CN105906348B - A kind of compact silicon nitride ceramic lift tube and the preparation method and application thereof - Google Patents
A kind of compact silicon nitride ceramic lift tube and the preparation method and application thereof Download PDFInfo
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- CN105906348B CN105906348B CN201610230674.XA CN201610230674A CN105906348B CN 105906348 B CN105906348 B CN 105906348B CN 201610230674 A CN201610230674 A CN 201610230674A CN 105906348 B CN105906348 B CN 105906348B
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Abstract
The present invention relates to a kind of compact silicon nitride ceramic lift tube and preparation method thereof, the silicon nitride ceramics stalk is by including that the raw material of 85~95 parts of silicon nitrides and 5~15 component sintering additives is prepared；The sintering aid is selected from one of aluminium oxide, magnesia, yttrium oxide, cerium oxide, titanium carbide or a variety of.The features such as silicon nitride ceramics stalk provided by the invention, density is high, hardness is high, bending strength is high, fracture toughness is strong, and long service life, can be used continuously 1 year or more on conventional low-voltage cast aluminum machine；The present invention passes through the fully optimized to raw material composition and preparation method, solves the problems, such as the production preparation of silicon nitride stalk in cast aluminium industry, improve the quality of critical component in domestic cast aluminium industry, substantially improve aluminum casting production efficiency, production cost is reduced, production efficiency is significantly improved, reduces production cost, be conducive to monopoly position of the breaks through foreign silicon nitride enterprise in the sector, improve China's silicon nitride ceramics level in the cognition degree in the whole world.
Description
Technical field
The present invention relates to extraordinary large-scale silicon nitride ceramics technical fields, and in particular to compact silicon nitride ceramic lift tube and its
Preparation method and application.
Background technique
Silicon nitride ceramics is the best special ceramic material of comprehensive performance, and silicon nitride has high intensity, high rigidity, high fracture
Toughness, heat shock resistance, coefficient of friction are low to be had been widely used in photovoltaic, automobile, metallurgy, chemical industry, the energy, environmental protection, aerospace etc.
Multiple fields.
Stalk is one of the critical component on low-voltage cast aluminum machine, its performance directly affects the quality and life of cast aluminium product
Efficiency is produced, the use environment of stalk is higher to the performance requirement of material, and material requirements has excellent high-temperature behavior, heat-resisting
Pinking is good, resists the erosion of high temperature molten aluminum, does not invade profit with molten aluminum, and have good air-tightness and heat shock resistance fatigability.
The material category of country's stalk mainly has silicon nitride reaction bonded silicon carbide, silicon carbide reaction-sintered, titanium at present
Sour aluminium, cast iron, this kind of material porosity height, intensity difference, accumulated slag are serious, are affected to production efficiency and the quality of production.At present
The reactive sintering of silicon nitride carbofrax material that the enterprise of the country 70% uses Beijing Golden Rainbow Silicon Nitride Company to produce,
Its unit price is 2000 yuan/root.But since mortality is poor, intensity is low, causes service life short, and average out to 2 months.
The production of compact silicon nitride stalk still belongs to blank at home, and production difficulty essentially consists in the formula of suitable performance
Adjustment, molding and the research of sintering process.
Summary of the invention
The purpose of the present invention is overcoming the deficiencies of existing technologies, by raw material composition and preparation method it is comprehensive excellent
Change, a kind of thermal conductivity height, good thermal shock, corrosion-resistant, silicon nitride ceramics stalk with long service life are provided.The present invention is simultaneously
The preparation method of the silicon nitride ceramics stalk is provided, it is scientific and reasonable, it reduces costs.
Specifically, the present invention provides a kind of compact silicon nitride ceramic lift tubes, by the raw material including following parts by weight
It is prepared: 85~95 parts of silicon nitride, 5~15 parts of sintering aid；
The sintering aid is selected from one of aluminium oxide, magnesia, yttrium oxide, cerium oxide, titanium carbide or a variety of.
Parts by weight of the present invention can be the unit of weight well known in the art such as μ g, mg, g, kg, be also possible to it again
Number, such as 1/10,1/100,10 times, 100 times.
