CN1092390C - Sol-gel process for preparing thermosensitive film resistor with negative temp. coefficient - Google Patents
Sol-gel process for preparing thermosensitive film resistor with negative temp. coefficient Download PDFInfo
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- CN1092390C CN1092390C CN98123522A CN98123522A CN1092390C CN 1092390 C CN1092390 C CN 1092390C CN 98123522 A CN98123522 A CN 98123522A CN 98123522 A CN98123522 A CN 98123522A CN 1092390 C CN1092390 C CN 1092390C
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Abstract
The present invention relates to a sol-gel process for preparing a thermosensitive film resistor with negative temperature coefficients. Firstly, acetate or nitrate of transition metal, such as manganese, cobalt, nickel and copper is dissolved in solvent, and a chelating agent is added and is used as initial solution. Then, the solution is stably placed; a well washed base plate is immersed into the solution and is lifted and pulled to the air; after the well washed base plate is dried, the well washed base is baked, and the process is repeated. Accordingly, thin films with the required thickness can be obtained; annealing and crystallization are carried out under high temperature, and the electrode plating, the scribing, the welding of lead wires, and the final encapsulation of the burnt thin film materials are carried out. The method has the advantages of simple manufacture and high stability, and the present invention can be widely applied to the fields of quick monitoring of the temperature, temperature compensation, surface temperature measurement, integrated temperature sensors, etc.
Description
The present invention relates to a kind of sol-gel method for preparing thin-film thermistor
Transition metal oxide such as manganese, cobalt, nickel, copper etc. mix by a certain percentage, behind forming and sintering, enable to obtain to have the semiconductive ceramic of very big temperature coefficient.With the thermistor stable performance that this semiconductive ceramic is made, the operation temperature area of broad is arranged, can be widely used in thermometric, temperature control, compensation, flow velocity measurement and the time delay circuit.Thin-film thermistor receives publicity because of it has that size is little, reaction speed is fast, be easy to resistance trimming, be easy to advantage such as integrated.At present, about thin-film thermistor more report and patent are arranged abroad, its preparation method includes evaporation, sputter, chemical vapour deposition (CVD).
The object of the invention has been to provide a kind of sol-gel method for preparing the negative temperature coefficient thin-film thermistor, be that acetate or nitrate with manganese, cobalt, nickel, copper transition metal is dissolved in the solvent, and interpolation chelating agent, as the solution that sets out, then this solution is placed stable, to clean clean substrate again immerses in the solution, lift 450 ℃ of bakings to the air drying, repeat this process, needing can obtain the film of thickness, the crystallization of annealing again, with the thin-film material plated electrode that burns till, scribing, solder taul to encapsulation.This manufacture method is simple, and good stability can be widely used in fields such as quick observing and controlling temperature, temperature-compensating, surface temperature measurement, integrated temperature sensor.
A kind of sol-gel method for preparing the negative temperature coefficient thin-film thermistor of the present invention, at first with manganese, cobalt or except cobalt, add nickel outside the manganese again, a kind of ratio in the copper is mol ratio (2-6): (1-2): the acetate of transition metal (0-3) or nitrate are dissolved in the solvent, and interpolation chelating agent, as the solution that sets out, then this solution is placed stable, solution concentration is 0.1-0.5M, pH value is 2-6, to clean clean substrate again immerses in the solution, lift 450 ℃ of bakings to the air drying, repeat this process, needing can obtain the film of thickness, again 500-700 ℃ of annealing crystallization, with the thin-film material plated electrode that burns till, scribing, solder taul is to encapsulation; Solvent is the alcohol of ethanol or methyl alcohol or isopropyl alcohol or butanols and acetate or glacial acetic acid or acetone and the mixed liquor of acid, and alcohol is 2-10 with the volume ratio of acid; Substrate is slide or quartz base plate; Chelating agent is acetylacetone,2,4-pentanedione or trifluoroacetylacetone (TFA) or ethanedioic acid or ethylenediamine two acetic acid, and its addition is that the mol ratio of chelating agent and salt is 1-4.
Further describe and provide embodiment below in conjunction with accompanying drawing
Fig. 1 is the coefficient thin-film thermistor structural representation of subzero temperature of the present invention
Fig. 2 is resistance-temperature relation figure of embodiment 1
Fig. 3 is resistance-temperature relation figure of embodiment 2
Fig. 4 is resistance-temperature relation figure of embodiment 3
Electrode (1) among Fig. 1 wherein, negative temperature coefficient film (2), substrate (3).
Embodiment 1:
With cobalt acetate, manganese nitrate, the nickel nitrate mol ratio is to be dissolved in ethanol at 3: 2: 1, acetate, in the mixed solvent of glacial acetic acid, and adding chelating agent acetylacetone,2,4-pentanedione stirs, this solution is placed stable, its solution concentration is 0.1M, again slide or the quartz base plate of cleaning immersed in this solution, speed with 4cm/s lifts to air drying, 450 ℃ of bakings down, repeat this process, needing can obtain the film of thickness, the crystallization of annealing under 500 ℃ temperature then is with the material plated electrode that burns till, electrode spacing 0.5mm, film thickness is 1100nm, scribing, solder taul gets final product to encapsulation, and Fig. 2 resistance of sample-temperature relation Figure 25 ℃ resistance for this reason is about 700K, and material constant is 3070.
