CN108558411A - 一种Si3N4陶瓷及其制备方法 - Google Patents
一种Si3N4陶瓷及其制备方法 Download PDFInfo
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- CN108558411A CN108558411A CN201810553737.4A CN201810553737A CN108558411A CN 108558411 A CN108558411 A CN 108558411A CN 201810553737 A CN201810553737 A CN 201810553737A CN 108558411 A CN108558411 A CN 108558411A
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- ceramics
- silica flour
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- mass ratio
- sintering aid
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000919 ceramic Substances 0.000 claims abstract description 57
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 56
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000003054 catalyst Substances 0.000 claims abstract description 36
- 238000005245 sintering Methods 0.000 claims abstract description 32
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 31
- 235000013312 flour Nutrition 0.000 claims abstract description 28
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 28
- 238000005238 degreasing Methods 0.000 claims abstract description 19
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 18
- 239000002002 slurry Substances 0.000 claims abstract description 17
- -1 silicon powder nitride Chemical class 0.000 claims abstract description 14
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical group O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000005469 granulation Methods 0.000 claims abstract description 8
- 230000003179 granulation Effects 0.000 claims abstract description 8
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 4
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 4
- 229910052691 Erbium Inorganic materials 0.000 claims abstract description 4
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 4
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 4
- 229910052689 Holmium Inorganic materials 0.000 claims abstract description 4
- 229910052765 Lutetium Inorganic materials 0.000 claims abstract description 4
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 4
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 4
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 4
- 229910052771 Terbium Inorganic materials 0.000 claims abstract description 4
