CN109437928A - 氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体及其制备方法 - Google Patents
氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体及其制备方法 Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 134
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 42
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 41
- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 35
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 35
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 35
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910001928 zirconium oxide Inorganic materials 0.000 title claims abstract description 32
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 30
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000919 ceramic Substances 0.000 claims abstract description 50
- 239000010936 titanium Substances 0.000 claims abstract description 15
- 239000002002 slurry Substances 0.000 claims abstract description 14
- 239000000853 adhesive Substances 0.000 claims abstract description 10
- 230000001070 adhesive effect Effects 0.000 claims abstract description 10
- 238000000498 ball milling Methods 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 8
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 6
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002019 doping agent Substances 0.000 claims abstract description 4
- 238000003746 solid phase reaction Methods 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract 2
- 238000001035 drying Methods 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 15
- 238000005507 spraying Methods 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 8
- 238000005336 cracking Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229910052727 yttrium Inorganic materials 0.000 claims description 4
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 3
- 229910052691 Erbium Inorganic materials 0.000 claims description 3
- 229910052693 Europium Inorganic materials 0.000 claims description 3
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 3
- 229910052779 Neodymium Inorganic materials 0.000 claims description 3
- 229910052772 Samarium Inorganic materials 0.000 claims description 3
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 239000004615 ingredient Substances 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 238000010671 solid-state reaction Methods 0.000 claims description 3
- 229910052765 Lutetium Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 229910052573 porcelain Inorganic materials 0.000 claims 1
- 238000002390 rotary evaporation Methods 0.000 claims 1
- 239000012071 phase Substances 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 7
- 239000007921 spray Substances 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 4
- 229910000420 cerium oxide Inorganic materials 0.000 abstract description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 abstract description 3
- 239000008187 granular material Substances 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 9
