CN114853473A - 一种耐高温cmas腐蚀的稀土硅酸盐陶瓷与制备方法 - Google Patents
一种耐高温cmas腐蚀的稀土硅酸盐陶瓷与制备方法 Download PDFInfo
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Abstract
一种耐高温CMAS腐蚀的稀土硅酸盐的陶瓷与制备方法，该陶瓷为高熵稀土单硅酸盐和高熵稀土双硅酸盐复合的复相陶瓷结构。通过固相反应法将RE2O3和SiO2分别合成单相(xRE1/x)2SiO5粉体和单相(xRE1/x)2Si2O7粉体，然后将单相(xRE1/x)2SiO5粉体和单相(xRE1/x)2Si2O7粉体按一定比例进行复合，形成(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相粉体，再将粉体压片后无压烧结形成(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相陶瓷块体；该结构的高熵稀土硅酸盐陶瓷具有良好的耐高温CMAS腐蚀能力等优异的性能。
Description
技术领域
本发明属于环境障涂层材料的制备技术领域，涉及一种高熵稀土单硅酸盐和高熵稀土双硅酸盐复合的复相陶瓷的结构设计及制备方法。
背景技术
SiC陶瓷基复合材料(CMCs)，是以SiC陶瓷为基体，C或SiC纤维增强的复合材料。SiC-CMCs具备密度低、耐高温、力学性能优异、抗氧化等特点，将其应用于航空发动机如燃烧室，涡轮等，可达到结构减重、燃烧效率提高的效果，实现高推重比发展，SiC-CMCs因此得到研究者的广泛关注。
SiC-CMCs在干燥氧化气氛中，表面能形成致密、抗氧化的SiO2保护层。但在航空发动机燃气环境中，SiO2保护层会与水蒸气反应生成挥发性Si(OH)4，造成氧化膜失效及复合材料的挥发与损伤，降低结构部件的力学性能与服役可靠性。
因此，需要在SiC-CMCs表面涂覆一层环境障涂层(EBCs)，可以将SiC-CMCs与燃烧室腐蚀环境隔离开，提高基体材料的高温稳定性，延长服役寿命。稀土硅酸盐陶瓷具有优异的抗氧化性、耐高温水汽腐蚀性能，以及与SiC基陶瓷相匹配的热膨胀系数和良好的化学相容性等优点，成为目前SiC基陶瓷表面EBCs的热门材料。但是，单组元稀土硅酸盐在长时间、高温环境中结构稳定性较差，稀土双硅酸盐易发生晶型转变、晶粒异常长大等现象，而稀土单硅酸盐易与SiO2反应生成稀土双硅酸盐，并存在热膨胀系数较大，与基体不匹配的问题。与此同时，在沙漠或火山附近，沙子或者火山灰常常会被吸入飞机发动机内，该类物质主要成分为A12O3-MgO-CaO-SiO2(CMAS)，其熔点较低，会在叶片等热端部件表面熔融，从而不断与表面稀土硅酸盐涂层发生反应而导致涂层失效。
“高熵”是21世纪提出的新材料设计理论，是由四种或多种组分构成的固溶体材料，其特点可以概括为四种效应：热力学的高熵效应、结构的晶格畸变效应、动力学的迟滞扩散效应、性能上的“鸡尾酒”效应。近年来，一些研究人员对高熵稀土硅酸盐展开了一系列工作，研究发现，与单组元稀土硅酸盐相比，高熵稀土硅酸盐不仅表现出优异的高温结构稳定性，而且具有较低的热导率、与SiC基陶瓷相匹配的热膨胀系数、良好的耐高温水汽腐蚀和高温CMAS腐蚀能力。与单组元稀土硅酸盐相比，尽管高熵稀土硅酸盐具有优异的耐高温CMAS腐蚀能力，但在长时间、高温CMAS腐蚀后其反应层厚度仍然较厚，约为300μm，并伴有应力裂纹和气泡缺陷产生。这对只有几十至几百微米厚的EBCs来说仍然是灾难性的，腐蚀能力差，限制了EBCs在高温下的应用。因此，现有的涂层均无法满足高温极端环境下的使用要求。
发明内容
发明目的
本发明针对高熵稀土硅酸盐在长时间、高温CMAS腐蚀后其反应层厚，并伴有应力裂纹和气泡缺陷，且腐蚀能力差，提供了一种耐高温CMAS腐蚀的高熵稀土硅酸盐的复相结构陶瓷与制备方法。
技术方案