- 229910052775 Thulium Inorganic materials 0.000 claims abstract description 4
- 229910052769 Ytterbium Inorganic materials 0.000 claims abstract description 4
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 4
- 229910052706 scandium Inorganic materials 0.000 claims abstract description 4
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 4
- 239000008187 granular material Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000011812 mixed powder Substances 0.000 claims description 11
- 239000002270 dispersing agent Substances 0.000 claims description 10
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- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid group Chemical group C(CCCCCCC\C=C/CCCCCCCC)(=O)O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 4
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- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 3
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 3
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- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 2
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- 238000000465 moulding Methods 0.000 abstract description 7
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
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- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000002518 antifoaming agent Substances 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 2
- MHIITNFQDPFSES-UHFFFAOYSA-N 25,26,27,28-tetrazahexacyclo[16.6.1.13,6.18,11.113,16.019,24]octacosa-1(25),2,4,6,8(27),9,11,13,15,17,19,21,23-tridecaene Chemical class N1C(C=C2C3=CC=CC=C3C(C=C3NC(=C4)C=C3)=N2)=CC=C1C=C1C=CC4=N1 MHIITNFQDPFSES-UHFFFAOYSA-N 0.000 description 2
- YFPJFKYCVYXDJK-UHFFFAOYSA-N Diphenylphosphine oxide Chemical compound C=1C=CC=CC=1[P+](=O)C1=CC=CC=C1 YFPJFKYCVYXDJK-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000001723 curing Methods 0.000 description 2
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- AUHZEENZYGFFBQ-UHFFFAOYSA-N 1,3,5-trimethylbenzene Chemical class CC1=CC(C)=CC(C)=C1 AUHZEENZYGFFBQ-UHFFFAOYSA-N 0.000 description 1
- ZDQNWDNMNKSMHI-UHFFFAOYSA-N 1-[2-(2-prop-2-enoyloxypropoxy)propoxy]propan-2-yl prop-2-enoate Chemical compound C=CC(=O)OC(C)COC(C)COCC(C)OC(=O)C=C ZDQNWDNMNKSMHI-UHFFFAOYSA-N 0.000 description 1