As a preferred solution of the present invention, the silicon nitride ceramics stalk is by including prepared by the raw material of following component
It forms: 85~88 parts of silicon nitride, 12~15 parts of sintering aid；The sintering aid is by the oxidation of 4~5:4 of weight ratio~7:3~4
Yttrium, aluminium oxide and cerium oxide composition；
It is further preferred that the silicon nitride ceramics stalk is by including that the raw material of following component is prepared: silicon nitride
85~88 parts, 4~5 parts of yttrium oxide, 4~7 parts of aluminium oxide, 3~4 parts of cerium oxide.
As a preferred solution of the present invention, the silicon nitride ceramics stalk is by including prepared by the raw material of following component
It forms: 88~90 parts of silicon nitride, 10~12 parts of sintering aid；The sintering aid is by the oxidation of 4~5:4 of weight ratio~7:1~4
Yttrium, magnesia and titanium carbide composition；
It is further preferred that the silicon nitride ceramics stalk is by including that the raw material of following component is prepared: silicon nitride
88~90 parts, 4~5 parts of yttrium oxide, 4~7 parts of magnesia, 1~4 part of titanium carbide.
As a preferred solution of the present invention, the silicon nitride ceramics stalk is by including prepared by the raw material of following component
It forms: 90~92 parts of silicon nitride, 8~10 parts of sintering aid；The sintering aid by weight ratio 3~5:3~5 yttrium oxide and oxygen
Change aluminium composition；
It is further preferred that the silicon nitride ceramics stalk is by including that the raw material of following component is prepared: silicon nitride
90~92 parts, 3~5 parts and 3~5 parts of aluminium oxide of yttrium oxide.
The silicon nitride that the present invention uses is preferably powdered, and the silicon nitride powder that average particle size is 50 μm~80 μm can be selected.
In silicon nitride ceramics stalk of the present invention, the total weight parts of preferably above-mentioned each raw material are 100 parts.
In silicon nitride ceramics stalk provided by the invention, raw material composition is simple, carries out to the relative usage of each raw material excellent
Choosing can ensure that obtained product has the comprehensive excellent properties such as density is high, hardness is high, intensity is high, performance is stablized.
Invention also provides the preparation methods of the silicon nitride ceramics stalk, specifically includes the following steps:
(1) by with each raw material is measured, abrasive media deionized water is added, is fully ground to obtain slurry；
(2) slurry is subjected to spray drying treatment, obtains partial size D50For 20 μm~100 μm of granulating raw material powder；
(3) by the granulating raw material it is powder filled enter mold in, handled by cold isostatic compaction, green body be made；
(4) green body obtained by step (3) carries out gas pressure sintering under inert gas conditions, obtains silicon nitride stalk.
In method of the present invention, the total weight of step (1) each raw material and the weight ratio of deionized water are preferred
For 1:1~1.5.The grinding carries out in vertical mixing mill；Preferably in vertical circulation Ball-stirring mill milling time be 4h~
24h.Milling time is controlled the uniformity consistency for being conducive to improve powder in 4h~for 24 hours by the present invention.
In method of the present invention, step (2) spray drying is granulated by way of spray drying, excellent
It is selected as being spray-dried while stirring, to ensure to obtain mobility height, good moldability, the uniform powder of sintering shrinkage.
The granulating raw material diameter of particle D of the acquisition50It is 20 μm~100 μm, preferably 50 μm~80 μm.The present invention is to granulating raw material powder
The partial size of body is controlled, and the efficient molding for improving silicon nitride ceramics stalk is conducive to.
In method of the present invention, step (3) the cold isostatic compaction processing carries out in cold isostatic press.Processing
Pressure is specially 120MPa~300MPa, preferably 120MPa~250MPa.Under above-mentioned pressure condition, the dwell time is preferred
For 5S~60S.The present invention preferably, be further defined the dwell time, be conducive to the pressure of cold isostatic compaction
Improve the consistency of the biscuit of silicon nitride ceramics stalk.
In method of the present invention, step (4) described gas pressure sintering carries out in gas pressure sintering furnace.The item of gas pressure sintering
Part specifically: it with nitrogen is protection gas, 1700~1900 DEG C, be sintered under the conditions of 0.1MPa~10MPa.Under the above conditions, it burns
The time of knot is preferably 1h~2.5h.The present invention carries out preferably, further to sintering time the temperature and pressure of gas pressure sintering
It is defined, is conducive to the compactness for improving the finished product of silicon nitride ceramics stalk.
