CN103096529B - There is the manufacture method of the silicon nitride heat generating body of higher reliability and fail safe - Google Patents
There is the manufacture method of the silicon nitride heat generating body of higher reliability and fail safe Download PDFInfo
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- CN103096529B CN103096529B CN201310004176.XA CN201310004176A CN103096529B CN 103096529 B CN103096529 B CN 103096529B CN 201310004176 A CN201310004176 A CN 201310004176A CN 103096529 B CN103096529 B CN 103096529B
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Abstract
The manufacture method that the present invention relates to a kind of silicon nitride heat generating body comprises: inserted in absolute ethyl alcohol with a small amount of high-temperature liquid-phase sintering agent by silicon nitride powder and mix, after batch mixing 10-72 hour, make formulation material through mist projection granulating; Then metal heating wire is imbedded formulation material and dry-pressing formed, then compressing further by the isostatic cool pressing of 180-220MPa, and pressurize 3-10 minute, to make biscuit; Then, one deck boron nitride separator post-drying is applied at described biscuit surface uniform; Then hot pressed sintering is carried out, sintering pressure 20-30MPa, sintering temperature 1600-1900 DEG C, temperature retention time 0.5-4 hour, to make blank; Finally, blank is put into vacuum atmosphere oven, keep 1300-1600 DEG C of constant temperature 10-24 hour, then naturally cool to room temperature.Described boron nitride separator is by the thick shape slurry that boron nitride powder and silicon nitride powder mix afterwards and absolute ethyl alcohol reconciles into.
Description
The application is divisional application, the application number of original application: 201010582116.2, the applying date: 2010-12-09, invention and created name: the manufacture method of silicon nitride heat generating body.
Technical field
The present invention relates to the technical field of the manufacture method of electric heating element, specifically a kind of manufacture method of silicon nitride heat generating body.
Background technology
Silicon nitride is a kind of covalent bond pottery, pure Si
3n
4powder cannot sinter, and must add a small amount of sintering agent and form liquid phase at high temperature, carry out liquid-phase sintering, just can obtain the silicon nitride material of excellent performance.Conventional additive comprises: Al
2o
3, MgO, SiO
2deng metal oxide, Y
2o
3, La
2o
3, CeO
2deng rare earth oxide, and AlN, Mg
3n
2, the nitride such as TiN, ZrN.High-performance silicon nitride ceramics has the excellent electricity such as insulation, high-strength, high temperature resistant, resistance to oxidation, heat shock resistance and high-termal conductivity, calorifics and mechanical property.
Silicon nitride heating plate is a kind of device in conjunction with high-performance silicon nitride ceramics matrix and long-life powerful high-temperature metal heating wire.There is volume little, the large and heat efficiency high of power, while be also proved to be a kind of safe and reliable heating system.After direct-electrifying, temperature is done on surface can reach 1200 degrees Celsius, and working life reaches more than 5000 hours.High-temperature metal heating wire material comprises, the materials such as tungsten filament, molybdenum filament and various tungsten-molybdenum alloy silks.
At present, more there is the phenomenon of carburizing in the silicon nitride heating sheet material in market, surface distributed has the phenomenons such as bulk blackspot, black patch from the appearance, and color and luster is uneven.Pure Si
3n
4the true qualities of dense sintering material should be canescence, and existing product exists matrix color blackout mostly, and surface uniform or uneven distribution pore, more have surface distributed to have the phenomenons such as bulk blackspot, black patch.This mainly in hot pressed sintering process because biscuit directly contacts with graphite, carbon infiltrates along liquid channel, dissolves in liquid phase, or reacts with silicon nitride and produce.The infiltration of carbon can the insulation property of deteriorated material, reduce safety and reliability.Simultaneously because the hot pressed sintering time is short, rely on mechanical pressure to strengthen fine and close effect, there is the microstructure that boundary stress is large, liquid phase crystallization is insufficient in the material obtained, affects the useful life of basis material.
