CN109665851A - The preparation method of multistage twin structure silicon nitride high-temperature ceramic materials - Google Patents
The preparation method of multistage twin structure silicon nitride high-temperature ceramic materials Download PDFInfo
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 67
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 35
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 32
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 26
- 238000000465 moulding Methods 0.000 claims abstract description 17
- 238000005238 degreasing Methods 0.000 claims abstract description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 16
- 235000013312 flour Nutrition 0.000 claims abstract description 14
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 14
- 239000003292 glue Substances 0.000 claims description 26
- 238000010304 firing Methods 0.000 claims description 15
- 230000015572 biosynthetic process Effects 0.000 claims description 14
- 238000009527 percussion Methods 0.000 claims description 14
- 238000012545 processing Methods 0.000 claims description 14
- 238000003786 synthesis reaction Methods 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 12
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 12
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 12
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 10
- 238000005452 bending Methods 0.000 claims description 4
- 230000006835 compression Effects 0.000 claims description 4
- 238000007906 compression Methods 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000001476 alcoholic effect Effects 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 3
- 238000005728 strengthening Methods 0.000 abstract description 3
- 238000003825 pressing Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 239000007788 liquid Substances 0.000 description 10
- 239000013078 crystal Substances 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 5
- 229910003978 SiClx Inorganic materials 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000002635 electroconvulsive therapy Methods 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011214 refractory ceramic Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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- C04B35/593—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride obtained by pressure sintering
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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- C04B35/62605—Treating the starting powders individually or as mixtures
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Abstract
The invention discloses a kind of preparation methods of multistage twin structure silicon nitride high-temperature ceramic materials, first heavy impulse handles simple substance silica flour, it reacts to obtain nano silicon nitride powders with nitrogen again, then plus glueballsization and degreasing form to obtain cold pressing green body, finally molding blank high pressure high temperature is sintered, finally obtains multistage twin structure silicon nitride high-temperature ceramic materials.The method has Composition Control precision height, and technology stability and repeatability are relatively by force, it can be achieved that the high temperature Strengthening and Toughening of silicon nitride ceramic material.
Description
Technical field
The present invention relates to refractory ceramics preparation technical field, in particular to a kind of multistage twin silicon nitride high-temperature ceramic materials
Preparation method.
Background technique
Silicon nitride ceramics is a kind of high temperature resistant structure ceramics, and high temperature obdurability is the most heavy of restriction its high-temperature field application
Want one of index.Silicon nitride ceramics is mainly prepared using traditional powder low pressure sintering method, higher firing temperature (> 1500
DEG C) crystal grain is made seriously to grow up, commonly add grain inhibitor, the method for superfines raw material has the inhibiting effect of crystal grain
Limit.Therefore, a kind of new method is found, silicon nitride ceramics crystal grain is refined, it is most important to improve its high temperature obdurability.
Summary of the invention
The present invention be directed to common approach to be difficult to solve the problems, such as the research and development field status for causing performance to weaken of growing up because of crystal grain,
A kind of preparation method of multistage twin silicon nitride high-temperature ceramic materials is provided.The method has Composition Control precision high, and technique is steady
It is qualitative and repeated relatively by force, it can be achieved that the high temperature Strengthening and Toughening of silicon nitride ceramic material.
To achieve the above objectives, the present invention, which adopts the following technical scheme that, is achieved:
A kind of preparation method of multistage twin structure silicon nitride high-temperature ceramic materials, comprising the following steps:
1) simple substance silica flour is subjected to high-frequency percussion processing, then high―temperature nuclei in a nitrogen atmosphere, obtains nano-silicon nitride
Powder；
2) by nano silicon nitride powders ball adding glue and it is centrifuged nodularization, and carries out degreasing, after degreasing in two-way weight device
Molding, obtains polycrystalline silicon nitride green body；
3) molding blank is placed in super-pressure in four-way superpressure heat collector to form by a firing, finally obtains multistage twin structure
Silicon nitride high-temperature ceramic materials.
As a further improvement of the present invention, in step 1), high-frequency percussion processing uses three-dimensional eddy current resonance ball-grinding machine,
150~300 revs/min of the speed of mainshaft, 6~12 hertz of vibration frequency.
As a further improvement of the present invention, in step 1), high―temperature nuclei carries out in high temperature process furnances, and nitrogen flow is
100~240 ml/mins, keep the temperature 100~120 minutes, 4~6 DEG C/minute of temperature rate by 1520~1590 DEG C of synthesis temperature.
