CN111960823A - 一种碱土金属离子掺杂稀土钽酸盐或铌酸盐热障涂层及其制备方法 - Google Patents
一种碱土金属离子掺杂稀土钽酸盐或铌酸盐热障涂层及其制备方法 Download PDFInfo
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Abstract
本发明涉及热障涂层技术领域，具体公开了一种碱土金属离子掺杂稀土钽酸盐或铌酸盐热障涂层及其制备方法，该涂层为多元梯度涂层，包括两种以上不同陶瓷组份，且至少有一种以上的陶瓷组份的体积分数沿涂层梯度连续递增或递减的变化，该涂层中陶瓷组份的化学通式为RE1‑xM1 xM2O4‑x/2(0<x<1)，M1为Mg、Ca、Sr或Ba元素中的一种；M2为Ta或Nb元素。本专利中方案既能够保证热障涂层具备原本碱土金属掺杂的稀土钽/铌酸盐的高膨胀系数，同时其热导率也大幅度的下降，通过实验检测得到热导率未超过1.10W·m‑1·K‑1，满足热障涂层对低热导率的需求。
Description
技术领域
本发明涉及热障涂层技术领域，特别涉及一种碱土金属离子掺杂稀土钽酸盐或铌酸盐热障涂层及其制备方法。
背景技术
热障涂层是利用陶瓷的隔热和抗腐蚀性特点来保护基体材料，在航空、航天、舰船、武器等方面有着重要的应用价值。目前，广泛使用的热障涂层材料主要为6％-8％的氧化钇稳定氧化锆(6-8YSZ)和锆酸镧(La2Zr2O7)，这两种陶瓷均有一定程度的不足：6-8YSZ的使用温度较低(≤1200℃)，热导率也较高(约2.5W·m-1k-1，900℃)，La2Zr2O7则有着热膨胀系数较低的问题，随着发动机和燃气轮机高推重比，高出口温度的未来发展需要，寻找新型热障涂层材料迫在眉睫。
稀土铌/钽酸盐陶瓷(RENb/TaO4)凭借着高的熔点，低热导率(1.38～1.94W·m-1·K-1)，高热膨胀系数(11×10-6K-1，1200℃)和铁弹韧性等优异的热物理性能和力学性能，被认为是最具潜力的新一代热障涂层材料。铁弹增韧机制赋予稀土铌/钽酸盐陶瓷优异的高温断裂韧性，这是其他潜在热障涂层材料所不具备的独特优势，另外有研究发现通过掺杂离子的引入能够在稀土钽/铌酸盐内产生氧空位和点缺陷，对降低热障涂层的热导率有一定效果；因此要如何最大化的体现出离子掺杂稀土铌/钽酸盐陶瓷(RENb/TaO4)陶瓷涂层对基体合金的保护作用依旧是当前研究的重点。
发明内容
本发明提供了一种碱土金属离子掺杂稀土钽酸盐或铌酸盐热障涂层及其制备方法，以得到热导率更低，符合热障涂层高温环境使用需求的离子掺杂稀土铌/钽酸盐陶瓷(RENb/TaO4)陶瓷涂层。
为了达到上述目的，本发明的技术方案为：
一种碱土金属离子掺杂稀土钽酸盐或铌酸盐热障涂层，该涂层为多元梯度涂层，包括两种以上不同陶瓷组份，且至少有一种以上的陶瓷组份的体积分数沿涂层梯度连续递增或递减的变化，该涂层中陶瓷组份的化学通式为RE1-xM1 xM2O4-x/2(0<x<1)，M1为Mg、Ca、Sr或Ba元素中的一种；M2为Ta或Nb元素。
本技术方案的技术原理和效果在于：
1、本方案中通过引入碱土金属离子掺杂稀土钽/铌酸盐，使其内部产生氧空位和点缺陷改善陶瓷涂层的热导率，另外通过对热障涂层各个梯度涂层的成分进行设计得到多元梯度涂层，即涂层中至少一种陶瓷组份的体积分数是在连续变化，这样的方式能够保证热障涂层具备原本碱土金属掺杂的稀土钽/铌酸盐的高膨胀系数，同时其热导率也大幅度的下降，通过实验检测得到热导率未超过1.10W·m-1·K-1，满足热障涂层对低热导率的需求。
