WO2022089378A1 - 一种具有裂纹愈合能力的陶瓷材料及其制备方法 - Google Patents
一种具有裂纹愈合能力的陶瓷材料及其制备方法 Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 60
- 230000035876 healing Effects 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000725 suspension Substances 0.000 claims abstract description 50
- 239000000843 powder Substances 0.000 claims abstract description 35
- 238000005245 sintering Methods 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 30
- 238000000498 ball milling Methods 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 239000002270 dispersing agent Substances 0.000 claims abstract description 7
- 229910006249 ZrSi Inorganic materials 0.000 claims description 46
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 18
- 238000002490 spark plasma sintering Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 15
- 239000011812 mixed powder Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 239000002612 dispersion medium Substances 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- RSAQARAFWMUYLL-UHFFFAOYSA-N tic-10 Chemical compound CC1=CC=CC=C1CN1C(CCN(CC=2C=CC=CC=2)C2)=C2C(=O)N2CCN=C21 RSAQARAFWMUYLL-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000010907 mechanical stirring Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 229940093429 polyethylene glycol 6000 Drugs 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 abstract description 13
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 229910021354 zirconium(IV) silicide Inorganic materials 0.000 abstract 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 2
- 229910052593 corundum Inorganic materials 0.000 abstract 2
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 2
- 229910005091 Si3N Inorganic materials 0.000 abstract 1
- 229910052581 Si3N4 Inorganic materials 0.000 abstract 1
- 238000005452 bending Methods 0.000 abstract 1
- 238000000227 grinding Methods 0.000 description 9
- 238000007731 hot pressing Methods 0.000 description 9
- 239000011159 matrix material Substances 0.000 description 8
- 239000013003 healing agent Substances 0.000 description 7
- 238000003825 pressing Methods 0.000 description 5
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000008439 repair process Effects 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229910016006 MoSi Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 1
- 238000007676 flexural strength test Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- 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
- C04B35/584—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
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
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- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3891—Silicides, e.g. molybdenum disilicide, iron silicide
Definitions
- the invention relates to the technical field of ceramic materials, in particular to a ceramic material with crack healing ability and a preparation method thereof.
- Ceramic materials have received more and more attention and applications in the past decades due to their excellent properties, such as high temperature resistance, corrosion resistance, wear resistance and high strength.
- ceramic materials also have obvious shortcomings, such as micro-cracks easily generated by mechanical shock and thermal shock during high-speed dry cutting, high friction coefficient, and sensitivity to defects. This will cause the ceramic material to reach the failure standard in advance, resulting in a great waste of resources and economy.
- the ceramic material with crack healing ability refers to adding a suitable repair agent to the ceramic material matrix.
- the self-healing ceramic material is by adding a specific healing agent to the ceramic matrix.
- the chemical reaction of the agent or healing agent to heal the crack of the ceramic material has shown that after the healing agent heals the crack, the strength of the ceramic material is restored and the service life is prolonged.
- the preparation of self-healing ceramic materials by adding SiC, MoSi 2 , MAX and other materials has been disclosed in the prior art.
- the heat treatment temperature of SiC materials needs to be 1000-1300 ° C.
- the lower the heat treatment temperature the longer the time required, and when the temperature is lower than 1000 ° C cracks. Healing takes tens of hours to heal etc.
- the present invention discloses a Si 3 N 4 /TiC/ZrSi 2 ceramic material with crack healing ability and a preparation method thereof.
- a repairing agent ZrSi 2 By adding a repairing agent ZrSi 2 , the Si 3 N 4
- the /TiC ceramic material has good crack repair ability and good sintering compactness, which enhances the comprehensive mechanical properties of the ceramic tool material.
- a ceramic material with crack healing ability the composition of which is ⁇ -Si 3 N 4 60-80%, TiC 5-15%, ZrSi 2 0-20%, Al 2 according to volume percentage O 3 3-7%, Y 2 O 3 5-7%.
