CN1357512A - Microwave sintering process of thermosensitive ceramic with negative temperature coefficient - Google Patents
Microwave sintering process of thermosensitive ceramic with negative temperature coefficient Download PDFInfo
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- CN1357512A CN1357512A CN 01124430 CN01124430A CN1357512A CN 1357512 A CN1357512 A CN 1357512A CN 01124430 CN01124430 CN 01124430 CN 01124430 A CN01124430 A CN 01124430A CN 1357512 A CN1357512 A CN 1357512A
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- temperature coefficient
- negative temperature
- manganese
- nickel
- coefficient thermistor
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Abstract
The present invention relates to the microwave sintering process of thermosensitive resistor ceramic with negative temperature coefficient. Thermosensitive material with negative temperature coefficient of binary, ternary or quaternary oxide is first compounded; and raw powder blank prepared through conventional coprecipitation process is sintered by setting in a thermal insulating body inside a multimode microwave sintering oven with power lower than 2.5 KW. The thermaosensitive resistor ceramic thus prepared has fine and dense crystal grain and the process has high finished product rate and short sintering time, 4 hr, and high production efficiency.
Description
The present invention relates to a kind of microwave sintering method of negative temperature coefficient thermosensitive ceramics
Microwave sintering has been obtained a lot of progress in recent years for the preparation of pottery and has been come into one's own day by day.Because the not available multiple advantages of ordinary method such as it have fast, sensitive, energy-conservation, efficient and function is cut out, its application prospect on ceramic post sintering prepares is quite wide.Microwave heating is microwave direct and interior of articles atom or molecule generation coupling absorption micro-wave energy with the difference of routine heating, makes object self heating thereby reach, and does not need to make the object intensification by thermal conduction.Microwave energy is effectively utilized like this, cuts down the consumption of energy, and also makes the heating and cooling control of object sensitive rapidly, can realize rapid heating and cooling to sample.Owing to the difference of specific inductivity, different atoms or molecule have nothing in common with each other to the absorption of micro-wave energy simultaneously, can realize the selectivity heating of the different components of sample is reached the purpose that function is cut out.In addition because the uniqueness of microwave heating produces the phenomenon of a kind of being referred to as " microwave effect ", as strengthening atomic diffusion, reducing activation energy etc.The report of the sintering of all useful microwave success of home and overseas at present function ceramics, but also mainly be confined to prepare the structural ceramics of high strength, toughness and hardness, as Al
2O
3, Si
3N
4, SiC etc., at electronic ceramics, especially the application of thermal sensitive ceramics aspect is also less.The electronic ceramics preparation that is sintered to that microwave is used for electronic ceramics provides new approaches and methods.
The present invention is in process years of researches and a large amount of experiments, develop a kind of microwave sintering method of negative temperature coefficient thermosensitive ceramics, this method is utilized microwave sintering NTC thermal sensitive ceramics and in conjunction with the technology of Chinese patent ZL971172560, the NTC thermal sensitive ceramics that preparation has less grain-size and pore is little, be evenly distributed; And utilize the microwave sintering reduction to sinter the porcelain temperature into, reduce sintering time and save the energy.
The object of the invention is, the microwave sintering method of the negative temperature coefficient thermosensitive ceramics of development is prepared the negative temperature coefficient thermistor composition of two component system or three component system or quaternary system oxide compound at first respectively; Coprecipitation method with routine prepares the negative temperature coefficient heat-sensitive powder green compact; Green compact are put into have Al
2O
3Fiber thermal insulation body, Al
2O
3In the double platinum rhodium thermopair thermal insulator of corundum thermal insulator, NiCrAl compo pipe shield microwaves, again thermal insulator integral body is put into 2.45GHz multi-mode reaction chamber microwave sintering device, carried out sintering under the power of 2.5KW and get final product being lower than.This method has the energy-and time-economizing, has shortened the explained hereafter cycle significantly, has improved the production efficiency of negative temperature coefficient unit.
