CN1793042A - In-situ flexible silicon nitride base ceramic and super-speed sintering process - Google Patents
In-situ flexible silicon nitride base ceramic and super-speed sintering process Download PDFInfo
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- CN1793042A CN1793042A CN 200610011114 CN200610011114A CN1793042A CN 1793042 A CN1793042 A CN 1793042A CN 200610011114 CN200610011114 CN 200610011114 CN 200610011114 A CN200610011114 A CN 200610011114A CN 1793042 A CN1793042 A CN 1793042A
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Abstract
The invention relates to a home position plasticizing silicon nitride ceramic and the quickly sintering method that belongs to ceramic field. It adopts silicon nitride powder and oxide/oxide mixture additive as raw material, and quickly sinters with SPS. The additive is rare earth oxide, and the oxide mixture additive is alumina, aluminum nitride and rare earth oxide. The method could quickly transform alpha-Si<SUB>3</SUB>N<SUB>4</SUB> to beta-Si<SUB>3</SUB>N<SUB>4</SUB> or beta-sialon crystal grain. The ceramic would have high rigidity and high tenacity.
Description
Technical field
The present invention relates to a kind of in-situ flexible silicon nitride base ceramic and super-speed sintering process thereof, belong to technical field of ceramic material.
Background technology
Silicon-nitride-based ceramic (comprising silicon nitride ceramics and Sialon pottery) 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.
Yet fine and close silicon-nitride-based ceramic normally adopts gas pressure sintering (Gas Pressure Sintering, GPS), hot pressed sintering (Hot-Pressed Silicon Nitride, HPSN) and HIP sintering (Hot Isostatic Pressing HIP) obtains.The GPS method normally the silicon nitride base substrate in the nitrogen of 5-20MPa at 1800-2100 ℃ of following sintering 1-3 hour because the nitrogen pressure height, thereby the decomposition that has suppressed silicon nitride can be at very high sintering temperature and densification.The hot pressed sintering silicon nitride is earlier with powder cold-press moulding in punching block, and compacting pressure is generally 50MPa, is placed on induction heating then or has in the graphite mo(u)ld of other heating elements to carry out hot pressing, and whole process has nitrogen to do protection.Hot pressing temperature is generally 1750-1900 ℃, and mechanical pressure is 20-30MPa, and soaking time is generally 1-3 hour.The HIP sintering silicon nitride then normally under up to the barometric information about 200Mpa, the about 1700-1850 of temperature ℃ sintering 1-3h.These sintering methods something in common is as can be seen: they all are to make silicon nitride be able to densification through the sintering of very long time (not waiting from 1 hour to a few hours) under High Temperature High Pressure.As everyone knows, the long sintering under this High Temperature High Pressure is very huge to the consumption of the energy, thus be very uneconomic, and also greatly reduce production efficiency.
Discharge plasma sintering (Spark Plasma Sintering, SPS) as a kind of new material preparation technology, the part electric current that passes through sample by instantaneous generation punctures entrap bubble in the space, shelf depreciation also produces plasma body and makes and be sintered intravital each uniform particles ground self-heating and make the particle surface activation, thereby have very high thermo-efficiency, can in the quite short time, prepare stupalith near complete densification.The SPS technology has that heat-up rate is fast as can be seen, sintering time is short and characteristics such as energy-conserving and environment-protective.
Summary of the invention
The objective of the invention is to oxide compound or oxide mixture is additive, prepares the silicon nitride ceramic material with in-situ flexible structure by a kind of supper-fast sintering process, thereby raises the efficiency greatly and reduce cost.
A kind of in-situ flexible silicon nitride base ceramic that the present invention proposes, it is characterized in that, described stupalith contains α phase silicon nitride powder, oxide addition or oxide mixture additive, the weight percent of described α phase silicon nitride powder is 80～95%, and the weight percent of described oxide addition or oxide mixture additive is 5～20%.
In above-mentioned silicon nitride ceramic material, described oxide addition is a rare earth oxide, and described oxide mixture additive is aluminum oxide, aluminium nitride and rare earth oxide.
In above-mentioned silicon nitride ceramic material, described rare earth oxide is single rare earth oxide compound or two kinds and two or more rare earth oxide.。
In above-mentioned silicon nitride ceramic material, described aluminum oxide and aluminium nitride additional proportion satisfy Si
6-zAl
zO
zN
8-z, 0＜z＜4.2 wherein.
