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CN110627495B - 一种低热导高熵铝酸盐陶瓷及其制备方法 - Google Patents

一种低热导高熵铝酸盐陶瓷及其制备方法 Download PDF

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CN110627495B
CN110627495B CN201910900428.4A CN201910900428A CN110627495B CN 110627495 B CN110627495 B CN 110627495B CN 201910900428 A CN201910900428 A CN 201910900428A CN 110627495 B CN110627495 B CN 110627495B
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向会敏
赵子樊
周延春
彭志坚
戴付志
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China Academy of Launch Vehicle Technology CALT
Aerospace Research Institute of Materials and Processing Technology
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Abstract

本发明涉及一种低热导高熵铝酸盐陶瓷及其制备方法，尤其涉及一种高纯度、高相对密度、低热导率高熵铝酸盐陶瓷及利用真空条件下放电等离子烧结法制备低热导高熵铝酸盐陶瓷的方法，属于高温隔热陶瓷领域，所述的高纯度密度是指纯度不低于95wt％，高相对密度是指相对密度不低于97％，低热导率是指室温热导率不高于4.1W·m‑1·K‑1，高熵是指铝酸盐陶瓷中金属元素的种类不低于五种。

Description

一种低热导高熵铝酸盐陶瓷及其制备方法
技术领域
本发明涉及一种低热导高熵铝酸盐陶瓷及其制备方法，尤其涉及一种高纯度、高相对密度、低热导率高熵铝酸盐陶瓷及利用真空条件下放电等离子烧结法制备低热导高熵铝酸盐陶瓷的方法，属于高温隔热陶瓷领域，所述的高纯度密度是指纯度不低于95wt％，高相对密度是指相对密度不低于97％，低热导率是指室温热导率不高于4.1W·m-1·K-1，高熵是指铝酸盐陶瓷中金属元素的种类不低于五种。
背景技术
新一代的陶瓷基航空发动机叶片的高温环境障/热障涂层材料以稀土硅酸盐、稀土铝酸盐等体系为主，其中稀土铝酸盐以其良好的抗水蒸汽腐蚀能力及与基体良好的化学相容性具备更优异的实际应用潜力。但单相的稀土铝酸盐由于热导率过高，不利于降低发动机叶片表面温度，这将提高基体所承受的温度压力，威胁发动机的可靠性。
发明内容
本发明的技术解决问题是：克服现有技术的不足，提出一种低热导高熵铝酸盐陶瓷及其制备方法。通过高熵的技术，在铝酸盐中同时引入不低于5种稀土金属元素，可有效降低铝酸盐的热导率。
本发明的技术解决方案是：
一种低热导高熵铝酸盐陶瓷，该铝酸盐陶瓷的原料包括Y(NO3)3·6H2O粉末、Nd(NO3)3·6H2O粉末、Sm(NO3)3·6H2O粉末、Eu(NO3)3·6H2O粉末、Er(NO3)3·6H2O粉末和Al(NO3)3·9H2O粉末，其中Y(NO3)3·6H2O粉末、Nd(NO3)3·6H2O粉末、Sm(NO3)3·6H2O粉末、Eu(NO3)3·6H2O粉末、Er(NO3)3·6H2O粉末和Al(NO3)3·9H2O粉末的摩尔比为1:1:1:1:1:5；该铝酸盐陶瓷的结构式为(Y0.2Nd0.2Sm0.2Eu0.2Er0.2)AlO3；该铝酸盐陶瓷的纯度不低于95wt％；该铝酸盐陶瓷的相对密度不低于97％；该铝酸盐陶瓷的室温热导率不高于4.1W·m-1·K-1。
一种低热导高熵铝酸盐陶瓷的制备方法，该方法的步骤包括：
(1)将铝酸盐陶瓷的原料在去离子水中进行溶解，溶解时间为0.5-2小时，溶解完成后得到溶液，在得到的溶液中加入过量氨水，使溶液的pH值调至9-10，有沉淀物质析出，过滤，取滤饼即为沉淀物质；
(2)将步骤(1)得到的沉淀物质进行干燥处理得到混合粉末，将干燥后的混合粉末放入高温炉中进行煅烧，煅烧温度为1550-1600℃，煅烧时间为2-4小时，得到陶瓷粉体；
(3)将步骤(2)得到陶瓷粉体放入放电等离子烧结炉中进行高温烧结，气氛为真空，烧结温度为1600-1650℃，烧结时间为3-10分钟，烧结压强为30-35MPa，真空度为8-15Pa，升温速率为50-100℃/分，得到铝酸盐陶瓷，制备得到的铝酸盐陶瓷的纯度不低于95wt％，相对密度不低于97％，室温热导率不高于4.1W·m-1·K-1。
本发明与现有技术相比具有如下有益效果：