As a further improvement of the present invention, in step 2), nodularization glue is polyvinyl butyral alcoholic solution, nanometer nitrogen
The mass ratio of SiClx powder and nodularization glue is (86.3~94.3): (5.7~13.7).
As a further improvement of the present invention, in step 2), skimming temp is 500~530 DEG C, cold moudling pressure 250
~280MPa.
As a further improvement of the present invention, in step 3), high pressure forms by a firing 5.4~11.2GPa of pressure, temperature 1640
~1750 DEG C, keep the temperature 20~40 minutes.
As a further improvement of the present invention, silicon nitride material obtained has multistage twin structure, and the impact of material is tough
Property >=13.2MPam1/2, microhardness >=38GPa, bending strength >=1160MPa, 1000 DEG C of compression strength >=2650MPa.
Compared with prior art, the invention has the characteristics that and advantage:
Elder generation's heavy impulse of the present invention handles simple substance silica flour, reacts to obtain nano silicon nitride powders with nitrogen, then plus glueballsization simultaneously
Degreasing forms to obtain cold pressing green body, is finally sintered molding blank high pressure high temperature；Wherein silicon powder obtains after heavy impulse is handled
Nano particle containing a large amount of dislocations provides basic lattice defect for subsequent synthesis twin nano-silicon nitride powder, obtains I grade of nanometer
Twin structure.Spheroidising provides powder size and shape basis for improving powder flowbility, for high-densit green body.Super-pressure
On the one hand high temperature sintering technique accelerates blank Densification, II grade of micron twin and whole on the other hand can be formed inside nodularization powder
III grade of micron twin structure of a green body.By introduce it is nanocrystalline with design multistage twin structure, give full play to nanocrystalline big
The tough sexual clorminance of surface and twin structure is that crystal grain is inhibited to grow up, strengthen the key means of performance.Nitridation produced by the present invention
Silicon materials have multistage twin structure, impact flexibility >=13.2MPam of material1/2, microhardness >=38GPa, bending strength
>=1160MPa, high temperature (1000 DEG C) compression strength >=2650MPa.
Further, during preparing silicon nitride ceramic material, the present invention is to solve have addition grain inhibitor, ultra-fine
Powder raw material etc. is difficult to effectively solve the problems, such as to grow up because of crystal grain that performance is caused to weaken, but uses synthesis of nanopowder, powder
Nodularization and multistage twin structure design, research shock treatment parameter, spheroidizing process, moulding process and silicon nitride ceramics obdurability,
The relationship of mechanical behavior under high temperature, it may be assumed that for multistage twin structure silicon nitride high-temperature ceramic materials, keep compared with high-strength tenacity and high temperature
The best shock treatment parameter of mechanical property, spheroidizing process, moulding process.The method has Composition Control precision high, and technique is steady
It is qualitative and repeated relatively by force, it can be achieved that the high temperature Strengthening and Toughening of silicon nitride ceramic material.
Specific embodiment
A kind of preparation method of multistage twin structure silicon nitride high-temperature ceramic materials of the present invention, includes the following steps:
(1) using three-dimensional eddy current resonance ball-grinding machine to simple substance silica flour carry out high-frequency percussion processing, the speed of mainshaft 150~
It 300 revs/min, 6~12 hertz of vibration frequency, is then synthesized in nitrogen atmosphere high temperature process furnances, nitrogen flow is 100~240
Ml/min, keeps the temperature 100~120 minutes, 4~6 DEG C/minute of temperature rate, obtains a nanometer nitrogen by 1520~1590 DEG C of synthesis temperature
SiClx powder；
(2) nano silicon nitride powders are added into glue and is centrifuged nodularization, nodularization glue is that 35mol/L polyvinyl butyral alcohol is molten
Liquid, arogel mass ratio are (86.3~94.3): (5.7~13.7) form in two-way weight device after degreasing, and skimming temp is
500~530 DEG C, 250~280MPa of cold moudling pressure.Obtain polycrystalline silicon nitride green body；
(3) molding blank super-pressure in four-way superpressure heat collector is placed in form by a firing, briquetting pressure 5.4~
11.2GPa, keeps the temperature 20~40 minutes, finally obtains multistage twin structure silicon nitride refractory ceramics material by 1640~1750 DEG C of temperature
Material.
The obdurability and high-temperature behavior of the silicon nitride ceramic material of following embodiment preparation are as shown in table 1.
