CN1727307A - Ceramics of silicon nitride with high antioxygenic property and preparation method - Google Patents
Ceramics of silicon nitride with high antioxygenic property and preparation method Download PDFInfo
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- CN1727307A CN1727307A CN 200510085369 CN200510085369A CN1727307A CN 1727307 A CN1727307 A CN 1727307A CN 200510085369 CN200510085369 CN 200510085369 CN 200510085369 A CN200510085369 A CN 200510085369A CN 1727307 A CN1727307 A CN 1727307A
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 56
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000000919 ceramic Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims description 12
- 230000003026 anti-oxygenic effect Effects 0.000 title claims description 5
- 239000000843 powder Substances 0.000 claims abstract description 39
- 239000013078 crystal Substances 0.000 claims abstract description 35
- 238000005245 sintering Methods 0.000 claims abstract description 26
- 238000007731 hot pressing Methods 0.000 claims abstract description 5
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 28
- 238000000498 ball milling Methods 0.000 claims description 20
- 239000002002 slurry Substances 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 17
- 239000000758 substrate Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- 238000003825 pressing Methods 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000000654 additive Substances 0.000 claims description 10
- 230000000996 additive effect Effects 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000000280 densification Methods 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 2
- 229910052691 Erbium Inorganic materials 0.000 claims description 2
- 229910052693 Europium Inorganic materials 0.000 claims description 2
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 229910052689 Holmium Inorganic materials 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 2
- 229910052772 Samarium Inorganic materials 0.000 claims description 2
- 229910052771 Terbium Inorganic materials 0.000 claims description 2
- 229910052775 Thulium Inorganic materials 0.000 claims description 2
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 2
- 238000011284 combination treatment Methods 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- 239000011812 mixed powder Substances 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 229910052706 scandium Inorganic materials 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- 230000003064 anti-oxidating effect Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 description 34
- 230000003647 oxidation Effects 0.000 description 33
- 239000012299 nitrogen atmosphere Substances 0.000 description 13
- 229910052710 silicon Inorganic materials 0.000 description 13
- 239000010703 silicon Substances 0.000 description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 12
- 206010013786 Dry skin Diseases 0.000 description 12
- 239000012612 commercial material Substances 0.000 description 12
- 238000005520 cutting process Methods 0.000 description 12
- 238000002474 experimental method Methods 0.000 description 12
- 229910002804 graphite Inorganic materials 0.000 description 12
- 239000010439 graphite Substances 0.000 description 12
- 230000004224 protection Effects 0.000 description 12
- -1 silicon nitrides Chemical class 0.000 description 12
- 238000005452 bending Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000013001 point bending Methods 0.000 description 6
- 230000004584 weight gain Effects 0.000 description 6
- 235000019786 weight gain Nutrition 0.000 description 6
- 230000003078 antioxidant effect Effects 0.000 description 5
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
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Abstract
A silicon nitride ceramics with high antioxidizing performance is prepared from silicon nitride powder (60-90 Wt %), RE oxide (5-25) and prefabricated silicon nitride crystal seeds (5-15) through hot pressing or SPS sintering. It has also high strength and toughness.
Description
Technical field
The present invention relates to a kind of silicon nitride ceramics and preparation method thereof, belong to the stupalith field.
Background technology
Silicon nitride ceramic material has premium propertiess such as high strength, high rigidity, resistance to oxidation, corrosion-resistant and shock resistance, is a kind of up-and-coming high-temperature structural material.Utilize that it is heat-resisting, the performance of preventing corrosion from molten metals, can be used for metallurgical industry, utilize its erosion resistance, can be used for chemical industry, utilize its high strength, high-fracture toughness and high rigidity, can be used for mechanical industry, on large-sized structural parts, also used to some extent in the last few years, such as: high speed wire rod roller and guide wheel etc.Because the appearance of world energy sources crisis and the special requirement of aerospace and military field, silicon nitride ceramic material become the important candidate material of the ceramic component in development internal combustion turbine and the diesel motor.Because High Temperature High Pressure and corrosive environment under the engine behaviour, the antioxidant anticorrosive performance of silicon nitride ceramics just seems very important.
