CN107651965A - A kind of silicon nitride ceramic material and preparation method thereof - Google Patents
A kind of silicon nitride ceramic material and preparation method thereof Download PDFInfo
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- CN107651965A CN107651965A CN201711132092.9A CN201711132092A CN107651965A CN 107651965 A CN107651965 A CN 107651965A CN 201711132092 A CN201711132092 A CN 201711132092A CN 107651965 A CN107651965 A CN 107651965A
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Abstract
The present invention relates to silicon nitride ceramic material field, and in particular to a kind of silicon nitride ceramic material and preparation method thereof.The silicon nitride ceramic material by weight percentage, including silicon nitride 86~95%, magnesia 2~4%, aluminum oxide 1~3%, yittrium oxide 2~7%.The preparation method of the silicon nitride ceramic material includes mixing material powder, adds deionized water, polyvinyl alcohol water solution and ammonium polyacrylate and is made into slurry, after drying-granulating, pressing blank, normal pressure, low-temperature sintering obtain finished product.Silicon nitride ceramic material provided by the invention and preparation method thereof, with when ratio, is significantly improved the sintering characteristic of silicon nitride ceramic material, it is sintered under normal pressure, cryogenic conditions by preferred feedstock;By optimization technological process and parameter, the production cost of silicon nitride ceramic material is significantly reduced, improves operating efficiency, make obtained silicon nitride ceramic material that there is higher density, mechanical strength and heat-resisting quantity.
Description
Technical field
The present invention relates to silicon nitride ceramic material field, and in particular to a kind of preparation method of silicon nitride ceramic material.
Background technology
Silicon nitride (Si3N4) ceramics due to height than by force, Gao Bimo, high temperature resistant, anti-oxidant, wear-resistant and anti-thermal shock
The advantages that, high temperature, high speed, strong corrosive medium working environment in there is special use value.In recent years, both at home and abroad competitively
It is researched and developed, its application is constantly expanded.
The technology of preparing of current existing silicon nitride ceramic material mainly has pressure sintering, gas pressure sintering method and normal pressure-sintered
Method.The efficiency of pressure sintering is low, energy consumption is big, allowance is big, cost is high, and can only manufacture the extremely simple product of shape, no
Adapt to the requirement of industrialization;Gas pressure sintering method is the production technology of the silicon nitride ceramic material of current main flow, but gas pressure sintering method
Requirement to sintering furnace is high, virtually increases the manufacturing cost of silicon nitride ceramic material.Normal pressure-sintered method is simplest burning
Knot mode, but very high sintering temperature is needed, beta-silicon nitride powder easily decomposes at high temperature, therefore has both ensured that silicon nitride ceramics existed
Densification sintering at relatively low temperature, while ensure beta-silicon nitride powder not severe decomposition again, it is that normal pressure-sintered silicon nitride ceramics needs
The subject matter to be solved.
The content of the invention
For the efficiency in existing silicon nitride ceramics technology of preparing is low, cost is high, high temperature easily decomposes beta-silicon nitride powder
The problem of, the present invention provides a kind of silicon nitride ceramic material.
Further, the present invention also provides a kind of preparation method of silicon nitride ceramic material.
To achieve the above object of the invention, the embodiment of the present invention employs following technical scheme:
A kind of silicon nitride ceramic material, counted using the raw material gross weight of the silicon nitride ceramic material as 100%, including it is following
The raw material of percentage by weight:
In silicon nitride ceramic material provided by the invention, silicon nitride is main component, and magnesia, can be with as sintering aid
Ensure that raw material forms liquid phase and highdensity silicon nitride material is made at a lower temperature, aluminum oxide can not only strengthen oxidation
Effect of the yttrium as sintering aid, improve made ceramic density under sintering temperature and low, moreover it is possible to suppress growing up for crystal grain, improve system
The mechanical strength of product, yittrium oxide can form the liquid phase for promoting ceramic material sintering, make this mutually in sintering with nitrogenizing pasc reaction, shape
Into resistant to elevated temperatures Binder Phase, so as to generate heat-resisting quantity more preferably ceramic material.The present invention uses preferable raw material proportioning, can be with
It is more suitable for the preparation technology of normal pressure, low temperature, and make there is higher density, mechanical strength and stronger heat-resisting quantity
Silicon nitride ceramic material.