2、本方案中能够得到低热导率的多元梯度陶瓷涂层，其原因在于，各梯度涂层之间成分呈渐变的形式，这样各梯度涂层之间形成的界面少，使得界面效应弱，同时最重要的一点在于，在各梯度涂层沉积过程中，每一层的成分还会不断的扩散，使得界面效应继续减弱，从而使得热导率下降。
进一步，所述多元梯度涂层的厚度为200～400μm。
有益效果：通过实验证明，多元梯度涂层的厚度设定为200～400μm，得到的热障涂层热导率较低。
进一步，所述多元梯度涂层的梯度层数n为6～21层。
有益效果：通过实验证明，多元梯度涂层的梯度层数设置为6～21层，既满足了各梯度层之间成分的扩散效果，又符合实际的沉积工艺难度。
进一步，所述稀土钽酸盐或铌酸盐粉末的制备方法，包括以下步骤：
步骤1：按照结构式为RE1-xM1 xM2O4-x/2取RE2O3和M1CO3粉末溶入浓硝酸中，使PH值低于1.5，将M2OCl3溶液逐滴加入，并不断搅拌，同时加入氨水使体系PH稳定在9～10，在水浴环境内继续搅拌，用无水乙醇或去离子水先后洗涤沉淀，直至PH＝7，将得到的滤饼置于烘箱内烘干，然后过筛并在中温环境下进行烧结，将烧结后的粉末再次过筛备用；
步骤2：将步骤1所制备的粉末与其质量不低于30wt.％的水混合获得浆料A，将浆料A与粘结剂以及聚乙二醇、正辛醇、增粘剂和增孔剂混合获得浆料B，再将浆料B送入离心喷雾干燥机对其进行离心喷雾造粒，得到粉体颗粒尺寸为20-70μm的球形碱土金属离子掺杂稀土钽酸盐或铌酸盐陶瓷粉末。
有益效果：采用本方法制备陶瓷粉体，不仅耗时少，且纯度高，且制备的碱土金属掺杂稀土钽/铌酸盐(RE1-xM1 xM2O4-x/2)粉末成相完全，成分均匀，粉末损耗量小。
进一步，所述步骤1中M2OCl3溶液的滴加速度为200～400mL/min，水浴温度为50～100℃，搅拌时间为30～120min，烘干温度为80～120℃，时间为5～10h；中温烧结温度为900-1100℃，时间为3-5h，所用筛子为300～500目。
有益效果：上述参数设定能够满足共沉淀法制备陶瓷粉体的要求。
进一步，步骤2中，粘结剂含量为0.5～3wt.％，添加剂含量为0.1～1wt.％，浆料B的进料速度控制在300～500mL/h，喷雾离心速度为8000～10000r/min。
有益效果：这样的参数下保证得到的粉末成分均匀。
本申请还公开了一种碱土金属离子掺杂稀土钽酸盐或铌酸盐热障涂层的制备方法，包括以下步骤：
步骤1：取两种以上不同RE1-xM1 xM2O4-x/2陶瓷粉末混合成n份混合陶瓷粉体，n份混合陶瓷粉体中至少一种以上的钽酸盐陶瓷组份的体积分数为连续递增或递减的变化；
步骤2：将步骤1得到的n份混合陶瓷粉体依次沉积到基体材料上得到多元梯度的碱土金属掺杂稀土钽酸盐或铌酸盐热障涂层。
有益效果：采用上述工艺得到的热障涂层具备多元梯度特征。
进一步，所述步骤2中在基体材料表面预先沉积厚度为100～200μm的金属粘结层，金属粘结层的成分为MCrAlY，其中M为Ni或Co。
有益效果：金属粘接层的设置能够提高稀土钽酸盐与基体材料之间的粘接性。
进一步，所述步骤2中采用APS、HVOF、EB-PVD或者超音速电弧喷涂法进行涂层沉积处理。