Guo. (reference is seen: S.Q.Guo to wait the investigator to make silicon nitride ceramics by the rare earth doped oxide compound of pressure sintering, N.Hirosaki, T.Nishimura, Y.Yamamoto, and M.Mitomo, " Hot-Pressed Silicon Nitridewith Lu203 Additives:Oxidation and Its Effect on Strength; " J.Am.Ceram.Soc., 86[11] 1900-905 (2003)), has the good oxidization resistance energy, but its mechanical property is relatively poor, and improve its mechanical property need sintering theory or preparation technology's further improvement.(the patent No.s: ZL951918354 such as the interior hero for a long time of bamboo, patent name: silicon nitride sinter and manufacture method thereof) prepared silicon nitride ceramics by reaction sintering, shortened the nitridation time in the reaction sintering when making silicon nitride sinter, thereby improved productivity, but its mechanical property and antioxidant property can also further improve raising.
Summary of the invention
The objective of the invention is with the rare earth oxide is additive, and adds ready-formed silicon nitride crystal seed, and preparation has the silicon nitride ceramic material of high antioxygenic property strong mechanical performance.
A kind of silicon nitride ceramics that the present invention proposes with high antioxygenic property, it is characterized in that: described silicon nitride ceramics is based on beta-silicon nitride powder, add rare earth oxide as additive and prefabricated silicon nitride crystal seed, be prepared from through hot pressing or SPS sintering process;
In above-mentioned silicon nitride ceramics, the weight percent of described beta-silicon nitride powder is 60～90%, and the weight percent of rare earth oxide is 5～25%, and the weight percent of prefabricated silicon nitride crystal seed is 5～15%.
In above-mentioned silicon nitride ceramics, the weight percent of described rare earth oxide is 10%, and the weight percent of described prefabricated silicon nitride crystal seed is 8%.
In above-mentioned silicon nitride ceramics, described beta-silicon nitride powder is the α phase silicon nitride powder; Described additive is Sc, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, a kind of in 17 kinds of rare earth oxides such as Lu.
In above-mentioned silicon nitride ceramics, described prefabricated silicon nitride crystal seed is β-Si
3N
4Crystal seed, by following prepared: in α phase silicon nitride powder, add a certain amount of RE oxide powder, add dehydrated alcohol and be made into slurry, high temperature drying obtains powder behind the ball milling, this powder is incubated 0.5～1.5 hour down for 1600～1800 ℃ at nitrogen atmosphere makes β-Si
3N
4Crystal seed.
The preparation method of a kind of silicon nitride ceramics that the present invention proposes, it is characterized in that: described method is to add rare earth oxide in the raw material alpha-silicon nitride powders, and adds ready-formed β-Si simultaneously
3N
4Crystal seed, its concrete preparation method comprises following each step:
(1) combination treatment of raw material: in raw material α phase silicon nitride powder, add rare earth oxide and prefabricated β-Si
3N
4Crystal seed is made into mixed powder, adds dehydrated alcohol and is made into slurry, ball milling;
(2) slurry behind the ball milling at high temperature drying obtain powder, sieve, dry-pressing formed;
(3) make the material densification with hot pressed sintering or discharge plasma sintering, the base substrate that is about to after dry-pressing formed is placed in the protective atmosphere sinter molding under High Temperature High Pressure.
In above-mentioned preparation method, the described sintering temperature of step 3 is 1700～1950 ℃, and pressure is 2～7 tons, and soaking time is 40～80 minutes, and protective atmosphere is argon gas or nitrogen.
In above-mentioned preparation method, the described sintering temperature of step 3 is 1800 ℃, and pressure is 4 tons.