- ⁇ -Si 3 N 4 is the matrix
- TiC is the reinforcing phase
- ZrSi 2 is the healing agent
- Al 2 O 3 and Y 2 O 3 are the sintering aids.
- a method for preparing the ceramic material with crack healing ability described in the first aspect comprising the following steps:
- step (3) pour the final suspension obtained in step (3) into the ball milling tank, add ball milling balls according to the weight ratio of balls to material 10:1, and carry out ball milling for 48h under protective atmosphere;
- step (4) drying the ball milling liquid obtained in step (4) at 80-120 ° C for 12-24 h in a vacuum drying oven, and then sieving through a 100-120 mesh sieve to obtain mixed powder, which is sealed and stored for later use;
- step (6) Load the mixed powder obtained in step (5) into a graphite mold, and after cold-pressing, put it into an SPS sintering furnace for sintering.
- the selected healing agent ZrSi 2 in the present invention can react with oxygen at a lower temperature to form ZrO which can heal cracks 2 and SiO 2 , effectively heal the cracks in the ceramic tool material; the flexural strength of the ceramic material can be restored to more than 80% of the smooth sample, which improves the service life of the ceramic tool material;
- ZrSi 2 also acts as a conductive phase to promote the SPS sintering of Si 3 N 4 , and the addition of ZrSi 2 can act as a sintering aid;
- the preparation method has the advantages of simple process, low equipment requirements and strong reliability.
- Fig. 1 is the SEM image of the cross-section of the Si 3 N 4 /TiC/ZrSi 2 ceramic material prepared in Example 1 of the present invention
- Fig. 2 is the crack morphology of the Si 3 N 4 /TiC/ZrSi 2 ceramic material prepared in Example 1 of the present invention
- Example 3 is the morphology of the Si 3 N 4 /TiC/ZrSi 2 ceramic material prepared in Example 1 of the present invention after crack healing;
- FIG. 4 is an EDS detection diagram of the crack healing area of the Si 3 N 4 /TiC/ZrSi 2 ceramic material prepared in Example 1 of the present invention
- FIG. 5 is an XRD test diagram of the Si 3 N 4 /TiC/ZrSi 2 ceramic material prepared in Example 1 of the present invention after crack healing and post-crack healing.
- the present invention discloses a Si 3 N 4 /TiC/ZrSi 2 ceramic material with crack healing ability and a preparation method thereof.
- a ceramic material with crack healing capability is provided, which is based on ⁇ -Si 3 N 4 as a matrix, TiC as a reinforcing phase, ZrSi 2 as a healing agent, Al 2 O 3 and Y 2 O 3 is a sintering aid, the volume percentage of each component is ⁇ -Si 3 N 4 60-80%, TiC 5-15%, ZrSi 2 0-20%, Al 2 O 3 3-7%, Y 2 O 3 5-7%.
- ZrSi 2 is added to the matrix of the Si 3 N 4 /TiC ceramic tool material to achieve the function of crack healing in the ceramic tool material.
- the healing agent ZrSi 2 can react with oxygen at a lower temperature of 600° C. to generate ZrO 2 and SiO 2 that can heal cracks can effectively heal cracks in ceramic tool materials; the flexural strength of ceramic materials can be restored to more than 80% of that of smooth samples, and the service life of tools such as tools prepared from ceramic materials can be improved.
- the volume percentage of each component is: ⁇ -Si 3 N 4 65-75%, TiC 10%, ZrSi 2 5-15%, Al 2 O 3 4%, Y 2 O 3 6%; the sum of the components is 100%.
- the average particle size of the ⁇ -Si 3 N 4 powder is 0.5-1 ⁇ m; the average particle size of the TiC powder is 0.5-1 ⁇ m; the average particle size of the ZrSi 2 powder is 1-3 ⁇ m; the average particle size of the Al 2 O 3 powder is The diameter of the powder is 0.5-2 ⁇ m; the average particle size of the Y 2 O 3 powder is 0.1-0.5 ⁇ m.