A kind of in-situ flexible silicon nitride base ceramic super-speed sintering process that the present invention proposes is characterized in that, described method is to add oxide compound or oxide mixture additive in raw material α phase silicon nitride powder, and its concrete preparation method comprises following each step:
(1) combination treatment of raw material: in raw material α phase silicon nitride powder, add oxide compound or oxide mixture additive, be made into mixed powder, add dehydrated alcohol and be made into the slurry ball milling;
(2) the slurry drying behind the ball milling obtains powder, sieves;
(3) superfast sintering: the gained powder graphite jig of packing into is placed in the heating chamber of discharging plasma sintering equipment, carry out discharge plasma sintering after vacuumizing, temperature was raised to 600 ℃ automatically within three minutes, after this heat-up rate is 100-450 ℃/min, sintering temperature is 1550-1900 ℃, sintering pressure is 20-80MPa, and highest temperature soaking time is 1-2 minute.
Because this super-speed sintering process that the present invention proposes makes primary α-Si
3N
4Be on good terms and in the extremely short time, change β-Si rapidly fully into
3N
4Or β-sialon phase, and original position has formed the β-Si of long column shape in silicon-nitride-based ceramic
3N
4Or β-sialon crystal grain, the silicon-nitride-based ceramic of gained has high rigidity and high tenacity, is a kind of up-and-coming structured material.So and this sintering method is owing to also be the high and very cheap ceramic sintering process of cost of a kind of efficient very fast.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is described further:
Embodiment one:
With 80 gram commercial materials α phase silicon nitrides, 7 gram aluminum oxide, 3 gram aluminium nitride and 10 gram Yb
2O
3Mix, add dehydrated alcohol after ball milling obtain uniform slurry, this slurry is sieved after the thorough drying in baking oven obtains powder.Taking by weighing 3.5 these powders of gram packs into and is placed in discharging plasma sintering equipment (SPS) chamber behind the graphite jig of internal diameter 20mm, vacuumize in back three minutes and be raised to 600 ℃ automatically, after this with 200 ℃/min be warmed up to 1700 ℃ and under 50MPa pressure insulation obtained the sample that thickness is about 3mm in 1 minute.Other 4 identical samples also make with same process.With diamond paste sample surfaces is polished to 0.5 micron.The phase composite of sample obtains by X-ray diffraction (XRD) analysis.The length-to-diameter ratio of long column shape crystal grain obtains by measuring field emission scanning electron microscope (FESEM) photo.Sample hardness (H
v) and fracture toughness property (K
IC) obtain under 196N load with Vickers hardness tester, fracture toughness property is that the method that proposes according to Antis calculates, the Young's modulus and the Poisson's ratio of wherein getting silicon nitride are respectively 310GPa and 0.27.The gained results averaged.
The testing of materials result is as follows:
The principal phase of sample is β-sialon phase.The length-to-diameter ratio of long column shape β-sialon crystal grain is 4.1.Sample hardness is 15.3GPa, and fracture toughness property is 5.8MPa.m
1/2
Embodiment two:
With 80 gram commercial materials α phase silicon nitrides, 7 gram aluminum oxide, 3 gram aluminium nitride and 10 gram Yb
2O
3Mix, add dehydrated alcohol after ball milling obtain uniform slurry, this slurry is sieved after the thorough drying in baking oven obtains powder.Taking by weighing 3.5 these powders of gram packs into and is placed in discharging plasma sintering equipment (SPS) chamber behind the graphite jig of internal diameter 20mm, vacuumize in back three minutes and be raised to 600 ℃ automatically, after this with 300 ℃/min be warmed up to 1800 ℃ and under 50MPa pressure insulation obtained the sample that thickness is about 3mm in 1 minute.Other 4 identical samples also make with same process.With diamond paste sample surfaces is polished to 0.5 micron.The phase composite of sample obtains by X-ray diffraction (XRD) analysis.The length-to-diameter ratio of long column shape crystal grain obtains by measuring field emission scanning electron microscope (FESEM) photo.Sample hardness (H
v) and fracture toughness property (K
IC) obtain under 196N load with Vickers hardness tester, fracture toughness property is that the method that proposes according to Antis calculates, the Young's modulus and the Poisson's ratio of wherein getting silicon nitride are respectively 310GPa and 0.27.The gained results averaged.
