CN101154485A - Microwave sintering method for thermal resistor with positive temperature coefficient and its special device - Google Patents

Microwave sintering method for thermal resistor with positive temperature coefficient and its special device Download PDF

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Publication number
CN101154485A
CN101154485A CNA2006100629894A CN200610062989A CN101154485A CN 101154485 A CN101154485 A CN 101154485A CN A2006100629894 A CNA2006100629894 A CN A2006100629894A CN 200610062989 A CN200610062989 A CN 200610062989A CN 101154485 A CN101154485 A CN 101154485A
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China
Prior art keywords
sintering
thermal insulator
microwave
crucible
semistor
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Pending
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CNA2006100629894A
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Chinese (zh)
Inventor
郜长福
张大牛
宋文杰
陈闻杰
郑阳
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Shenzhen Jinke Special Materials Co., Ltd.
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郜长福
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Priority to CNA2006100629894A priority Critical patent/CN101154485A/en
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Abstract

A microwave sintering method of posiode and special hardware belong to the preparation method field of electronic heating element. The microwave sintering method comprises the following art procedures: a posiode green ware body of the series of barium titanate made by the prior art is placed into a crucible and a sintering special thermal insulator, and then the whole is placed into a micro-wave oven to sinter; the sintering procedure is that the speed of temperature rise is controlled between 5 degrees per minute and 100 degrees per minute, after the temperature is up to 1100 degrees to 1300 degrees, the whole is kept at a constant temperature for 5 to 60 minutes, and then the whole is cooled down to the room temperature at the cooling rate of 3 to 30 degrees per minute; the special hardware is a sintering special thermal insulator arranged in the micro-wave oven body, the sintering special thermal insulator comprises a fibre thermal insulator in the outer layer and a thermal insulator in the sub outer layer; a fibre insulation ball packed layer is arranged between the thermal insulator in the sub outer layer and the crucible in the inner layer. The invention is of short cycle of sintering art, good quality of products and high rate of finished products, thereby improving the production benefit and saving energy sources.

