CN102170716B - Method for manufacturing silicon nitride heating body - Google Patents
Method for manufacturing silicon nitride heating body Download PDFInfo
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- CN102170716B CN102170716B CN 201010582116 CN201010582116A CN102170716B CN 102170716 B CN102170716 B CN 102170716B CN 201010582116 CN201010582116 CN 201010582116 CN 201010582116 A CN201010582116 A CN 201010582116A CN 102170716 B CN102170716 B CN 102170716B
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- silicon nitride
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- biscuit
- boron nitride
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Abstract
The invention relates to a method for manufacturing a silicon nitride heating body, which comprises the following steps of: charging silicon nitride powder and a small amount of high-temperature liquid phase combustion assisting agent into anhydrous ethanol for mixing; after mixing for 10-72 hours, spraying and granulating to obtain a prescription material; then embedding a metal heating wire into the prescription material and drily pressing for moulding; further pressing for moulding by the cold isostatic pressure of 180-220MPa and keeping for 3-12 minutes to obtain a biscuit; then uniformly coating a boron nitride isolating layer on the surface of the biscuit, drying; carrying out hot press sintering at the sintering pressure of 20-30MPa, the sintering temperature of 1,600-1,900 DEG C and the temperature keeping time of 0.5-4 hours to obtain a blank; and finally, charging the blank into a vacuum atmosphere furnace, keeping the constant temperature of 1,300-1,600 DEG C for 10-24 hours and then naturally cooling to room temperature. The born nitride isolating layer is thick slurry which is formed by mixing boron nitride powder with the silicon nitride powder and blending the mixture with the anhydrous ethanol.
Description
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 can't sintering, must add a small amount of sintering agent and form liquid phase at high temperature, carries out liquid-phase sintering, just can obtain the silicon nitride material of excellent performance.Additive commonly used 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, TiN, the nitride such as ZrN.The high-performance silicon nitride ceramics has excellent electricity, calorifics and the mechanical property such as insulation, high-strength, high temperature resistant, resistance to oxidation, heat shock resistance and high-termal conductivity.
Silicon nitride heating plate is a kind of device in conjunction with high-performance silicon nitride ceramics matrix and powerful high-temperature metal heating wire of long-life.It is little to have volume, and the large and heat efficiency high of power also is proved to be a kind of safe and reliable heating system simultaneously.Behind the direct-electrifying, temperature is done on the surface can reach 1200 degrees centigrade, and working life reached 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, there is the phenomenon of carburizing in the silicon nitride heating sheet material in market more, and surface distributed has the phenomenons such as bulk blackspot, black patch from the appearance, and color and luster is inhomogeneous.Pure Si
3N
4The true qualities of dense sintering material should be canescence, and existing product exists matrix black mostly, and surface uniform or uneven distribution pore more have surface distributed that the phenomenons such as bulk blackspot, black patch are arranged.This mainly be in the hot pressed sintering process since biscuit directly contact with graphite, carbon infiltrates along liquid channel, dissolve in the liquid phase, or with silicon nitride react the generation.The insulation property of the deteriorated material of infiltration meeting of carbon reduce safety and reliability.Simultaneously because the hot pressed sintering time is short, rely on mechanical pressure to strengthen fine and close effect, the material that obtains exists that boundary stress is large, the inadequate microstructure of liquid phase crystallization, affects the useful life of basis material.
Summary of the invention
The technical problem to be solved in the present invention provides 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 comprises:
Step 1, silicon nitride powder and high-temperature liquid-phase sintering agent inserted in the 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, described formulation material is dry-pressing formed after, further compressing 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 ℃, temperature retention time 0.5-4 hour, to make blank;
Step 5, described blank is put into vacuum atmosphere oven, keep 1300-1600 ℃ constant temperature 10-24 hour, then naturally cool to room temperature.
Further, described boron nitride separator is to mix thick shape slurry rear and that absolute ethyl alcohol reconciles into by boron nitride powder and silicon nitride powder; Wherein, the part by weight of silicon nitride powder and boron nitride powder is: 0.10: 0.90 to 0: 1.00.