The testing of materials result is as follows:
The principal phase of sample is β-sialon phase.The length-to-diameter ratio of long column shape β-sialon crystal grain is 5.3.Sample hardness is 14.7GPa, and fracture toughness property is 6.3MPa.m
1/2
Embodiment three:
With 80 gram commercial materials α phase silicon nitrides, 7 gram aluminum oxide, 3 gram aluminium nitride and 10 gram Yb
2O
3Mix, add dehydrated alcohol after ball milling obtain uniform slurry, this slurry is sieved after the thorough drying in baking oven obtains powder.Taking by weighing 3.5 these powders of gram packs into and is placed in discharging plasma sintering equipment (SPS) chamber behind the graphite jig of internal diameter 20mm, vacuumize in back three minutes and be raised to 600 ℃ automatically, after this with 100 ℃/min be warmed up to 1550 ℃ and under 20MPa pressure insulation obtained the sample that thickness is about 3mm in 1 minute.Other 4 identical samples also make with same process.With diamond paste sample surfaces is polished to 0.5 micron.The phase composite of sample obtains by X-ray diffraction (XRD) analysis.The length-to-diameter ratio of long column shape crystal grain obtains by measuring field emission scanning electron microscope (FESEM) photo.Sample hardness (H
v) and fracture toughness property (K
IC) obtain under 196N load with Vickers hardness tester, fracture toughness property is that the method that proposes according to Antis calculates, the Young's modulus and the Poisson's ratio of wherein getting silicon nitride are respectively 310GPa and 0.27.The gained results averaged.
The testing of materials result is as follows:
The principal phase of sample is β-sialon phase.The length-to-diameter ratio of long column shape β-sialon crystal grain is 3.7.Sample hardness is 16.2GPa, and fracture toughness property is 4.0MPa.m
1/2
Embodiment four:
With 80 gram commercial materials α phase silicon nitrides, 7 gram aluminum oxide, 3 gram aluminium nitride and 10 gram Yb
2O
3Mix, add dehydrated alcohol after ball milling obtain uniform slurry, this slurry is sieved after the thorough drying in baking oven obtains powder.Taking by weighing 3.5 these powders of gram packs into and is placed in discharging plasma sintering equipment (SPS) chamber behind the graphite jig of internal diameter 20mm, vacuumize in back three minutes and be raised to 600 ℃ automatically, after this with 450 ℃/min be warmed up to 1900 ℃ and under 80MPa pressure insulation obtained the sample that thickness is about 3mm in 2 minutes.Other 4 identical samples also make with same process.With diamond paste sample surfaces is polished to 0.5 micron.The phase composite of sample obtains by X-ray diffraction (XRD) analysis.The length-to-diameter ratio of long column shape crystal grain obtains by measuring field emission scanning electron microscope (FESEM) photo.Sample hardness (H
v) and fracture toughness property (K
IC) obtain under 196N load with Vickers hardness tester, fracture toughness property is that the method that proposes according to Antis calculates, the Young's modulus and the Poisson's ratio of wherein getting silicon nitride are respectively 310GPa and 0.27.The gained results averaged.
The testing of materials result is as follows:
The principal phase of sample is β-sialon phase.The length-to-diameter ratio of long column shape β-sialon crystal grain is 5.6.Sample hardness is 14.6GPa, and fracture toughness property is 6.4MPa.m
1/2
Embodiment five:
With 90 gram commercial materials α phase silicon nitrides, 10 gram Yb
2O
3Mix, add dehydrated alcohol after ball milling obtain uniform slurry, this slurry is sieved after the thorough drying in baking oven obtains powder.Taking by weighing 3.5 these powders of gram packs into and is placed in discharging plasma sintering equipment (SPS) chamber behind the graphite jig of internal diameter 20mm, vacuumize in back three minutes and be raised to 600 ℃ automatically, after this with 200 ℃/min be warmed up to 1700 ℃ and under 50MPa pressure insulation obtained the sample that thickness is about 3mm in 1 minute.Other 4 identical samples also make with same process.With diamond paste sample surfaces is polished to 0.5 micron.The phase composite of sample obtains by X-ray diffraction (XRD) analysis.The length-to-diameter ratio of long column shape crystal grain obtains by measuring field emission scanning electron microscope (FESEM) photo.Sample hardness (H
v) and fracture toughness property (K
IC) obtain under 196N load with Vickers hardness tester, fracture toughness property is that the method that proposes according to Antis calculates, the Young's modulus and the Poisson's ratio of wherein getting silicon nitride are respectively 310GPa and 0.27.The gained results averaged.