Description

The microwave sintering method of semistor and special equipment
Technical field:
The present invention relates to a kind of microwave sintering method and special equipment of semistor, it belongs to a kind of preparation method field of electronic heating element, particularly the preparing technical field of barium titanate series semistor.
Background technology:
In recent years, development along with microwave high-temperature sintering technology and microwave high-temperature agglomerating plant, the microwave sintering pottery has been obtained bigger progress, and more and more be subject to people's attention, because the multiple advantage that normal sintering methods such as it has fast, sensitive, energy-conservation, efficient are not had, it has broad prospects on ceramic post sintering prepares.The difference of microwave sintering and normal sintering is that normal sintering is to rely on heater that heat is passed to heating object by convection current, conduction or radiation mode to make it reach a certain temperature, and the generation of microwave heating heat is to lead loss and generate heat owing to microwave directly produces coupling absorption microwave energy or electricity with interior of articles atom or molecule, be that heating object generates heat from body, rather than from other heaters, microwave energy is effectively utilized like this, cut down the consumption of energy, and can realize Fast Heating and cooling sample.Because the uniqueness of microwave heating produces the phenomenon of a kind of being referred to as " microwave effect ", can strengthen atom diffusion, reduce activation energy, reduce sintering temperature thus, shorten sintering time, and can make uniformity and the good ceramic material of consistency.Gone out as aluminium oxide Al with microwave success sintering both at home and abroad at present 2O 3, silicon nitride Si 3N 4, pottery such as carborundum SiC, but all be confined to prepare the structural ceramics of high strength, high rigidity, high tenacity, in electronic ceramic fields, especially the application of thermal sensitive ceramics aspect is less, does not particularly also utilize at present the technology of microwave sintering barium titanate series semistor pottery.
Summary of the invention:
The object of the present invention is to provide and a kind ofly can under low-temp low-pressure, can carry out large-scale production, and the microwave sintering method and the special equipment of the barium titanate of energy savings series semistor.
The object of the present invention is achieved like this:
A kind of microwave sintering method of semistor, it comprises following processing step:
A) ceramic green of the barium titanate series semistor that will make through existing technology is put into crucible, will be equipped with then the crucible of ceramic green and sintering special-purpose thermal insulation body together integral body put into microwave oven and carry out sintering;
B) the sintering flow process is: set programming rate and be controlled between 5 ℃/min~100 ℃/min, after being warming up to 1200 ℃ ± 100 ℃, constant temperature kept 5~60 minutes, was cooled to room temperature with 3~30 ℃/min cooling rate then, promptly finished the preparation of semistor.
A kind of special equipment that is used for the microwave sintering method of above-mentioned semistor, it comprises a microwave oven body and crucible, it is characterized in that in described microwave oven body, being provided with sintering special-purpose thermal insulation body, described sintering special-purpose thermal insulation body comprises: outer layer fiber thermal insulator, inferior outer field thermal insulator; Between described inferior outer thermal insulator and inner crucible, be provided with fiber thermal insulation ball packed layer.
Be provided with keeping warmth space between described outer layer fiber thermal insulator and the inferior outer field thermal insulator.
Described outer layer fiber thermal insulator is cuboid or the cylindrical structure that has upper and lower cover plate.
The special equipment of the microwave sintering method of described semistor is characterized in that described outer layer fiber thermal insulator is an aluminium oxide Al 2O 3Material; Described time outer thermal insulator is magnesium aluminate spinel-chromic acid lanthanum MgAl 2O 4-LaCrO 3Material; Described fiber thermal insulation ball is Al 2O 3The fiber thermal insulation ball.
Described crucible is to have the cuboid of upper and lower cover plate or the corundum crucible of cylindrical structure.
The present invention has advantage: the sintering process cycle is short, the production efficiency height: 12 hours of normal sintering technology are shortened to 3 hours of microwave sintering, improve the production efficiency of barium titanate series semistor pottery greatly; Energy-saving and cost-reducing: because the microwave sintering sample generates heat, strengthens uniquenesses such as atom diffusion, reduction activation energy from body, the capacity usage ratio height, sintering temperature is low, constant temperature time is short, process cycle is short, under the identical situation of sintered sample quantity, can cut down the consumption of energy at double.Good product quality, rate of finished products height: owing to being rapidly heated and fast cooling and whole heating property of microwave sintering, make the uniformity and the consistency of material be improved, electric property consistency such as resistance, Curie point, side reaction coefficient are fine, the rate of finished products height, thus improved productivity effect.
