CN109534814B - 氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐(RETa/NbO4)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(RETa/NbO4)陶瓷粉体及其制备方法 Download PDF

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CN109534814B
CN109534814B CN201811647659.0A CN201811647659A CN109534814B CN 109534814 B CN109534814 B CN 109534814B CN 201811647659 A CN201811647659 A CN 201811647659A CN 109534814 B CN109534814 B CN 109534814B
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powder
ceramic powder
rare earth
reta
niobate
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CN109534814A (zh
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冯晶
吴鹏
葛振华
宋鹏
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Shaanxi Tianxuan Coating Technology Co ltd
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Kunming University of Science and Technology
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Priority to CN201811647659.0A priority Critical patent/CN109534814B/zh
Priority to US17/418,207 priority patent/US11584692B2/en
Priority to JP2021538498A priority patent/JP7220794B2/ja
Priority to EP19902209.6A priority patent/EP3882227A4/en
Priority to PCT/CN2019/070804 priority patent/WO2020133575A1/zh
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Abstract

本发明属于陶瓷粉体制备技术领域，公开了氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RETa/NbO4陶瓷粉体及其制备方法。氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RETa/NbO4陶瓷粉体，其化学通式为RE1‑x(Ta/Nb)1‑x(Zr/Ce/Ti)2xO4，0＜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10‑70μm，该陶瓷粉体呈球形。制备时，通过对原料进行球磨，再采用高温固相法反应后，与溶剂、有机粘接剂混合得到浆料C，并进行离心雾化后得到干燥的粒料，再烧结，得到一种满足APS技术对陶瓷粉体的要求的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐RETa/NbO4陶瓷粉体。