The testing of materials result is as follows:
The principal phase of sample is β-Si
3N
4Phase.Long column shape β-Si
3N
4The length-to-diameter ratio of crystal grain is 5.9.Sample hardness is 13.6GPa, and fracture toughness property is 6.1MPa.m
1/2
Embodiment six:
With 95 gram commercial materials α phase silicon nitrides, 5 gram Yb
2O
3Mix, add dehydrated alcohol after ball milling obtain uniform slurry, this slurry is sieved after the thorough drying in baking oven obtains powder.Taking by weighing 3.5 these powders of gram packs into and is placed in discharging plasma sintering equipment (SPS) chamber behind the graphite jig of internal diameter 20mm, vacuumize in back three minutes and be raised to 600 ℃ automatically, after this with 100 ℃/min be warmed up to 1550 ℃ and under 20MPa pressure insulation obtained the sample that thickness is about 3mm in 1 minute.Other 4 identical samples also make with same process.With diamond paste sample surfaces is polished to 0.5 micron.The phase composite of sample obtains by X-ray diffraction (XRD) analysis.The length-to-diameter ratio of long column shape crystal grain obtains by measuring field emission scanning electron microscope (FESEM) photo.Sample hardness (H
v) and fracture toughness property (K
IC) obtain under 196N load with Vickers hardness tester, fracture toughness property is that the method that proposes according to Antis calculates, the Young's modulus and the Poisson's ratio of wherein getting silicon nitride are respectively 310GPa and 0.27.The gained results averaged.
The testing of materials result is as follows:
The principal phase of sample is β-Si
3N
4Phase.Long column shape β-Si
3N
4The length-to-diameter ratio of crystal grain is that 2.7 sample hardness are 16.6GPa, and fracture toughness property is 3.5MPa.m
1/2
Embodiment seven:
With 80 gram commercial materials α phase silicon nitrides, 20 gram Yb
2O
3Mix, add dehydrated alcohol after ball milling obtain uniform slurry, this slurry is sieved after the thorough drying in baking oven obtains powder.Taking by weighing 3.5 these powders of gram packs into and is placed in discharging plasma sintering equipment (SPS) chamber behind the graphite jig of internal diameter 20mm, vacuumize in back three minutes and be raised to 600 ℃ automatically, after this with 200 ℃/min be warmed up to 1700 ℃ and under 50MPa pressure insulation obtained the sample that thickness is about 3mm in 1 minute.Other 4 identical samples also make with same process.With diamond paste sample surfaces is polished to 0.5 micron.The phase composite of sample obtains by X-ray diffraction (XRD) analysis.The length-to-diameter ratio of long column shape crystal grain obtains by measuring field emission scanning electron microscope (FESEM) photo.Sample hardness (H
v) and fracture toughness property (K
IC) obtain under 196N load with Vickers hardness tester, fracture toughness property is that the method that proposes according to Antis calculates, the Young's modulus and the Poisson's ratio of wherein getting silicon nitride are respectively 310GPa and 0.27.The gained results averaged.
The testing of materials result is as follows:
The principal phase of sample is β-Si
3N
4Phase.Long column shape β-Si
3N
4The length-to-diameter ratio of crystal grain is 5.6.Sample hardness is 14.6GPa, and fracture toughness property is 6.5MPa.m
1/2
Embodiment eight:
With 90 gram commercial materials α phase silicon nitrides, 10 gram Yb
2O
3Mix, add dehydrated alcohol after ball milling obtain uniform slurry, this slurry is sieved after the thorough drying in baking oven obtains powder.Taking by weighing 3.5 these powders of gram packs into and is placed in discharging plasma sintering equipment (SPS) chamber behind the graphite jig of internal diameter 20mm, vacuumize in back three minutes and be raised to 600 ℃ automatically, after this with 450 ℃/min be warmed up to 1900 ℃ and under 80MPa pressure insulation obtained the sample that thickness is about 3mm in 2 minutes.Other 4 identical samples also make with same process.With diamond paste sample surfaces is polished to 0.5 micron.The phase composite of sample obtains by X-ray diffraction (XRD) analysis.The length-to-diameter ratio of long column shape crystal grain obtains by measuring field emission scanning electron microscope (FESEM) photo.Sample hardness (H
v) and fracture toughness property (K
IC) obtain under 196N load with Vickers hardness tester, fracture toughness property is that the method that proposes according to Antis calculates, the Young's modulus and the Poisson's ratio of wherein getting silicon nitride are respectively 310GPa and 0.27.The gained results averaged.