(1)本发明首次以Y(NO3)3·6H2O、Nd(NO3)3·6H2O、Sm(NO3)3·6H2O、Eu(NO3)3·6H2O、Er(NO3)3·6H2O和Al(NO3)3·9H2O为原料，获得了高熵铝酸盐陶瓷；在真空条件下通过放电等离子体烧结获得高纯度、高相对密度、低热导率高熵铝酸盐陶瓷，经分析表明高熵铝酸盐陶瓷具有纯度高、相对密度高、热导率低的特点，纯度在95wt％以上，相对密度在97％以上，热导率在4.1W·m-1·K-1以下。
(2)本发明制备高熵铝酸盐粉体工艺过程简单快速，从Y(NO3)3·6H2O、Nd(NO3)3·6H2O、Sm(NO3)3·6H2O、Eu(NO3)3·6H2O、Er(NO3)3·6H2O和Al(NO3)3·9H2O原料直接得到高熵铝酸盐粉体，通过放电等离子烧结法短时间内快速获得高熵铝酸盐陶瓷。
(3)本发明制备得到的高纯度、高相对密度、低热导率高熵铝酸盐陶瓷的纯度、相对密度及颗粒尺寸可调节性好，可以通过真空高温烧结工艺调节纯度、相对密度及颗粒尺寸，制备过程灵活可控。
(4)目的在于克服现有技术的上述不足，提供一种低热导率高熵铝酸盐陶瓷及其制备方法，该制备方法工艺简单快速、实用性强，在工艺过程中不需要加入高温助烧结剂，制备得到的高熵铝酸盐陶瓷具有纯度高、相对密度高、热导率低等优点。
(5)一种低热导率高熵铝酸盐陶瓷的制备方法，以Y(NO3)3·6H2O、Nd(NO3)3·6H2O、Sm(NO3)3·6H2O、Eu(NO3)3·6H2O、Er(NO3)3·6H2O和Al(NO3)3·9H2O为原料，按照摩尔比为1:1:1:1:1:5在去离子水中进行溶解混合，混合时间为0.5小时，在混合均匀的溶液中加入过量氨水，使混合溶液pH值调至10，得到沉淀物质；将得到的沉淀物过滤并进行干燥处理得到混合物粉末，将干燥后的粉末放入高温炉中进行煅烧，煅烧温度为1550-1600℃，煅烧时间为2-4小时，得到高熵铝酸盐粉体；将得到的高熵铝酸盐粉体放入放电等离子烧结炉中进行高温烧结，气氛为真空，烧结温度为1600-1650℃，烧结时间为3-10分钟，烧结压强控制为30MPa，真空度均为8-15Pa，升温速率为50-100℃/分。
附图说明
图1为本发明实施例1制备得到的低热导高熵铝酸盐陶瓷粉体的示意图；
图2为本发明实施例1制备得到的低热导高熵铝酸盐陶瓷成分的X-射线衍射图谱；
图3为本发明实施例2制备得到的低热导高熵铝酸盐陶瓷的显微结构照片及各成分分布图；
图4为本发明实施例2制备得到的低热导高熵铝酸盐陶瓷的热膨胀曲线。
具体实施方式
下面结合附图和具体实施例对本发明作进一步详细的描述：
实施例1
将Y(NO3)3·6H2O、Nd(NO3)3·6H2O、Sm(NO3)3·6H2O、Eu(NO3)3·6H2O、Er(NO3)3·6H2O和Al(NO3)3·9H2O按Y(NO3)3·6H2O:Nd(NO3)3·6H2O:Sm(NO3)3·6H2O:Eu(NO3)3·6H2O:Er(NO3)3·6H2O:Al(NO3)3·9H2O＝1:1:1:1:1:5的摩尔比称重，加入去离子水溶解，溶解时间为0.5小时，在混合均匀的溶液中加入过量氨水，使混合溶液pH值调至10，过滤得到沉淀物质；将得到的沉淀物进行干燥处理得到混合粉末，将干燥后的混合粉末放入高温炉中进行煅烧，煅烧温度为1550℃，煅烧时间为2小时，得到高熵铝酸盐粉体。将高熵铝酸盐粉体放入放电等离子烧结炉中进行高温烧结，气氛为真空，烧结温度为1650℃，烧结时间为3分钟，烧结压强控制为30MPa，真空度均为8Pa，升温速率为100℃/分，得到的低热导高熵铝酸盐陶瓷纯度为96wt％，相对密度为97％。粉体制备过程如图1所示，得到的低热导高熵铝酸盐陶瓷成分如图2的X-射线衍射图谱所示，表明当高温反应温度为1550℃时即可制备得到纯度不小于96wt％的低热导高熵铝酸盐陶瓷。相对密度为98％。显微结构如图3所示，可以观察到其中无气孔分布，各组成元素分布均匀，表明陶瓷相对密度较高。得到的低热导高熵铝酸盐陶瓷热膨胀系数如图4所示，得到高熵铝酸盐陶瓷热膨胀系数为9.1×10-6K-1。
实施例2
将Y(NO3)3·6H2O、Nd(NO3)3·6H2O、Sm(NO3)3·6H2O、Eu(NO3)3·6H2O、Er(NO3)3·6H2O和Al(NO3)3·9H2O按Y(NO3)3·6H2O:Nd(NO3)3·6H2O:Sm(NO3)3·6H2O:Eu(NO3)3·6H2O:Er(NO3)3·6H2O:Al(NO3)3·9H2O＝1:1:1:1:1:5的摩尔比称重，加入去离子水溶解，混合时间为0.5小时，在混合均匀的溶液中加入过量氨水，使混合溶液pH值调至10，过滤得到沉淀物质；将得到的沉淀物进行干燥处理得到混合物粉末，将干燥后的粉末放入高温炉中进行煅烧，煅烧温度为1600℃，煅烧时间为3小时，得到高熵铝酸盐粉体。将高熵铝酸盐粉体放入放电等离子烧结炉中进行高温烧结，气氛为真空，烧结温度为1700℃，烧结时间为5分钟，烧结压强控制为30MPa，真空度均为10Pa，升温速率为80℃/分，得到的低热导高熵铝酸盐陶瓷纯度为98wt％，相对密度为98％。显微结构如图3所示，可以观察到其中无气孔分布，各组成元素分布均匀，表明陶瓷相对密度较高。得到的低热导高熵铝酸盐陶瓷热膨胀系数如图4所示，得到高熵铝酸盐陶瓷热膨胀系数为9.1×10-6K-1。