Summary of the invention
The technical problem to be solved in the present invention is to provide the manufacture method of the simple silicon nitride heat generating body of a kind of technique, to produce the silicon nitride heat generating body with higher reliability and fail safe.
For solving the problems of the technologies described above, the manufacture method of silicon nitride heat generating body provided by the invention, comprising:
Step 1, silicon nitride powder and high-temperature liquid-phase sintering agent inserted in absolute ethyl alcohol by weight 0.96:0.04 to 0.80:0.20 mix, after batch mixing 10-72 hour, make formulation material through mist projection granulating;
Step 2, metal heating wire is imbedded in described formulation material dry-pressing formed, then compressing further by the isostatic cool pressing of 180-220MPa, and pressurize 3-10 minute, to make biscuit; Described metal heating wire is molybdenum filament;
Step 3, apply one deck boron nitride separator post-drying at described biscuit surface uniform;
Step 4, then carry out hot pressed sintering, sintering pressure 20-30MPa, sintering temperature 1600-1900 DEG C, temperature retention time 0.5-4 hour, to make blank;
Step 5, described blank is put into vacuum atmosphere oven, keep 1300-1600 DEG C of constant temperature 10-24 hour, then naturally cool to room temperature.
Further, described boron nitride separator is by the thick shape slurry that boron nitride powder and silicon nitride powder mix afterwards and absolute ethyl alcohol reconciles into; Wherein, the part by weight of silicon nitride powder and boron nitride powder is: 0.10:0.90 to 0:1.00.
Further, in described step 4, when carrying out hot pressed sintering, the hot pressing graphite jig of employing with the contact-making surface of biscuit on scribble boron nitride separator described in one deck.
The preferred Al of described high-temperature liquid-phase sintering agent
2o
3, MgO, SiO
2deng metal oxide, Y
2o
3, La
2o
3, CeO
2deng rare earth oxide, AlN, Mg
3n
2, the nitride such as TiN, ZrN, addition is 4wt%-20wt%.Wherein, the addition of described metal oxide is 0-20wt%, and the addition of rare earth oxide is 0-20wt%, and the addition of nitride is 0-5wt%.Common metal oxides can reduce sintering temperature, and rare earth oxide and a small amount of nitride can increase the viscosity of high-temperature liquid-phase and help high temperature crystallization.
The technique effect that the present invention has: (1) silicon nitride heat generating body of the present invention adopts high purity silicon nitride (Si
3n
4) powder, a small amount of liquid phase sintering and high-temperature metal heating wire composition, through forming of green body, after hot pressed sintering and high-temperature heat treatment, make compact silicon nitride base heater.This heater has the feature of high-strength, high thermal conductance, high reliability.Wherein biscuit surface has boron nitride powder (BN) coating, this process eliminates the infiltration of carbon in production process.High-temperature heat treatment process eliminates material stress, facilitates the crystallization of grain boundary glassy phase, substantially increases reliability and the fail safe of device.(2) in the manufacture method of silicon nitride heat generating body of the present invention, with absolute ethyl alcohol (99.9% purity) as medium, ball milling mixing 10-72 hour, both ensure that batch mixing was even, had again reduced oxidative phenomena.Any macromolecule modifier is not added in manufacturing process of the present invention.Some polymeric additive can improve the performance of biscuit and improve shaping finished product rate, but the technique that the biscuit of this technological forming must glue through row, get rid of polymeric additive.In general, under oxygen atmosphere, row is sticky can get rid of to greatest extent and burn the carbon in polymeric additive.And silicon nitride can only be arranged sticky under vacuum or nitrogen protection atmosphere, thoroughly eliminate carbon more difficult, so the residue always leaving some carbon containings is evenly distributed in biscuit, insulated with material and reliability can be reduced.The present invention does not adopt any macromolecule additive, but relies on dry-pressing and isostatic cool pressing technique to prepare the biscuit of high strength.(3) in the present invention, biscuit surface uniform is coated with BN separator, biscuit can be stoped to contact with the direct of graphite, eliminate the possibility of high temperature case-carbonizing element.(4) the present invention is after hot pressed sintering, and the material stress of silicon nitride heat generating body is comparatively large, is slow cooling to room temperature, can eliminates the stress of material after at high temperature annealing in process 10-24 hour.In addition, in high-temperature process, make the glassy phase crystallization in material, remaining carbon can be eliminated further and reduce material stress.(5) silicon nitride heating matrix of the present invention contains high-purity Si 3N4 powder and a small amount of high-temperature liquid-phase sintering agent.Initial substrate raw material and heating wire make biscuit through dry-pressing and isostatic cool pressing, biscuit surface-coated BN material.Biscuit at high temperature under high pressure hot pressed sintering becomes blank.Sintering blank high-temperature heat treatment process eliminates material stress and glass ceramics phase, has the feature of higher reliability and fail safe.