Further, the present invention also provides a kind of preparation method of silicon nitride ceramic material, and the preparation method is at least wrapped
Include following steps:
Step 1, the powder for weighing according to the raw material proportioning of silicon nitride ceramic material each raw material components, obtained after well mixed
Mixed-powder;
Step 2, deionized water is added into step 1 gained mixed-powder, be that abrasive media mixes to described using silicon nitride ball
Close powder to be ground, polyvinyl alcohol water solution and ammonium polyacrylate are added in process of lapping, is made into slurry;
Step 3, after step 2 gained slurry is dried into granulation, it is pressed into base substrate;
Step 4, step 3 gained base substrate is warming up to 500~600 DEG C under vacuum, is incubated 1~3h;
Step 5, under inert atmosphere conditions, step 4 gained base substrate is warming up to 1550~1650 DEG C, 1~4h is sintered, obtains
To finished product.
Relative to prior art, the preparation method of silicon nitride ceramic material provided by the invention need to only be burnt at ambient pressure
Knot, required sintering temperature are less than normal temperature sintering temperature of the prior art, silicon nitride can be avoided to decompose.And the preparation method is grasped
Make simply, process is easily controlled, and is suitable for big production operation.
Brief description of the drawings
Technical scheme in order to illustrate the embodiments of the present invention more clearly, it will use below required in embodiment
Accompanying drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for ability
For the those of ordinary skill of domain, on the premise of not paying creative work, it can also be obtained according to these accompanying drawings other attached
Figure.
Fig. 1 is the X-ray diffractogram for the silicon nitride ceramic material being prepared using the preparation method of the embodiment of the present invention
Spectrum.
Fig. 2 is the section SEM spectrum for the silicon nitride ceramic material being prepared using the preparation method of the embodiment of the present invention.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
The embodiment of the present invention provides a kind of silicon nitride ceramics, using the raw material gross weight of the silicon nitride ceramic material as
100% meter, include the raw material of following percentage by weight:
In silicon nitride ceramic material provided by the invention, silicon nitride is main component, and magnesia, can be with as sintering aid
Ensure and form liquid phase at a lower temperature and highdensity silicon nitride material is made, content of magnesia is too high, then can influence material
The mechanical property of material;The liquid phase of acceleration of sintering can be formed by introducing yittrium oxide in silicon nitride in sintering or relative low temperature hot pressing,
This mutually sintering when higher temperature under with nitrogenize pasc reaction, form resistant to elevated temperatures Binder Phase, these Binder Phases along nitridation silicon wafer
Boundary configures, and can ensure material has more preferably heat-resisting quantity, with the increase of yttria levels, excessive bonding phase oxidation
When with great volume it is corresponding, the inoxidizability of silicon nitride material can be reduced;Aluminum oxide is introduced in silicon nitride material, no
Effect of the yittrium oxide as sintering aid can only be strengthened, improve the density under sintering temperature and low, moreover it is possible to suppress growing up for crystal grain,
The mechanical strength of product is improved, but aluminum oxide introduction volume is too high, can cause uneven distribution of each component in Grain-Boundary Phase, reduces
Life of product.The present invention uses preferable raw material proportioning, it can be made to be more suitable for the preparation technology of normal pressure, low temperature, and make tool
There is the silicon nitride ceramic material of higher density, mechanical strength and stronger heat-resisting quantity.
Specifically, the mass percentage content of α-siliconnitride is 90~99.94% in the silicon nitride, the matter of beta-silicon nitride
It is 0~9% to measure degree, the mass percentage content that the mass percentage content of oxygen is 0~1.5%, Fe is 0.05~
0.2%, Ca mass percentage content are 0.01~0.07%.Too high oxygen level can influence the machinery after silicon nitride ceramics sintering
Performance;More than 90% α phase contents are the basic demands of the beta-silicon nitride powder for ceramic post sintering;Fe in silicon nitride powder body,
Ca contents contribute to the raising of sintering activity, and too low Fe, Ca content is difficult in 1600 DEG C of sintering, and too high Fe, Ca content
Finished product machinery intensity decreases can be caused.