有益效果：上述几种涂层的制备工艺均为现有比较成熟的工艺，可根据具体的生产环境进行选择。
具体实施方式
下面通过具体实施方式进一步详细说明：
实施例1：
一种碱土金属离子掺杂稀土钽酸盐热障涂层，该涂层为多元梯度涂层，包括两种不同的陶瓷组份，且至少有一种以上的陶瓷组份的体积分数沿涂层梯度连续递增或递减的变化，本实施例1中两种陶瓷组份的化学通式为Dy0.8Ca0.2TaO3.9和Gd0.8Sr0.2TaO3.9，两种陶瓷组份在每一个梯度涂层中的体积分数配比如表1所示。
另外上述碱土金属离子掺杂稀土钽酸盐或铌酸盐的制备方法，以制备Dy0.8Ca0.2TaO3.9为例，包括以下步骤：
步骤1：按照Dy0.8Ca0.2TaO3.9的结构式将Dy2O3和CaCO3粉末溶入浓硝酸中进行反应，并将PH调至1左右，然后将制备好的TaOCl3溶液逐滴加入(滴加的速度为200mL/min)，不停的搅拌，同时加入氨水使体系PH稳定在9～10，搅拌1小时后，在60℃水浴环境内继续搅拌120min，然后用去离子水不断洗涤沉淀，直至PH＝7，将滤饼置于120℃烘箱内公干5h，然后过500目筛并在900℃进行5h烧结，将烧结后的粉末再次过500目筛备用。
步骤2：将步骤1所制备的粉末与其质量30wt.％的水混合获得浆料A，将浆料A与粉末质量分数为0.5％的粘结剂以及0.2％的聚乙二醇、0.1％正辛醇和0.1％增孔剂均匀混合获得浆料B，然后将浆料B送入离心喷雾干燥机对其进行离心喷雾造粒，干燥气体为N2，喷雾干燥机进料速度控制在350mL/h，离心速度为9000r/min，进口和出口温度分别为350℃和170℃，获得粉体颗粒尺寸介于20～70μm的Ca掺杂稀土钽酸镝(Dy0.8Ca0.2TaO3.9)球形粉末。
上述碱土金属离子掺杂稀土钽酸盐热障涂层的制备方法，包括以下步骤：
步骤1：取上述方法制备的Dy0.8Ca0.2TaO3.9和Gd0.8Sr0.2TaO3.9粉末按照表1所示混合成6份混合陶瓷粉体。
步骤2：将基体材料(本实施例中镍基高温合金)进行表面粗糙化处理，再在其表面预先沉积厚度为100μm的金属粘结层，金属粘结层的成分为NiCrAlY，采用APS方法将步骤1得到的6份混合陶瓷粉体依次沉积到金属粘接层上得到多元梯度的碱土金属离子掺杂稀土钽酸盐热障陶瓷涂层，该涂层的厚度为200μm。
表1为实施例1中Dy0.8Ca0.2TaO3.9和Gd0.8Sr0.2TaO3.9粉末的体积分数(％)
实施例2：
与实施例1的区别在于，参照表2所示，梯度层数n＝11，碱土金属离子掺杂稀土钽酸盐涂层的厚度为300μm，各梯度层中Dy0.8Ca0.2TaO3.9和Gd0.8Sr0.2TaO3.9粉末的体积分数见下表2所示。
表2为实施例2各梯度层中Dy0.8Ca0.2TaO3.9和Gd0.8Sr0.2TaO3.9粉末的体积分数(％)
| 梯度层数n | Dy<sub>0.8</sub>Ca<sub>0.2</sub>TaO<sub>3.9</sub>粉末 | Gd<sub>0.8</sub>Sr<sub>0.2</sub>TaO<sub>3.9</sub>粉末 |
| 1 | 100 | 0 |
| 2 | 90 | 10 |
| 3 | 80 | 20 |
| 4 | 70 | 30 |
| 5 | 60 | 40 |
| 6 | 50 | 50 |
| 7 | 40 | 60 |
| 8 | 30 | 70 |
