CN112851365A - 一种氮化硅基复相导电陶瓷的制备方法 - Google Patents
一种氮化硅基复相导电陶瓷的制备方法 Download PDFInfo
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- CN112851365A CN112851365A CN202110140908.2A CN202110140908A CN112851365A CN 112851365 A CN112851365 A CN 112851365A CN 202110140908 A CN202110140908 A CN 202110140908A CN 112851365 A CN112851365 A CN 112851365A
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- silicon nitride
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- microwave sintering
- oxide
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 85
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 239000000919 ceramic Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000009768 microwave sintering Methods 0.000 claims abstract description 65
- 238000005245 sintering Methods 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- 238000009694 cold isostatic pressing Methods 0.000 claims description 13
- 150000004706 metal oxides Chemical class 0.000 claims description 13
- 238000003825 pressing Methods 0.000 claims description 13
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 9
- 229910044991 metal oxide Inorganic materials 0.000 claims description 9
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 9
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000395 magnesium oxide Substances 0.000 claims description 7
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 7
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 7
- 230000002745 absorbent Effects 0.000 claims description 6
- 239000002250 absorbent Substances 0.000 claims description 6
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 229910020968 MoSi2 Inorganic materials 0.000 claims description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 5
- 239000006096 absorbing agent Substances 0.000 claims description 5
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 229910052718 tin Inorganic materials 0.000 claims description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 4