Further, the silicon nitride is as obtained by prepared by nitride metal method.Nitride metal method can be by controlling gold
The addition of metal catalyst controls the mass percentage content of α-siliconnitride and beta-silicon nitride in silicon nitride, and controls silicon nitride
In tenor, meet the required silicon nitride raw material of the present invention so as to produce.
Further, the embodiment of the present invention also provides a kind of preparation method of silicon nitride ceramic material, the preparation method
Including at least following steps:
Step 1, the powder for weighing according to the raw material proportioning of silicon nitride ceramic material each raw material components, obtained after well mixed
Mixed-powder;
Step 2, deionized water is added into step 1 gained mixed-powder, be that abrasive media mixes to described using silicon nitride ball
Close powder to be ground, polyvinyl alcohol water solution and ammonium polyacrylate are added in process of lapping, is made into slurry;
Step 3, after step 2 gained slurry is dried into granulation, it is pressed into base substrate;
Step 4, step 3 gained base substrate is warming up to 500~600 DEG C under vacuum, is incubated 1~3h;
Step 5, under inert atmosphere conditions, step 4 gained base substrate is warming up to 1550~1650 DEG C, 1~4h is sintered, obtains
To finished product.
Relative to prior art, the preparation method of silicon nitride ceramic material provided by the invention need to only be burnt at ambient pressure
Knot, required sintering temperature are less than normal temperature sintering temperature of the prior art, silicon nitride can be avoided to decompose.And the preparation method is grasped
Make simply, process is easily controlled, and is suitable for big production operation.
Specifically, in above-mentioned steps 1, the powder diameter of the raw material components is 0.1~1 μm.Powder granularity is small, sinters
It is active high, contribute to the sintering of ceramics, the sintering character of material powder of the granularity more than 1 μm is excessively poor, influences the suitable of preparation technology
Profit carries out and product quality.
In above-mentioned steps 2, the solid content of the slurry is 40~60%.The too high then slurry of solid content is excessively thick, easily makes
Raw material mixing is uneven, and solid content is too low, causes grinding efficiency to reduce, and reduces production efficiency;The polyvinyl alcohol water solution
Mass concentration is 5~8%, and preferable polyvinyl alcohol water solution concentration has preferable viscosity, is advantageous to make slurry form particle;
The mass percent concentration of polyvinyl alcohol and the ammonium polyacrylate described in the slurry is 0.8~1.2%, preferable poly-
The dosage of vinyl alcohol and ammonium polyacrylate is more beneficial for forming slurry to be molded during drying-granulating.
In above-mentioned steps 3, the drying-granulating include ball milling be granulated, mist projection granulating, preferable drying-granulating mode can be with
It is dried simultaneously during granulation, dry particl can be made within a short period of time, reduce time cost;The compacting
Including dry-pressing, isostatic cool pressing, pressure is 80~200MPa, and more than 80MPa briquetting pressure just can guarantee that base substrate has enough
Intensity, but briquetting pressure is excessive, easily ceramic body is ftractureed.
In above-mentioned steps 4, the sintering at least comprises the following steps:500~600 DEG C are warming up under vacuum condition, insulation 1
~3h.500-600 DEG C of dump temperature is the decomposition temperature of institute's adding additives, can ensure to arrange as far as possible under the temperature, time conditions
The completion of glue.
It is further preferred that the speed of the heating is 1~6 DEG C/min.Heat up at such speeds, base substrate can be made faster
Ground reaches 500~600 DEG C, hence it is evident that shortens the production cycle.
In above-mentioned steps 5, under inert atmosphere conditions, step 4 gained base substrate is warming up to 1550~1650 DEG C, sintering 1
~4h, obtains finished product.Temperature can cause a large amount of decomposition of silicon nitride more than 1650 DEG C when normal pressure-sintered, therefore preferably by silicon nitride
Ceramics carry out dense sintering below 1650 DEG C.
It is further preferred that the inert atmosphere is nitrogen atmosphere, nitrogen does not chemically react with material, can avoid producing
Raw impurity;One of silicon nitride catabolite is nitrogen, and increase nitrogen pressure can suppress the positive progress of the decomposition reaction, reduce
The decomposition of silicon nitride.