The testing of materials result is as follows:
The principal phase of sample is β-Si
3N
4Phase.Long column shape β-Si
3N
4The length-to-diameter ratio of crystal grain is 6.1.Sample hardness is 13.3GPa, and fracture toughness property is 6.6MPa.m
1/2
Embodiment nine:
With 85 gram commercial materials α phase silicon nitrides, 7.5 gram La
2O
3With 7.5 gram Yb
2O
3Mix, add dehydrated alcohol after ball milling obtain uniform slurry, this slurry is sieved after the thorough drying in baking oven obtains powder.Taking by weighing 3.5 these powders of gram packs into and is placed in discharging plasma sintering equipment (SPS) chamber behind the graphite jig of internal diameter 20mm, vacuumize in back three minutes and be raised to 600 ℃ automatically, after this with 200 ℃/min be warmed up to 1700 ℃ and under 50MPa pressure insulation obtained the sample that thickness is about 3mm in 1 minute.Other 4 identical samples also make with same process.With diamond paste sample surfaces is polished to 0.5 micron.The phase composite of sample obtains by X-ray diffraction (XRD) analysis.The length-to-diameter ratio of long column shape crystal grain obtains by measuring field emission scanning electron microscope (FESEM) photo.Sample hardness (H
v) and fracture toughness property (K
IC) obtain under 196N load with Vickers hardness tester, fracture toughness property is that the method that proposes according to Antis calculates, the Young's modulus and the Poisson's ratio of wherein getting silicon nitride are respectively 310GPa and 0.27.The gained results averaged.
The testing of materials result is as follows:
The principal phase of sample is β-Si
3N
4Phase.Long column shape β-Si
3N
4The length-to-diameter ratio of crystal grain is 5.7.Sample hardness is 13.8GPa, and fracture toughness property is 5.9MPa.m
1/2
Embodiment ten:
With 85 gram commercial materials α phase silicon nitrides, 7.5 gram Y
2O
3With 7.5 gram Lu
2O
3Mix, add dehydrated alcohol after ball milling obtain uniform slurry, this slurry is sieved after the thorough drying in baking oven obtains powder.Taking by weighing 3.5 these powders of gram packs into and is placed in discharging plasma sintering equipment (SPS) chamber behind the graphite jig of internal diameter 20mm, vacuumize in back three minutes and be raised to 600 ℃ automatically, after this with 200 ℃/min be warmed up to 1700 ℃ and under 50MPa pressure insulation obtained the sample that thickness is about 3mm in 1 minute.Other 4 identical samples also make with same process.With diamond paste sample surfaces is polished to 0.5 micron.The phase composite of sample obtains by X-ray diffraction (XRD) analysis.The length-to-diameter ratio of long column shape crystal grain obtains by measuring field emission scanning electron microscope (FESEM) photo.Sample hardness (H
v) and fracture toughness property (K
IC) obtain under 196N load with Vickers hardness tester, fracture toughness property is that the method that proposes according to Antis calculates, the Young's modulus and the Poisson's ratio of wherein getting silicon nitride are respectively 310GPa and 0.27.The gained results averaged.
The testing of materials result is as follows:
The principal phase of sample is β-Si
3N
4Phase.Long column shape β-Si
3N
4The length-to-diameter ratio of crystal grain is 6.1.Sample hardness is 13.4GPa, and fracture toughness property is 6.5MPa.m
1/2
Comparative Examples one:
With 90 gram commercial materials α phase silicon nitrides, 10 gram Yb
2O
3Mix, add dehydrated alcohol after ball milling obtain uniform slurry, this slurry is sieved after the thorough drying in baking oven obtains powder.Taking by weighing 3.5 these powders of gram packs into and is placed in discharging plasma sintering equipment (SPS) chamber behind the graphite jig of internal diameter 20mm, vacuumize in back three minutes and be raised to 600 ℃ automatically, after this with 200 ℃/min be warmed up to 1700 ℃ and under 50MPa pressure insulation obtained the sample that thickness is about 3mm in 3 minutes.Other 4 identical samples also make with same process.With diamond paste sample surfaces is polished to 0.5 micron.The phase composite of sample obtains by X-ray diffraction (XRD) analysis.The length-to-diameter ratio of long column shape crystal grain obtains by measuring field emission scanning electron microscope (FESEM) photo.Sample hardness (H
v) and fracture toughness property (K
IC) obtain under 196N load with Vickers hardness tester, fracture toughness property is that the method that proposes according to Antis calculates, the Young's modulus and the Poisson's ratio of wherein getting silicon nitride are respectively 310GPa and 0.27.The gained results averaged.