Embodiment 2:
With cobalt acetate, the manganese acetate mol ratio is to be dissolved in methyl alcohol at 2: 1, acetate, in the mixed solvent of glacial acetic acid, and adding chelating agent trifluoroacetylacetone (TFA) stirs, this solution is placed stable, its solution concentration is 0.2M, again slide or the quartz base plate of cleaning immersed in this solution, speed with 4cm/s lifts to air drying, 450 ℃ of bakings down, repeat this process, needing can obtain the film of thickness, the crystallization of annealing under 600 ℃ temperature is with the material plated electrode that burns till, electrode spacing 0.5mm, film thickness is 1100nm, scribing, solder taul gets final product to encapsulation, and Fig. 3 resistance of sample-temperature relation Figure 25 ℃ resistance for this reason is about 4785K, and material constant is 3600.
Embodiment 3:
With cobalt acetate, manganese nitrate, the Schweinfurt green mol ratio is to be dissolved in isopropyl alcohol at 6: 1.48: 2.52, butanols, in the acetone mixed solvent, and adding chelating agent ethanedioic acid stirs, this solution is placed stable, its solution concentration is 0.5M, again slide or the quartz base plate of cleaning immersed in this solution, speed with 4cm/s lifts to air drying, 450 ℃ of bakings down, repeat this process, needing can obtain the film of thickness, the crystallization of annealing under 700 ℃ temperature is with the material plated electrode that burns till, electrode spacing 0.5mm, film thickness is 550nm, scribing, solder taul gets final product to encapsulation, and Fig. 2 resistance of sample-temperature relation Figure 25 ℃ resistance for this reason is about 20.7K, and material constant is 2580.
Claims (4)
1, a kind of sol-gel method for preparing the negative temperature coefficient thin-film thermistor, it is characterized in that at first with manganese, cobalt or except cobalt, add nickel outside the manganese again, a kind of ratio in the copper is mol ratio (2-6): (1-2): the acetate of transition metal (0-3) or nitrate are dissolved in the solvent, and interpolation chelating agent, as the solution that sets out, then this solution is placed stable, solution concentration is 0.1-0.5M, pH value is 2-6, to clean clean substrate again immerses in the solution, lift 450 ℃ of bakings to the air drying, repeat this process, needing can obtain the film of thickness, again 500-700 ℃ of annealing crystallization, with the thin-film material plated electrode that burns till, scribing, solder taul is to encapsulation.
2, the sol-gel method of preparation negative temperature coefficient thin-film thermistor according to claim 1, it is characterized in that solvent is the alcohol of ethanol or methyl alcohol or isopropyl alcohol or butanols and acetate or glacial acetic acid or acetone and the mixed liquor of acid, alcohol is 2-10 with the volume ratio of acid.
3, the sol-gel method of preparation negative temperature coefficient thin-film thermistor according to claim 1 is characterized in that, substrate is slide or quartz base plate.
4, the sol-gel method of preparation negative temperature coefficient thin-film thermistor according to claim 1, it is characterized in that chelating agent is acetylacetone,2,4-pentanedione or trifluoroacetylacetone (TFA) or ethanedioic acid or ethylenediamine two acetic acid, its addition is that the mol ratio of chelating agent and salt is 1-4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98123522A CN1092390C (en) | 1998-10-08 | 1998-10-08 | Sol-gel process for preparing thermosensitive film resistor with negative temp. coefficient |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98123522A CN1092390C (en) | 1998-10-08 | 1998-10-08 | Sol-gel process for preparing thermosensitive film resistor with negative temp. coefficient |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1250940A CN1250940A (en) | 2000-04-19 |
| CN1092390C true CN1092390C (en) | 2002-10-09 |
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| CN98123522A Expired - Fee Related CN1092390C (en) | 1998-10-08 | 1998-10-08 | Sol-gel process for preparing thermosensitive film resistor with negative temp. coefficient |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100443631C (en) * | 2006-08-17 | 2008-12-17 | 中国科学院上海技术物理研究所 | Preparation method of manganese-cobalt-nickel thin film heat-sensitive material |
| CN102544221B (en) * | 2012-01-20 | 2014-08-13 | 中国科学院上海技术物理研究所 | Method for preparing sapphire substrate-based wide-band film type photoelectric detector |
| CN104700970B (en) * | 2015-03-30 | 2017-12-22 | 东莞理工学院 | A kind of adjusting method of negative temperature coefficient thin-film thermistor and preparation method thereof and its resistance value |
| CN108151913A (en) * | 2017-12-27 | 2018-06-12 | 赛特科（唐山）科技有限公司 | A kind of heat-sensitive material of sensor |
| CN112735709A (en) * | 2020-12-26 | 2021-04-30 | 广东工业大学 | Film type negative temperature coefficient sensor and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05135913A (en) * | 1991-11-12 | 1993-06-01 | Matsushita Electric Ind Co Ltd | Manufacture of oxide semiconductor for thermistor |
| CN1185632A (en) * | 1996-12-14 | 1998-06-24 | 中国科学院新疆物理研究所 | Oxidate semi-conductor thermosensitive resistance and mfg. method thereof |
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1998
- 1998-10-08 CN CN98123522A patent/CN1092390C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05135913A (en) * | 1991-11-12 | 1993-06-01 | Matsushita Electric Ind Co Ltd | Manufacture of oxide semiconductor for thermistor |
| CN1185632A (en) * | 1996-12-14 | 1998-06-24 | 中国科学院新疆物理研究所 | Oxidate semi-conductor thermosensitive resistance and mfg. method thereof |
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| CN1250940A (en) | 2000-04-19 |
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