Sintering processing in step (4) preferably hangs burning or one of horizontal, during product short transverse keep
It is uniform to shrink deformation and higher verticality.
As a preferred solution of the present invention, the preparation method comprises the following steps:
(1) by deionized water with each raw material is measured, is added, the weight ratio of the raw material and deionized water is 1:1~1.5；
4h~for 24 hours is ground in vertical circulation Ball-stirring mill, obtains slurry；
(2) slurry is subjected to spray drying treatment while stirring, obtains partial size D50It is former for 50 μm~80 μm of granulations
Feed powder body；
(3) by the granulating raw material it is powder filled enter mold in, be placed in cold isostatic press, 120MPa~250MPa into
The processing of row isostatic cool pressing, dwell time are 5S~60S, and green body is made；
(4) green body obtained by step (3) is protection gas in 1700~1900 DEG C, 0.1MPa with nitrogen in gas pressure sintering furnace
Gas pressure sintering 1h~2.5h is carried out under the conditions of~10MPa, obtains silicon nitride stalk.
In the method for the invention, without processing to idiosome after sintering, the production of silicon nitride stalk can be obtained
Product.
In preparation method provided by the invention, concrete operations and parameter are carried out preferably, association to be played between each step
Same-action, the silicon nitride ceramics stalk being prepared have the spies such as density is high, hardness is high, bending strength is high, fracture toughness is strong
Point, and long service life can be used continuously 1 year or more on conventional low-voltage cast aluminum machine.
The present invention further protects application of the silicon nitride ceramics stalk on low-voltage cast aluminum.It specifically can be used as low
Component in die casting aluminium machine.
This patent passes through the selection to material system, mist projection granulating, isostatic cool pressing near-net-shape, gas pressure sintering equipment
The research of improvement and design, Fixture Design and sintering process solves the problems, such as the production preparation of silicon nitride stalk in cast aluminium industry,
So as to substantially improve aluminum casting production efficiency by the quality for improving critical component in domestic cast aluminium industry, production is reduced
Cost is conducive to the aluminium casting fast development in market and the competitiveness for improving domestic aluminum casting industry that updates at home, separately
Outside, can monopoly position of the breaks through foreign silicon nitride enterprise in the sector, improve China's silicon nitride ceramics level the whole world recognizing
Degree of knowing.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
The raw material related in following embodiment is all known commercial product.
In order to adapt to the needs of actual production, and it is adapted with technical solution provided by the invention, nitrogen provided by the invention
The specification of SiClx ceramic lift tube is Ф 178* Ф 100*860.
Embodiment 1
A kind of silicon nitride ceramics stalk is present embodiments provided, is made of the following raw material: silicon nitride powder 85kg, oxidation
Yttrium 5kg, aluminium oxide 7kg, cerium oxide 3kg.
The present embodiment provides the preparation method of the silicon nitride ceramics stalk, specific steps simultaneously are as follows:
(1) each raw material is taken, deionized water is added, the total weight of the raw material and the weight ratio of deionized water are 1:1,
10h is ground in vertical circulation Ball-stirring mill, obtains slurry；
(2) slurry is subjected to spray drying treatment while stirring, obtains partial size D50For 50 μm of granulating raw material powder
Body；
(3) by the granulating raw material it is powder filled enter mold in, be placed in cold isostatic press, carried out in 120MPa cold etc. quiet
Green body is made in pressure processing, dwell time 20s；
(4) green body obtained by step (3) is in gas pressure sintering furnace, with nitrogen be protection gas under the conditions of 1730 DEG C, 6MPa into
Row gas pressure sintering, soaking time 2h obtain silicon nitride stalk.
Sample detection (being detected using conventional process in the industry) is carried out on the resulting stalk of the present embodiment, product refers to
Mark specifically: averag density 3.25g/cm3, three-point bending resistance intensity 710MPa, fracture toughness 7.2MPa.m1/2, Vickers hardness
1560, linear expansion coefficient 3.0*10-6/ K, Poisson's ratio 0.28, degree of porosity≤0.06%.Through detecting, provided in this embodiment liter of liquid
Pipe can be used continuously on conventional low-voltage cast aluminum machine more than 1 year.
Embodiment 2
A kind of silicon nitride ceramics stalk similar to Example 1 is present embodiments provided, distinctive points are, described in preparation
The formula of silicon nitride ceramics stalk is different, specifically: silicon nitride powder 88kg, yttrium oxide 4kg, aluminium oxide 4kg, cerium oxide 4kg,
Preparation method is completely the same as embodiment 1.