Embodiment 1
(1) using three-dimensional eddy current resonance ball-grinding machine to simple substance silica flour carry out high-frequency percussion processing, 150 turns of the speed of mainshaft/
Point, it 6 hertz of vibration frequency, is then synthesized in nitrogen atmosphere high temperature process furnances, nitrogen flow is 240 ml/mins, synthesis temperature
1520 DEG C, 100 minutes are kept the temperature, 5 DEG C/minute of temperature rate, obtains nano silicon nitride powders；
(2) nano silicon nitride powders are added into glue and is centrifuged nodularization, nodularization glue is that 35mol/L polyvinyl butyral alcohol is molten
Liquid, arogel mass ratio are 87:13, are formed in two-way weight device after degreasing, and skimming temp is 500 DEG C, cold moudling pressure
280MPa obtains polycrystalline silicon nitride green body；
(3) molding blank is placed in super-pressure in four-way superpressure heat collector to form by a firing, briquetting pressure 11.2GPa, temperature
1640 DEG C of degree keeps the temperature 30 minutes, finally obtains multistage twin structure silicon nitride high-temperature ceramic materials.
Embodiment 2
(1) using three-dimensional eddy current resonance ball-grinding machine to simple substance silica flour carry out high-frequency percussion processing, 170 turns of the speed of mainshaft/
Point, it 7 hertz of vibration frequency, is then synthesized in nitrogen atmosphere high temperature process furnances, nitrogen flow is 120 ml/mins, synthesis temperature
1530 DEG C, 100 minutes are kept the temperature, 5 DEG C/minute of temperature rate, obtains nano silicon nitride powders；
(2) nano silicon nitride powders are added into glue and is centrifuged nodularization, nodularization glue is that 35mol/L polyvinyl butyral alcohol is molten
Liquid, arogel mass ratio are 88:12, are formed in two-way weight device after degreasing, and skimming temp is 520 DEG C, cold moudling pressure
250MPa obtains polycrystalline silicon nitride green body；
(3) molding blank is placed in super-pressure in four-way superpressure heat collector to form by a firing, briquetting pressure 5.9GPa, temperature
1650 DEG C, 20 minutes are kept the temperature, multistage twin structure silicon nitride high-temperature ceramic materials are finally obtained.
Embodiment 3
(1) using three-dimensional eddy current resonance ball-grinding machine to simple substance silica flour carry out high-frequency percussion processing, 170 turns of the speed of mainshaft/
Point, it 8 hertz of vibration frequency, is then synthesized in nitrogen atmosphere high temperature process furnances, nitrogen flow is 160 ml/mins, synthesis temperature
1560 DEG C, 120 minutes are kept the temperature, 4 DEG C/minute of temperature rate, obtains nano silicon nitride powders；
(2) nano silicon nitride powders are added into glue and is centrifuged nodularization, nodularization glue is that 35mol/L polyvinyl butyral alcohol is molten
Liquid, arogel mass ratio are 89:11, are formed in two-way weight device after degreasing, and skimming temp is 520 DEG C, cold moudling pressure
230MPa obtains polycrystalline silicon nitride green body；
(3) molding blank is placed in super-pressure in four-way superpressure heat collector to form by a firing, briquetting pressure 7.2GPa, temperature
1680 DEG C, 30 minutes are kept the temperature, multistage twin structure silicon nitride high-temperature ceramic materials are finally obtained.
Embodiment 4
(1) using three-dimensional eddy current resonance ball-grinding machine to simple substance silica flour carry out high-frequency percussion processing, 210 turns of the speed of mainshaft/
Point, it 9 hertz of vibration frequency, is then synthesized in nitrogen atmosphere high temperature process furnances, nitrogen flow is 190 ml/mins, synthesis temperature
1570 DEG C, 100 minutes are kept the temperature, 5 DEG C/minute of temperature rate, obtains nano silicon nitride powders；
(2) nano silicon nitride powders are added into glue and is centrifuged nodularization, nodularization glue is that 35mol/L polyvinyl butyral alcohol is molten
Liquid, arogel mass ratio are 90:10, are formed in two-way weight device after degreasing, and skimming temp is 500 DEG C, cold moudling pressure
280MPa obtains polycrystalline silicon nitride green body；
(3) molding blank is placed in super-pressure in four-way superpressure heat collector to form by a firing, briquetting pressure 8.2GPa, temperature
1690 DEG C, 30 minutes are kept the temperature, multistage twin structure silicon nitride high-temperature ceramic materials are finally obtained.