一种耐高温CMAS腐蚀的稀土硅酸盐陶瓷，其特征在于：该陶瓷结构为高熵稀土单硅酸盐(xRE1/x)2SiO5和高熵稀土双硅酸盐(xRE1/x)2Si2O7形成的复合相陶瓷，其中，(xRE1/x)2SiO5与(xRE1/x)2Si2O7的质量比为1/3~3/1；其中的RE为稀土元素，x为组元数。
一种如上所述的耐高温CMAS腐蚀的稀土硅酸盐陶瓷的制备方法，其特征在于：步骤如下：
步骤1，高熵稀土单、双硅酸盐粉体制备：首先，将RE2O3、SiO2粉体按照摩尔比1:1的比例在球磨机中湿球磨混合24 h。之后将所得浆液放入烘箱，在80 ℃下干燥10 h。然后将干燥后粉体在1450~1550 ℃温度下煅烧2 h，再经过球磨破碎10 h，合成出单相高熵稀土单硅酸盐(xRE1/x)2SiO5粉体；将RE2O3、SiO2粉体按照摩尔比1:2的比例在球磨机中湿球磨混合24 h。之后将所得浆液放入烘箱，在80 ℃下干燥10 h。然后，将混合粉体在1450~1550 ℃温度下煅烧2 h，经过球磨破碎10 h，合成出单相高熵稀土双硅酸盐(xRE1/x)2Si2O7粉体；
步骤2，(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相粉体制备：将步骤1制备好的单相(xRE1/x)2SiO5粉体和单相(xRE1/x)2Si2O7粉体，在球磨机中湿球磨混合24 h，然后将所得浆液放入烘箱，在80 ℃下干燥10 h，再过200目筛获得(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相粉体；
步骤3，试样烧结：将得到的(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相粉体压制成陶瓷块体，随后采用无压烧结，在1600~1700 ℃下保温10 h，升温速率5 ℃/min，制备成致密的(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相陶瓷块体。
优选的，步骤1所述的RE2O3中RE为稀土元素，x为2~6组元。
优选的，步骤2所述(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相粉体中，(xRE1/x)2SiO5和(xRE1/x)2Si2O7的质量比为1/3~3/1。
优选的，步骤3所述致密的(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相陶瓷块体的相对密度为96%~98%。
优点及效果
与现有方法相比，本发明具有如下优点：（1）该方法具有工艺简单，成本低、可以大批量生产等优点；（2）高熵稀土单硅酸盐能够与SiO2发生反应，消除了高熵稀土双硅酸盐晶界处的SiO2相，净化了晶界，抑制高温CMAS熔体的渗入，显著提高了材料耐高温CMAS腐蚀能力；（3）由于“高熵稳定效应”和复相陶瓷结构特征，极大改善耐高温CMAS腐蚀能力。
附图说明
图1为本发明(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相陶瓷的表面形貌；
图2为本发明(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相陶瓷的截面形貌。
具体实施方式
下面结合附图对本发明做进一步的说明：
一种耐高温CMAS腐蚀的稀土硅酸盐陶瓷，该陶瓷结构为高熵稀土单硅酸盐(xRE1/x)2SiO5和高熵稀土双硅酸盐(xRE1/x)2Si2O7形成的复合相陶瓷，其中，(xRE1/x)2SiO5与(xRE1/x)2Si2O7的质量比为1/3~3/1；其中的RE为稀土元素，x为组元数。
一种耐高温CMAS腐蚀的稀土硅酸盐的制备方法，制备步骤为：首先，通过固相反应法将RE2O3和SiO2合成单相(xRE1/x)2SiO5粉体和单相(xRE1/x)2Si2O7粉体，然后将单相(xRE1/x)2SiO5粉体和单相(xRE1/x)2Si2O7粉体进行复合形成(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相粉体，（参见图1、图2）再将粉体压片无压烧结后形成(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相陶瓷块体；该结构的陶瓷具有良好的耐高温CMAS腐蚀能力等优异性能。