- 125000006188 2-phenyl benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C1=C(C([H])=C([H])C([H])=C1[H])C([H])([H])* 0.000 description 1
- 238000010146 3D printing Methods 0.000 description 1
- OSBSXTGABLIDRX-UHFFFAOYSA-N 5-methylidenecyclohexa-1,3-diene Chemical compound C=C1CC=CC=C1 OSBSXTGABLIDRX-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Natural products C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 description 1
- 241000233855 Orchidaceae Species 0.000 description 1
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- ZCZFEIZSYJAXKS-UHFFFAOYSA-N [3-hydroxy-2,2-bis(hydroxymethyl)propyl] prop-2-enoate Chemical compound OCC(CO)(CO)COC(=O)C=C ZCZFEIZSYJAXKS-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001555 benzenes Chemical class 0.000 description 1
- 125000003236 benzoyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C(*)=O 0.000 description 1
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- MTZQAGJQAFMTAQ-UHFFFAOYSA-N ethyl benzoate Chemical compound CCOC(=O)C1=CC=CC=C1 MTZQAGJQAFMTAQ-UHFFFAOYSA-N 0.000 description 1
- JZMPIUODFXBXSC-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.OC(=O)C=C.CCOC(N)=O JZMPIUODFXBXSC-UHFFFAOYSA-N 0.000 description 1
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- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- LYXOWKPVTCPORE-UHFFFAOYSA-N phenyl-(4-phenylphenyl)methanone Chemical class C=1C=C(C=2C=CC=CC=2)C=CC=1C(=O)C1=CC=CC=C1 LYXOWKPVTCPORE-UHFFFAOYSA-N 0.000 description 1
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- MDDUHVRJJAFRAU-YZNNVMRBSA-N tert-butyl-[(1r,3s,5z)-3-[tert-butyl(dimethyl)silyl]oxy-5-(2-diphenylphosphorylethylidene)-4-methylidenecyclohexyl]oxy-dimethylsilane Chemical compound C1[C@@H](O[Si](C)(C)C(C)(C)C)C[C@H](O[Si](C)(C)C(C)(C)C)C(=C)\C1=C/CP(=O)(C=1C=CC=CC=1)C1=CC=CC=C1 MDDUHVRJJAFRAU-YZNNVMRBSA-N 0.000 description 1
- YRHRIQCWCFGUEQ-UHFFFAOYSA-N thioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=CC=CC=C3SC2=C1 YRHRIQCWCFGUEQ-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- C04B35/591—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride obtained by reaction sintering
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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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