| 9 | 20 | 80 |
| 10 | 10 | 90 |
| 11 | 0 | 100 |
实施例3：
与实施例1的区别在于，参照表3所示，陶瓷涂层的梯度层数n＝21，碱土金属掺杂稀土钽酸盐涂层的厚度为400μm，各梯度层中Dy0.8Ca0.2TaO3.9和Gd0.8Sr0.2TaO3.9粉末的体积分数见下表3所示。
表3为实施例3各梯度层中Dy0.8Ca0.2TaO3.9和Gd0.8Sr0.2TaO3.9粉末的体积分数(％)
实施例4：
与实施例2的区别在于，本实施例中还包括采用实施例1的方法制备的La0.9Ba0.1TaO3.95粉体，梯度层数n＝11，陶瓷涂层的厚度为300μm，各梯度层中Dy0.8Ca0.2TaO3.9、Gd0.8Sr0.2TaO3.9和La0.9Ba0.1TaO3.95粉末的体积分数见下表4所示。
表4为实施例4各梯度层中各陶瓷组份的体积分数(％)
实施例5：
与实施例2的区别在于，本实施例中的陶瓷组份包括采用实施例1的方法制备的Y0.6Ca0.4NbO3.8和Y0.8Mg0.2NbO3.8粉体，梯度涂层n＝11，碱土金属离子掺杂稀土钽酸盐涂层的厚度为300μm，各梯度层中Y0.6Ca0.4NbO3.8和Y0.8Mg0.2NbO3.8粉体的体积分数见下表5所示。
表5为实施例5各梯度层中陶瓷组份的体积分数(％)
对比例1：
与实施例1的区别在于，对比例1中两种陶瓷粉末采用球磨后高温烧结而成。
对比例2：
与实施例1的区别在于，步骤2中先将Dy0.8Ca0.2TaO3.9粉末采用APS方法沉积到金属粘接层上得到涂层A，再将Gd0.8Sr0.2TaO3.9粉末采用APS方法沉积到涂层A上得到涂层B，涂层A与涂层B的总厚度为200μm。
选取实施例1～5、对比例1～2得到的材料试件进行热导率实验检测：
采用激光热导仪进行测试，在800K温度时，测试结果如下表6所示：
表6为实施例1～5与对比例1～2的热导率(W·m-1·K-1)
| 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 对比例1 | 对比例2 | |
| 热导率 | 1.07 | 1.05 | 1.02 | 1.04 | 1.05 | 1.21 | 1.69 |
从上表6可以得出：
1、采用本申请中的技术方案得到的陶瓷热障涂层，其热导率未超过1.10W·m-1·K-1，满足热障涂层对低热导率的需求，而通过对比例2可以看出，未进行成分设计的陶瓷涂层，其热导率明显偏高，而采用高温烧结得到的碱金属掺杂稀土钽/铌酸盐粉体虽热导率满足热障涂层的需求，但仍然要高于本申请中采用共沉淀法制备的陶瓷粉末。
2、通过对热障涂层各个梯度涂层的成分进行设计得到多元梯度涂层，即涂层中至少一种陶瓷组份的体积分数是在连续变化，这样的方式能够保证热障涂层具备原本碱土金属掺杂的稀土钽/铌酸盐的高膨胀系数，同时其热导率也大幅度的下降，原因在于采用这样的方式进行沉积得到的热障涂层，各梯度涂层之间成分呈渐变的形式，各梯度涂层之间形成的界面少，使得界面效应弱，同时最重要的一点在于，在各梯度涂层沉积过程中，每一层的成分还会不断的扩散，使得界面效应继续减弱，从而使得热导率下降，而本申请中实施例3的热导率最低，说明梯度层数越高，对热导率的改善越显著。
以上所述的仅是本发明的实施例，方案中公知的具体材料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 (9)