The testing of materials result is as follows:
The principal phase of sample is β-Si
3N
4Phase.Long column shape β-Si
3N
4The length-to-diameter ratio of crystal grain is 6.2.Sample hardness is 13.2GPa, and fracture toughness property is 6.3MPa.m
1/2When soaking time is brought up to 3 minutes, but the identical sample that only is incubated 1 minute with other condition is compared, though the length-to-diameter ratio of crystal grain and mechanical property raising to some extent, but this as can be seen raising is very few, basically be within the scope that allows in error, we can say also that therefore the length-to-diameter ratio of crystal grain and mechanical property do not change basically.
Comparative Examples two:
With 90 gram commercial materials α phase silicon nitrides, 10 gram Yb
2O
3Mix, add dehydrated alcohol after ball milling obtain uniform slurry, this slurry is sieved after the thorough drying in baking oven obtains powder.Taking by weighing 3.5 these powders of gram packs into and is placed in discharging plasma sintering equipment (SPS) chamber behind the graphite jig of internal diameter 20mm, vacuumize in back three minutes and be raised to 600 ℃ automatically, after this with 200 ℃/min be warmed up to 1700 ℃ and under 50MPa pressure insulation obtained the sample that thickness is about 3mm in 10 minutes.Other 4 identical samples also make with same process.With diamond paste sample surfaces is polished to 0.5 micron.The phase composite of sample obtains by X-ray diffraction (XRD) analysis.The length-to-diameter ratio of long column shape crystal grain obtains by measuring field emission scanning electron microscope (FESEM) photo.Sample hardness (H
v) and fracture toughness property (K
IC) obtain under 196N load with Vickers hardness tester, fracture toughness property is that the method that proposes according to Antis calculates, the Young's modulus and the Poisson's ratio of wherein getting silicon nitride are respectively 310GPa and 0.27.The gained results averaged.
The testing of materials result is as follows:
The principal phase of sample is β-Si
3N
4Phase.Long column shape β-Si
3N
4The length-to-diameter ratio of crystal grain is 5.8.Sample hardness is 13.9GPa, and fracture toughness property is 6.0MPa.m
1/2As can be seen, when soaking time is brought up to 10 minutes, but the identical sample that only is incubated 1 minute with other condition compare, the length-to-diameter ratio of crystal grain does not improve, and mechanical property does not change basically yet.
Claims (5)
1, a kind of in-situ flexible silicon nitride base ceramic, it is characterized in that, described pottery contains α phase silicon nitride powder, oxide addition or oxide mixture additive, the weight percent of described α phase silicon nitride powder is 80～95%, and the weight percent of described oxide addition or oxide mixture additive is 5～20%.
According to the described silicon-nitride-based ceramic of claim 1, it is characterized in that 2, described oxide addition is a rare earth oxide, described oxide mixture additive is aluminum oxide, aluminium nitride and rare earth oxide.
According to claim 1 or 2 described silicon-nitride-based ceramics, it is characterized in that 3, described oxide compound is single rare earth oxide compound or two kinds and two or more rare earth oxide.
4, according to claim 1 or 2 described silicon-nitride-based ceramics, it is characterized in that the additional proportion of described aluminum oxide and aluminium nitride satisfies Si
6-zAl
zO
zN
8-z0＜z＜4.2 wherein.
5, a kind of in-situ flexible silicon nitride base ceramic super-speed sintering process as claimed in claim 1, it is characterized in that, described method is to add oxide compound or oxide mixture additive in raw material α phase silicon nitride powder, and its concrete preparation method comprises following each step:
(1) combination treatment of raw material: in raw material α phase silicon nitride powder, add oxide compound or oxide mixture additive, be made into mixed powder, add dehydrated alcohol and be made into the slurry ball milling;
(2) the slurry drying behind the ball milling obtains powder, sieves;
(3) superfast sintering: the gained powder graphite jig of packing into is placed in the heating chamber of discharging plasma sintering equipment, carry out discharge plasma sintering after vacuumizing, temperature was raised to 600 ℃ automatically within three minutes, after this heat-up rate is 100-450 ℃/min, sintering temperature is 1550-1900 ℃, sintering pressure is 20-80MPa, and highest temperature soaking time is 1-2 minute.
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| GB2506287B (en) * | 2011-08-05 | 2019-07-31 | Univ South China Tech | Tungsten Carbide Composite Containing Alumina Grains and Silicon Nitride Whiskers and the Preparation Method Thereof |
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