Because the present invention adds a certain amount of rare earth oxide as additive in α phase silicon nitride powder, and adds ready-formed β-Si
3N
4Crystal seed is through mixing drying, dry-pressing formed, and prepare the silicon nitride ceramic material of densification by hot pressing or plasma discharging (SPS) sintering process, therefore this material has high-intensity high-tenacity, having good antioxidant property, is a kind of promising high-temperature structural material, can make turibine rotor, the combustion chamber inwall, bearing, valve, component such as fixture of heat treatment are applied to metallurgy, chemical industry, machinery, space flight and military field.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is described further:
(1) raw material: based on α phase silicon nitride powder, add weight ratio therein and be 5～25% rare earth oxide (Lu for example of (preferably 10%)
2O
3) as additive, and add weight ratio (preferably 8%) ready-formed β-Si that is 5～15%
3N
4Crystal seed.Add rare earth oxide as additive, can make alpha-silicon nitride powders sintering densification at a lower temperature, because its less ionic radius and higher intergranular refractoriness mutually, improved the antioxidant property of material effectively.Add ready-formed β-Si
3N
4Crystal seed can make it obtain preferred growth as plus seed under bigger growth motivating force effect, thereby the microstructure of stupalith is developed towards the direction with high length-diameter ratio crystal grain, guarantees that material has high-intensity high-tenacity.
(2) technology: in order to make additive Lu
2O
3And β-Si
3N
4Crystal seed mixes in raw material a phase silicon nitride powder, uses dehydrated alcohol as ball-milling medium, and with at high temperature dry 4～40 hours (preferably 8 hours) of slurry, the dry-pressing of sieving becomes base substrate behind the ball milling 4～40 hours (preferably 24 hours).
(3) sintering densification of material:, adopt hot pressed sintering or plasma discharging (SPS) sintering method in order to make the material densification.Hot pressing temperature is 1700～1950 ℃ (preferably 1800 ℃); Pressure is 2～7 tons (preferably 4 tons); Soaking time is 40～80 minutes (preferably 60 minutes); Protective atmosphere is argon gas or nitrogen (preferably nitrogen).
Embodiment 1:
With 14.8 gram commercial materials α phase silicon nitrides and 1.8 gram rare earth oxide Sc
2O
3Mix, join and carried out ball milling in the 100ml dehydrated alcohol 24 hours, slurry was obtained 16 gram powders in 12 hours 80 ℃ of dryings, powder is put into graphite jig, insulation made β-Si in 30 minutes under 1600 ℃ of nitrogen atmosphere protections
3N
4Crystal seed.With 60 gram commercial materials α phase silicon nitrides, 25 gram rare earth oxide Sc
2O
3With 15 gram ready-formed β-Si
3N
4Crystal seed mixes, and joins and carries out ball milling in the 200ml dehydrated alcohol 24 hours, and slurry is crossed 80 mesh sieves 80 ℃ of dryings after 12 hours, and is dry-pressing formed, makes two diameter 50mm, the cylindrical base substrate of high 15mm.Base substrate is put into graphite jig, and hot pressed sintering is 40 minutes under 1700 ℃, 2 tons pressure, nitrogen atmosphere protection, obtains two blocks of disk materials of high compactionization.With 3 of the meticulous strips of cutting 3 of strips wearing into 3 * 4 * 40mm and 4 * 6 * 40mm of disk,,, use for the high temperature oxidation experiment with the meticulous rectangular tab of wearing into 30 * 18 * 4mm of cutting of another piece disk for mechanical property experiment usefulness.
Experimental result is as follows:
It is 900MPa that three-point bending method records room temperature bending strength, and fracture toughness property is 7.87MPa*m
1/2, good mechanical performance.High-temperature oxidation test oxidation 100 hours under 1400 ℃ of air atmospheres, final oxidation weight gain is 0.23mg/cm
24.Mechanical properties decrease 7～10% after the oxidation.