Accompanying drawing explanation
In order to make content of the present invention be more likely to be clearly understood, below basis specific embodiment and by reference to the accompanying drawings, the present invention is further detailed explanation, wherein
Fig. 1 is the structural representation of the silicon nitride heat generating body in embodiment.
Reference numeral: 1--silicon nitride heat generating body, 2--metal heating wire, 3--electrode.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in detail:
(embodiment 1)
The silicon nitride heat generating body of the present embodiment is made up of silicon nitride heating and the high-temperature metal heating wire be located in silicon nitride heat generating body.Metal heating wire is tungsten filament, molybdenum filament or tungsten-molybdenum alloy silk.
The manufacture method of above-mentioned silicon nitride heat generating body comprises:
Step 1, silicon nitride powder and high-temperature liquid-phase sintering agent inserted in absolute ethyl alcohol by weight 0.96:0.04 to 0.80:0.20 mix (ballmillmixer specifically can be adopted to mix), after batch mixing 10-72 hour, make formulation material through mist projection granulating;
Step 2, metal heating wire is imbedded in described formulation material dry-pressing formed, then compressing further by the isostatic cool pressing of 180-220MPa, and pressurize 3-10 minute, to make biscuit;
Step 3, apply one deck boron nitride separator post-drying at described biscuit surface uniform;
Step 4, then carry out hot pressed sintering, sintering pressure 20-30MPa, sintering temperature 1600-1900 DEG C, temperature retention time 0.5-4 hour, to make blank;
Step 5, described blank is put into vacuum atmosphere oven, keep 1300-1600 DEG C of constant temperature 10-24 hour, then naturally cool to room temperature, finally at metal heating wire two ends welding electrode.
Described boron nitride separator is by the thick shape slurry that boron nitride powder and silicon nitride powder mix afterwards and absolute ethyl alcohol reconciles into; Wherein, the part by weight of silicon nitride powder and boron nitride powder is: 0.10:0.90 to 0:1.00.
In described step 4, when carrying out hot pressed sintering, the hot pressing graphite jig of employing with the contact-making surface of biscuit on scribble boron nitride separator described in one deck.
(embodiment 2)
On the basis of embodiment 1, the manufacture method of the silicon nitride heat generating body of the present embodiment comprises:
By the silicon nitride powder of 92wt%, the Al of 3wt%
2o
3, the Y of 3wt%
2o
3, the AlN of the MgO of 1wt%, 1wt% adds 99.9% absolute ethyl alcohol Homogeneous phase mixing 72 hours, then inserts mist projection granulating in explosion-proof mist projection granulating tower and makes formulation material.
