • the object of the present invention is to provide a high-temperature and high-efficiency multifunctional inorganic electric heating film and a manufacturing method thereof, so as to solve the disadvantages existing in the prior art.
  • the electric heating film of the present invention has the advantages of high thermal efficiency, high temperature resistance, dry burning, oxidation resistance, stable electrical conductivity, long life and many uses.
  • the object of the present invention is achieved according to the following technical scheme.
  • the invention is a high-temperature, high-efficiency, multifunctional, electromechanical-free thermal film, which is characterized in that it is composed of the following components by weight ratio:
  • the manufacturing method of the high-temperature and high-efficiency multifunctional inorganic electric heating film includes the following steps:
  • the carrier material is an insulating material, including quartz glass, borosilicate glass, microcrystalline glass, or ordinary glass.
  • the cleaning carrier is acid washing, water washing, deionized water washing, and absolute ethanol washing of the carrier; in the film forming in the step (4), the The dehumidification treatment includes water separation, filtration, fine filtration, and heating; when spraying, the preheating temperature of the compressed air is 30-50 ° C, and the air pressure is 0.02-0.05Mp a ; the preheating temperature of the carrier is 600- 800 ° C.
  • the main film-forming substance of the electrothermal film of the present invention is a metal oxide, so it is called an inorganic electrothermal film. Its main raw material is anhydrous SnCl 4 .
  • the present invention removes water or crystal water that is harmful in chemical reactions in order to prevent the generation of unsaturated valence ions during film formation at high temperature; High thermal efficiency, high temperature resistance, dry burning, anti-oxidation, stable conductivity and long life.
  • the film-forming principle of the present invention is different from that of a semiconductor electrothermal film, and raw materials and methods are also different.
  • the present invention adopts a redox reaction to prepare an Sn0 2 inorganic electrothermal film.
  • the reaction In the reaction, the interference of moisture is eliminated, and the deficiency of ions that generate unsaturated valence during film formation at high temperature is eliminated; the invention uses oxygen in the air to heat, so that the oxygen in the air is dissolved in anhydrous ethanol and sprayed into a mist
  • the shaped SnCl 4 particles react directly at high temperature to complete the reaction, and the reaction is completed in one step.
  • the reaction formula is: SnCl 4 + 0 2 ⁇ Sn0 2 + 2C1 2
  • the electrothermal film has certain transparency and has electrothermal conversion function, infrared radiation function, photoelectric conversion function, electro-optical display function, and reflected infrared light. Series features. There are also some metal oxides that have a clear role in forming a film together. They also do not contain impurities and are pure inorganic substances.
  • SbCl 3 is used as the resistance value modifier, InCl 3 is used as the high-temperature stabilizer, and BiCl 3 is used as the resistance-value stabilizer to enhance the resistance value stability at high temperature; MnCl 2 and NiCl 2 are anti-aging and stable MnCl 2 and NiCl 2 are additives to improve the infrared radiation and reflection function of the inorganic electrothermal film. The high temperature stability of the product is guaranteed from the formula.
  • the main measures in the process are:
  • the compressed air used for spray film formation does not contain moisture and impurities, so as to prevent the unsaturated valence ions from remaining in the electrothermal film.
  • the non-electromechanical thermal film achieves high thermal efficiency, high temperature resistance, dry burning, oxidation resistance, stable electrical conductivity, and improved life.
  • the inorganic electrothermal film of the present invention has higher visible light transmittance, higher hardness, higher surface smoothness, and metallic luster than the semiconductor electrothermal film, and does not require annealing treatment after film formation, which is successful in one time and improves productivity.
  • the inorganic electrothermal film of the present invention can be used as a high-temperature heating electrothermal film, and can also be used as a photoelectric conversion film of a solar cell. After adding components, it can also be made into an infrared radiation electrothermal film and a conductive glass for a liquid crystal electro-optic display, which has a wide range of uses.
  • FIG. 1 is a temperature rise performance curve graph of an inorganic electrothermal film of the present invention and a prior art semiconductor electrothermal film.
  • DETAILED DESCRIPTION Example 1 To produce a high-temperature and high-efficiency multifunctional inorganic electric heating film.
  • Composition It is composed of the following components by weight (unit: gram):
  • the SnCl 4 used is an anhydrous tin tetrachloride colorless and transparent liquid. The remaining components do not contain water and crystal water, and deionized water cannot be added as a solvent to dilute the film application solution.
  • Each of the components is analytically pure with chemical reagents.
  • the method in this embodiment is a method for manufacturing an inorganic electrothermal film for dry firing heating, and includes the following 1. Prepare the materials, prepare the components of the inorganic electrothermal film according to the group, and prepare the electrothermal film carrier; the electrothermal film carrier adopts high temperature resistant and low linear expansion coefficient insulating material, and quartz glass is selected in this embodiment. tube,
  • composition It consists of the following components by weight (unit: gram):
  • the electrothermal film carrier is selected as a quartz glass plate
  • the compressed air needs to be dehumidified before use; the dehumidification process includes water separation, filtration, fine filtration, heating and dehumidification operations; during spraying, the compressed air
  • the pressure is 0.03Mp a ; the preheating temperature of compressed air is 40 ° C; the preheating temperature of the carrier is 630 ° C; the electric heating film made according to the embodiment 1 of the present invention can be used for dry-baking heating, and is suitable for 3-220V AC or DC power supply, the power density can be 0.1- 40W / cm 2 , the heating speed is extremely fast, the thermal inertia is very small, the dry life at 600 ° C, the service life is more than 8000 hours, the resistance has not changed for
  • Figure 1 is a graph of the temperature rise performance of the inorganic electrothermal film of the present invention and the prior art electrothermal film.
  • curve 1 is the measured heating state of the Sn0 2 inorganic electrothermal film of the present invention. Its power density is 30W / C m 2 , the heating rate is extremely fast, and the highest is 100CTC (non-working state).
  • No. Curve 2 is the measured heating state of the Sn0 2 inorganic electrothermal film of the present invention. Its power density is 10W / cm 2 , and the heating rate is very fast.
  • the highest temperature can be more than 800 ° C, and the working range is 600- 800 ° C, at 600 ° C. When used, the service life is greater than 8000 hours.
  • Curve 3 is the heating state of the prior art Sn0 2 -Sb semiconductor electrothermal film with a power density of lOW / cm 2 , and the heating rate is relatively fast, up to 600 ° C, and the operating temperature range is 400-600 ° C, at 400 ° ⁇ When used, the life is more than 3000 hours.
  • Curve 4 is the heating state of the PTC inorganic ceramic electrothermal film (0.2 mil thick film, opaque) in the prior art.
  • the power density is 5W / cm 2 , which is a typical representative of the inorganic thick film.
  • the operating temperature is 200 300 ° C. When the working temperature is 200 ° C, it can be used.
  • the life is more than 2000 hours.
  • Curve 5 is a good-quality organic electrothermal film, with a maximum temperature of 200 ° C, an operating temperature of 80-150 ° C, and a working life of more than 2000 hours at 80 ° C. As can be seen, the performance of electric inorganic Sn0 2 film of the invention is significantly better than the prior art electric membrane.