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63424—Polyacrylates; Polymethacrylates
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- 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
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/428—Silicon
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- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- Chemical & Material Sciences (AREA)
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- Manufacturing & Machinery (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
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Abstract
本申请属于陶瓷技术领域，具体涉及一种Si3N4陶瓷及其制备方法。本发明提供的Si3N4陶瓷包括：硅粉、氮化催化剂和烧结助剂；硅粉经氮化催化剂氮化处理后生成Si3N4，氮化催化剂与硅粉的质量比为(1～20):(80～99)；氮化催化剂选自ZrO2、TiO2或Eu2O3；烧结助剂为MgO和Re2O3，Re选自Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu。制备时，依次进行配料混合、制粒、形成陶瓷浆料，再依次光固化成型、脱脂、氮化处理和高温烧结，即可。因而，本申请技术方案通过利用硅粉氮化体积膨胀对样品收缩进行补偿，实现了复杂形状氮化硅陶瓷净尺寸成型，原材料来源广，制备成本低，方法简便。
Description
技术领域
本发明属于陶瓷技术领域，具体涉及一种Si3N4陶瓷及其制备方法。
背景技术
Si3N4陶瓷材料作为一种结构材料，具有优异的力学性能，例如高硬度、高强、耐磨、耐高温、物理化学稳定性等优异性能，可广泛应用于结构件、催化剂载体、过滤材料和散热材料等多个方面。然而，正是因为其优异的力学性能限制了其加工的多样性，如果仅仅依靠传统的加工工艺无法得到具有复杂形状的陶瓷材料，难以满足对个性化、精细化、轻量化和复杂化的高端产品快速制造的需求，限制了高性能陶瓷产品的开发与应用。因而，开发一种可获得任意复杂形状的陶瓷材料的成型工艺具有巨大的应用场景。
目前，Si3N4陶瓷的主流成型工艺为增材制造工艺，但其在烧结后样品出现收缩的现象，严重影响到陶瓷制备的精度。为了解决该方法，常规的做法是：通过估算陶瓷烧结后的收缩率，在设计模型时进行补偿。然而，该法不仅实施起来比较复杂，而且需要保证样品能在三维方向均匀收缩，更严重的是收缩太严重可能破坏其最终结构，产生裂纹或者鼓包。
发明内容
为了解决上述技术问题，本发明的目的在于提供一种Si3N4陶瓷及其制备方法，其具体技术方案如下：
一种Si3N4陶瓷，其制备原材料包括：硅粉、氮化催化剂和烧结助剂；所述硅粉经所述氮化催化剂氮化处理后生成Si3N4，所述氮化催化剂与硅粉的质量比为(1～20):(80～99)；
所述氮化催化剂选自ZrO2、TiO2或Eu2O3；
所述烧结助剂为MgO和Re2O3，所述Re选自Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu。
优选的，所述Si3N4和烧结助剂的质量比为(80～99):(1～20)。
优选的，所述MgO和Re2O3的质量比为(30～60):(40～70)。
优选的，所述硅粉和所述氮化催化剂的质量比为95∶5，所述Si3N4和烧结助剂的质量比为90∶10，所述MgO和Re2O3的质量比为55∶45。
一种上述Si3N4陶瓷的制备方法，包括以下步骤：
a)按配比称取硅粉、氮化催化剂和烧结助剂，混合球磨，得到混合粉体；
b)将步骤a)的混合粉体与分散剂混合，进行喷雾制粒，得到球形颗粒；
c)将步骤b)的球形颗粒与预混溶剂混合，得到陶瓷浆料；
d)将步骤c)的陶瓷浆料置于预置光源波长下进行光固化成型，脱脂，得到脱脂坯体；
e)将步骤d)的脱脂坯体以第一升温速率升温至第一温度，在氮气气氛下进行氮化处理，得到氮化产物；将所述氮化产物以第二升温速率升温至第二温度进行烧结，得到所述Si3N4陶瓷。
优选的，步骤e)所述氮气气氛的压力为5MPa～10MPa。
优选的，步骤e)所述第一升温速率为20℃/min，所述第一温度为1250℃～1600℃，保温时间为0.5h～24h；
所述第二升温速率为10℃/min，所述第二温度为1600℃～2000℃，保温时间为0.5h～24h。
优选的，所述陶瓷浆料中所述球形颗粒的体积百分比含量为45％～70％；
所述硅粉的纯度为95％～100％，粒径小于10μm。