Description

氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐(RETa/NbO4)陶瓷 粉体及其制备方法
技术领域
本发明属于陶瓷粉体制备领域，具体涉及一种氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐(RETa/NbO4)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。
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114相RETa/NbO4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。
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分布等，而对于粒径分布通常要在10～200μm范围内，而粉体的形状要呈球形或近球形。而目前还没有一种工艺能够制备得到满足APS工艺的掺杂稀土钽酸盐陶瓷粉体。
发明内容
本发明意在提供一种氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐(RETa/NbO4)陶瓷粉体及其制备方法，以满足APS技术对陶瓷粉体的要求，并且在将氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐(RETa/NbO4)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。
为实现上述目的，本发明提供如下基础技术方案，氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐(RETa/NbO4)陶瓷粉体，该陶瓷粉体的化学通式为RE1-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO4，0＜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10-70μm，该陶瓷粉体呈球形。
本技术方案的有益效果：
1、本基础方案中氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐(RETa/NbO4)陶瓷粉体的粒径为10-70μm，一方面，这样的粒径分布满足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(RETa/NbO4)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RETa/NbO4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(RETa/NbO4)陶瓷粉体粒径较为均匀。
本发明还提供另一基础方案，氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐(RETa/NbO4)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(1-x):(1-x):2x的RE2O3粉末、Ta2O5粉末/Nb2O5粉末、掺杂物加入溶剂中，形成混合溶液，掺杂物为ZrO2粉末、CeO2粉末或TiO2粉末，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300r/min，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1500-1800℃，反应时间为6-20h，得到成分为RE1-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO4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400-800℃的温度下对浆料C进行离心雾化实现干燥，离心速度为8000-9000r/min，得到干燥的料粒D；
步骤(4)：
将步骤(3)得到的料粒D在温度800-1300℃下烧结，烧结时间为7-9h，制得氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐(RETa/NbO4)陶瓷粉体。
本技术方案的有益效果为：
1、采用步骤(1)～步骤(4)的工艺制备得到的了粒径为10～70μm的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐(RETaO4/RENbO4)陶瓷粉体，以满足APS喷涂技术的要求，同时实现了对稀土钽/铌酸盐(RE3TaO4/RE3NbO4)陶瓷粉体作为热障涂层的使用。
2、采用步骤(1)和步骤(2)得到目标相RE1-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO4陶瓷粉末。
3、步骤(3)采用离心雾化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RE1-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO4陶瓷粉末中细小的粉末颗粒团聚在一起，而离心雾化干燥的原理为：浆料C进入高速旋转的喷雾盘，被喷成极小的雾化液滴，使浆料C表面积大大增加，与热空气接触，水分迅速蒸发，能在极短的时间内干燥，进而得到近球形的粉末。
4、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)得到的稀土钽/铌酸盐(RETa/NbO4)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)中离心雾化的温度为600℃，离心速度为8500r/min。
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较为均匀，且均呈球状的形貌。
进一步，所述步骤(1)中的RE2O3粉末、Ta2O5粉末/Nb2O5粉末在称量之前进行预干燥，预干燥温度为400-700℃，干燥时间为5-8h。
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RE2O3粉末、Ta2O5粉末/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。
进一步，所述步骤(3)中浆料C中粉末B的质量百分比为25％，有机粘接剂的质量百分比为2％。
有益效果：发明人通过实验的验证得出，该参数下能实现目标相RETa/NbO4粉末中细小的粉末颗粒团聚的效果佳。
进一步，所述步骤(4)中的烧结温度为1200℃，烧结时间为8h。
有益效果：发明人通过实验的验证得出，该参数下能料粒D结合强度大，密度大，并形成球状的形貌。
附图说明
图1为本发明实施例5制得的氧化锆掺杂稀土钽酸盐(Sc0.8Ta0.8Zr0.4O4)的XRD图；
图2为本发明实施例5制得的氧化锆掺杂稀土钽酸盐(Sc0.8Ta0.8Zr0.4O4)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(RETa/NbO4)陶瓷粉体，该陶瓷粉体的化学通式为RE1-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO4，0＜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10-70μm，该陶瓷粉体呈球形。
申请人对在研究过程中，对本发明氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐(RETa/NbO4)陶瓷粉体及其制备方法进行了大量的实验，现以其中12组实验进行说明。氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐(RETa/NbO4)陶瓷粉体及其制备方法的实施例1-12的各参数如表1、表2所示：(表1为实施例1-6的具体参数、表2为实施例7-12的具体参数)
表1
Figure GDA0002388861190000051
Figure GDA0002388861190000061
表2
Figure GDA0002388861190000062
Figure GDA0002388861190000071
现以实施例1为例，对本发明氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐(RETa/NbO4)陶瓷粉体的制备方法，进行说明。
氧化锆(ZrO2)掺杂稀土碳酸盐(RETaO4)陶瓷粉体(Sc0.8Ta0.8Zr0.4O4)的制备方法，包括以下几个步骤：
步骤(1)：
将氧化锆(ZrO2)粉末、稀土氧化物粉末Sc2O3、五氧化二钽(Ta2O5)粉末进行预干燥，预干燥的温度为600℃，预干燥的时间为8h；并称取5.58g氧化锆(ZrO2)粉末、6.24g稀土氧化物粉末Sc2O3、20g氧化二钽(Ta2O5)粉末加入到乙醇溶剂中，得到混合溶液，使得混合溶液中Sc:Ta:Zr的摩尔比为2:2:1；再采用球磨机对混合溶液进行球磨10h，球磨机的转速为300r/min。
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60℃，干燥的时间为2h，将干燥后的粉末采用300目的筛子过筛，得到粉末A。
步骤(2)：
将步骤(1)中得到的粉末A采用高温固相反应法制得成分为ZrO2掺杂ScTaO4的粉末B，反应温度为1700℃，反应时间为10h；并采用300目的筛子对粉末B进行过筛。
步骤(3)：
将步骤(2)中过筛后的粉末B与去离子水溶剂、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25％，有机粘接剂的质量百分比为2％，其余为溶剂，有机粘接剂采用聚乙烯醇或者阿拉伯树胶，本实施例使用聚乙烯醇；再利用离心雾化法对浆料C进行干燥，干燥时的温度为600℃，离心速度为8500r/min，得到干燥的料粒D。
步骤(4)：
将步骤(3)得到的料粒D在1200℃的温度下烧结8h，再采用300目的筛子对烧结后的料粒D过筛，得到粒径为10～70nm并且形貌呈球形的氧化锆(ZrO2)掺杂ScTaO4陶瓷粉体(Sc0.8Ta0.8Zr0.4O4)。
实施例2-6与实施例1的不同之处仅在于参数不同，以及最后形成的陶瓷粉体不同。
对实施例1-12进行XRD表征、SEM表征，现以实施例1为例，对得到的氧化锆掺杂稀土钽酸盐陶瓷粉体(Sc0.8Ta0.8Zr0.4O4)材料的表征进行说明：
1XRD表征：
X射线衍射图谱如图1所示，由图1可知，实施例1得到的氧化锆掺杂稀土钽酸盐陶瓷粉体(Sc0.8Ta0.8Zr0.4O4)为正交相，无杂相，晶格空间群为C2221。而实施例2-12得到的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐(RETa/NbO4)陶瓷粉体均为正交相，无杂相，晶格空间群均为C2221。
2SEM表征：
实施例1制备的氧化锆掺杂稀土钽酸盐陶瓷粉体(Sc0.8Ta0.8Zr0.4O4)的SEM图谱如图2所示，从图2可知粉体的粒径范围为10-70μm，且呈球形的形貌。而实施例2-12得到的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐(RETa/NbO4)陶瓷粉体粒径范围均为10-70μm，且均呈球形的形貌。
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，未采用离心雾化的方式进行干燥，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(RETa/NbO4)陶瓷粉体，粒径为10-70μm内，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喷涂技术的陶瓷粉体。
对于本领域的技术人员来说，在不脱离本发明技术方案构思的前提下，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，这些都不会影响本专利实施的效果和专利的实用性。