The performance parameter that Examples 1 to 4 prepares silicon nitride material is shown in Table 1:
Table 1
From upper table, it can be concluded that, silicon nitride material prepared by the present invention has multistage twin structure, the impact flexibility of material
≥13.2MPa·m1/2, microhardness >=38GPa, bending strength >=1160MPa, high temperature (1000 DEG C) compression strength >=
2650MPa。
Embodiment 5
(1) using three-dimensional eddy current resonance ball-grinding machine to simple substance silica flour carry out high-frequency percussion processing, 220 turns of the speed of mainshaft/
Point, it 10 hertz of vibration frequency, is then synthesized in nitrogen atmosphere high temperature process furnances, nitrogen flow is 190 ml/mins, synthesis temperature
1580 DEG C of degree keeps the temperature 100 minutes, 5 DEG C/minute of temperature rate, obtains nano silicon nitride powders；
(2) nano silicon nitride powders are added into glue and is centrifuged nodularization, nodularization glue is that 35mol/L polyvinyl butyral alcohol is molten
Liquid, arogel mass ratio are 87.4:12.6, are formed in two-way weight device after degreasing, and skimming temp is 500 DEG C, cold moudling
Pressure 280MPa obtains polycrystalline silicon nitride green body；
(3) molding blank is placed in super-pressure in four-way superpressure heat collector to form by a firing, briquetting pressure 9.4GPa, temperature
1700 DEG C, 40 minutes are kept the temperature, multistage twin structure silicon nitride high-temperature ceramic materials are finally obtained.
Embodiment 6
(1) using three-dimensional eddy current resonance ball-grinding machine to simple substance silica flour carry out high-frequency percussion processing, 270 turns of the speed of mainshaft/
Point, it 11 hertz of vibration frequency, is then synthesized in nitrogen atmosphere high temperature process furnances, nitrogen flow is 210 ml/mins, synthesis temperature
1590 DEG C of degree keeps the temperature 100 minutes, 5 DEG C/minute of temperature rate, obtains nano silicon nitride powders；
(2) nano silicon nitride powders are added into glue and is centrifuged nodularization, nodularization glue is that 35mol/L polyvinyl butyral alcohol is molten
Liquid, arogel mass ratio are 88.5:11.5, are formed in two-way weight device after degreasing, and skimming temp is 500 DEG C, cold moudling
Pressure 280MPa obtains polycrystalline silicon nitride green body；
(3) molding blank is placed in super-pressure in four-way superpressure heat collector to form by a firing, briquetting pressure 11.2GPa, temperature
1750 DEG C of degree keeps the temperature 30 minutes, finally obtains multistage twin structure silicon nitride high-temperature ceramic materials.
Embodiment 7
(1) using three-dimensional eddy current resonance ball-grinding machine to simple substance silica flour carry out high-frequency percussion processing, 280 turns of the speed of mainshaft/
Point, it 12 hertz of vibration frequency, is then synthesized in nitrogen atmosphere high temperature process furnances, nitrogen flow is 210 ml/mins, synthesis temperature
1580 DEG C of degree keeps the temperature 100 minutes, 5 DEG C/minute of temperature rate, obtains nano silicon nitride powders；
(2) nano silicon nitride powders are added into glue and is centrifuged nodularization, nodularization glue is that 35mol/L polyvinyl butyral alcohol is molten
Liquid, arogel mass ratio are 94.3:5.7, are formed in two-way weight device after degreasing, and skimming temp is 500 DEG C, cold moudling pressure
Power 280MPa obtains polycrystalline silicon nitride green body；
(3) molding blank is placed in super-pressure in four-way superpressure heat collector to form by a firing, briquetting pressure 7GPa, temperature
1730 DEG C, 30 minutes are kept the temperature, multistage twin structure silicon nitride high-temperature ceramic materials are finally obtained.