The microwave sintering method of negative temperature coefficient thermosensitive ceramics of the present invention follows these steps to carry out:
A, prepare the negative temperature coefficient thermistor composition of two component system or three component system or quaternary system oxide compound at first respectively;
B, the oxide compound negative temperature coefficient thermistor composition for preparing is prepared negative temperature coefficient thermistor composition powder green compact with conventional coprecipitation method;
C, green compact are put into thermal insulator (3), then with (1) Al
2O
3Fiber thermal insulation body, (2) Al
2O
3The double platinum rhodium thermopair integral body of corundum thermal insulator, (3) thermal insulator, (4) green compact, (5) NiCrAl compo pipe shield microwaves is put into 2.45GH
zIn the multi-mode reaction chamber microwave sintering device, carry out sintering under the power of 2.5KW being lower than; The sintering flow process is, heating schedule is that 5.-15 ℃/min is adjustable, is raised to 1150 ℃ ± 50 ℃, constant temperature 30 minutes, 8 ℃/min is cooled to 700 ℃ and closes the microwave source naturally cooling then, promptly gets the large size φ 50 negative tempperature coefficient thermistor potteries that do not have the cracking even compact.
D, in sintering, adopt NiCrAl compo pipe shield microwaves thermocouple temperature measurement, the computer acquisition Temperature numerical;
Wherein the negative temperature coefficient thermistor composition of two component system oxide compound is manganese-nickel; The negative temperature coefficient thermistor composition of three component system oxide compound is cobalt-manganese-nickel or manganese-Ni-Fe or cobalt-manganese-copper or manganese-nickel-magnesium or manganese-nickel-aluminium; The negative temperature coefficient thermistor composition of quaternary system oxide compound is manganese-nickel-magnesium-aluminium or cobalt-manganese-copper-iron or cobalt-manganese-nickel-aluminium;
In step c, can regulate material constant B value by regulating temperature rise rate.
The microwave sintering method of negative temperature coefficient thermosensitive ceramics of the present invention, this method has following characteristics:
1), 36 hours of normal sintering technology are shortened to 4 hours of microwave sintering process, because microwave sintering is whole heating, the homogeneity and the consistence of material are improved, and the consistence of resistance and B value is fine.This technology has the advantage of energy-and time-economizing, and has significantly shortened the explained hereafter cycle, thereby improves the production efficiency of NTC element.
2), the NTC element resistance is brought up to the 50%-60% of microwave sintering process 1% with interior yield rate by the 15%-45% of normal sintering technology; Resistance is brought up to the 80%-85% of microwave sintering process 2% with the interior 60%-75% by normal sintering technology, has improved the high precision components yield rate of NTC element, thereby has improved productivity effect.
3), material parameter B value can carry out adjusting in 2% scope by regulating temperature rise rate under the prerequisite that does not change thermostat temperature and time, this is that normal sintering technology can't realize.
Referring to accompanying drawing
Fig. 1 is the placement and the thermal insulator structural representation of sample of the present invention
(1) is the cylindric Al of cover plate about the band among the figure
2O
3The fiber thermal insulation body;
(2) for being with the cylindric Al of cover plate up and down
2O
3The corundum thermal insulator;
(3) be Chinese patent ZL97117256.0 MgAl2O4-LaCrO3 thermal insulator;
(4) the NTC thermo-sensitive material green compact sample for being sintered;
(5) for adopting the double platinum rhodium thermopair of NiCrAl compo pipe shield microwaves.