- 239000010955 niobium Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 5
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 239000012720 thermal barrier coating Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229920000084 Gum arabic Polymers 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 241000978776 Senegalia senegal Species 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000000205 acacia gum Substances 0.000 description 1
- 235000010489 acacia gum Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 description 1
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 1
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 description 1
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003116 impacting effect Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 1
- 229910003443 lutetium oxide Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 1
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 description 1
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium(III) oxide Inorganic materials O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及陶瓷粉体制备技术领域，具体公开了氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体，采用掺杂物(氧化锆/氧化钛/氧化铈)、RE2O3粉末、Ta2O5粉末或Nb2O5粉末球磨后，经固相反应得到目标相，后与有机粘接剂混合形成浆料，采用高温喷雾裂解的方法进行干燥，得到类球状的粉体颗粒，后烧结得到氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐陶瓷粉体；该陶瓷粉体的化学通式为RE3‑x(Ta/Nb)1‑x(Zr/Ce/Ti)2xO7，0＜x＜1，晶体结构为正交相，晶格空间群为C2221，粒径为10‑50μm，该陶瓷粉体呈球形。采用本发明的技术方案得到能够满足APS技术要求的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐陶瓷粉体。
Description
技术领域
本发明涉及陶瓷粉体制备技术领域，特别涉及稀土钽/铌酸盐陶瓷粉体及其制备方法。
背景技术
热障涂层材料主要应用于航空发动机工业，具有低热导率、高热膨胀系数、抗烧结、高温稳定性良好等优点，主要起到隔热、防氧化、有效抵抗粒子冲击从而保护航空发动机高温区域零部件基底的作用。
大气等离子喷涂(APS)以及电子束物理气象沉积(EBPVD)技术是目前工业上制备热障涂层材料所通用的制备技术，EBPVD多用于制备柱状晶形貌的热障涂层，而APS技术多用于制备片层状结构的热障涂层，且涂层紧密，气孔率少。但APS技术对粉体具有诸多要求，包括粉体需要具有一定的密度，有机粘接剂要适量，粉体的形状，以及具有一定的粒径范围等，而对于粒径范围通常要在10～200μm范围内，而粉体的形状要呈球形或近球形。
YSZ(氧化钇稳定氧化锆)是当前研究以及应用最为广泛的热障涂层，但由于在1200℃以上时，YSZ会发生相变而导致涂层失效，促使研究人员去寻找能够替代YSZ的热障涂层，2007年哈佛大学Clarke教授课题组同加州大学圣巴巴拉分校的Levi教授等提出了钽酸钇(YTaO4)铁弹体有望作为新型热障涂层材料，但关于稀土钽酸盐的研究主要集中在其晶体结构和发光性能等方面的理论计算；2016年Wang等人通过固相反应法制得了致密的稀土钽酸盐块体材料，得出了热导率远小于YSZ材料的结论，另外还有研究表明，在317相RE3Ta/NbO7的化合物中掺杂四价离子能够进一步降低基底材料的热导率、提升基底材料的热膨胀系数等，研究人员的大量研究与实验结论为稀土钽酸盐在热障涂层上的应用提供了理论的基础。
但目前还没有一种工艺能够制备得到满足APS工艺的掺杂稀土钽/铌酸盐陶瓷粉体。
发明内容
本发明提供了氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体及其制备方法，以满足APS技术对陶瓷粉体粒径和形状的要求，并且在将稀土钽/铌酸盐陶瓷粉体喷涂在合金基体上后，能够起到降低热传导的作用。
为了达到上述目的，本发明的基础方案为：
氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体，该陶瓷粉体的化学通式为RE3-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO7，0＜x＜1，该陶瓷粉体晶体结构为正交相，晶格空间群为C2221，粒径为10-50μm，该陶瓷粉体呈球形。
本基础方案的技术原理和效果在于：
1、本基础方案中氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体的粒径范围在10-50μm范围内，一方面，这样的粒径范围满足APS喷涂技术的粉体要求，不会因粉体粒径太大将喷枪的喷嘴堵塞住，从而导致喷涂失败的问题；另一方面，也不会因粉体的粒径太小，使得粉体质量太小，导致粉末在喷枪的等离子火线的外表面，而未进入其心部，这样粉末在长时间加热作用下直接挥发掉，而导致喷涂失败。
2、本基础方案中氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体呈球形，这样粉体表面较为光滑，这就使得粉体的流动性较好，这样既满足了APS喷涂技术的要求，同时还得到了高质量的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐涂层。