It is further preferred that the pressure of the inert atmosphere is 10~50kPa, under the pressure condition, inert gas can
So that the air in sintering furnace is discharged out of the furnace, influence of the oxygen to production process and product quality in air, pressure are avoided
It is too small, it is insufficient to allow air to be fully drained, pressure is excessive, can cause the energy waste of nitrogen and dynamical system.
It is further preferred that the speed of the heating is 1~6 DEG C/min.At such speeds, base substrate can be made quickly to reach
To sintering temperature, hence it is evident that shorten the production cycle.Generally, should be heated up during sintering under extremely slow speed, but the application is excellent
The raw material proportioning and technological process and parameter of silicon nitride ceramics are changed, it is possible to heated up, carried under faster speed
High production efficiency, reduces time cost and power source cost.
It is further preferred that described be sintered in high-temperature vacuum sintering furnace is carried out.The application optimizes silicon nitride ceramics
It raw material proportioning and production technology, can at ambient pressure be sintered, and not need too high sintering temperature, therefore need not make
With special sintering furnace, conventional high-temperature vacuum sintering furnace can be used, so as to reduce production cost.
Silicon nitride ceramic material provided by the invention, with when ratio, significantly improves silicon nitride pottery by preferred feedstock
The sintering characteristic of ceramic material, it is set to be sintered under normal pressure, cryogenic conditions.The present invention passes through optimization technological process and ginseng
Number, the production cost of silicon nitride ceramic material is significantly reduced, improve operating efficiency, and make obtained silicon nitride ceramic material tool
There are higher density, mechanical strength and heat-resisting quantity.
In order to better illustrate embodiment of the present invention, illustrated below by embodiment is further.
Embodiment 1
The embodiment of the present invention provides a kind of preparation method of silicon nitride ceramic material, comprises the following steps:
Step 1, by mass percent be 92% silicon nitride powder, 2% magnesium oxide powder, 2% aluminum oxide thing powder,
4% yttrium oxide powder mixing, mixed-powder is obtained, wherein silicon nitride raw material powder contains α-nitrogen that mass percent is 95%
SiClx, 3.8% beta-silicon nitride, 1.1% oxygen, 0.08% Fe impurity, 0.02% Ca impurity, and average grain diameter is 0.86
μm;
Step 2, deionized water is added into step 1 gained mixed-powder, be that abrasive media mixes to described using silicon nitride ball
Close powder to be ground 24 hours, the polyvinyl alcohol water solution and poly- third that mass percent concentration is 6% is added in process of lapping
Olefin(e) acid ammonium, slurry is made into, the solid content of gained slurry is 40%, and wherein the mass percentage content of polyvinyl alcohol is 0.8%, is gathered
The mass percentage content of ammonium acrylate is 1.2%;
Step 3, after step 2 gained slurry is dried into granulation with ball milling comminutor, under 160MPa molding pressure
It is pressed into the base substrate of multiple 50mm*50mm*5mm for bending strength and hardness test;
Step 4, step 3 gained base substrate is warming up to 500 DEG C with 2 DEG C/min speed under vacuum, is incubated 3h.
Step 5,20kPa nitrogen protection under, step 4 gained base substrate is warming up to 1600 DEG C with 2 DEG C/min speed,
3h is sintered, obtains finished product.
Embodiment 2
The embodiment of the present invention provides a kind of silicon nitride ceramic material, and its preparation method comprises the following steps:
Step 1, by mass percent be 90% silicon nitride powder, 2% magnesium oxide powder, 3% aluminum oxide thing powder,
The oxide powder mixing of 5% yttrium, obtains mixed-powder, wherein silicon nitride raw material powder contain α that mass percent is 92%-
Silicon nitride, 6.49% beta-silicon nitride, 1.3% oxygen, 0.15% Fe impurity, 0.06% Ca impurity, and average grain diameter is
0.70μm;
Step 2, deionized water is added into step 1 gained mixed-powder, be that abrasive media mixes to described using silicon nitride ball
Close powder to be ground 24 hours, the polyvinyl alcohol water solution and poly- third that mass percent concentration is 5% is added in process of lapping
Olefin(e) acid ammonium, slurry is made into, the solid content of gained slurry is 60%, and wherein the mass percentage content of polyvinyl alcohol is 1.0%, is gathered
The mass percentage content of ammonium acrylate is 1.0%;
Step 3, after step 2 gained slurry is dried into granulation with sponging granulator, under 200MPa molding pressure
It is pressed into the base substrate of multiple 50mm*50mm*5mm for bending strength and hardness test;
Step 4, step 3 gained base substrate is warming up to 550 DEG C with 3 DEG C/min speed under vacuum, is incubated 2h.