Embodiment 1
A, prepare the negative temperature coefficient thermistor composition of two component system manganese-nickel oxide at first respectively;
B, manganese-nickel oxide negative temperature coefficient thermistor composition of preparing is prepared the negative temperature coefficient heat-sensitive powder green compact with conventional coprecipitation method;
C, green compact are put into thermal insulator (3), then with (1) Al
2O
3The fiber thermal insulation body,
(2) Al
2O
3The double platinum rhodium thermopair integral body of corundum thermal insulator, (3) thermal insulator, (4) green compact, (5) NiCrAl compo pipe shield microwaves is put into 2.45GH
zIn the multi-mode reaction chamber microwave sintering device, adding microwave power at room temperature to 600 a ℃ warm area is 0.8KW, temperature rise rate is 6 ℃/min, at 600-1150 ℃ of warm area temperature rise rate is 10 ℃/min, at 1150 ℃, constant temperature 30 minutes, 8 ℃/min is cooled to 700 ℃ and closes the microwave source naturally cooling then, promptly get the block negative tempperature coefficient thermistor pottery that does not have the cracking even compact, becoming porcelain density is 5.26g/cm
3, material constant B value is 3560 ± O.3% and the good thermal sensitive ceramic material of consistence.The NTC thermistor element resistance of making is brought up to 60%. of microwave sintering process with interior element yield rate by 45% of normal sintering technology 1%
D, in sintering, adopt NiCrAl compo pipe shield microwaves thermocouple temperature measurement, the computer acquisition Temperature numerical.
Embodiment 2
A, prepare the negative temperature coefficient thermistor composition of three component system cobalt-manganese-nickel or manganese-Ni-Fe or cobalt-manganese-copper or manganese-nickel-magnesium or manganese-nickel-aluminum oxide at first respectively;
B, the three component system oxide compound negative temperature coefficient thermistor composition for preparing is prepared the negative temperature coefficient heat-sensitive powder green compact with conventional coprecipitation method;
C, green compact are put into thermal insulator (3), then with (1) Al
2O
3Fiber thermal insulation body, (2) Al
2O
3The double platinum rhodium thermopair integral body of corundum thermal insulator, (3) thermal insulator, (4) green compact, (5) NiCrAl compo pipe shield microwaves is put into 2.45GH
zIn the multi-mode reaction chamber microwave sintering device, adding microwave power at room temperature to 600 a ℃ warm area is 1.0KW, temperature rise rate is 10 ℃/min, add microwave power 1.5-2.2KW at 600-1150 ℃ of warm area, temperature rise rate is 15 ℃/min, and 1150 ℃ of constant temperature 30 minutes, 8 ℃/min was cooled to 700 ℃ and closes the microwave source naturally cooling then, promptly get the block negative tempperature coefficient thermistor pottery that does not have the cracking even compact, becoming porcelain density is 4.99-5.32g/cm
3, material constant B value is 3250-3650 ± 0.3% and the good thermal sensitive ceramic material of consistence.The NTC thermistor element resistance of making is brought up to 50%. of microwave sintering process with interior element yield rate by 15% of normal sintering technology 1%
D, in sintering, adopt NiCrAl compo pipe shield microwaves thermocouple temperature measurement, the computer acquisition Temperature numerical.
Embodiment 3
A, prepare the negative temperature coefficient thermistor composition of quaternary system manganese-nickel-magnesium-aluminium or cobalt-manganese-copper-iron or cobalt-manganese-nickel-aluminum oxide at first respectively;
B, the quaternary system oxide compound negative temperature coefficient thermistor composition for preparing is prepared the negative temperature coefficient heat-sensitive powder green compact with conventional coprecipitation method;
C, green compact are put into thermal insulator (3), then with (1) Al
2O
3Fiber thermal insulation body, (2) Al
2O
3The double platinum rhodium thermopair integral body of corundum thermal insulator, (3) thermal insulator, (4) green compact, (5) NiCrAl compo pipe shield microwaves is put into 2.45GH
zIn the multi-mode reaction chamber microwave sintering device, adding microwave power at room temperature to 600 a ℃ warm area is 1.0KW, temperature rise rate is 10 ℃/min, add microwave power 1.5-2.2KW at 600-1150 ℃ of warm area, temperature rise rate is 15 ℃/min, and 1150 ℃ of constant temperature 30 minutes, 8 ℃/min was cooled to 700 ℃ and closes the microwave source naturally cooling then, promptly get the block negative tempperature coefficient thermistor pottery that does not have the cracking even compact, becoming porcelain density is 5.0-5.40g/cm
3, material constant B value is 3450-3850 ± 0.3% and the good thermal sensitive ceramics of consistence.The NTC thermistor element resistance of making is brought up to 60% of microwave sintering process with interior element yield rate by 25% of normal sintering technology 1%.