3、本基础方案中在RE3Ta/NbO7的化合物中掺杂四价离子(Zr4+或Ce4+或Ti4+)能够进一步降低基底的热导率、提升基底的热膨胀系数。
进一步，RE为Sc、Y、La、Nd、Sm、Eu、Gd、Dy、Er、Yb、Lu中的一种或几种的混合。
有益效果：发明人通过实验的验证，采用这几种或几种的混合的稀土元素，得到的稀土钽/铌酸盐(RE3Ta/NbO7)陶瓷粉体粒径范围较为均匀。
进一步，氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐(RE3TaO7/RE3NbO7)陶瓷粉体的制备方法，包括以下步骤：
步骤(1)：称取RE:(Ta/Nb):(Zr/Ce/Ti)的摩尔比为(3-x):(1-x):2x的Ta2O5粉末或Nb2O5粉末、掺杂物(ZrO2粉末或CeO2粉末或TiO2粉末)、RE2O3粉末加入溶剂中，形成混合溶液，采用球磨机对混合溶液进行球磨，球磨的时间不小于10h，球磨机的转速不小于300转/分，经干燥后得到干燥的粉末A；
步骤(2)：将步骤(1)得到的粉末A进行高温固相反应，反应温度为1600-1800℃，反应时间为6-20h，得到成分为RE3-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO7的粉末B；
步骤(3)：将步骤(2)得到的粉末B与溶剂、有机粘接剂混合得到浆料C，所述浆料C中粉末B的质量百分比为10％～40％，有机粘接剂的质量百分比为0.1％～3％，其余为溶剂，在温度1000-1200℃下对浆料C进行喷雾裂解干燥，干燥时间为30-60min，得到干燥的料粒D；
步骤(4)：将步骤(3)得到的料粒D在温度1400-1600℃下烧结，烧结时间为2-4h，得到的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体。
有益效果：采用步骤(1)～步骤(4)的工艺制备得到的了粒径为10～50μm的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐(RE3TaO7/RE3NbO7)陶瓷粉体。
采用步骤(1)和步骤(2)得到目标相RE3-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO7陶瓷粉末。
步骤(3)采用高温喷雾裂解的方式对制得的浆料C进行干燥，其中有机粘接剂是为了将目标相RE3-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO7陶瓷粉末中细小的粉末颗粒团聚在一起，而喷雾裂解干燥的原理为：将制得的浆料C，通过高压气体雾化，使得浆料C形成细小的液滴，在1000-1200℃高温下，液滴中的液体快速蒸发，进而得到近球形的粉末。
步骤(4)的烧结是为了将步骤(3)得到的料粒D形成一定的结合强度，具有一定的密度，进而形成球状的形貌。
进一步，所述步骤(1)中的干燥采用旋转蒸发仪进行干燥，干燥温度为40-60℃，旋转蒸发时间为2-4h。
有益效果：采用旋转蒸发仪进行干燥，干燥的时间较短，且粉体在旋转过程中可以得到较为充分的干燥。
进一步，所述步骤(1)得到的粉末A、步骤(2)得到的粉末B和步骤(4)得到的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体均采用200-500目的筛子过筛。
有益效果：将各步骤得到的粉体过筛，避免出现颗粒较大的粉末，以烧结步骤为例，由于烧结过程中，可能会产生块体，因此过筛可以将这些块体清除掉。
进一步，所述步骤(3)中的喷雾裂解温度为1200℃，时间为60min。
有益效果：发明人通过实验的验证得出，该参数下得到粉体的粒径范围较为均匀，且均呈球状的形貌。
进一步，所述步骤(1)在称量粉末之前对粉末进行预干燥，预干燥温度为600-800℃，干燥时间为8-10h。
有益效果：预干燥能降低前驱粉体中的含水量，从而降低水分对准确称量的影响。
进一步，所述步骤(1)中ZrO2粉末或CeO2粉末或TiO2粉末、RE2O3粉末、Ta2O5粉末或Nb2O5粉末的纯度不低于99.9％。
有益效果：采用纯度较高的前驱粉体，降低引入的杂质元素，降低杂质对粉体制备的不良影响。
附图说明
图1为本发明实施例2制得的氧化铈掺杂稀土钽酸盐(Y2.8Ta0.8Ce0.4O7)的XRD图；
图2为本发明实施例2制得的氧化铈掺杂稀土钽酸盐(Y2.8Ta0.8Ce0.4O7)的SEM图。
具体实施方式
下面通过具体实施方式进一步详细说明：
氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体，该陶瓷粉体的化学通式为RE3-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO7，0＜x＜1，RE为Sc、Y、La、Nd、Sm、Eu、Gd、Dy、Er、Yb、Lu中的一种或几种的混合，该陶瓷粉体晶体结构为正交相，晶格空间群为C2221，粒径为10-50μm，该陶瓷粉体呈球形。
氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体的制备方法，包括以下几个步骤：
步骤(1)：将掺杂物(氧化锆(ZrO2)粉末或氧化铈(CeO2)粉末或氧化钛(TiO2)粉末中的一种)、稀土氧化物粉末(稀土氧化物为Sc2O3、Y2O3、La2O3、Nd2O3、Sm2O3、Eu2O3、Gd2O3、Dy2O3、Er2O3、Yb2O3、Lu2O3中的一种或几种)、五氧化二钽(Ta2O5)粉末或五氧化二铌(Nb2O5)粉末进行预干燥，预干燥的温度为600-800℃，预干燥的时间为8-10h，按照RE3-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO7对应元素的化学计量比分别称取预干燥后的粉末，加入到去离子水或乙醇溶剂中，得到混合溶液，使得混合溶液中RE:(Ta/Nb):(Zr/Ce/Ti)的摩尔比为(3-x):(1-x):2x，采用球磨机对混合溶液进行球磨，球磨的时间不小于10h，球磨机的转速不小于300转/分。
将球磨后得到的浆料采用旋转蒸发仪(型号：N-1200B)进行干燥，干燥温度为40-60℃，干燥的时间为2-4h，得到粉末A，将粉末A采用200-500目的筛子过筛。
步骤(2)：将步骤(1)中得到过筛后的粉末A进行高温固相反应，反应温度为1600-1800℃，反应时间为6-20h，得到成分为RE3-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO7的粉末B，将粉末B采用200-500目的筛子过筛。