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 claims description 3
- 229910033181 TiB2 Inorganic materials 0.000 claims description 3
- -1 TiCN Chemical compound 0.000 claims description 3
- 229910007948 ZrB2 Inorganic materials 0.000 claims description 3
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 3
- 238000001746 injection moulding Methods 0.000 claims description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 16
- 238000000280 densification Methods 0.000 abstract description 12
- 238000005452 bending Methods 0.000 abstract description 6
- 230000005012 migration Effects 0.000 abstract description 5
- 238000013508 migration Methods 0.000 abstract description 5
- 239000000758 substrate Substances 0.000 abstract description 5
- 238000009792 diffusion process Methods 0.000 abstract description 4
- 239000002245 particle Substances 0.000 description 18
- 239000000203 mixture Substances 0.000 description 17
- 238000001816 cooling Methods 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 9
- 238000000465 moulding Methods 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 6
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 4
- 229910026551 ZrC Inorganic materials 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 229910008322 ZrN Inorganic materials 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 238000003754 machining Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910034327 TiC Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 229910007946 ZrB Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000010892 electric spark Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005324 grain boundary diffusion Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
本发明提供了一种氮化硅基复相导电陶瓷的制备方法，本发明以氮化硅为基体，同时添加导电相以及烧结助剂，采用两步微波烧结法，制备的氮化硅基复相导电陶瓷晶粒细小且均匀、致密度高，且强度、硬度等力学性能也得到了显著提升。本发明采用的两步微波烧结法，可抑制晶界迁移，并利用晶界扩散使坯体达到致密化；因此，该方法既可以抑制烧结后期晶粒的生长，同时又不会影响致密化的进行。实施例的结果显示，本发明提供的氮化硅基复相导电陶瓷的相对密度大于99％，维氏硬度大于15GPa，断裂韧性大于6MPa·m1/2，抗弯强度大于900MPa，电阻率小于1Ω·cm。
Description
技术领域