- a method for preparing the above-mentioned ceramic material with crack healing ability comprising the following steps:
- step (3) pour the final suspension obtained in step (3) into the ball milling tank, add ball milling balls according to the weight ratio of balls to material 10:1, and carry out ball milling for 48h under protective atmosphere;
- step (4) drying the ball milling liquid obtained in step (4) at 80-120 ° C for 12-24 h in a vacuum drying oven, and then sieving through a 100-120 mesh sieve to obtain mixed powder, which is sealed and stored for later use;
- step (5) The mixed powder obtained in step (5) is put into a graphite mold, and after being cold-pressed, it is put into a spark plasma sintering furnace for sintering.
- the dispersant described in step (3) is polyethylene glycol 6000;
- the ball grinding balls in step (5) are cemented carbide balls YG6 or YG8, and the protective atmosphere is nitrogen;
- the spark plasma sintering parameters of step (6) heating rate: before 1300 °C, 90-110 °C/min, higher than 1300 °C, 30-50 °C/min; sintering temperature 1700 -1750°C; holding time 20-35min, holding at 1600°C and after reaching the sintering temperature for 10-17min; axial pressure 25-35MPa.
- Spark plasma sintering can greatly improve the sinterability of most materials and enable them to sinter rapidly at relatively low temperatures and in a short period of time, thereby expanding the possibilities for developing new advanced materials.
- the essential difference between spark plasma sintering and the traditional sintering method (hot pressing) is the heating method, because hot pressing sintered material is heated only by heat conduction from the container, while spark plasma sintering is a form of dual heat generation by current and container. If spark plasma sintering is used for rapid sintering of ceramic materials, better mechanical properties can be obtained on the basis of maintaining the ability of ceramic materials to heal cracks.
- ZrSi 2 can also act as a conductive phase, and its addition also promotes the spark plasma sintering of Si 3 N 4 , and the addition of ZrSi 2 can act as a sintering aid.
- the ceramic material prepared by the invention has good sintering compactness and enhances the comprehensive mechanical property capability of the ceramic material.
- the average particle size of ⁇ -Si 3 N 4 powder is 0.5-1 ⁇ m; the average particle size of TiC powder is 0.5-1 ⁇ m; the average particle size of ZrSi 2 powder is 1-3 ⁇ m; Al 2 The average particle size of the O 3 powder is 0.5-2 ⁇ m; the average particle size of the Y 2 O 3 powder is 0.1-0.5 ⁇ m.
- the obtained ball milling liquid was dried at 110 °C for 12 hours in a vacuum drying oven, and then sieved through a 100-mesh sieve to obtain a mixed powder.
- the obtained mixed powder was put into a graphite mold, and then put into an SPS sintering furnace after cold pressing. Hot-pressing sintering in medium; SPS sintering parameters: 100°C/min before 1300°C; 1300°C-1450°C 50°C/min; 1450°C-1600°C 30°C/min; 1600°C hold for 15min; /min; 1700°C for 10min; pressure 30MPa.
- the ceramic material prepared in this example is cut into standard strip samples of 3mm ⁇ 4mm ⁇ 35mm, and then the strips are subjected to rough grinding, grinding, chamfering and polishing.
- the mechanical properties were tested, and the results showed that the flexural strength of the material was 751MPa, the hardness was 15.91GPa, and the fracture toughness was 6.96MPa ⁇ M 1/2 .
- Cracks of 350-450 ⁇ m were prefabricated on the surface of the tool using a Vickers hardness tester.
- the cracked sample was heat-treated in a high-temperature air furnace at a heat treatment temperature of 600 °C and held for 30 minutes; the cracked sample after heat treatment was tested for flexural strength at room temperature. 90.14% of the sample.
- Fig. 3 shows the crack surface morphology after heat treatment, and it is found that the crack is basically healed.