Description of drawings:
Accompanying drawing 1 is the structural representation of microwave sintering special equipment of the present invention
Embodiment:
Be special equipment in the embodiment of the invention with accompanying drawing 1 below, the present invention be further detailed:
Embodiment 1:
At first prepare the special equipment that the present invention uses, this device-specific equipment, as shown in accompanying drawing 1, it comprises a microwave oven body 1, in described microwave oven body 1, be provided with sintering special-purpose thermal insulation body, described sintering special-purpose thermal insulation body comprises: outer field fiber thermal insulation body 1, and the crucible 4 of inferior outer field thermal insulator 2 and internal layer is provided with fiber thermal insulation ball packed layer 3 between described outer thermal insulator 2 and inner crucible 4; At described outer field fiber thermal insulation body 1, be provided with keeping warmth space 6 between the inferior outer field thermal insulator 2.In the present embodiment, described outer field fiber thermal insulation body 1 is Al 2O 3Material; Described time outer field thermal insulator 2 is MgAl 2O 4-LaCrO 3Material, the crucible 4 of described internal layer is Al 2O 3The corundum crucible of material; Described fiber thermal insulation ball is Al 2O 3The fiber thermal insulation ball.Described outer layer fiber thermal insulator 1 is for having the rectangular structure of upper and lower cover plate; Described crucible 4 is for having the rectangular structure of upper and lower cover plate.
Formulated barium titanate series posistor material of the prior art at first on request; Then with the barium titanate for preparing series posistor material with the serial posistor material powder of conventional sintering reaction synthesis of barium titanate and be molded into ceramic green; Above-mentioned process procedure is prior art.Then ready ceramic green 5 is put into Al 2O 3Corundum crucible 4 will be filled the Al of ceramic green then 2O 3Corundum crucible, Al 2O 3Fiber thermal insulation ball 3, MgAl 2O 4-LaCrO 3 Thermal insulator 2, Al 2O 3Fiber thermal insulation body 1 integral body is put into the microwave sintering device, and this microwave oven should have a 2.45GHz multi-mode reaction chamber.Carry out sintering under the power of 6.0KW being lower than, adding microwave power at room temperature to 400 a ℃ warm area is 1.0KW, heating rate is 10 ℃/min, at 400 ℃~1150 ℃ warm area heating rates is 15 ℃/min, then when temperature reaches 1150 ℃, constant temperature 30 minutes is closed the microwave source natural cooling after being cooled to 500 ℃ with 10 ℃/min then, so promptly finishes the sintering that does not have the barium titanate of cracking even compact series semistor pottery.
Embodiment 2:
Ceramic green 5 is put into Al 2O 3Corundum crucible will be filled the Al of green compact then 2O 3Corundum crucible, Al 2O 3Fiber thermal insulation ball 3, MgAl 2O 4-LaCrO 3 Thermal insulator 2, Al 2O 3Fiber thermal insulation body 1 integral body is put into 2.45GHz multi-mode reaction chamber microwave oven sintering device, carry out sintering under the power of 6.0KW being lower than, adding microwave power at room temperature to 400 a ℃ warm area is 1.2KW, heating rate is 15 ℃/min, at 400 ℃~1150 ℃ warm area heating rates is 10 ℃/min, at 1200 ℃, and constant temperature 20 minutes, close the microwave source natural cooling after being cooled to 500 ℃ with 10 ℃/min then, get final product to such an extent that do not have a barium titanate series semistor pottery of cracking even compact.Described outer layer fiber thermal insulator 1 is for having the cylindrical structure of upper and lower cover plate; Described corundum crucible 4 is for having the cylindrical structure of upper and lower cover plate.
The other parts of present embodiment and embodiment 1 are identical.
Embodiment 3:
Ceramic green 5 is put into Al 2O 3Corundum crucible 4 will be filled the Al of green compact then 2O 3Corundum crucible, Al 2O 3Fiber thermal insulation ball 3, MgAl 2O 4-LaCrO 3 Thermal insulator 2, Al 2O 3Fiber thermal insulation body 1 integral body is put into 2.45GHz multi-mode reaction chamber microwave sintering device, carry out sintering under the power of 6.0KW being lower than, adding microwave power at room temperature to 400 a ℃ warm area is 1.5KW, heating rate is 18 ℃/min, at 400 ℃~1150 ℃ warm area heating rates is 20 ℃/min, at 1250 ℃, and constant temperature 15 minutes, close the microwave source natural cooling after being cooled to 500 ℃ with 10 ℃/min then, get final product to such an extent that do not have a barium titanate series semistor pottery of cracking even compact.
The other parts of present embodiment and embodiment 1 are identical.