1.一种碱土金属离子掺杂稀土钽酸盐或铌酸盐热障涂层，其特征在于：该涂层为多元梯度涂层，包括两种以上不同陶瓷组份，且至少有一种以上的陶瓷组份的体积分数沿涂层梯度连续递增或递减的变化，该涂层中陶瓷组份的化学通式为RE1-xM1 xM2O4-x/2(0<x<1)，M1为Mg、Ca、Sr或Ba元素中的一种；M2为Ta或Nb元素。
2.根据权利要求1所述的一种碱土金属离子掺杂稀土钽酸盐或铌酸盐热障涂层，其特征在于：所述多元梯度涂层的厚度为200～400μm。
3.根据权利要求2所述的一种碱土金属离子掺杂稀土钽酸盐或铌酸盐热障涂层，其特征在于：所述多元梯度涂层的梯度层数n为6～21层。
4.根据权利要求3所述的一种碱土金属离子掺杂稀土钽酸盐或铌酸盐热障涂层，其特征在于：所述稀土钽酸盐或铌酸盐粉末的制备方法，包括以下步骤：
步骤1：按照结构式为RE1-xM1 xM2O4-x/2取RE2O3和M1CO3粉末溶入浓硝酸中，使PH值低于1.5，将M2OCl3溶液逐滴加入，并不断搅拌，同时加入氨水使体系PH稳定在9～10，在水浴环境内继续搅拌，用无水乙醇或去离子水先后洗涤沉淀，直至PH＝7，将得到的滤饼置于烘箱内烘干，然后过筛并在中温环境下进行烧结，将烧结后的粉末再次过筛备用；
步骤2：将步骤1所制备的粉末与其质量不低于30wt.％的水混合获得浆料A，将浆料A与粘结剂以及聚乙二醇、正辛醇、增粘剂和增孔剂混合获得浆料B，再将浆料B送入离心喷雾干燥机对其进行离心喷雾造粒，得到粉体颗粒尺寸为20-70μm的球形碱土金属离子掺杂稀土钽酸盐或铌酸盐陶瓷粉末。
5.根据权利要求4所述的一种碱土金属离子掺杂稀土钽酸盐或铌酸盐热障涂层，其特征在于：所述步骤1中M2OCl3溶液的滴加速度为200～400mL/min，水浴温度为50～100℃，搅拌时间为30～120min，烘干温度为80～120℃，时间为5～10h；中温烧结温度为900-1100℃，时间为3-5h，所用筛子为300～500目。
6.根据权利要求4所述的一种碱土金属离子掺杂稀土钽酸盐或铌酸盐热障涂层，其特征在于：步骤2中，粘结剂含量为0.5～3wt.％，添加剂含量为0.1～1wt.％，浆料B的进料速度控制在300～500mL/h，喷雾离心速度为8000～10000r/min。
7.一种制备如权利要求6所述的碱土金属离子掺杂稀土钽酸盐或铌酸盐热障涂层的方法，其特征在于：包括以下步骤：
步骤1：取两种以上不同RE1-xM1 xM2O4-x/2陶瓷粉末混合成n份混合陶瓷粉体，n份混合陶瓷粉体中至少一种以上的钽酸盐陶瓷组份的体积分数为连续递增或递减的变化；
步骤2：将步骤1得到的n份混合陶瓷粉体依次沉积到基体材料上得到多元梯度的碱土金属掺杂稀土钽酸盐或铌酸盐热障涂层。
8.根据权利要求7所述的一种碱土金属离子掺杂稀土钽酸盐或铌酸盐热障涂层，其特征在于：所述步骤2中在基体材料表面预先沉积厚度为100～200μm的金属粘结层，金属粘结层的成分为MCrAlY，其中M为Ni或Co。
9.根据权利要求7所述的一种碱土金属离子掺杂稀土钽酸盐或铌酸盐热障涂层，其特征在于：所述步骤2中采用APS、HVOF、EB-PVD或者超音速电弧喷涂法进行涂层沉积处理。
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