- EDS analysis as shown in Figure 4, it can be seen from the distribution of Zr, Si and O elements at the crack that this is due to the TiO 2 and SiO 2 generated by the oxidation of ZrSi 2 to repair the crack.
- the detection pattern of Fig. 5XRD also proves the existence of ZrO 2 and SiO 2 .
- the volume percentages of the raw material components are ⁇ -Si 3 N 4 70%, TiC 10%, ZrSi 2 10%, Al 2 O 3 4%, Y 2 O 3 6%
- the obtained ball milling liquid was dried in a vacuum drying oven at 120°C for 24 hours, and then sieved through a 100-mesh sieve to obtain a mixed powder.
- the obtained mixed powder was put into a graphite mold, and then put into SPS for sintering after cold pressing.
- the ceramic material prepared in this example is cut into standard strip samples of 3mm ⁇ 4mm ⁇ 35mm, and then the strips are subjected to rough grinding, grinding, chamfering and polishing.
- the mechanical properties were tested, and the results showed that the flexural strength of the material was 802MPa, the hardness was 15.36GPa, and the fracture toughness was 8.02MPa ⁇ M 1/2 .
- Figure 1 is the SEM image of the fracture surface of the ceramic material. It can be found that ZrSi 2 is evenly distributed in the ceramic matrix, and the ⁇ -Si 3 N 4 has uniform grains and good density, which is beneficial to the mechanical properties of the ceramic material. Cracks of 350-450 ⁇ m were prefabricated on the surface of the tool using a Vickers hardness tester. The cracked sample was heat-treated in a high-temperature air furnace at a heat treatment temperature of 600 °C and held for 30 minutes; the cracked sample after heat treatment was subjected to a room temperature flexural strength test. 88.78% of the sample.
- the volume percentages of the raw material components are ⁇ -Si 3 N 4 60%, TiC 15%, ZrSi 2 15%, Al 2 O 3 4%, Y 2 O 3 6%
- the obtained ball milling liquid was dried in a vacuum drying oven at 120°C for 24 hours, and then sieved through a 100-mesh sieve to obtain a mixed powder.
- the obtained mixed powder was put into a graphite mold, and then put into SPS for sintering after cold pressing. Hot pressing sintering in the furnace; hot pressing sintering parameters: 100°C/min before 1300°C; 1300°C-1450°C 50°C/min; 1450°C-1600°C 30°C/min
- the ceramic material prepared in this example is cut into standard strip samples of 3mm ⁇ 4mm ⁇ 35mm, and then the strips are subjected to rough grinding, grinding, chamfering and polishing.
- the mechanical properties were tested, and the results showed that the flexural strength of the material was 685MPa, the hardness was 14.82GPa, and the fracture toughness was 7.53MPa ⁇ M 1/2 .
- Cracks of 350-450 ⁇ m were prefabricated on the surface of the tool using a Vickers hardness tester. The cracked sample was heat treated in a high temperature air furnace, the heat treatment temperature was 600 °C, and the temperature was kept for 30 minutes; the cracked sample after heat treatment was tested for flexural strength at room temperature. 80.43% of the sample.
- the volume percentage of raw material components is ⁇ -Si 3 N 4 75%, TiC 10%, ZrSi 2 5%, Al 2 O 3 4%, Y 2 O 3 6%
- the obtained ball milling liquid was dried in a vacuum drying oven at 120 ° C for 24 hours, and then sieved through a 100-mesh sieve to obtain a mixed powder.
- the obtained mixed powder was put into a graphite mold, and then put into an SPS sintering furnace after cold pressing. Hot-pressing sintering is carried out in the middle; hot-pressing sintering parameters: 100°C/min before 1300°C; 1300°C-1450°C 50°C/min; 1450°C-1600°C 30°C/min
- the ceramic material prepared in this example is cut into standard strip samples of 3mm ⁇ 4mm ⁇ 35mm, and then the strips are subjected to rough grinding, grinding, chamfering and polishing.