实施例1
本实施例是选取了Y、Yb元素，制备二组元高熵(2RE1/2)2Si2O7/(2RE1/2)2SiO5复相陶瓷，包括以下步骤：
步骤1，高熵稀土单、双硅酸盐粉体制备：将RE2O3（RE为稀土元素）、SiO2分别按摩尔比1:1和1:2比例进行混合。将混合粉体在球磨机中湿球磨混合24 h，之后将所得浆液放入烘箱，在80 ℃下干燥10 h，然后将干燥后的粉体在1450 ℃温度下煅烧2 h，再经过球磨破碎10h，分别合成出单相高熵稀土单硅酸盐(2RE1/2)2SiO5粉体和单相高熵稀土双硅酸盐(2RE1/2)2Si2O7粉体。
步骤2，(2RE1/2)2Si2O7/(2RE1/2)2SiO5复相粉体制备：将步骤1制备好的单相粉体，按(2RE1/2)2SiO5：(2RE1/2)2Si2O7的质量比为1:1比例在球磨机中湿球磨混合24 h，然后将所得浆液放入烘箱，在80 ℃下干燥10 h，再过200目筛获得(2RE1/2)2Si2O7/(2RE1/2)2SiO5复相粉体。
步骤3，试样烧结：将得到的(2RE1/2)2Si2O7/(2RE1/2)2SiO5复相粉体压制陶瓷块体，采用无压烧结，在1700 ℃下保温10 h，升温速率5 ℃/min，制备成致密的(2RE1/2)2Si2O7/(2RE1/2)2SiO5复相陶瓷块体。
本实施例制备的(2RE1/2)2Si2O7/(2RE1/2)2SiO5复相陶瓷结构致密，相对密度达到96.6 %，在1400 ℃下经CMAS腐蚀48 h后，反应层厚度仅为150μm，与单组元稀土硅酸盐相比，耐腐蚀性能得到了显著提高。
实施例2
本实施例是选取了Y、Yb、Er元素，制备三组元高熵(3RE1/3)2Si2O7/(3RE1/3)2SiO5复相陶瓷，包括以下步骤：
步骤1，高熵稀土单、双硅酸盐粉体制备：将RE2O3（RE为稀土元素）、SiO2分别按摩尔比1:1和1:2比例进行混合。将混合粉体在球磨机中湿球磨混合24 h，之后将所得浆液放入烘箱，在80 ℃下干燥10 h，然后将干燥后的粉体在1500 ℃温度下保温2 h，再经过球磨破碎10h，分别合成出单相高熵稀土单硅酸盐(3RE1/3)2SiO5粉体和单相高熵稀土双硅酸盐(3RE1/3)2Si2O7粉体。
步骤2，(3RE1/3)2Si2O7/(3RE1/3)2SiO5复相粉体制备：将步骤1制备好的单相粉体，按(3RE1/3)2SiO5：(3RE1/3)2Si2O7的质量比为1:3比例在球磨机中湿球磨混合24 h，然后将所得浆液放入烘箱，在80 ℃下干燥10 h，再过200目筛获得(3RE1/3)2Si2O7/(3RE1/3)2SiO5复相粉体。
步骤3，试样烧结：将得到的(3RE1/3)2Si2O7/(3RE1/3)2SiO5复相粉体压制成陶瓷块体，采用无压烧结，在1650 ℃下保温10 h，升温速率5 ℃/min，制备成致密的(3RE1/3)2Si2O7/(3RE1/3)2SiO5复相陶瓷块体。
本实施例制备的(3RE1/3)2Si2O7/(3RE1/3)2SiO5复相陶瓷结构致密，相对密度达到97.1 %，在1500 ℃下经CMAS腐蚀48 h后，反应层厚度仅为95μm，耐腐蚀性能得到了显著提高。
实施例3
结合图1-2，本实施例是选取了Y、Yb、Er、Sc元素，制备四组元高熵(4RE1/4)2Si2O7/(4RE1/4)2SiO5复相陶瓷，包括以下步骤：
步骤1，高熵稀土单、双硅酸盐粉体制备：将RE2O3（RE为稀土元素）、SiO2分别按摩尔比1:1和1:2比例进行混合。将混合粉体在球磨机中湿球磨混合24 h，之后将所得浆液放入烘箱，在80 ℃下干燥10 h，然后将干燥后的粉体在1500 ℃温度下保温2 h，再经过球磨破碎10h，分别合成出单相高熵稀土单硅酸盐(4RE1/4)2SiO5粉体和单相高熵稀土双硅酸盐(4RE1/4)2Si2O7粉体。