Embodiment 2:
With 14 gram commercial materials α phase silicon nitrides and 1 gram rare earth oxide La
2O
3Mix, join and carried out ball milling in the 100ml dehydrated alcohol 24 hours, slurry was obtained 8 gram powders in 12 hours 80 ℃ of dryings, powder is put into graphite jig, insulation made β-Si in 45 minutes under 1650 ℃ of nitrogen atmosphere protections
3N
4Crystal seed.With 70 gram commercial materials α phase silicon nitrides, 20 gram rare earth oxide La
2O
3With 10 gram ready-formed β-Si
3N
4Crystal seed mixes, and joins and carries out ball milling in the 200ml dehydrated alcohol 24 hours, and slurry is crossed 80 mesh sieves 80 ℃ of dryings after 12 hours, and is dry-pressing formed, makes two diameter 50mm, the cylindrical base substrate of high 15mm.Base substrate is put into graphite jig, and hot pressed sintering is 50 minutes under 1750 ℃, 3 tons pressure, nitrogen atmosphere protection, obtains two blocks of disk materials of high compactionization.With 3 of the meticulous strips of cutting 3 of strips wearing into 3 * 4 * 40mm and 4 * 6 * 40mm of disk,,, use for the high temperature oxidation experiment with the meticulous rectangular tab of wearing into 30 * 18 * 4mm of cutting of another piece disk for mechanical property experiment usefulness.
Experimental result is as follows:
It is 980MPa that three-point bending method records room temperature bending strength, and fracture toughness property is 7.42MPa*m
1/2, good mechanical performance.High-temperature oxidation test oxidation 100 hours under 1400 ℃ of air atmospheres, final oxidation weight gain is 0.35mg/cm
2Mechanical properties decrease 10～12% after the oxidation.
Embodiment 3:
With 7.5 gram commercial materials α phase silicon nitrides and 0.5 gram rare earth oxide Nd
2O
3Mix, join and carried out ball milling in the 100ml dehydrated alcohol 24 hours, slurry was obtained 8 gram powders in 12 hours 80 ℃ of dryings, powder is put into graphite jig, insulation made β-Si in 60 minutes under 1800 ℃ of nitrogen atmosphere protections
3N
4Crystal seed.With 80 gram commercial materials α phase silicon nitrides, 15 gram rare earth oxide Nd
2O
3With 5 gram ready-formed β-Si
3N
4Crystal seed mixes, and joins and carries out ball milling in the 200ml dehydrated alcohol 24 hours, and slurry is crossed 80 mesh sieves 80 ℃ of dryings after 12 hours, and is dry-pressing formed, makes two diameter 50mm, the cylindrical base substrate of high 15mm.Base substrate is put into graphite jig, and discharge plasma sintering is 60 minutes under 1950 ℃, 7 tons pressure, nitrogen atmosphere protection, obtains two blocks of disk materials of high compactionization.With 3 of the meticulous strips of cutting 3 of strips wearing into 3 * 4 * 40mm and 4 * 6 * 40mm of disk,,, use for the high temperature oxidation experiment with the meticulous rectangular tab of wearing into 30 * 18 * 4mm of cutting of another piece disk for mechanical property experiment usefulness.
Experimental result is as follows:
It is 940MPa that three-point bending method records room temperature bending strength, and fracture toughness property is 8.21MPa*m
1/2, good mechanical performance.High-temperature oxidation test oxidation 100 hours under 1400 ℃ of air atmospheres, final oxidation weight gain is 0.41mg/cm
2Mechanical properties decrease 7～14% after the oxidation.