本发明涉及导电陶瓷技术领域，尤其涉及一种氮化硅基复相导电陶瓷的制备方法。
背景技术
氮化硅陶瓷综合力学性能优异，尤其是兼具高强度、高硬度、高韧性和耐磨性能良好的优点，而且具有较高的化学稳定性和抗热震性，是一种理想的工程陶瓷材料，广泛用于机械、化工、航空航天及国防军工等领域。但是，由于氮化硅陶瓷具有电绝缘性，因而只能采用传统的金刚石工具进行机械加工，加工效率低、成本高，且无法加工成形状复杂的部件，严重限制了氮化硅陶瓷的应用。
通过在氮化硅陶瓷中引入钛基化合物(TiN、TiC、TiCN、TiB2)、锆基化合物(ZrN、ZrC、ZrB2)或MoSi2等导电相，可以提高氮化硅陶瓷的导电性，进而可以采用电火花加工，提高了加工效率，解决了上述无法加工成形状复杂的部件的问题。但是，导电相的加入会阻碍氮化硅的烧结致密化，使得制备复相导电陶瓷时，需要采用热压烧结或高温(≥1800℃)气压烧结才能实现致密化，而采用上述烧结方法又会导致氮化硅陶瓷硬度、强度等力学性能的下降。
因此，为了实现形状复杂的氮化硅陶瓷部件的快速加工，亟需提供一种能够实现氮化硅基复相陶瓷致密化的同时保证氮化硅陶瓷力学性能的方法。
发明内容
本发明的目的在于提供一种氮化硅基复相导电陶瓷的制备方法，本发明提供的制备方法可抑制晶界迁移，并利用晶界扩散使坯体达到致密化，因此，提升了氮化硅基复相导电陶瓷的强度、硬度等力学性能。
为了实现上述发明目的，本发明提供了以下技术方案：
本发明提供了一种氮化硅基复相导电陶瓷的制备方法，包括以下步骤：
(1)将氮化硅、导电相以及烧结助剂混合后通过成型，得到坯体；所述烧结助剂包括稀土氧化物和金属氧化物，所述金属氧化物包括氧化铝或氧化镁；
(2)将所述步骤(1)得到的坯体依次进行高温微波烧结和低温微波烧结，得到氮化硅基复相导电陶瓷。
优选地，所述步骤(1)的坯体中氮化硅的质量含量为40～60％，导电相的质量含量为30～50％，金属氧化物的质量含量为1～5％，稀土氧化物的质量含量为2～10％。
优选地，所述导电相包括TiN、TiC、TiCN、TiB2、ZrN、ZrC、ZrB2或MoSi2。
优选地，所述稀土氧化物包括氧化钇、氧化镧或氧化铈。
优选地，所述氮化硅中β-Si3N4的质量含量为≥85％，所述氮化硅的平均粒径D50≤1.0μm。
优选地，所述步骤(1)中坯体的原料还包括微波吸收剂；所述微波吸收剂包括碳化硅或氧化锆。
优选地，所述步骤(1)中成型的方式包括干压、冷等静压、注塑、注凝和注浆中的一种或几种。
优选地，所述步骤(2)中高温微波烧结的温度为1500～1700℃，所述高温微波烧结的保温时间为0～30min；所述低温微波烧结的温度为1400～1600℃，所述低温微波烧结的保温时间为10～120mim；所述高温微波烧结和低温微波烧结的温度差为50～150℃。
优选地，所述步骤(2)中高温微波烧结的升温速率为2～30℃/min，高温微波烧结后降温至所述低温微波烧结的温度的降温速率为30～80℃/min。
优选地，所述步骤(2)中的高温微波烧结和低温微波烧结均在氮气气氛中进行，所述氮气的流量独立地为0.5～5L/min。
本发明提供了一种氮化硅基复相导电陶瓷的制备方法，包括以下步骤：将氮化硅、导电相以及烧结助剂混合后通过成型，得到坯体；将所述坯体依次进行高温微波烧结和低温微波烧结，得到氮化硅基复相导电陶瓷；所述烧结助剂包括稀土氧化物和金属氧化物，所述金属氧化物包括氧化铝或氧化镁。本发明以氮化硅为基体，同时添加导电相以及烧结助剂，采用两步微波烧结法，制备的氮化硅基复相导电陶瓷晶粒细小且均匀、致密度高，且强度、硬度等力学性能也得到了显著提升。本发明通过添加导电相，在氮化硅基体中形成连续的导电网络，提高氮化硅基陶瓷的导电性，并且导电相具有比氮化硅基体更强的吸收微波能力，能对微波烧结起到促进作用，有利于降低氮化硅基复相导电陶瓷的微波烧结温度；通过添加烧结助剂，有利于促进烧结致密化。本发明采用的两步微波烧结法，可抑制晶界迁移，并利用晶界扩散使坯体达到致密化；因此，该方法既可以抑制烧结后期晶粒的生长，同时又不会影响致密化的进行。实施例的结果显示，本发明提供的氮化硅基复相导电陶瓷的相对密度大于99％，维氏硬度大于15GPa，断裂韧性大于6MPa·m1/2，抗弯强度大于900MPa，电阻率小于1Ω·cm。
附图说明
图1为本发明实施例1～4和对比例1～4制备的氮化硅基复相导电陶瓷的显微结构示意图；
图2为本发明中采用的微波烧结炉的示意图；
其中，1-氧化铝纤维炉膛，2-测温装置，3-坩埚，4-碳化硅，5-待烧结坯体。
具体实施方式
本发明提供了一种氮化硅基复相导电陶瓷的制备方法，包括以下步骤：
(1)将氮化硅、导电相以及烧结助剂混合后通过成型，得到坯体；所述烧结助剂包括稀土氧化物和金属氧化物，所述金属氧化物包括氧化铝或氧化镁；