Claims (10)

1.氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐(RETa/NbO4)陶瓷粉体，其特征在于：该陶瓷粉体的化学通式为RE1-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO4，0＜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10-70μm，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(RETa/NbO4)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(RETa/NbO4)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(1-x):(1-x):2x的RE2O3粉末、Ta2O5粉末/Nb2O5粉末、掺杂物加入溶剂中，形成混合溶液，掺杂物为ZrO2粉末、CeO2粉末或TiO2粉末，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300r/min，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1500-1800℃，反应时间为6-20h，得到成分为RE1-x(Ta/Nb)1-x(Zr/Ce/Ti)2xO4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400-800℃的温度下对浆料C进行离心雾化实现干燥，离心速度为8000-9000r/min，得到干燥的料粒D；
步骤(4)：
将步骤(3)得到的料粒D在温度800-1300℃下烧结，烧结时间为7-9h，制得氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐(RETa/NbO4)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(RETa/NbO4)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(RETa/NbO4)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)得到的稀土钽/铌酸盐(RETa/NbO4)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(RETa/NbO4)陶瓷粉体的制备方法，其特征在于：所述步骤(3)中离心雾化的温度为600℃，离心速度为8500r/min。
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(RETa/NbO4)陶瓷粉体的制备方法，其特征在于：所述步骤(1)中的RE2O3粉末、Ta2O5粉末/Nb2O5粉末在称量之前进行预干燥，预干燥温度为400-700℃，干燥时间为5-8h。
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(RETa/NbO4)陶瓷粉体的制备方法，其特征在于：所述步骤(1)中RE2O3粉末、Ta2O5粉末/Nb2O5粉末的纯度不低于99.9％。
9.根据权利要求8所述的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐(RETa/NbO4)陶瓷粉体的制备方法，其特征在于：所述步骤(3)中浆料C中粉末B的质量百分比为25％，有机粘接剂的质量百分比为2％。
10.根据权利要求9所述的氧化锆/氧化钛/氧化铈掺杂稀土钽/铌酸盐(RETa/NbO4)陶瓷粉体的制备方法，其特征在于：所述步骤(4)中的烧结温度为1200℃，烧结时间为8h。
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