Embodiment 4:
With 7.5 gram commercial materials α phase silicon nitrides and 0.5 gram rare earth oxide Dy
2O
3Mix, join and carried out ball milling in the 100ml dehydrated alcohol 24 hours, slurry was obtained 8 gram powders in 12 hours 80 ℃ of dryings, powder is put into graphite jig, insulation made β-Si in 75 minutes under 1750 ℃ of nitrogen atmosphere protections
3N
4Crystal seed.With 90 gram commercial materials α phase silicon nitrides, 7 gram rare earth oxide Dy
2O
3With 3 gram ready-formed β-Si
3N
4Crystal seed mixes, and joins and carries out ball milling in the 200ml dehydrated alcohol 24 hours, and slurry is crossed 80 mesh sieves 80 ℃ of dryings after 12 hours, and is dry-pressing formed, makes two diameter 50mm, the cylindrical base substrate of high 15mm.Base substrate is put into graphite jig, and hot pressed sintering is 70 minutes under 1850 ℃, 5 tons pressure, nitrogen atmosphere protection, obtains two blocks of disk materials of high compactionization.With 3 of the meticulous strips of cutting 3 of strips wearing into 3 * 4 * 40mm and 4 * 6 * 40mm of disk,,, use for the high temperature oxidation experiment with the meticulous rectangular tab of wearing into 30 * 18 * 4mm of cutting of another piece disk for mechanical property experiment usefulness.
Experimental result is as follows:
It is 1020MPa that three-point bending method records room temperature bending strength, and fracture toughness property is 8.18MPa*m
1/2, good mechanical performance.High-temperature oxidation test oxidation 100 hours under 1400 ℃ of air atmospheres, final oxidation weight gain is 0.33mg/cm
2Mechanical properties decrease 8～12% after the oxidation.
Embodiment 5:
With 7.4 gram commercial materials α phase silicon nitrides and 0.6 gram rare earth oxide Yb
2O
3Mix, join and carried out ball milling in the 100ml dehydrated alcohol 24 hours, slurry was obtained 8 gram powders in 12 hours 80 ℃ of dryings, powder is put into graphite jig, insulation made β-Si in 90 minutes under 1800 ℃ of nitrogen atmosphere protections
3N
4Crystal seed.With 82 gram commercial materials α phase silicon nitrides, 10 gram rare earth oxide Yb
2O
3With 8 gram ready-formed β-Si
3N
4Crystal seed mixes, and joins and carries out ball milling in the 200ml dehydrated alcohol 24 hours, and slurry is crossed 80 mesh sieves 80 ℃ of dryings after 12 hours, and is dry-pressing formed, makes two diameter 50mm, the cylindrical base substrate of high 15mm.Base substrate is put into graphite jig, and hot pressed sintering is 80 minutes under 1950 ℃, 6 tons pressure, nitrogen atmosphere protection, obtains two blocks of disk materials of high compactionization.With 3 of the meticulous strips of cutting 3 of strips wearing into 3 * 4 * 40mm and 4 * 6 * 40mm of disk,,, use for the high temperature oxidation experiment with the meticulous rectangular tab of wearing into 30 * 18 * 4mm of cutting of another piece disk for mechanical property experiment usefulness.
Experimental result is as follows:
It is 1060MPa that three-point bending method records room temperature bending strength, and fracture toughness property is 8.67MPa*m
1/2, good mechanical performance.High-temperature oxidation test oxidation 100 hours under 1400 ℃ of air atmospheres, final oxidation weight gain is 0.29mg/cm
2Mechanical properties decrease 10～19% after the oxidation.