(2)将所述步骤(1)得到的坯体依次进行高温微波烧结和低温微波烧结，得到氮化硅基复相导电陶瓷。
本发明将氮化硅、导电相以及烧结助剂混合后通过成型，得到坯体。
在本发明中，所述坯体中氮化硅的质量含量优选为40～60％，更优选为45～55％。在本发明中，所述氮化硅中β-Si3N4的质量含量优选为≥85％，更优选为≥95％。本发明优选将所述氮化硅中β-Si3N4的质量含量控制在上述范围，有利于使烧结后的氮化硅形成均匀细小的等轴状晶粒。在本发明中，所述氮化硅的平均粒径D50优选为≤1.0μm。本发明优选将所述氮化硅的平均粒径控制在上述范围，能够防止氮化硅的平均粒径过大时阻碍烧结致密化，使烧结温度升高。本发明对所述氮化硅的来源没有特殊的限定，采用本领域技术人员熟知的市售产品即可。
在本发明中，所述坯体中导电相的质量含量优选为30～50％，更优选为30～45％。在本发明中，所述导电相优选包括TiN、TiC、TiCN、TiB2、ZrN、ZrC、ZrB2或MoSi2，更优选为TiN、TiC、ZrC或MoSi2。本发明通过添加导电相，在氮化硅基体中形成连续的导电网络，提高氮化硅基复相导电陶瓷的导电性，并且导电相具有比氮化硅基体更强的吸收微波能力，能对微波烧结起到促进作用，有利于降低氮化硅基复相导电陶瓷的微波烧结温度。本发明对所述导电相的来源没有特殊的限定，采用本领域技术人员熟知的市售产品即可。
在本发明中，所述烧结助剂包括稀土氧化物和金属氧化物。在本发明中，所述烧结助剂的添加，有利于促进烧结致密化。
在本发明中，所述坯体中金属氧化物的质量含量优选为1～5％，更优选为3～5％。在本发明中，所述金属氧化物包括氧化铝或氧化镁，优选为氧化铝。本发明对所述氧化铝或氧化镁的来源没有特殊的限定，采用本领域技术人员熟知的市售产品即可。
在本发明中，所述坯体中稀土氧化物的质量含量优选为2～10％，更优选为3～8％，最优选为4～6％。在本发明中，所述稀土氧化物优选包括氧化钇、氧化镧或氧化铈。本发明对所述稀土氧化物的来源没有特殊的限定，采用本领域技术人员熟知的市售产品即可。
在本发明中，所述坯体的原料还优选包括微波吸收剂。在本发明中，所述微波吸收剂优选包括碳化硅或氧化锆。在本发明中，所述坯体中微波吸收剂的质量含量优选为1～10％，更优选为1～5％。在本发明中，所述碳化硅或氧化锆的介质损耗高，具有极强的吸收微波能力，可以进一步增强氮化硅基复相导电陶瓷对微波的吸收能力，降低烧结温度。本发明对所述微波吸收剂的来源没有特殊的限定，采用本领域技术人员熟知的市售产品即可。
在本发明中，所述导电相、烧结助剂和微波吸收剂的纯度优选独立地为≥98％。
在本发明中，所述导电相、烧结助剂和微波吸收剂的平均粒径D50优选独立地为≤2.0μm。本发明优选将所述导电相、烧结助剂和微波吸收剂的平均粒径控制在上述范围，有利于促进烧结致密化，进一步降低烧结温度。
在本发明中，所述成型的方式优选包括干压、冷等静压、注塑、注凝和注浆中的一种或几种。在本发明中，所述成型优选包括：将原料混合均匀后先进行干压成型，再进行冷等静压处理，得到坯体。在本发明中，所述干压成型的压力优选为10～25MPa。在本发明中，所述干压成型得到的产物的尺寸优选为45×45×8mm。在本发明中，所述冷等静压处理的压力优选为200～300MPa。
得到坯体后，本发明将所述坯体依次进行高温微波烧结和低温微波烧结，得到氮化硅基复相导电陶瓷。本发明采用两步微波烧结法制备氮化硅基复相导电陶瓷，可抑制晶界迁移，并利用晶界扩散使坯体达到致密化；因此，该方法既可以抑制烧结后期晶粒的生长，同时又不会影响致密化的进行。
在本发明中，所述高温微波烧结和低温微波烧结的装置优选为微波烧结炉。在本发明中，所述微波烧结炉优选如图2所示，所述微波烧结炉优选包括氧化铝纤维炉膛、测温装置、坩埚以及碳化硅。在本发明中，所述氧化铝纤维炉膛用于隔热保温；所述测温装置用于观测烧结温度；所述坩埚用于放置待烧结坯体，所述坩埚的材质优选为氮化硼；所述碳化硅用于辅助加热。
在本发明中，所述高温微波烧结的温度优选为1500～1700℃。在本发明中，所述高温微波烧结的保温时间优选为0～30min，更优选为0～15min。
在本发明中，所述低温微波烧结的温度优选为1400～1600℃。在本发明中，所述低温微波烧结的保温时间优选为10～120mim，更优选为20～80min。
在本发明中，所述高温微波烧结和低温微波烧结的温度差优选为50～150℃。
在本发明中，所述高温微波烧结的升温速率优选为2～30℃/min。在本发明中，高温微波烧结后降温至所述低温微波烧结的温度的降温速率优选为30～80℃/min。