Embodiment 8
(1) using three-dimensional eddy current resonance ball-grinding machine to simple substance silica flour carry out high-frequency percussion processing, 250 turns of the speed of mainshaft/
Point, it 7 hertz of vibration frequency, is then synthesized in nitrogen atmosphere high temperature process furnances, nitrogen flow is 190 ml/mins, synthesis temperature
1560 DEG C, 100 minutes are kept the temperature, 5 DEG C/minute of temperature rate, obtains nano silicon nitride powders；
(2) nano silicon nitride powders are added into glue and is centrifuged nodularization, nodularization glue is that 35mol/L polyvinyl butyral alcohol is molten
Liquid, arogel mass ratio are 90.6:9.4, are formed in two-way weight device after degreasing, and skimming temp is 500 DEG C, cold moudling pressure
Power 280MPa obtains polycrystalline silicon nitride green body；
(3) molding blank is placed in super-pressure in four-way superpressure heat collector to form by a firing, briquetting pressure 8GPa, temperature
1680 DEG C, 30 minutes are kept the temperature, multistage twin structure silicon nitride high-temperature ceramic materials are finally obtained.
Embodiment 9
(1) using three-dimensional eddy current resonance ball-grinding machine to simple substance silica flour carry out high-frequency percussion processing, 300 turns of the speed of mainshaft/
Point, it 7 hertz of vibration frequency, is then synthesized in nitrogen atmosphere high temperature process furnances, nitrogen flow is 190 ml/mins, synthesis temperature
1560 DEG C, 100 minutes are kept the temperature, 4 DEG C/minute of temperature rate, obtains nano silicon nitride powders；
(2) nano silicon nitride powders are added into glue and is centrifuged nodularization, nodularization glue is that 35mol/L polyvinyl butyral alcohol is molten
Liquid, arogel mass ratio are 86.3:13.7, are formed in two-way weight device after degreasing, and skimming temp is 530 DEG C, cold moudling
Pressure 250MPa obtains polycrystalline silicon nitride green body；
(3) molding blank is placed in super-pressure in four-way superpressure heat collector to form by a firing, briquetting pressure 5.4GPa, temperature
1680 DEG C, 20 minutes are kept the temperature, multistage twin structure silicon nitride high-temperature ceramic materials are finally obtained.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the principle of the present invention, it can also make several improvements and retouch, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (7)
1. a kind of preparation method of multistage twin structure silicon nitride high-temperature ceramic materials, which comprises the following steps:
1) simple substance silica flour is subjected to high-frequency percussion processing, then high―temperature nuclei in a nitrogen atmosphere, obtains nano silicon nitride powders；
2) by nano silicon nitride powders ball adding glue and it is centrifuged nodularization, and carries out degreasing, formed in two-way weight device after degreasing,
Obtain polycrystalline silicon nitride green body；
3) molding blank is placed in super-pressure in four-way superpressure heat collector to form by a firing, finally obtains multistage twin structure nitridation
Silicon high-temperature ceramic materials.
2. the preparation method of multistage twin structure silicon nitride high-temperature ceramic materials as described in claim 1, which is characterized in that step
It is rapid 1) in, high-frequency percussion processing use three-dimensional eddy current resonance ball-grinding machine, 150~300 revs/min of the speed of mainshaft, vibration frequency 6~
12 hertz.
3. the preparation method of multistage twin structure silicon nitride high-temperature ceramic materials as described in claim 1, which is characterized in that step
It is rapid 1) in, high―temperature nuclei carries out in high temperature process furnances, nitrogen flow be 100~240 ml/mins, synthesis temperature 1520~
1590 DEG C, keep the temperature 100~120 minutes, 4~6 DEG C/minute of temperature rate.
4. the preparation method of multistage twin structure silicon nitride high-temperature ceramic materials as described in claim 1, which is characterized in that step
It is rapid 2) in, nodularization glue is polyvinyl butyral alcoholic solution, the mass ratio of nano silicon nitride powders and nodularization glue be (86.3~
94.3): (5.7~13.7).
5. the preparation method of multistage twin structure silicon nitride high-temperature ceramic materials as described in claim 1, which is characterized in that step
It is rapid 2) in, skimming temp be 500~530 DEG C, 250~280MPa of cold moudling pressure.
6. the preparation method of multistage twin structure silicon nitride high-temperature ceramic materials as described in claim 1, which is characterized in that step
It is rapid 3) in, high pressure forms by a firing 5.4~11.2GPa of pressure, 1640~1750 DEG C of temperature, keeps the temperature 20~40 minutes.
7. the preparation method of the multistage twin structure silicon nitride high-temperature ceramic materials as described in claim 1 to 5 any one,
It is characterized in that, silicon nitride material obtained has multistage twin structure, impact flexibility >=13.2MPam of material1/2, micro- hard
Degree >=38GPa, bending strength >=1160MPa, 1000 DEG C of compression strength >=2650MPa.
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