优选的，所述分散剂选自油酸、硬脂酸、聚乙烯吡咯烷酮、六偏磷酸钠、聚丙烯酸钠、酯基季铵盐和聚乙二醇辛基苯基醚中的至少一种。
优选的，所述混合粉末与分散剂的混合质量比为(95～99.99):(0.01～5)。
综上所述，本发明提供了一种Si3N4陶瓷，其制备原材料包括：硅粉、氮化催化剂和烧结助剂，氮化催化剂与Si的质量比为(1～20):(80～99)，氮化催化剂为ZrO2、TiO2或Eu2O3，烧结助剂为MgO和Re2O3。在氮源存在的高温条件下，氮化催化剂可加快硅粉氮化速率，硅粉在经过氮化处理后体积膨胀，可对烧结成型会发生收缩的样品进行补偿，使得产品的尺寸在陶瓷浆料固含量稳定的情况下不变，保证陶瓷样品的精度。
在制备上述Si3N4陶瓷时，通过将硅粉、氮化催化剂和烧结助剂的混合物混合球磨，然后喷雾制粒，获得具有恰当粒径范围和良好球形度的球形颗粒，流动性良好，成型性能优异；然后，将球形颗粒与预混溶剂混合形成陶瓷浆料，依次经过光固化成型、脱脂，得到脱脂坯体；接着，脱脂坯体依次进行氮化处理和烧结，即得具有高致密度、尺寸稳定且形状复杂的氮化硅陶瓷。
经实验证明，通过上述技术方案可制备任意复杂形状的Si3N4陶瓷，其相对密度大于95％，硬度为16GPa～22GPa，断裂韧性为9MPa·m1/2～14MPa·m1/2，抗弯强度为1000MPa～1500MPa。
与现有技术相比，本发明具有下述优点：
1)选用低成本的硅粉为原料快速制备氮化硅，极大的降低制造成本；
2)通过利用硅粉氮化体积膨胀对样品收缩进行补偿，实现复杂形状氮化硅陶瓷净尺寸成型；
3)氮化硅陶瓷采用光固化3D打印成型，具有极高的分辨率，最高达到25μm。
具体实施方式
为了解决现有技术中，陶瓷坯体在高温烧结后出现收缩的现象，本发明提供了一种Si3N4陶瓷及其制备方法。
本发明Si3N4陶瓷的制备方法包括以下步骤：
1、配料
硅粉与氮化催化剂的质量比优选为(80～99):(1～20)，较优选为(90～99):(1～100)，最优选为95∶5；氮化催化剂为ZrO2、TiO2何Eu2O3中的任意一种。
当氮化催化剂与硅粉的质量比低于1：99，可能出现氮化不完全，甚至在较快的升温速率下出现熔硅现象，残余的硅在Si3N4陶瓷中作为一种缺陷会极大地降低制备陶瓷的性能；当氮化催化剂与硅粉的质量比高于20：80，氮化催化剂虽然可以促进硅粉的快速氮化，但是过多的氮化催化剂会引入副产物，例如TiO2作为氮化催化剂添加量超过20％时，过多的TiO2会与Si3N4反应产生Si2N2O的副产物，作为主相的Si3N4则被消耗，得不到本申请所需的Si3N4陶瓷。
Si3N4和烧结助剂的质量比为(80～99):(1～20)，较优选为(90～99):(1～10)，最优选为90∶10。
烧结助剂为MgO和Re2O3，MgO和Re2O3的质量比为(30～60):(40～70)，较优选为(50～60):(40～50)，最优选为55∶45；
其中，Re选自Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu。
硅粉的纯度为99％；粒径小于10μm，优选为0.1μm～10μm，最优选为0.1μm；
氮化催化剂纯度为99％；粒径为<10μm；
MgO粉纯度为99％，Re2O3粉纯度为99.9％。
2、混合球磨
将上述配比的硅粉、氮化催化剂和烧结助剂混合，置于行星式球磨机中，以乙醇为溶剂，以Si3N4球为球磨介质，球料比为(1～5):1，球磨混合4～18h，干燥后得到Si3N4-ZrO2-MgO-Y2O3混合粉体。
3、喷雾制粒
将混合粉体与分散剂混合，进行喷雾制粒，得到球形颗粒，粒径为1μm。
在本发明中，混合粉体与分散剂的混合质量比优选为(95～99.99):(0.01～5)，较优选为(99～99.99):(0.01～1)，最优选为99.95:0.05；
分散剂选自油酸、硬脂酸、聚乙烯吡咯烷酮、六偏磷酸钠、聚丙烯酸钠、酯基季铵盐和聚乙二醇辛基苯基醚中的至少一种。
4、制备陶瓷浆料
将球形颗粒和预混溶剂进行混合，得到陶瓷浆料。
其中，陶瓷浆料的固含量(即球形颗粒含量)优选为45％～70％，较优选为50％～70％，最优选为60％；
预混溶剂包括：单体10重量份～90重量份，低聚物10重量份～90重量份，光引发剂0.1重量份～5重量份，光敏剂0.1重量份～5重量份，增感剂0.1重量份～5重量份，消泡剂0.1重量份～5重量份；
单体选自已二醇二丙烯酸酯、烷氧基丙烯酸酯、聚氨酯二丙烯酸酯、聚氨酯丙烯酸酯、聚氨酯六丙烯酸酯、季戊四醇丙烯酸酯、三丙二醇二丙烯酸酯中的至少一种；
低聚物选自丙烯酸酯、丙烯酸胺和硅烷丙烯酸酯中的至少一种；
光引发剂选自(2,4,6-三甲基苯甲酰基)二苯基氧化膦、苯基双(2,4,6-三甲基苯甲酰基)氧化膦、2,4,6-三甲基苯甲酰基磷酸乙酯、双2,6-二氟-3-吡咯苯基二茂铁、2-异丙基硫杂蒽酮、4-苯基二苯甲酮和2-苯基苄-2-二甲基胺-1-(4-吗啉苄苯基)丁酮中的至少一种；
光敏剂选自间-四羟基苯基二氢卟酚、初卟啉锡、苯卟啉衍生物、苯并卟啉衍生物单酸、亚甲苯兰、酞青类和N-天门冬酰基二氢卟酚中的至少一种；
增感剂选自脂肪族叔胺、乙醇胺类叔胺、叔胺型苯甲酸酯和丙烯酰氧基叔胺中的至少一种；
消泡剂选自巴斯夫-8034A、巴斯夫-NXZ和毕克-555中的一种或多种。
5、固化成型、脱脂