本发明优选先升温到一个较高的温度1500～1700℃烧结坯体，并保温0～10min，再快速降温到相对较低的温度1400～1600℃，并进行10～120min的保温，从而抑制晶界迁移，并利用晶界扩散使坯体达到致密化。因此，采用该方法既可以抑制烧结后期晶粒的生长，同时又不会影响致密化的进行，制备的氮化硅基复相导电陶瓷晶粒细小且均匀，致密度高，强度、硬度等力学性能也得到了显著提升。
在本发明中，所述高温微波烧结和低温微波烧结的微波频率优选为2.45GHz。
在本发明中，所述高温微波烧结和低温微波烧结优选均在氮气气氛中进行。在本发明中，所述氮气的流量优选独立地为0.5～5L/min。
本发明以氮化硅为基体，同时添加导电相以及烧结助剂，采用两步微波烧结法，制备的氮化硅基复相导电陶瓷晶粒细小且均匀、致密度高，且强度、硬度等力学性能也得到了显著提升。
下面将结合本发明中的实施例，对本发明中的技术方案进行清楚、完整地描述。显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
原料：
氮化硅(β-Si3N4的质量含量≥95％，平均粒径D50为0.5μm)：53％，
氮化钛(纯度≥99％，平均粒径D50为0.1μm)：35％，
氧化铝(纯度≥99％，平均粒径D50为0.5μm)：3％，
氧化钇(纯度≥99％，平均粒径D50为0.2μm)：6％，
碳化硅(纯度≥98.5％，平均粒径D50为0.5μm)：3％。
将上述原料混合均匀后先进行干压成型，所得产物的尺寸为45×45×8mm，干压成型的压力为20MPa，再进行冷等静压处理，冷等静压处理的压力为300MPa，得到坯体。将上述坯体放入微波烧结炉的炉腔中，抽真空至炉内真空度小于100Pa，然后通入氮气使炉内压力达到0.1MPa，反复两次进行洗炉后，在0.1MPa的流动氮气气氛中开始升温，氮气流量为1L/min，先以15℃/min的速率升温到1600℃，保温5min，然后以50℃/min的速率降温到1550℃，保温30mim，之后自然冷却至室温，得到氮化硅基复相导电陶瓷。
实施例2
原料：
氮化硅(β-Si3N4的质量含量≥95％，平均粒径D50为0.5μm)：50％，
氮化钛(纯度≥99％，平均粒径D50为0.1μm)：40％，
氧化铝(纯度≥99％，平均粒径D50为0.5μm)：3％，
氧化钇(纯度≥99％，平均粒径D50为0.2μm)：5％，
碳化硅(纯度≥98.5％，平均粒径D50为0.5μm)：2％。
将上述原料混合均匀后先进行干压成型，所得产物的尺寸为45×45×8mm，干压成型的压力为20MPa，再进行冷等静压处理，冷等静压处理的压力为300MPa，得到坯体。将上述坯体放入微波烧结炉的炉腔中，抽真空至炉内真空度小于100Pa，然后通入氮气使炉内压力达到0.1MPa，反复两次进行洗炉后，在0.1MPa的流动氮气气氛中开始升温，氮气流量为1L/min，先以15℃/min的速率升温到1650℃，保温0min，然后以50℃/min的速率降温到1550℃，保温40mim，之后自然冷却至室温，得到氮化硅基复相导电陶瓷。
实施例3
原料：
氮化硅(β-Si3N4的质量含量≥95％，平均粒径D50为0.5μm)：48％，
氮化钛(纯度≥99％，平均粒径D50为0.1μm)：45％，
氧化铝(纯度≥99％，平均粒径D50为0.5μm)：3％，
氧化钇(纯度≥99％，平均粒径D50为0.2μm)：4％。
将上述原料混合均匀后先进行干压成型，所得产物的尺寸为45×45×8mm，干压成型的压力为20MPa，再进行冷等静压处理，冷等静压处理的压力为300MPa，得到坯体。将上述坯体放入微波烧结炉的炉腔中，抽真空至炉内真空度小于100Pa，然后通入氮气使炉内压力达到0.1MPa，反复两次进行洗炉后，在0.1MPa的流动氮气气氛中开始升温，氮气流量为1L/min，先以15℃/min的速率升温到1650℃，保温5min，然后以50℃/min的速率降温到1600℃，保温30mim，之后自然冷却至室温，得到氮化硅基复相导电陶瓷。
实施例4
原料：
氮化硅(β-Si3N4的质量含量≥95％，平均粒径D50为0.5μm)：50％，
氮化钛(纯度≥99％，平均粒径D50为0.1μm)：40％，
氧化镁(纯度≥98％，平均粒径D50为0.2μm)：3％，
氧化钇(纯度≥99％，平均粒径D50为0.2μm)：5％，
氧化锆(纯度≥99％，平均粒径D50为0.5μm)：2％。
将上述原料混合均匀后先进行干压成型，所得产物的尺寸为45×45×8mm，干压成型的压力为20MPa，再进行冷等静压处理，冷等静压处理的压力为300MPa，得到坯体。将上述坯体放入微波烧结炉的炉腔中，抽真空至炉内真空度小于100Pa，然后通入氮气使炉内压力达到0.1MPa，反复两次进行洗炉后，在0.1MPa的流动氮气气氛中开始升温，氮气流量为1L/min，先以15℃/min的速率升温到1600℃，保温3min，然后以50℃/min的速率降温到1550℃，保温30mim，之后自然冷却至室温，得到氮化硅基复相导电陶瓷。