Claims (5)

1.一种低热导高熵铝酸盐陶瓷，其特征在于：该铝酸盐陶瓷的原料包括Y(NO3)3·6H2O粉末、Nd(NO3)3·6H2O粉末、Sm(NO3)3·6H2O粉末、Eu(NO3)3·6H2O粉末、Er(NO3)3·6H2O粉末和Al(NO3)3·9H2O粉末，其中Y(NO3)3·6H2O粉末、Nd(NO3)3·6H2O粉末、Sm(NO3)3·6H2O粉末、Eu(NO3)3·6H2O粉末、Er(NO3)3·6H2O粉末和Al(NO3)3·9H2O粉末的摩尔比为1:1:1:1:1:5；
该低热导高熵铝酸盐陶瓷的制备方法，该方法的步骤包括：
(1)将铝酸盐陶瓷的原料在去离子水中进行溶解，溶解时间为0.5-2小时，溶解完成后得到溶液，在得到的溶液中加入过量氨水，使溶液的pH值调至9-10，有沉淀物质析出，过滤，取滤饼即为沉淀物质；
(2)将步骤(1)得到的沉淀物质进行干燥处理得到混合粉末，将干燥后的混合粉末放入高温炉中进行煅烧，煅烧温度为1550-1600℃，煅烧时间为2-4小时，得到陶瓷粉体；
(3)将步骤(2)得到陶瓷粉体放入放电等离子烧结炉中进行高温烧结，气氛为真空，烧结温度为1600-1650℃，烧结时间为3-10分钟，烧结压强为30-35MPa，真空度为8-15Pa，升温速率为50-100℃/分，得到铝酸盐陶瓷。
2.根据权利要求1所述的一种低热导高熵铝酸盐陶瓷，其特征在于：该铝酸盐陶瓷的结构式为(Y0.2Nd0.2Sm0.2Eu0.2Er0.2)AlO3。
3.根据权利要求1所述的一种低热导高熵铝酸盐陶瓷，其特征在于：该铝酸盐陶瓷的纯度不低于95wt％。
4.根据权利要求1所述的一种低热导高熵铝酸盐陶瓷，其特征在于：该铝酸盐陶瓷的相对密度不低于97％。
5.根据权利要求1所述的一种低热导高熵铝酸盐陶瓷，其特征在于：该铝酸盐陶瓷的室温热导率不高于4.1W·m-1·K-1。
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