Step 5,15kPa nitrogen protection under, step 4 gained base substrate is warming up to 1570 DEG C with 3 DEG C/min speed,
4h is sintered, obtains finished product.
Embodiment 3
The embodiment of the present invention provides a kind of silicon nitride ceramic material, and its preparation method comprises the following steps:
Step 1, by mass percent be 86% silicon nitride powder, 4% magnesium oxide powder, 3% aluminum oxide thing powder,
The oxide powder mixing of 7% yttrium, obtains mixed-powder, wherein silicon nitride raw material powder contain α that mass percent is 96%-
Silicon nitride, 3.06% beta-silicon nitride, 0.8% oxygen, 0.11% Fe impurity, 0.03% Ca impurity, and average grain diameter is
0.72μm;
Step 2, deionized water is added into step 1 gained mixed-powder, be that abrasive media mixes to described using silicon nitride ball
Close powder to be ground 24 hours, the polyvinyl alcohol water solution and poly- third that mass percent concentration is 8% is added in process of lapping
Olefin(e) acid ammonium, slurry is made into, the solid content of gained slurry is 50%, and wherein the mass percentage content of polyvinyl alcohol is 1.2%, is gathered
The mass percentage content of ammonium acrylate is 0.8%;
Step 3, after step 2 gained slurry is dried into granulation with sponging granulator, under 100MPa molding pressure
It is pressed into the base substrate of multiple 50mm*50mm*5mm for bending strength and hardness test;
Step 4, step 3 gained base substrate is warming up to 570 DEG C with 1 DEG C/min speed under vacuum, is incubated 1h.
Step 5,15kPa nitrogen protection under, step 4 gained base substrate is warming up to 1550 DEG C with 4 DEG C/min speed,
2h is sintered, obtains finished product.
Embodiment 4
The embodiment of the present invention provides a kind of silicon nitride ceramic material, and its preparation method comprises the following steps:
Step 1, by mass percent be 95% silicon nitride powder, 2% magnesium oxide powder, 1% aluminum oxide thing powder,
The oxide powder mixing of 2% yttrium, obtains mixed-powder, wherein silicon nitride raw material powder contain α that mass percent is 94%-
Silicon nitride, 4.98% beta-silicon nitride, 0.9% oxygen, 0.07% Fe impurity, 0.05% Ca impurity, and average grain diameter is
0.75μm;
Step 2, deionized water is added into step 1 gained mixed-powder, be that abrasive media mixes to described using silicon nitride ball
Close powder to be ground 24 hours, the polyvinyl alcohol water solution and poly- third that mass percent concentration is 7% is added in process of lapping
Olefin(e) acid ammonium, slurry is made into, the solid content of gained slurry is 45%, and wherein the mass percentage content of polyvinyl alcohol is 1.2%, is gathered
The mass percentage content of ammonium acrylate is 1.2%;
Step 3, after with ball milling comminutor, step 2 gained slurry is dried, it is pressed under 80MPa molding pressure
For bending strength and multiple 50mm*50mm*5mm of hardness test base substrate;
Step 4, step 3 gained base substrate is warming up to 600 DEG C with 5 DEG C/min speed under vacuum, is incubated 1.5h.
Step 5,15kPa nitrogen protection under, step 4 gained base substrate is warming up to 1650 DEG C with 6 DEG C/min speed,
1h is sintered, obtains finished product.
In order to better illustrate the characteristic of silicon nitride ceramic material provided in an embodiment of the present invention, prepared by embodiment 1
Silicon nitride ceramic material carries out XRD detections, SEM electron-microscope scannings respectively, as a result respectively as shown in Figure 1 and Figure 2.