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Surface Treatment Of Glass (AREA)
  • Formation Of Insulating Films (AREA)

Abstract

L'invention concerne un film chauffant électrique inorganique multifonction, à haute efficacité, résistant aux températures élevées, comprenant (en % en poids):SnCl4: 400-500; InCl3: 60-100; SbCl3: 10-30; MnCl2: 1-5; BiCl3: 1-5; NiCl2: 1-5; C2H5OH: 400-600; C3H5(OH)3: 60-120. Cette composition ne contient pas d'eau, y compris sous forme cristalline. Il importe de ne pas d'ajouter d'eau déionisée comme solvant. Les matières premières utilisées dans cette composition sont analytiquement pures. Par rapport à l'art antérieur, le film selon l'invention présente les avantages suivants: rendement thermique élevé, résistance aux températures élevées, résistance à l'oxydation, conductivité stable, longévité et polyvalence.
PCT/CN2004/001381 2003-12-02 2004-11-30 Film chauffant electrique inorganique multifonction, a haute efficacite, resistant aux temperatures elevees, et son procede de production WO2005055662A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CNB2003101171358A CN100426936C (zh) 2003-12-02 2003-12-02 一种耐高温无机电热膜及其制作方法
CN200310117135.8 2003-12-02

Publications (1)

Publication Number Publication Date
WO2005055662A1 true WO2005055662A1 (fr) 2005-06-16

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Country Status (2)

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CN (1) CN100426936C (fr)
WO (1) WO2005055662A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108882410A (zh) * 2018-08-02 2018-11-23 青岛在宇工贸有限公司 一种石墨烯远红外电热膜自动化生产设备

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102843793B (zh) * 2011-06-24 2015-05-20 北京万众光通科技发展有限公司 一种电热转换体涂层及使用方法
SG11201605692WA (en) 2014-01-16 2016-08-30 Sony Corp Audio processing device and method, and program therefor
CN104529182A (zh) * 2014-11-26 2015-04-22 山西长生伟业热能科技有限公司 一种普通电热玻璃的制备方法
CN106793195B (zh) * 2017-02-24 2020-01-07 江苏一森电采暖科技有限公司 长寿命电热元件及其制备方法
CN109246871A (zh) * 2018-09-07 2019-01-18 南京运膜科技有限公司 一种电热膜施膜液、及电热膜的制备方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1074579A (zh) * 1992-12-11 1993-07-21 戴金利 一种半导体电热薄膜及其加工方法
EP0654956A1 (fr) * 1993-11-24 1995-05-24 U'LAMP ENTERPRISES Co., Ltd. Méthode de fabrication d'une couche chauffée électriquement
CN1136263A (zh) * 1996-03-12 1996-11-20 尹维平 无机氧化物电热薄膜及其制法

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* Cited by examiner, † Cited by third party
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CN1033225A (zh) * 1988-11-26 1989-05-31 上海大华化轻工业公司 掺杂半导体电热膜
CN1036432C (zh) * 1992-07-09 1997-11-12 连铁军 一种耐高温透明电热膜及其生产方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1074579A (zh) * 1992-12-11 1993-07-21 戴金利 一种半导体电热薄膜及其加工方法
EP0654956A1 (fr) * 1993-11-24 1995-05-24 U'LAMP ENTERPRISES Co., Ltd. Méthode de fabrication d'une couche chauffée électriquement
CN1136263A (zh) * 1996-03-12 1996-11-20 尹维平 无机氧化物电热薄膜及其制法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108882410A (zh) * 2018-08-02 2018-11-23 青岛在宇工贸有限公司 一种石墨烯远红外电热膜自动化生产设备

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CN1625305A (zh) 2005-06-08
CN100426936C (zh) 2008-10-15

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