Correlated performance is under equal conditions detected, this comparative example specific product index and embodiment 1 are without significant difference.
Embodiment 3
A kind of silicon nitride ceramics stalk similar to Example 1 is present embodiments provided, distinctive points are, described in preparation
The formula of silicon nitride ceramics stalk is different, specifically: silicon nitride powder 86kg, yttrium oxide 5kg, aluminium oxide 6kg, cerium oxide 3kg,
Preparation method is completely the same as embodiment 1.
Correlated performance is under equal conditions detected, this comparative example specific product index and embodiment 1 are without significant difference.
Embodiment 4
A kind of silicon nitride ceramics stalk similar to Example 1 is present embodiments provided, distinctive points are, described in preparation
The formula of silicon nitride ceramics stalk is different, specifically: silicon nitride powder 85kg, yttrium oxide 6kg, aluminium oxide 7kg, cerium oxide 2kg,
Preparation method is completely the same as embodiment 1.
Correlated performance is under equal conditions detected, this comparative example specific product index is as follows: averag density 3.24g/
cm3, bending strength 690MPa, fracture toughness 6.5MPa.m1/2, Vickers hardness 1500, remaining parameter and embodiment 1 are without significance difference
It is different.
Embodiment 5
A kind of silicon nitride ceramics stalk is present embodiments provided, is made of the following raw material: silicon nitride powder 88kg, oxidation
Yttrium 4kg, magnesia 5kg, titanium carbide 3kg.
The present embodiment provides the preparation method of the silicon nitride ceramics stalk, specific steps simultaneously are as follows:
(1) each raw material is taken, deionized water is added, the total weight of the raw material and the weight ratio of deionized water are 1:1.5,
8h is ground in vertical circulation Ball-stirring mill, obtains slurry；
(2) slurry is subjected to spray drying treatment while stirring, obtains partial size D50For 60 μm of granulating raw material powder
Body；
(3) by the granulating raw material it is powder filled enter mold in, be placed in cold isostatic press, carried out in 150MPa cold etc. quiet
Green body is made in pressure processing, dwell time 30s；
(4) green body obtained by step (3) is protection gas under the conditions of 1800 DEG C, 10MPa with nitrogen in gas pressure sintering furnace
Gas pressure sintering is carried out, soaking time 1h obtains silicon nitride stalk.
Sample detection, product index are carried out on the resulting stalk of the present embodiment specifically: density 3.26g/cm3,
Three-point bending resistance intensity is 800MPa, fracture toughness 7MPa.m1/2, Vickers hardness 1620, linear expansion coefficient 3.05*10-6/ K, Poisson
Than 0.27, degree of porosity≤0.02%.Through detecting, stalk provided in this embodiment can be continuous on conventional low-voltage cast aluminum machine
It uses more than 1 year.
Embodiment 6
A kind of silicon nitride ceramics stalk similar to Example 5 is present embodiments provided, distinctive points are, described in preparation
The formula of silicon nitride ceramics stalk is different, specifically: silicon nitride powder 89kg, yttrium oxide 4kg, magnesia 4kg, titanium carbide 3kg,
Preparation method is completely the same as embodiment 5.
Correlated performance is under equal conditions detected, this comparative example specific product index and embodiment 5 are without significant difference.
Embodiment 7
A kind of silicon nitride ceramics stalk similar to Example 5 is present embodiments provided, distinctive points are, described in preparation
The formula of silicon nitride ceramics stalk is different, specifically: silicon nitride powder 90kg, yttrium oxide 5kg, magnesia 4kg, titanium carbide 1kg,
Preparation method is completely the same as embodiment 5.
Correlated performance is under equal conditions detected, this comparative example specific product index and embodiment 5 are without significant difference.
Embodiment 8
A kind of silicon nitride ceramics stalk is present embodiments provided, is made of the following raw material: silicon nitride powder 92kg, oxidation
Aluminium 5kg, yttrium oxide 3kg.