From figure 1 it appears that α-nitridation in the silicon nitride ceramic material being prepared using method provided by the invention
Silicon is completely reformed into beta-silicon nitride, and silicon nitride ceramics made from explanation possesses sufficient intensity.Grain-Boundary Phase is mainly MgSiO3-
SiO2、Y4Si2O7N2Etc. compound, wherein Y4Si2O7N2There is fabulous intensity at high temperature, and the intensity of silicon nitride ceramics by
The influence of Grain-Boundary Phase is received, high Grain-Boundary Phase intensity can make final products possess high intensity.
From figure 2 it can be seen that the silicon nitride ceramic material being prepared using method provided by the invention is hardly deposited
In porosity, and crystal grain is tiny, uniform, and silicon nitride ceramic material made from explanation possesses good mechanical performance.
Silicon nitride ceramic material prepared by embodiment 1~4 carries out performance test, and testing result is as shown in table 1 below, specifically
's:The consistency of silicon nitride ceramic material>99%, bending strength>500MPa, material fracture toughness>6.2MPam1/2, Vickers
Hardness is 14.5~15.5GPa.
Table 1
From above experimental result, the preparation method of silicon nitride ceramic material provided by the present invention can drop in unobvious
On the premise of lower silicon nitride ceramic material mechanical performance, sintering temperature and sintering pressure are reduced, production cost is greatly reduced, makes
The application field of silicon nitride ceramics gets a promotion.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modification, equivalent substitution or improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (10)
1. a kind of silicon nitride ceramic material, it is characterised in that using the raw material gross weight of the silicon nitride ceramic material as 100%
Meter, include the raw material of following percentage by weight:
2. silicon nitride ceramic material according to claim 1, it is characterised in that:The quality of α-siliconnitride in the silicon nitride
Degree is 90~99.94%, and the mass percentage content of beta-silicon nitride is 0~9%, and the mass percentage content of oxygen is
The mass percentage content that 0~1.5%, Fe mass percentage content are 0.05~0.2%, Ca is 0.01~0.07%.
3. silicon nitride ceramic material according to claim 2, it is characterised in that:The silicon nitride is by nitride metal method
Prepare gained.
A kind of 4. preparation method of silicon nitride ceramic material, it is characterised in that:The preparation method comprises at least following steps:
Step 1, according to the raw material proportioning of the silicon nitride ceramic material described in any one of claims 1 to 3 weigh each raw material components
Powder, obtain mixed-powder after well mixed;
Step 2, deionized water is added into step 1 gained mixed-powder, be abrasive media to the mixed powder using silicon nitride ball
End is ground, and polyvinyl alcohol water solution and ammonium polyacrylate are added in process of lapping, is made into slurry;
Step 3, after step 2 gained slurry is dried into granulation, it is pressed into base substrate;
Step 4, step 3 gained base substrate is warming up to 500~600 DEG C under vacuum, is incubated 1~3h;
Step 5, under inert atmosphere conditions, step 4 gained base substrate is warming up to 1550~1650 DEG C, 1~4h is sintered, obtains into
Product.
5. the preparation method of silicon nitride ceramic material according to claim 4, it is characterised in that:Described in the step 4
The speed to be heated up described in heating and the step 5 is 1~6 DEG C/min.
6. the preparation method of silicon nitride ceramic material according to claim 4, it is characterised in that:Described in the step 5
Inert atmosphere includes nitrogen atmosphere.
7. the preparation method of silicon nitride ceramic material according to claim 4, it is characterised in that:Described in the step 5
The pressure of inert atmosphere is 10~50kPa.
8. the preparation method of silicon nitride ceramic material according to claim 4, it is characterised in that:Described in the step 1
The powder diameter of raw material components is 0.1~1 μm.
9. the preparation method of silicon nitride ceramic material according to claim 4, it is characterised in that:Described in the step 2
The solid content of slurry is 40~60%;And/or
The mass percent concentration of polyvinyl alcohol water solution described in the step 2 is 5~8%;And/or
The mass percent concentration of polyvinyl alcohol and the ammonium polyacrylate described in slurry is 0.8 described in the step 2
~1.2%.
10. the preparation method of silicon nitride ceramic material according to claim 4, it is characterised in that:Described in the step 3
Drying-granulating includes ball milling granulation, mist projection granulating;And/or
Compacting includes dry-pressing, isostatic cool pressing described in the step 3, and pressure is 80~200MPa.
It is sintered in high-temperature vacuum sintering furnace and carries out described in the step 5.
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