步骤(3)：将步骤(2)得到过筛后的粉末B与去离子水或乙醇溶剂、有机粘接剂混合得到浆料C，其中浆料C中粉末B的质量百分比为10％～40％，有机粘接剂的质量百分比为0.1％～3％，其余为溶剂，有机粘接剂采用聚乙烯醇或者***树胶，在温度1000-1200℃下对浆料C进行喷雾裂解干燥，干燥时间为30-60min，得到干燥的料粒D；
步骤(4)：将步骤(3)得到的料粒D在温度1400-1600℃下烧结，烧结时间为2-4h，得到的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体，将得到的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体采用200-500目的筛子过筛。
采用上述方法得到了粒径为10～50μm的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体，且陶瓷粉体检测到的形貌呈球形。
表一为本发明实施例1-6的具体参数(表格中斜杠表示该实施例中不含有该成分)：
表二为本发明实施例7-12的具体参数(表格中斜杠表示该实施例中不含有该成分)：
实施例1-12采用扫描电镜检测，得到粉体的粒径范围均在10-50μm范围内，且均呈球形。
以实施例2为例，对得到的氧化铈掺杂稀土钽酸盐(Y2.8Ta0.8Ce0.4O7)陶瓷粉体材料进行表征：
1、XRD表征：
X射线衍射图谱如图1所示，可知实施例2得到的氧化铈掺杂稀土钽酸盐(Y2.8Ta0.8Ce0.4O7)陶瓷粉体为正交相，无杂相，晶格空间群为C2221。
2、SEM表征：
实施例2制备的氧化铈掺杂稀土钽酸盐(Y2.8Ta0.8Ce0.4O7)陶瓷粉体的SEM图谱如图2所示，从图2可知粉体的粒径范围在10-50μm，且呈球形的形貌。
列举对比例3组与实施例1-12得到的陶瓷粉体进行对比：
对比例1：与实施例1的区别在于，未采用喷雾裂解的方式进行干燥，干燥的温度为800℃，干燥时间为1.5h，最后得到的粉体粒径范围为180μm-220μm，且粉体呈不规则的形貌。
对比例2：与实施例1的区别仅在于，球磨的时间为7h，最后得到的粉体平均粒径大于200μm。
对比例3：与实施例1的区别仅在于，烧结后未进行过筛处理，最后得到的粉体中含有粒径大于220μm的块体。
综上，本实施例1-12制备的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体，粒径范围为10-50μm，且呈球状的形貌，符合APS喷涂技术对粉体的要求，而对比例1-3均未得到符合APS喷涂技术要求的陶瓷粉体。
以上所述的仅是本发明的实施例，方案中公知的具体结构及特性等常识在此未作过多描述。应当指出，对于本领域的技术人员来说，在不脱离本发明结构的前提下，还可以作出若干变形和改进，这些也应该视为本发明的保护范围，这些都不会影响本发明实施的效果和专利的实用性。本申请要求的保护范围应当以其权利要求的内容为准，说明书中的具体实施方式等记载可以用于解释权利要求的内容。
Claims (8)
1.氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体，其特征在于：该陶瓷粉体的化学通式为RE3-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO7，0＜x＜1，该陶瓷粉体晶体结构为正交相，晶格空间群为C2221，粒径范围为10-50μm，该陶瓷粉体呈球形。
2.根据权利要求1所述的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体，其特征在于：RE为Sc、Y、La、Nd、Sm、Eu、Gd、Dy、Er、Yb、Lu中的一种或几种的混合。
3.根据权利要求2所述的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体的制备方法，其特征在于：包括以下步骤：
步骤(1)：称取RE:(Ta/Nb):(Zr/Ce/Ti)的摩尔比为(3-x):(1-x):2x的Ta2O5粉末或Nb2O5粉末、掺杂物(ZrO2粉末或CeO2粉末或TiO2粉末)、RE2O3粉末加入溶剂中，形成混合溶液，采用球磨机对混合溶液进行球磨，球磨的时间不小于10h，球磨机的转速不小于300转/分，经干燥后得到干燥的粉末A；
步骤(2)：将步骤(1)得到的粉末A进行高温固相反应，反应温度为1600-1800℃，反应时间为6-20h，得到成分为RE3-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO7的粉末B；
步骤(3)：将步骤(2)得到的粉末B与溶剂、有机粘接剂混合得到浆料C，所述浆料C中粉末B的质量百分比为10％～40％，有机粘接剂的质量百分比为0.1％～3％，其余为溶剂，在温度1000-1200℃下对浆料C进行喷雾裂解干燥，干燥时间为30-60min，得到干燥的料粒D；
步骤(4)：将步骤(3)得到的料粒D在温度1400-1600℃下烧结，烧结时间为2-4h，得到氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体。
4.根据权利要求3所述的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体的制备方法，其特征在于：所述步骤(1)中的干燥采用旋转蒸发仪进行干燥，干燥温度为40-60℃，旋转蒸发时间为2-4h。
5.根据权利要求4所述的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体的制备方法，其特征在于：所述步骤(1)得到的粉末A、步骤(2)得到的粉末B和步骤(4)得到的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体均采用200-500目的筛子过筛。
6.根据权利要求5所述的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体的制备方法，其特征在于：所述步骤(3)中的喷雾裂解温度为1200℃，时间为60min。
7.根据权利要求6所述的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体的制备方法，其特征在于：所述步骤(1)在称量粉末之前对粉末进行预干燥，预干燥温度为600-800℃，干燥时间为8-10h。
8.根据权利要求7所述的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RE3Ta/NbO7陶瓷粉体的制备方法，其特征在于：所述步骤(1)中ZrO2粉末或CeO2粉末或TiO2粉末、RE2O3粉末、Ta2O5粉末或Nb2O5粉末的纯度不低于99.9％。
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