The present embodiment provides the preparation method of the silicon nitride ceramics stalk, specific steps simultaneously are as follows:
(1) each raw material is taken, deionized water is added, the total weight of the raw material and the weight ratio of deionized water are 1:1.2,
4h is ground in vertical circulation Ball-stirring mill, obtains slurry；
(2) slurry is subjected to spray drying treatment while stirring, obtains partial size D50For 80 μm of granulating raw material powder；
(3) by the granulating raw material it is powder filled enter mold in, be placed in cold isostatic press, carried out in 250MPa cold etc. quiet
Green body is made in pressure processing, dwell time 40s；
(4) green body obtained by step (3) is protection gas under the conditions of 1800 DEG C, 0.5MPa with nitrogen in gas pressure sintering furnace
Gas pressure sintering is carried out, soaking time 2.5h obtains silicon nitride stalk.
Sample detection, product index are carried out on the resulting stalk of the present embodiment specifically: density 3.24g/cm3,
Three-point bending resistance intensity is 730MPa, fracture toughness 7.5MPa.m1/2, Vickers hardness 1520, linear expansion coefficient 3.1*10-6/ K, Poisson
Than 0.26, degree of porosity≤0.06%.Through detecting, stalk provided in this embodiment can continuously make on conventional low-voltage cast aluminum machine
With more than 1 year.
Embodiment 9
A kind of silicon nitride ceramics stalk similar to Example 8 is present embodiments provided, distinctive points are, described in preparation
The formula of silicon nitride ceramics stalk is different, specifically: silicon nitride powder 90kg, aluminium oxide 5kg, yttrium oxide 5kg, preparation method are complete
Entirely with embodiment 8.
Correlated performance is under equal conditions detected, this comparative example specific product index and embodiment 8 are without significant difference.
Embodiment 10
A kind of silicon nitride ceramics stalk similar to Example 8 is present embodiments provided, distinctive points are, described in preparation
The formula of silicon nitride ceramics stalk is different, specifically: silicon nitride powder 91kg, aluminium oxide 4kg, yttrium oxide 5kg, preparation method are complete
Entirely with embodiment 8.
Correlated performance is under equal conditions detected, this comparative example specific product index and embodiment 8 are without significant difference.
Comparative example 1
This comparative example provides similar silicon nitride ceramics stalk known to one kind, certain specially commercially available domestic producer is raw
The silicon nitride stalk of production.
Correlated performance is under equal conditions detected, this comparative example specific product index is as follows: averag density 3.24g/
cm3, bending strength 652MPa, fracture toughness 6.1MPa.m1/2, Vickers hardness 1481.
Comparative example 2
This comparative example provides a kind of silicon nitride ceramics stalk similar to Example 1, and distinctive points are, described in preparation
The formula of silicon nitride ceramics stalk is different, specifically: silicon nitride powder 83kg, yttrium oxide 6kg, aluminium oxide 9kg, cerium oxide 2kg,
Preparation method is completely the same as embodiment 1.
Correlated performance is under equal conditions detected, this comparative example specific product index is as follows: averag density 3.23g/
cm3, bending strength 632MPa, fracture toughness 6.7MPa.m1/2, Vickers hardness 1480.
Comparative example 3
This comparative example provides a kind of silicon nitride ceramics stalk similar to Example 1, prepares the heater protecting
For the formula of pipe completely with embodiment 1, distinctive points are preparation method difference, specifically: the raw material mix grinding time is in step (1)
2h；Step (2) obtains D50For 120 μm of granulating raw material powder.
Correlated performance is under equal conditions detected, this comparative example specific product index is as follows: averag density 3.23g/
cm3, bending strength 680MPa, fracture toughness 7.2MPa.m1/2, Vickers hardness 1460.
Although above having used general explanation, specific embodiment and test, the present invention is made to retouch in detail
It states, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art
's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed
Range.
Claims (6)
1. a kind of compact silicon nitride ceramic lift tube, which is characterized in that by weight, by the raw material preparation of following component
At: 85~88 parts of silicon nitride, 12~15 parts of sintering aid；The sintering aid is by the oxidation of 4~5:4 of weight ratio~7:3~4
Yttrium, aluminium oxide and cerium oxide composition；Or 88~90 parts of silicon nitride, 10~12 parts of sintering aid；The sintering aid is by weight ratio 4
Yttrium oxide, magnesia and the titanium carbide composition of~5:4~7:1~4；
The ceramic lift tube is prepared using the method included the following steps:
(1) by with each raw material is measured, abrasive media deionized water is added, ground in vertical mixing mill 4h~for 24 hours afterwards slurry；
(2) slurry is spray-dried while stirring, obtains partial size D50For 50 μm~80 μm of granulating raw material powder；
(3) by the granulating raw material it is powder filled enter mold in, in cold isostatic press, pressure maintaining under the conditions of 120MPa~250MPa
Green body is made in 5S~60S；
(4) green body obtained by step (3) carries out gas pressure sintering under inert gas conditions, obtains silicon nitride stalk.