步骤2，(4RE1/4)2Si2O7/(4RE1/4)2SiO5复相粉体制备：将步骤1制备好的单相粉体，按(4RE1/4)2SiO5：(4RE1/4)2Si2O7的质量比为1:3比例在球磨机中湿球磨混合24 h，然后将所得浆液放入烘箱，在80 ℃下干燥10 h，再过200目筛获得(4RE1/4)2Si2O7/(4RE1/4)2SiO5复相粉体。
步骤3，试样烧结：将得到的(4RE1/4)2Si2O7/(4RE1/4)2SiO5复相粉体压制陶瓷块体，采用无压烧结，在1600 ℃下保温10 h，升温速率5 ℃/min，制备成致密的(4RE1/4)2Si2O7/(4RE1/4)2SiO5复相陶瓷块体。
本实施例制备的(4RE1/4)2Si2O7/(4RE1/4)2SiO5复相陶瓷结构致密，相对密度达到98%，在1500 ℃下经CMAS腐蚀48 h后，反应层厚度仅为60μm，耐腐蚀性能得到了显著提高。
实施例4
本实施例是选取了Y、Yb、Er、Sc、Tm、Lu元素，制备六组元高熵(6RE1/6)2Si2O7/(6RE1/6)2SiO5复相陶瓷，包括以下步骤：
步骤1，高熵稀土单、双硅酸盐粉体制备：将RE2O3（RE为稀土元素）、SiO2分别按摩尔比1:1和1:2比例进行混合。将混合粉体在球磨机中湿球磨混合24 h，之后将所得浆液放入烘箱，在80 ℃下干燥10 h，然后将干燥后的粉体在1550 ℃温度下保温2 h，再经过球磨破碎10h，分别合成出单相高熵稀土单硅酸盐(6RE1/6)2SiO5粉体和单相高熵稀土双硅酸盐(6RE1/6)2Si2O7粉体。
步骤2，(6RE1/6)2Si2O7/(6RE1/6)2SiO5复相粉体制备：将将步骤1制备好的单相粉体，按(6RE1/6)2SiO5：(6RE1/6)2Si2O7的质量比为3:1比例在球磨机中湿球磨混合24 h，然后将所得浆液放入烘箱，在80 ℃下干燥10 h，再过200目筛获得(6RE1/6)2Si2O7/(6RE1/6)2SiO5复相粉体。
步骤3，试样烧结：将得到的(6RE1/6)2Si2O7/(6RE1/6)2SiO5复相粉体压制成陶瓷块体，采用无压烧结，在1700 ℃下保温10 h，升温速率5 ℃/min，制备成致密的(6RE1/6)2Si2O7/(6RE1/6)2SiO5复相陶瓷块体。
本实施例制备的(6RE1/6)2Si2O7/(6RE1/6)2SiO5复相陶瓷结构致密，相对密度达到96.8 %，在1500 ℃下经CMAS腐蚀48 h后，反应层厚度仅为50 μm，耐腐蚀性能得到了显著提高。
需要说明的是：高熵稀土单、双硅酸盐粉体制备中，RE2O3、SiO2之间的比例关系是公知技术，本领域技术人员知晓它们在何种比例下，能够制备出高熵稀土单、双硅酸盐粉体。
在步骤2的(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相粉体制备中，(xRE1/x)2SiO5与(xRE1/x)2Si2O7可以为任意合理的比例混合，都能实现本发明的目的，但最优选为(xRE1/x)2SiO5与(xRE1/x)2Si2O7的质量比为1/3~3/1。
本发明的方法通过固相反应法将RE2O3和SiO2合成单相(xRE1/x)2SiO5粉体和单相(xRE1/x)2Si2O7粉体，然后将单相(xRE1/x)2SiO5粉体和单相(xRE1/x)2Si2O7粉体进行复合形成(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相粉体，再将粉体压片无压烧结后形成(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相陶瓷块体。所制备(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相陶瓷具有良好的耐高温CMAS腐蚀能力等优异性能。