对比例1
采用和实施例1相同的原料组成和成型工艺，得到坯体。
将得到的坯体进行气压烧结，烧结温度为1750℃，氮气压力为9.8MPa，保温3h，之后自然冷却至室温，得到氮化硅基复相导电陶瓷。
对比例2
采用和实施例2相同的原料组成和成型工艺，得到坯体。
将得到的坯体进行气压烧结，烧结温度为1800℃，氮气压力为9.8MPa，保温3h，之后自然冷却至室温，得到氮化硅基复相导电陶瓷。
对比例3
采用和实施例3相同的原料组成和成型工艺，得到坯体。
将得到的坯体进行气压烧结，烧结温度为1850℃，氮气压力为9.8MPa，保温2h，之后自然冷却至室温，得到氮化硅基复相导电陶瓷。
对比例4
采用和实施例4相同的原料组成和成型工艺，得到坯体。
将得到的坯体进行气压烧结，烧结温度为1780℃，氮气压力为9.8MPa，保温2h，之后自然冷却至室温，得到氮化硅基复相导电陶瓷。
性能测试
采用阿基米德排水法测试实施例1～4和对比例1～4制备的氮化硅基复相导电陶瓷的密度，并计算相对密度，结果见表1。
采用压痕法测试实施例1～4和对比例1～4制备的氮化硅基复相导电陶瓷的维氏硬度和断裂韧性，施加载荷为196N，测试结果见表1。
采用标准GB/T 6569-2006中测试抗弯强度的方法测试实施例1～4和对比例1～4制备的氮化硅基复相导电陶瓷的抗弯强度，其中，测试样品的规格为40×3×4mm，测试三点抗弯强度，跨距为30mm，测试结果见表1。
采用扫描电子显微镜观察实施例1～4和对比例1～4制备的氮化硅基复相导电陶瓷的显微结构，如图1所示，并在随机拍摄的SEM照片上完成晶粒尺寸的测量，每个样品统计的晶粒数目不少于500个，测试结果见表1。
表1 实施例1～4以及对比例1～4制备的氮化硅基复相导电陶瓷的性能
由以上实施例可以看出，本发明提供的制备方法在实现氮化硅基复相导电陶瓷致密化的同时提升了陶瓷的强度、硬度等力学性能。并且，本发明制备的氮化硅基复相导电陶瓷的相对密度大于99％，维氏硬度大于15GPa，断裂韧性大于6MPa·m1/2，抗弯强度大于900MPa，电阻率小于1Ω·cm。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。
Claims (10)
1.一种氮化硅基复相导电陶瓷的制备方法，包括以下步骤：
(1)将氮化硅、导电相以及烧结助剂混合后通过成型，得到坯体；所述烧结助剂包括稀土氧化物和金属氧化物，所述金属氧化物包括氧化铝或氧化镁；
(2)将所述步骤(1)得到的坯体依次进行高温微波烧结和低温微波烧结，得到氮化硅基复相导电陶瓷。
2.根据权利要求1所述的制备方法，其特征在于，所述步骤(1)的坯体中氮化硅的质量含量为40～60％，导电相的质量含量为30～50％，金属氧化物的质量含量为1～5％，稀土氧化物的质量含量为2～10％。
3.根据权利要求1或2所述的制备方法，其特征在于，所述导电相包括TiN、TiC、TiCN、TiB2、ZrN、ZrC、ZrB2或MoSi2。
4.根据权利要求1或2所述的制备方法，其特征在于，所述稀土氧化物包括氧化钇、氧化镧或氧化铈。
5.根据权利要求1或2所述的制备方法，其特征在于，所述氮化硅中β-Si3N4的质量含量为≥85％，所述氮化硅的平均粒径D50≤1.0μm。
6.根据权利要求1所述的制备方法，其特征在于，所述步骤(1)中坯体的原料还包括微波吸收剂；所述微波吸收剂包括碳化硅或氧化锆。
7.根据权利要求1所述的制备方法，其特征在于，所述步骤(1)中成型的方式包括干压、冷等静压、注塑、注凝和注浆中的一种或几种。
8.根据权利要求1所述的制备方法，其特征在于，所述步骤(2)中高温微波烧结的温度为1500～1700℃，所述高温微波烧结的保温时间为0～30min；所述低温微波烧结的温度为1400～1600℃，所述低温微波烧结的保温时间为10～120mim；所述高温微波烧结和低温微波烧结的温度差为50～150℃。
9.根据权利要求1或8所述的制备方法，其特征在于，所述步骤(2)中高温微波烧结的升温速率为2～30℃/min，高温微波烧结后降温至所述低温微波烧结的温度的降温速率为30～80℃/min。
10.根据权利要求1或8所述的制备方法，其特征在于，所述步骤(2)中的高温微波烧结和低温微波烧结均在氮气气氛中进行，所述氮气的流量独立地为0.5～5L/min。
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