2. silicon nitride ceramics stalk according to claim 1, which is characterized in that the total weight parts of each raw material are 100 parts.
3. the preparation method of silicon nitride ceramics stalk of any of claims 1 or 2, which comprises the following steps:
(1) by with each raw material is measured, deionized water is added, ground in vertical mixing mill 4h~for 24 hours afterwards slurry；
(2) slurry is spray-dried while stirring, obtains partial size D50For 50 μm~80 μm of granulating raw material powder；
(3) by the granulating raw material it is powder filled enter mold in, in cold isostatic press, pressure maintaining under the conditions of 120MPa~250MPa
Green body is made in 5S~60S；
(4) green body obtained by step (3) carries out gas pressure sintering under inert gas conditions, obtains silicon nitride stalk.
4. preparation method according to claim 3, which is characterized in that the total weight of step (1) each raw material and go from
The weight ratio of sub- water is 1:1~1.5.
5. preparation method according to claim 3 or 4, which is characterized in that step (4) described gas pressure sintering specifically:
It is protection gas with nitrogen in gas pressure sintering furnace, 1700~1900 DEG C, 1h~2.5h is sintered under the conditions of 0.1MPa~10MPa.
6. silicon nitride ceramics stalk of any of claims 1 or 2 or claim 3~5 any one the method preparation and
At application of the silicon nitride ceramics stalk on low-voltage cast aluminum.
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| CN107151144A (en) * | 2017-05-27 | 2017-09-12 | 陈国生 | A kind of aluminum alloy low-pressure casting silicon nitride accessory new material and preparation method thereof |
| CN107285740A (en) * | 2017-05-27 | 2017-10-24 | 陈国生 | A kind of aluminum alloy low-pressure casting silicon nitride accessory new material and preparation method thereof |
| CN109467441A (en) * | 2017-09-08 | 2019-03-15 | 苏州玄陶商务咨询有限公司 | The preparation method of bio-medical silicon nitride compositions and silicon nitride ceramics |
| CN107586135A (en) * | 2017-09-26 | 2018-01-16 | 陈凌 | Ceramic composite and its preparation method and application |
| CN107840663A (en) * | 2017-12-23 | 2018-03-27 | 洛阳名力科技开发有限公司 | A kind of silicon nitride ceramics |
| CN108407075A (en) * | 2018-01-02 | 2018-08-17 | 上海华培动力科技股份有限公司 | A kind of stalk preparation method for suction pouring |
| CN108863397A (en) * | 2018-07-13 | 2018-11-23 | 威海圆环先进陶瓷股份有限公司 | A kind of technique preparing SiN ceramic with high heat conductivity crucible |
| CN115667185A (en) * | 2020-05-26 | 2023-01-31 | 株式会社东芝 | Silicon nitride sintered body, wear-resistant member using same, and method for producing silicon nitride sintered body |
| CN111606716A (en) * | 2020-06-08 | 2020-09-01 | 浙江锐克特种陶瓷有限公司 | Silicon nitride wear-resistant sheet prepared based on atmosphere sintering method |
| CN112960984B (en) * | 2021-02-23 | 2022-11-18 | 北京中材人工晶体研究院有限公司 | Silicon nitride ceramic heat radiation protection tube and manufacturing method thereof |
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| CN101348371B (en) * | 2008-09-03 | 2011-02-02 | 山东硅苑新材料科技股份有限公司 | Lift tube for low-voltage cast aluminum and preparation thereof |
| CN101538162B (en) * | 2009-01-21 | 2011-09-14 | 北京中材人工晶体有限公司 | Preparation method for high reliability large-scale silicon nitride ceramic material |
| CN102531612A (en) * | 2010-12-15 | 2012-07-04 | 北京中材人工晶体研究院有限公司 | Silicon nitride material and preparation method of heat insulating disc cover prepared from same |
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