将陶瓷浆料置于300nm～460nm光源波长下进行光固化成型，打印层厚度为25μm～30μm，得到成型的原始坯体；然后脱脂，得到脱脂坯体。
本实步骤所述光固化成型和脱脂为常规技术手段，其具体条件参数可根据实际产品需要进行调节，此处不再一一赘述。
6、氮化处理
将脱脂坯体以20℃/min的升温速率升温至1200℃～1600℃，在氮气气氛下保温反应0.5h～4h，得到氮化产物。其中，氮气压力为5MPa。
7、高温烧结
将氮化产物以10℃/min的升温速率升温至1600℃～2000℃，保温反应0.5h～4h，得到所述Si3N4陶瓷。
下面将结合本发明的实施例，对本发明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
本实施例制备了一种Si3N4陶瓷，其制备的具体步骤如下：
1、配料
在本实施例中，硅粉：氮化催化剂＝95wt％:5wt％，Si3N4:烧结助剂(MgO-Y2O3)＝90wt％:10wt％，MgO:Y2O3＝55wt％:45wt％；
硅粉纯度为99％，粒径0.1μm；
氮化催化剂ZrO2纯度为99％，粒径为0.5μm；
MgO粉纯度为99％，Y2O3粉纯度为99％。
2、混合球磨
将上述配比的硅粉、氮化催化剂和烧结助剂混合，置于行星式球磨机中，以乙醇为溶剂，以Si3N4球为球磨介质，球磨混合8h，干燥后得到Si3N4-ZrO2-MgO-Y2O3混合粉体。
3、喷雾制粒
将混合粉体与分散剂0.03％油酸混合，进行喷雾制粒，得到球形颗粒，粒径为1μm。
4、制备陶瓷浆料
将球形颗粒和预混溶剂进行混合，得到陶瓷浆料。
其中，陶瓷浆料的固含量(即球形颗粒含量)为50％；
预混溶剂包括：单体20重量份，低聚物78重量份，光引发剂0.5重量份，光敏剂0.5重量份，增感剂0.5重量份，消泡剂0.5重量份；
单体选为已二醇二丙烯酸酯，低聚物选为丙烯酸酯，光引发剂选为(2,4,6-三甲基苯甲酰基)二苯基氧化膦，光敏剂选为苯并卟啉衍生物单酸，增感剂选为脂肪族叔胺，消泡剂选为巴斯夫-8034A。
5、固化成型、脱脂
将陶瓷浆料置于355nm光源波长下进行光固化成型，打印层厚度为30μm，得到成型的原始坯体；然后脱脂，得到脱脂坯体。
本实步骤所述光固化成型和脱脂为常规技术手段，其具体条件参数可根据实际产品需要进行调节，此处不再一一赘述。
6、氮化处理
将脱脂坯体以20℃/min的升温速率升温至1400℃，在氮气气氛下保温反应2h，得到氮化产物。其中，氮气压力保持为一个大气压左右即可。
7、高温烧结
将氮化产物以10℃/min的升温速率升温至1800℃，并保持氮气压力为5MPa，保温反应2h，得到所述Si3N4陶瓷。
对本实施例制得的Si3N4陶瓷进行性能检测，测得其相对密度为99％，硬度为18GPa，断裂韧性为10MPa·m1/2，抗弯强度为1200MPa。
实施例2
本实施例与实施例1的区别在于：氮化催化剂TiO2；高温烧结时的氮气压力为10MPa。其余地方与实施例1基本相同，此处不再一一赘述。
对本实施例制得的Si3N4陶瓷进行性能检测，测得其相对密度为99％，硬度为20GPa，断裂韧性为12MPa·m1/2，抗弯强度为1200MPa。
实施例3
本实施例与实施例1的区别在于：氮化催化剂Eu2O3；氮化处理4h；烧结温度为1900℃；高温烧结时的氮气压力为10MPa。其余地方与实施例1基本相同，此处不再一一赘述。
对本实施例制得的Si3N4陶瓷进行性能检测，测得其相对密度为99％，硬度为20GPa，断裂韧性为12MPa·m1/2，抗弯强度为1200MPa。
实施例4
本实施例与实施例1的区别在于：氮化催化剂TiO2；高温烧结时的氮气压力为10MPa；烧结温度为1900℃。其余地方与实施例1基本相同，此处不再一一赘述。
对本实施例制得的Si3N4陶瓷进行性能检测，测得其相对密度为99％，硬度为21GPa，断裂韧性为13MPa·m1/2，抗弯强度为1300MPa。
Claims (10)
1.一种Si3N4陶瓷，其特征在于，其制备原材料包括：硅粉、氮化催化剂和烧结助剂；所述硅粉经所述氮化催化剂氮化处理后生成Si3N4，所述氮化催化剂与硅粉的质量比为(1～20):(80～99)；
所述氮化催化剂选自ZrO2、TiO2或Eu2O3；
所述烧结助剂为MgO和Re2O3，所述Re选自Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu。
2.根据权利要求1所述的Si3N4陶瓷，其特征在于，所述Si3N4和烧结助剂的质量比为(80～99):(1～20)。
3.根据权利要求1或2所述的Si3N4陶瓷，其特征在于，所述MgO和Re2O3的质量比为(30～60):(40～70)。
4.根据权利要求1至3任意一项所述的Si3N4陶瓷，其特征在于，所述硅粉和所述氮化催化剂的质量比为95∶5，所述Si3N4和烧结助剂的质量比为90∶10，所述MgO和Re2O3的质量比为55∶45。
5.一种权利要求1至4任意一项所述的Si3N4陶瓷的制备方法，其特征在于，包括以下步骤：
a)按配比称取硅粉、氮化催化剂和烧结助剂，混合球磨，得到混合粉体；
b)将步骤a)的混合粉体与分散剂混合，进行喷雾制粒，得到球形颗粒；
c)将步骤b)的球形颗粒与预混溶剂混合，得到陶瓷浆料；
d)将步骤c)的陶瓷浆料置于预置光源波长下进行光固化成型，脱脂，得到脱脂坯体；