D, in sintering, adopt NiCrAl compo pipe shield microwaves thermocouple temperature measurement, the computer acquisition Temperature numerical.
Claims (3)
1, a kind of microwave sintering method of negative temperature coefficient thermosensitive ceramics is characterized in that following these steps to carrying out:
A, prepare the negative temperature coefficient thermistor composition of two component system or three component system or quaternary system oxide compound at first respectively;
B, the oxide compound negative temperature coefficient thermistor composition for preparing is prepared negative temperature coefficient thermistor composition powder green compact with conventional coprecipitation method;
C, green compact are put into thermal insulator (3), then with (1) Al
2O
3Fiber thermal insulation body, (2) Al
2O
3The double platinum rhodium thermopair integral body of corundum thermal insulator, (3) thermal insulator, (4) green compact, (5) NiCrAl compo pipe shield microwaves is put into 2.45GH
zIn the multi-mode reaction chamber microwave sintering device, carry out sintering under the power of 2.5KW being lower than; The sintering flow process is, heating schedule is that 5-15 ℃/min is adjustable, is raised to 1150 ℃ ± 50 ℃, constant temperature 30 minutes, and 8 ℃/min is cooled to 700 ℃ and closes the microwave source naturally cooling then, promptly gets the large size φ 50 negative tempperature coefficient thermistor potteries that do not have the cracking even compact.
D, in sintering, adopt NiCrAl compo pipe shield microwaves thermocouple temperature measurement, the computer acquisition Temperature numerical;
2, the microwave sintering method of negative temperature coefficient thermosensitive ceramics according to claim 1, the negative temperature coefficient thermistor composition that it is characterized in that the two component system oxide compound is manganese-nickel; The negative temperature coefficient thermistor composition of three component system oxide compound is cobalt-manganese-nickel or manganese-Ni-Fe or cobalt-manganese-copper or manganese-nickel-magnesium or manganese-nickel-aluminium; The negative temperature coefficient thermistor composition of quaternary system oxide compound is manganese-nickel-magnesium-aluminium or cobalt-manganese-copper-iron or cobalt-manganese-nickel-aluminium;
3, the microwave sintering method of negative temperature coefficient thermosensitive ceramics according to claim 1 is characterized in that can regulating material constant B value by regulating temperature rise rate in step c.
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|---|---|---|---|
| CNB011244305A CN1169750C (en) | 2001-07-27 | 2001-07-27 | Microwave sintering process of thermosensitive ceramic with negative temperature coefficient |
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|---|---|---|---|
| CNB011244305A CN1169750C (en) | 2001-07-27 | 2001-07-27 | Microwave sintering process of thermosensitive ceramic with negative temperature coefficient |
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| CN1169750C CN1169750C (en) | 2004-10-06 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100351207C (en) * | 2005-09-01 | 2007-11-28 | 陕西科技大学 | Ceramic parts quick making method |
| CN102173832A (en) * | 2011-01-10 | 2011-09-07 | 宜昌浩诚工贸有限公司 | Microwave sintering method of clay-graphite crucible |
| CN102211924A (en) * | 2011-04-01 | 2011-10-12 | 中国科学院新疆理化技术研究所 | Preparation method of composite phase negative temperature coefficient thermal sensitive ceramic material |