Formulation material is poured in mould, then metal heating wire is imbedded in powder dry-pressing formed, be of a size of 120*20*10.Encapsulated by dry-pressing formed biscuit, put into isostatic cool pressing equipment and carry out isostatic pressed process, the pressure of isostatic pressed is 200MPa, dwell time 3-10 minute again.Reconcile into thick shape slurry with high-pure anhydrous ethanol and boron nitride fine powder, adopt knife coating, at the uniform boron nitride separator of biscuit surface-coated one deck, drying and processing.Also be coated with one deck boron nitride separator at hot pressing graphite jig and biscuit contact-making surface, the biscuit handled well is put into mould.Mould is put into hot pressing furnace, and at 1800 degrees Celsius, 25MPa suppresses 2 hours, comes out of the stove within Temperature fall to 50 degree Celsius.Blank after sintering is put into heat-treatment furnace, and flowing nitrogen is protected, and at 1300-1500 degree Celsius, insulation is after 15 hours altogether, and slow cooling is come out of the stove to room temperature.Processed through surfacing by the fever tablet blank made, the subsequent techniques such as soldering make the silicon nitride heating plate of high-performance and high reliability.
Relevant isostatic cool pressing: under normal temperature, be placed in by powder in the middle of airtight liquid environment, liquid transfer superhigh pressure makes powder compacting.Because in liquid, pressure is equal everywhere, so be isostatic pressed.Again due under being normal temperature, so be isostatic cool pressing.Working temperature, when 100-200 DEG C, is warm isostatic pressed.Working temperature is higher is then high temperature insostatic pressing (HIP).What have reaches 2000 DEG C
Traditional spray granulation is all pass into hot blast in drying tower, by contacting with feed liquid is large-area, and transpiring moisture, and obtain shaping particle.
Hot pressed sintering is filled in model by dry powder, then add flanging heating from limit, single shaft direction, makes shaping and sinter a kind of sintering method simultaneously completed.Hot-press equipment: conventional hot press forms primarily of heating furnace, pressue device, mould and thermometric pressure tester.
Obviously, above-described embodiment is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all execution modes.And these belong to spirit institute's apparent change of extending out of the present invention or change and are still among protection scope of the present invention.
Claims (3)
1. a manufacture method for silicon nitride heat generating body, is characterized in that comprising:
Step 1, silicon nitride powder and high-temperature liquid-phase sintering agent inserted in absolute ethyl alcohol by weight 0.96:0.04 to 0.80:0.20 mix, after batch mixing 10-72 hour, make formulation material through mist projection granulating;
Step 2, metal heating wire is imbedded in described formulation material dry-pressing formed, then compressing further by the isostatic cool pressing of 180-220MPa, and pressurize 3-10 minute, to make biscuit; Described metal heating wire is molybdenum filament;
Step 3, apply one deck boron nitride separator post-drying at described biscuit surface uniform;
Step 4, then carry out hot pressed sintering, sintering pressure 20-30MPa, sintering temperature 1600-1900 DEG C, temperature retention time 0.5-4 hour, to make blank;
Step 5, described blank is put into vacuum atmosphere oven, keep 1300-1600 DEG C of constant temperature 10-24 hour, then naturally cool to room temperature, finally at metal heating wire two ends welding electrode.
2. the manufacture method of silicon nitride heat generating body according to claim 1, is characterized in that: described boron nitride separator is by the thick shape slurry that boron nitride powder and silicon nitride powder mix afterwards and absolute ethyl alcohol reconciles into; Wherein, the part by weight of silicon nitride powder and boron nitride powder is: 0.10:0.90 to 0:1.00.
3. the manufacture method of silicon nitride heat generating body according to claim 2, is characterized in that: in described step 4, when carrying out hot pressed sintering, the hot pressing graphite jig of employing with the contact-making surface of biscuit on scribble boron nitride separator described in one deck.