e)将步骤d)的脱脂坯体以第一升温速率升温至第一温度，在氮气气氛下进行氮化处理，得到氮化产物；将所述氮化产物以第二升温速率升温至第二温度进行烧结，得到所述Si3N4陶瓷。
6.根据权利要求5所述的制备方法，其特征在于，步骤e)所述氮气气氛的压力为5MPa～10MPa。
7.根据权利要求5所述的制备方法，其特征在于，步骤e)所述第一升温速率为20℃/min，所述第一温度为1250℃～1600℃，保温时间为0.5h～24h；
所述第二升温速率为10℃/min，所述第二温度为1600℃～2000℃，保温时间为0.5h～24h。
8.根据权利要求5所述的制备方法，其特征在于，所述陶瓷浆料中所述球形颗粒的体积百分比含量为45％～70％；
所述硅粉的纯度为95％～100％，粒径小于10μm。
9.根据权利要求5所述的制备方法，其特征在于，所述分散剂选自油酸、硬脂酸、聚乙烯吡咯烷酮、六偏磷酸钠、聚丙烯酸钠、酯基季铵盐和聚乙二醇辛基苯基醚中的至少一种。
10.根据权利要求5所述的制备方法，其特征在于，所述混合粉末与分散剂的混合质量比为(95～99.99):(0.01～5)。
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| CN109796208A (zh) * | 2019-03-28 | 2019-05-24 | 西安增材制造国家研究院有限公司 | 一种Si3N4陶瓷结构件及其制备方法 |
| CN110483062A (zh) * | 2019-08-21 | 2019-11-22 | 广东工业大学 | 一种高性能氮化硅陶瓷及其制备方法和应用 |
| CN111533561A (zh) * | 2020-07-06 | 2020-08-14 | 佛山华骏特瓷科技有限公司 | 氮化硅基陶瓷球及其制备方法和应用 |
| CN112341206A (zh) * | 2020-11-05 | 2021-02-09 | 衡阳凯新特种材料科技有限公司 | 一种稀土镨钬稳定氮化硅陶瓷的成型方法 |
| CN114621014A (zh) * | 2022-03-09 | 2022-06-14 | 中国科学院上海硅酸盐研究所 | 一种高强度高热导氮化硅陶瓷材料及其制备方法 |
| CN116813354A (zh) * | 2023-06-06 | 2023-09-29 | 东莞理工学院 | 一种原位制备氮化硅陶瓷的方法、制得的氮化硅陶瓷及其应用 |
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| CN105884376A (zh) * | 2016-04-01 | 2016-08-24 | 广东工业大学 | 一种硅粉流延制备氮化硅陶瓷基板的方法 |
| CN106810215A (zh) * | 2017-01-18 | 2017-06-09 | 深圳摩方新材科技有限公司 | 一种陶瓷浆料的制备及3d打印光固化成型方法 |
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| CN106699191A (zh) * | 2017-01-20 | 2017-05-24 | 广东工业大学 | 一种基于光固化成型的3d打印制备氮化硅陶瓷的方法 |
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| CN106810215A (zh) * | 2017-01-18 | 2017-06-09 | 深圳摩方新材科技有限公司 | 一种陶瓷浆料的制备及3d打印光固化成型方法 |
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| CN109796208A (zh) * | 2019-03-28 | 2019-05-24 | 西安增材制造国家研究院有限公司 | 一种Si3N4陶瓷结构件及其制备方法 |
| CN109796208B (zh) * | 2019-03-28 | 2022-04-19 | 西安增材制造国家研究院有限公司 | 一种Si3N4陶瓷结构件及其制备方法 |
| CN110483062A (zh) * | 2019-08-21 | 2019-11-22 | 广东工业大学 | 一种高性能氮化硅陶瓷及其制备方法和应用 |
| CN111533561A (zh) * | 2020-07-06 | 2020-08-14 | 佛山华骏特瓷科技有限公司 | 氮化硅基陶瓷球及其制备方法和应用 |
| CN112341206A (zh) * | 2020-11-05 | 2021-02-09 | 衡阳凯新特种材料科技有限公司 | 一种稀土镨钬稳定氮化硅陶瓷的成型方法 |
| CN114621014A (zh) * | 2022-03-09 | 2022-06-14 | 中国科学院上海硅酸盐研究所 | 一种高强度高热导氮化硅陶瓷材料及其制备方法 |
| CN116813354A (zh) * | 2023-06-06 | 2023-09-29 | 东莞理工学院 | 一种原位制备氮化硅陶瓷的方法、制得的氮化硅陶瓷及其应用 |
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