| CN101585707B (en) * | 2009-07-07 | 2012-05-23 | 西安交通大学 | Method for preparing high-temperature NTC heat-sensitive resistance material |
| CN103073278A (en) * | 2013-01-30 | 2013-05-01 | 广州新莱福磁电有限公司 | Manufacturing method of high-precision and high-reliability NTC thermistor chip |
| CN104370525A (en) * | 2013-08-15 | 2015-02-25 | 中国振华集团云科电子有限公司 | Preparation method for manganese-cobalt-copper system non-linear negative temperature coefficient thick-film electronic slurry |
| CN105000891A (en) * | 2015-06-01 | 2015-10-28 | 北京控制工程研究所 | MnCoNi oxide ceramic infrared sensitive element densifying method |
| CN108585795A (en) * | 2018-07-11 | 2018-09-28 | 中国科学院新疆理化技术研究所 | A kind of method that molten salt process prepares negative temperature coefficient thermal-sensitive ceramic material |
| CN109616268A (en) * | 2018-12-13 | 2019-04-12 | 中国科学院新疆理化技术研究所 | A kind of preparation method of compound high-temperature thermistor |
| CN112851313A (en) * | 2021-01-21 | 2021-05-28 | 南京理工大学 | High-temperature thermistor material and microwave preparation method thereof |
-
2001
- 2001-07-27 CN CNB011244305A patent/CN1169750C/en not_active Expired - Fee Related
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100351207C (en) * | 2005-09-01 | 2007-11-28 | 陕西科技大学 | Ceramic parts quick making method |
| CN101585707B (en) * | 2009-07-07 | 2012-05-23 | 西安交通大学 | Method for preparing high-temperature NTC heat-sensitive resistance material |
| CN102173832A (en) * | 2011-01-10 | 2011-09-07 | 宜昌浩诚工贸有限公司 | Microwave sintering method of clay-graphite crucible |
| CN102211924A (en) * | 2011-04-01 | 2011-10-12 | 中国科学院新疆理化技术研究所 | Preparation method of composite phase negative temperature coefficient thermal sensitive ceramic material |
| CN102211924B (en) * | 2011-04-01 | 2013-04-17 | 中国科学院新疆理化技术研究所 | Preparation method of composite phase negative temperature coefficient thermal sensitive ceramic material |
| CN103073278B (en) * | 2013-01-30 | 2014-10-08 | 广州新莱福磁电有限公司 | Manufacturing method of high-precision and high-reliability NTC thermistor chip |
| CN103073278A (en) * | 2013-01-30 | 2013-05-01 | 广州新莱福磁电有限公司 | Manufacturing method of high-precision and high-reliability NTC thermistor chip |
| CN104370525A (en) * | 2013-08-15 | 2015-02-25 | 中国振华集团云科电子有限公司 | Preparation method for manganese-cobalt-copper system non-linear negative temperature coefficient thick-film electronic slurry |
| CN104370525B (en) * | 2013-08-15 | 2016-09-07 | 中国振华集团云科电子有限公司 | A kind of preparation method of manganese cobalt copper system non-linear negative temperature coefficient thick-film electronic slurry |
| CN105000891A (en) * | 2015-06-01 | 2015-10-28 | 北京控制工程研究所 | MnCoNi oxide ceramic infrared sensitive element densifying method |
| CN108585795A (en) * | 2018-07-11 | 2018-09-28 | 中国科学院新疆理化技术研究所 | A kind of method that molten salt process prepares negative temperature coefficient thermal-sensitive ceramic material |
| CN108585795B (en) * | 2018-07-11 | 2021-02-05 | 中国科学院新疆理化技术研究所 | Method for preparing negative temperature coefficient thermal sensitive ceramic material by salt melting method |
| CN109616268A (en) * | 2018-12-13 | 2019-04-12 | 中国科学院新疆理化技术研究所 | A kind of preparation method of compound high-temperature thermistor |
| CN112851313A (en) * | 2021-01-21 | 2021-05-28 | 南京理工大学 | High-temperature thermistor material and microwave preparation method thereof |
| CN112851313B (en) * | 2021-01-21 | 2022-08-12 | 南京理工大学 | High-temperature thermistor material and microwave preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN1169750C (en) | 2004-10-06 |
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Granted publication date: 20041006 Termination date: 20100727 |