本发明制备了一种高熵稀土单/双硅酸盐复相陶瓷，来提高其耐高温CMAS腐蚀能力。一方面，高熵稀土硅酸盐具有高熵稳定效应，在高温CMAS熔体中，硅酸盐晶粒的溶解度较低，能够提高材料本征耐高温CMAS腐蚀的能力。在腐蚀过程中，高熵稀土硅酸盐为“溶解析出再沉淀”机制，高熵稀土硅酸盐溶解在CMAS中，并与CMAS反应生成磷灰石，形成反应层，与单组元稀土硅酸盐相比，构型熵的增加减缓了陶瓷在CMAS中的溶解，从而降低了反应层的厚度，增强了耐高温腐蚀性能。另一方面，将(xRE1/x)2Si2O7和(xRE1/x)2SiO5复合后，能够改变陶瓷的晶粒尺寸和晶界结构，从而改善其耐腐蚀能力。在CMAS熔体中(xRE1/x)2Si2O7晶粒的溶解速率较高，当大部分(xRE1/x)2Si2O7在反应前沿溶解后，(xRE1/x)2SiO5晶粒暴露出来，增大了在界面凹陷处(xRE1/x)2SiO5晶粒与CMAS熔体的接触面积，导致局部磷灰石相数量增多，从而形成更加致密的磷灰石阻挡层，能够阻止熔体的渗入。
Claims (5)
1.一种耐高温CMAS腐蚀的稀土硅酸盐陶瓷，其特征在于：该陶瓷结构为高熵稀土单硅酸盐(xRE1/x)2SiO5和高熵稀土双硅酸盐(xRE1/x)2Si2O7形成的复合相陶瓷，其中，(xRE1/x)2SiO5与(xRE1/x)2Si2O7的质量比为1/3~3/1；其中的RE为稀土元素，x为组元数。
2.一种如权利要求1所述的耐高温CMAS腐蚀的稀土硅酸盐陶瓷的制备方法，其特征在于：步骤如下：
步骤1，高熵稀土单、双硅酸盐粉体制备：首先，将RE2O3、SiO2粉体按照摩尔比1:1的比例在球磨机中湿球磨混合24 h；之后将所得浆液放入烘箱，在80 ℃下干燥10 h；然后将干燥后粉体在1450~1550 ℃温度下煅烧2 h，再经过球磨破碎10 h，合成出单相高熵稀土单硅酸盐(xRE1/x)2SiO5粉体；将RE2O3、SiO2粉体按照摩尔比1:2的比例在球磨机中湿球磨混合24 h；之后将所得浆液放入烘箱，在80 ℃下干燥10 h；然后，将混合粉体在1450~1550 ℃温度下煅烧2 h，经过球磨破碎10 h，合成出单相高熵稀土双硅酸盐(xRE1/x)2Si2O7粉体；
步骤2，(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相粉体制备：将步骤1制备好的单相(xRE1/x)2SiO5粉体和单相(xRE1/x)2Si2O7粉体，在球磨机中湿球磨混合24 h，然后将所得浆液放入烘箱，在80 ℃下干燥10 h，再过200目筛获得(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相粉体；
步骤3，试样烧结：将得到的(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相粉体压制成陶瓷块体，随后采用无压烧结，在1600~1700 ℃下保温10 h，升温速率5 ℃/min，制备成致密的(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相陶瓷块体。
3.根据权利要求2所述的耐高温CMAS腐蚀的稀土硅酸盐陶瓷的制备方法，其特征在于：步骤1所述的RE2O3中RE为稀土元素，x为2~6组元。
4.根据权利要求2所述的耐高温CMAS腐蚀的稀土硅酸盐陶瓷的制备方法，其特征在于：步骤2所述(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相粉体中，(xRE1/x)2SiO5和(xRE1/x)2Si2O7的质量比为1/3~3/1。
5.根据权利要求2所述的耐高温CMAS腐蚀的稀土硅酸盐陶瓷的制备方法，其特征在于：步骤3所述致密的(xRE1/x)2SiO5/(xRE1/x)2Si2O7复相陶瓷块体的相对密度为96%~98%。
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