Further, in the described step 4, when carrying out hot pressed sintering, scribble the described boron nitride separator of one deck on the hot pressing graphite jig and contact-making surface biscuit of employing.
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, TiN, the nitride such as ZrN, addition are 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%.The common metal oxide 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 form, and through forming of green body, makes compact silicon nitride base heater after hot pressed sintering and the high-temperature heat treatment.This heater has the characteristics of high-strength, high thermal conductance, high reliability.Wherein the biscuit surface has boron nitride powder (BN) coating, and this technique has been eliminated the infiltration of carbon in the production process.High-temperature heat treatment process has been eliminated material stress, has promoted the crystallization of grain boundary glassy phase, has greatly improved device reliability and fail safe.(2) in the manufacture method of silicon nitride heat generating body of the present invention, as medium, ball milling mixing 10-72 hour had both guaranteed that batch mixing was even, had reduced again oxidative phenomena with absolute ethyl alcohol (99.9% purity).Do not add any macromolecule modifier in the manufacturing process of the present invention.Some polymeric additive can improve the performance of biscuit and improve the shaping finished product rate, yet the biscuit of this technological forming must through the sticking technique of row, be got rid of polymeric additive.In general, the sticking carbon that can get rid of to greatest extent and burn in the polymeric additive of row under oxygen atmosphere.And that silicon nitride can only be arranged under vacuum or nitrogen protection atmosphere is sticking, thoroughly eliminates relatively difficulty of carbon, is evenly distributed in the biscuit so always stay the residue of some carbon containings, can reduce insulated with material and reliability.The present invention does not adopt any macromolecule additive, but relies on dry-pressing and isostatic cool pressing technique to prepare high-intensity biscuit.(3) among the present invention, the biscuit surface uniform is coated with the BN separator, can stop biscuit to contact with the direct of graphite, has eliminated the possibility of high temperature case-carbonizing element.(4) the present invention is behind hot pressed sintering, and the material stress of silicon nitride heat generating body is larger, is slow cooling to room temperature after at high temperature annealing in process 10-24 hour, can eliminate the stress of material.In addition, in high-temperature process, make the glassy phase crystallization in the material, can further eliminate remaining carbon 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 are made biscuit, biscuit surface-coated BN material through dry-pressing and isostatic cool pressing.Biscuit hot pressed sintering under HTHP becomes blank.Sintering blank high-temperature heat treatment process is eliminated material stress and glass ceramics mutually, has the characteristics of higher reliability and fail safe.
Description of drawings
For content of the present invention is more likely to be clearly understood, below the specific embodiment and by reference to the accompanying drawings of basis, the present invention is further detailed explanation, wherein
Fig. 1 is the structural representation of the silicon nitride heat generating body among the embodiment.
Reference numeral: 1--silicon nitride heat generating body, 2--metal heating wire, 3--electrode.
Embodiment
The present invention is described in detail below in conjunction with drawings and Examples:
(embodiment 1)
The silicon nitride heat generating body of present embodiment is comprised of silicon nitride heating and the high-temperature metal heating wire of being located in the silicon nitride heat generating body.The 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 the absolute ethyl alcohol by weight 0.96: 0.04 to 0.80: 0.20 mix (specifically can adopt ballmillmixer to mix), after batch mixing 10-72 hour, make formulation material through mist projection granulating;
Step 2, the metal heating wire is imbedded in the described formulation material dry-pressing formed, then the isostatic cool pressing by 180-220MPa is further compressing, 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 ℃, temperature retention time 0.5-4 hour, to make blank;
Step 5, described blank is put into vacuum atmosphere oven, keep 1300-1600 ℃ constant temperature 10-24 hour, then naturally cool to room temperature, at last at metal heating wire two ends welding electrode.
Described boron nitride separator is to mix thick shape slurry rear and that absolute ethyl alcohol reconciles into by boron nitride powder and silicon nitride powder; Wherein, the part by weight of silicon nitride powder and boron nitride powder is: 0.10: 0.90 to 0: 1.00.