- the mechanical properties were tested, and the results showed that the flexural strength of the material was 802MPa, the hardness was 15.36GPa, and the fracture toughness was 8.02MPa ⁇ M 1/2 .
- Cracks of 350-450 ⁇ m were prefabricated on the surface of the tool using a Vickers hardness tester.
- the cracked sample was heat treated under high temperature vacuum conditions, the heat treatment temperature was 600 °C, and the temperature was kept for 30 minutes; the cracked sample after heat treatment was tested for flexural strength at room temperature. 47.51% of the smooth specimen.
- the lower flexural strength recovery of ceramic materials is mainly due to the lack of oxidation reaction to generate oxides to repair cracks. However, the material strength is partially recovered, which is partly recovered by the release of residual stress inside the tool at high temperature.
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Abstract
Description
Claims (10)
- 一种具有裂纹愈合能力的陶瓷材料,其特征在于,按照体积百分数其组成为α-Si 3N 4 60-80%,TiC 5-15%,ZrSi 2 0-20%,Al 2O 3 3-7%,Y 2O 3 5-7%。
- 如权利要求1所述具有裂纹愈合能力的陶瓷材料,其特征在于,按照体积百分数其组成为:α-Si 3N 4 65-75%,TiC 10%,ZrSi 2 5-15%,Al 2O 3 4%,Y 2O 3 6%;各组分之和为100%。
- 如权利要求1所述具有裂纹愈合能力的陶瓷材料,其特征在于所述α-Si 3N 4粉体平均粒径为0.5-1μm。
- 如权利要求1所述具有裂纹愈合能力的陶瓷材料,其特征在于,TiC粉体平均粒径为0.5-1μm。
- 如权利要求1所述具有裂纹愈合能力的陶瓷材料,其特征在于,ZrSi 2粉体平均粒径为1-3μm。
- 如权利要求1所述具有裂纹愈合能力的陶瓷材料,其特征在于,Al 2O 3粉体平均粒径为0.5-2μm;Y 2O 3粉体平均粒径为0.1-0.5μm。
- 权利要求1所述具有裂纹愈合能力的陶瓷材料的制备方法,其特征在于,包括以下步骤:(1)按比例称取α-Si 3N 4、TiC和ZrSi 2粉体,分别加入适量的无水乙醇为分散介质,超声分散并机械搅拌15-25min,制得α-Si 3N 4悬浮液,TiC悬浮液和ZrSi 2悬浮液;(2)将上述三种悬浮液混合得到复相悬浮液;(3)称取Si 3N 4重量的1-4wt%的分散剂,以无水乙醇溶解后加入复相悬浮液中然后按比例添加Al 2O 3和Y 2O 3粉体,超声分散并机械搅拌20-40min;(4)将步骤(3)所得的最终悬浮液倒入球磨罐,按照球料重量比10:1加入球磨球,在保护气氛下进行球磨48h;(5)将步骤(4)得到的球磨液在真空干燥箱80-120℃下干燥12-24h,然后经100-120目筛过筛,得到混合粉料,密封保存备用;(6)将步骤(5)得到的混合粉料装入石墨模具中,经冷压成型后放入放电等离子烧结炉中进行放电等离子烧结。
- 如权利要求7所述具有裂纹愈合能力的陶瓷材料的制备方法,其特征在于,步骤(3)所述分散剂为聚乙二醇6000。
- 如权利要求7所述具有裂纹愈合能力的陶瓷材料的制备方法,其特征在于,步骤(5)所述球磨球为硬质合金小球YG6或YG8,保护气氛为氮气。
- 如权利要求7所述具有裂纹愈合能力的陶瓷材料的制备方法,其特征在于步骤(6)所述放电等离子烧结参数:升温速率:在1300℃之前,90-110℃/min,高于1300℃,30-50℃/min;烧结温度1700-1750℃;保温时间20-35min,分别在1600℃和达到烧结温度后保温10-17min;轴向压力25-35MPa。
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