Embodiment 6:
With 7.4 gram commercial materials α phase silicon nitrides and 0.6 gram rare earth oxide Lu
2O
3Mix, join and carried out ball milling in the 100ml dehydrated alcohol 24 hours, slurry was obtained 8 gram powders in 12 hours 80 ℃ of dryings, powder is put into graphite jig, insulation made β-Si in 60 minutes under 1700 ℃ of nitrogen atmosphere protections
3N
4Crystal seed.With 82 gram commercial materials α phase silicon nitrides, 10 gram rare earth oxide Lu
2O
3With 8 gram ready-formed β-Si
3N
4Crystal seed mixes, and joins and carries out ball milling in the 200ml dehydrated alcohol 24 hours, and slurry is crossed 80 mesh sieves 80 ℃ of dryings after 12 hours, and is dry-pressing formed, makes two diameter 50mm, the cylindrical base substrate of high 15mm.Base substrate is put into graphite jig, and hot pressed sintering is 60 minutes under 1800 ℃, 4 tons pressure, nitrogen atmosphere protection, obtains two blocks of disk materials of high compactionization.With 3 of the meticulous strips of cutting 3 of strips wearing into 3 * 4 * 40mm and 4 * 6 * 40mm of disk,,, use for the high temperature oxidation experiment with the meticulous rectangular tab of wearing into 30 * 18 * 4mm of cutting of another piece disk for mechanical property experiment usefulness.
Experimental result is as follows:
It is 1080MPa that three-point bending method records room temperature bending strength, and fracture toughness property is 8.97MPa*m
1/2, good mechanical performance.High-temperature oxidation test oxidation 100 hours under 1400 ℃ of air atmospheres, final oxidation weight gain is 0.13mg/cm
2, figure below is a material oxidation weightening finish curve.Mechanical properties decrease 5～12% after the oxidation, still keep higher level.This sample has good antioxidant property in same type of material.
Claims (8)
1, a kind of silicon nitride ceramics with high antioxygenic property is characterized in that: described silicon nitride ceramics adds rare earth oxide as additive and prefabricated silicon nitride crystal seed based on beta-silicon nitride powder, is prepared from through hot pressing or SPS sintering process.
2, according to the described silicon nitride ceramics of claim 1, it is characterized in that: the weight percent of described beta-silicon nitride powder is 60～90%, and the weight percent of rare earth oxide is 5～25%, and the weight percent of prefabricated silicon nitride crystal seed is 5～15%.
3, according to claim 1 or 2 described silicon nitride ceramics, it is characterized in that: the weight percent of described rare earth oxide is 10%, and the weight percent of described prefabricated silicon nitride crystal seed is 8%.
4, according to the described silicon nitride ceramics of claim 1, it is characterized in that: described beta-silicon nitride powder is the α phase silicon nitride powder; Described additive is Sc, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, a kind of in the Lu17 kind rare earth oxide.
5, according to the described silicon nitride ceramics of claim 1, it is characterized in that: described prefabricated silicon nitride crystal seed is β-Si
3N
4Crystal seed, by following prepared: in α phase silicon nitride powder, add a certain amount of RE oxide powder, add dehydrated alcohol and be made into slurry, behind the ball milling at high temperature drying obtain powder, with this powder 1600 ℃～1800 ℃ of nitrogen atmospheres down insulation made β-Si in 0.5～1.5 hour
3N
4Crystal seed.
6, a kind of method for preparing silicon nitride ceramics as claimed in claim 1 is characterized in that: described method is to add rare earth oxide in the raw material alpha-silicon nitride powders, and adds ready-formed β-Si simultaneously
3N
4Crystal seed, its concrete preparation method comprises following each step:
(1) combination treatment of raw material: in raw material α phase silicon nitride powder, add rare earth oxide and prefabricated β-Si
3N
4Crystal seed is made into mixed powder, adds dehydrated alcohol and is made into slurry, ball milling;
(2) slurry behind the ball milling at high temperature drying obtain powder, sieve, dry-pressing formed;
(3) make the material densification with hot pressed sintering or discharge plasma sintering, the base substrate that is about to after dry-pressing formed is placed in the protective atmosphere sinter molding under High Temperature High Pressure.
7, according to the described preparation method of claim 6, it is characterized in that: the described sintering temperature of step 3 is 1700～1950 ℃, and pressure is 2～7 tons, and soaking time is 40～80 minutes, and protective atmosphere is argon gas or nitrogen.
8, according to claim 6 or 7 described preparation methods, it is characterized in that: the described sintering temperature of step 3 is 1800 ℃, and pressure is 4 tons.
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