In the described step 4, when carrying out hot pressed sintering, scribble the described boron nitride separator of one deck on the hot pressing graphite jig and contact-making surface biscuit of employing.
(embodiment 2)
On the basis of embodiment 1, the manufacture method of the silicon nitride heat generating body of present embodiment comprises:
With the silicon nitride powder of 92wt%, the Al of 3wt%
2O
3, the Y of 3wt%
2O
3, the MgO of 1wt%, the AlN of 1wt% add 99.9% absolute ethyl alcohol and evenly mixed 72 hours, then insert in the explosion-proof mist projection granulating tower mist projection granulating and make formulation material.
Formulation material is poured in the mould, again the metal heating wire is imbedded in the powder dry-pressing formedly, be of a size of 120*20*10.With dry-pressing formed biscuit encapsulation, put into isostatic cool pressing equipment and wait static pressure to process again, the pressure that waits static pressure is 200MPa, dwell time 3-10 minute.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 of handling well is put into mould.Mould is put into hot pressing furnace, and at 1800 degrees centigrade, 25MPa compacting 2 hours naturally is cooled to 50 degrees centigrade and comes out of the stove with interior.Blank behind the sintering is put into heat-treatment furnace, flowing nitrogen protection, 1300-1500 degree centigrade be incubated altogether 15 hours after, slow cooling to room temperature is come out of the stove.The fever tablet blank of making is processed through surfacing, and the subsequent techniques such as soldering are made the silicon nitride heating plate of high-performance and high reliability.
Relevant isostatic cool pressing: under the normal temperature, powder is placed in the middle of the airtight liquid environment, liquid transfer superhigh pressure makes powder compacting.Because pressure equates in the liquid everywhere, so the static pressure such as be.Again owing to being under the normal temperature, so be isostatic cool pressing.Working temperature is the static pressure such as temperature in the time of 100-200 ℃.Working temperature is higher then to be high temperature insostatic pressing (HIP).What have reaches 2000 ℃
Traditional spray granulation all is to pass into hot blast in drying tower, by contacting with feed liquid is large-area, and transpiring moisture, and obtain the particle of moulding.
Hot pressed sintering is that dry powder is filled in the model, adds the flanging heating from single shaft direction limit, a kind of sintering method that moulding and sintering are finished simultaneously again.Hot-press equipment: hot press commonly used mainly is comprised of heating furnace, pressue device, mould and thermometric pressure tester.
Obviously, above-described embodiment only is for example of the present invention clearly is described, and is not to be 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 need not also can't give all execution modes exhaustive.And these belong to apparent variation or the change that spirit of the present invention extended out and still are among protection scope of the present invention.
Claims (3)
1. the manufacture method of a silicon nitride heat generating body is characterized in that comprising:
Step 1, silicon nitride powder and high-temperature liquid-phase sintering agent inserted in the 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, the metal heating wire is imbedded in the described formulation material dry-pressing formed, then the isostatic cool pressing by 180-220MPa is further compressing, 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 ℃, temperature retention time 0.5-4 hour, to make blank;
Step 5, described blank is put into vacuum atmosphere oven, keep 1300-1600 ℃ constant temperature 10-24 hour, then naturally cool to room temperature, at last 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 after being mixed by boron nitride powder and silicon nitride powder and the thick shape slurry that reconciles into of absolute ethyl alcohol; 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 the described step 4, when carrying out hot pressed sintering, scribble the described boron nitride separator of one deck on the hot pressing graphite jig and contact-making surface biscuit of employing.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010582116 CN102170716B (en) | 2010-12-09 | 2010-12-09 | Method for manufacturing silicon nitride heating body |
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| CN201310004176.XA Division 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 |
| CN201310003718.1A Division CN103096528B (en) | 2010-12-09 | 2010-12-09 | Preparation method for silicon nitride heating body |
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| CN102170716B true CN102170716B (en) | 2013-01-30 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Also Published As
| Publication number | Publication date |
|---|---|
| CN103096529A (en) | 2013-05-08 |
| CN103096529B (en) | 2016-04-06 |
| CN102170716A (en) | 2011-08-31 |
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