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| CN201310004176.XA CN103096529B (en) | 2010-12-09 | 2010-12-09 | There is the manufacture method of the silicon nitride heat generating body of higher reliability and fail safe |
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|---|---|---|---|
| CN 201010582116 CN102170716B (en) | 2010-12-09 | 2010-12-09 | Method for manufacturing silicon nitride heating body |
| CN201310004176.XA CN103096529B (en) | 2010-12-09 | 2010-12-09 | There is the manufacture method of the silicon nitride heat generating body of higher reliability and fail safe |
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| CN 201010582116 Division CN102170716B (en) | 2010-12-09 | 2010-12-09 | Method for manufacturing silicon nitride heating body |
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| CN103183512A (en) * | 2011-12-27 | 2013-07-03 | 浙江昱辉阳光能源有限公司 | Preparation method for powder for silicon nitride crucible |
| CN102595665B (en) * | 2012-02-28 | 2014-07-09 | 威海兴泰金属制造有限公司 | Silicon nitride heating sheet and manufacturing method thereof |
| CN105936595A (en) * | 2015-11-28 | 2016-09-14 | 衡阳凯新特种材料科技有限公司 | Silicon nitride heating element and preparation method thereof |
| CN105884375B (en) * | 2016-03-18 | 2018-05-22 | 北方民族大学 | A kind of Si3N4-TiZrN2The lqiuid phase sintering method of-TiN composite conductive ceramics |
| CN106007661A (en) * | 2016-05-23 | 2016-10-12 | 湖南省醴陵市电热电器瓷厂 | Making method of integral ceramic heating body and integral ceramic heating body |
| CN108191434B (en) * | 2018-03-01 | 2020-09-18 | 吉林师范大学 | High-pressure rapid preparation method of high-thermal-conductivity and high-compactness silicon nitride material |
| CN112390629B (en) * | 2020-12-04 | 2022-02-08 | 吉林大学 | Device and method for rapidly sintering ceramic |
| CN115703683B (en) * | 2021-08-17 | 2023-10-20 | 赛默肯(苏州)电子新材料有限公司 | High-strength high-heat-conductivity large-size silicon nitride ceramic and preparation method thereof |
| CN114773067A (en) * | 2022-05-23 | 2022-07-22 | 江苏方大正塬生态环境科技有限公司 | GSPL-SNCS silicon nitride tape-casting slurry |
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| CN1006886B (en) * | 1987-07-06 | 1990-02-21 | 国家建筑材料工业局山东工业陶瓷研究设计院 | Silicone nitride/boron nitride composite and prepn. thereof |
| US5593728A (en) * | 1994-11-01 | 1997-01-14 | Advanced Ceramics Corporation | Interface coating for ceramic fibers |
| CN1076944C (en) * | 1999-03-15 | 2001-12-26 | 广州石潮高性能陶瓷总公司 | Silicon nitride heat generating body and its prodn. method |
| JP4454191B2 (en) * | 2001-07-30 | 2010-04-21 | 日本特殊陶業株式会社 | Manufacturing method of ceramic heater |
| CN1204223C (en) * | 2001-10-09 | 2005-06-01 | 刘庆昌 | Nano-grade silicon nitride composite material heating body and its production process |
| CN1849017A (en) * | 2005-04-05 | 2006-10-18 | 郜长福 | Silicon nitride heating body and its pressureless lower temperature sintering producing method |
| CN101318822B (en) * | 2008-07-04 | 2010-09-01 | 冷水江市明玉陶瓷工具有限责任公司 | Silicon nitride composite ceramics heater |
| CN101434488B (en) * | 2008-12-12 | 2011-12-07 | 哈尔滨工业大学 | Silicon nitride-based composite ceramic with phosphates as sintering aid and preparation thereof |
| CN101665363B (en) * | 2009-09-25 | 2013-04-17 | 长沙隆泰微波热工有限公司 | Additive for silicon nitride sintered bodies |
| CN101885608A (en) * | 2010-07-15 | 2010-11-17 | 武汉工程大学 | Boron nitride nanotube strengthened silicon nitride ceramic material and preparation method thereof |
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| CN102170716B (en) | 2013-01-30 |
| CN103096529A (en) | 2013-05-08 |
| CN102170716A (en) | 2011-08-31 |
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