Claims (6)

1. the microwave sintering method of a semistor is characterized in that it comprises following processing step:
A) ceramic green of the barium titanate series semistor that will make through existing technology is put
Go into crucible (4), will be equipped with then the crucible (4) of ceramic green and sintering special-purpose thermal insulation body together integral body put into microwave oven and carry out sintering;
B) the sintering flow process is: set programming rate and be controlled between 5 ℃/min~100 ℃/min, after being warming up to 1200 ℃ ± 100 ℃, constant temperature kept 5~60 minutes, was cooled to room temperature with 3~30 ℃/min cooling rate then, promptly finished the preparation of ceramic positive temperature coefficient thermosensitive resistor.
2. special equipment that is used for the microwave sintering method of the semistor described in the claim 1, it comprises a microwave oven body (7) and crucible (4), it is characterized in that in described microwave oven body (7), being provided with sintering special-purpose thermal insulation body, described sintering special-purpose thermal insulation body comprises: outer layer fiber thermal insulator (1), inferior outer field thermal insulator (2); Between described inferior outer thermal insulator (2) and inner crucible (4), be provided with fiber thermal insulation ball packed layer (3).
3. the special equipment of the microwave sintering method of the semistor described in claim 2 is characterized in that being provided with keeping warmth space (6) between described outer layer fiber thermal insulator (1) and time outer field thermal insulator (2).
4. as the special equipment of the microwave sintering method that is used for semistor in the claim 2, it is characterized in that described outer layer fiber thermal insulator (1) is for having the cuboid or the cylindrical structure of upper and lower cover plate.
5. the special equipment of the microwave sintering method of the semistor described in claim 2 or 3 or 4 is characterized in that described outer layer fiber thermal insulator (1) is an aluminium oxide Al 2O 3Material; Described time outer thermal insulator (2) is magnesium aluminate spinel-chromic acid lanthanum MgAl 2O 4-LaCrO 3Material; Described fiber thermal insulation ball is Al 2O 3The fiber thermal insulation ball.
6. as the special equipment of the microwave sintering method that is used for semistor in the claim 2, it is characterized in that described crucible (4) is for having the cuboid of upper and lower cover plate or the corundum crucible of cylindrical structure.
CNA2006100629894A 2006-09-30 2006-09-30 Microwave sintering method for thermal resistor with positive temperature coefficient and its special device Pending CN101154485A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102030537A (en) * 2009-09-28 2011-04-27 广东南方宏明电子科技股份有限公司 Process for sintering ceramic capacitor dielectric
CN103030406A (en) * 2013-01-02 2013-04-10 桂林理工大学 Ptc ceramic sintering method
CN101565322B (en) * 2009-01-21 2014-09-17 徐艳姬 Ceramic fiber fabric-reinforced microwave heating plate and chamber and manufacturing method thereof
CN104602375A (en) * 2014-12-17 2015-05-06 内蒙古坤瑞玻璃工贸有限公司 Thermal sensitive ceramic electrically heated glass and preparation method thereof
CN105837227A (en) * 2016-03-28 2016-08-10 安徽石轩文化科技有限公司 Method of quickly sintering ceramic with ceramic sintering special-use microwave box-type oven
CN106518052A (en) * 2015-09-10 2017-03-22 华中科技大学 Method for preparing fine-grained barium titanate temperature-sensitive ceramic and product thereof
CN106992049A (en) * 2017-05-09 2017-07-28 句容市博远电子有限公司 A kind of high temperature modification resistance and preparation method thereof

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101565322B (en) * 2009-01-21 2014-09-17 徐艳姬 Ceramic fiber fabric-reinforced microwave heating plate and chamber and manufacturing method thereof
CN102030537A (en) * 2009-09-28 2011-04-27 广东南方宏明电子科技股份有限公司 Process for sintering ceramic capacitor dielectric
CN103030406A (en) * 2013-01-02 2013-04-10 桂林理工大学 Ptc ceramic sintering method
CN104602375A (en) * 2014-12-17 2015-05-06 内蒙古坤瑞玻璃工贸有限公司 Thermal sensitive ceramic electrically heated glass and preparation method thereof
CN106518052A (en) * 2015-09-10 2017-03-22 华中科技大学 Method for preparing fine-grained barium titanate temperature-sensitive ceramic and product thereof
CN105837227A (en) * 2016-03-28 2016-08-10 安徽石轩文化科技有限公司 Method of quickly sintering ceramic with ceramic sintering special-use microwave box-type oven
CN106992049A (en) * 2017-05-09 2017-07-28 句容市博远电子有限公司 A kind of high temperature modification resistance and preparation method thereof

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Effective date of registration: 20080229

Address after: Guangdong Province, Shenzhen City, Nanshan District science and Technology Park Qiong Yu Road No. 8 branch company

Applicant after: Shenzhen Jinke Special Materials Co., Ltd.

Address before: No. 8, Qiong Yu Road, Nanshan District science and Technology Park, Shenzhen, Guangdong

Applicant before: Gao Changfu

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Open date: 20080402