CN113105238A - 一种原位生成SiC掺杂Gd2Zr2O7热障涂层陶瓷材料及其制备方法 - Google Patents

一种原位生成SiC掺杂Gd2Zr2O7热障涂层陶瓷材料及其制备方法 Download PDF

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CN113105238A
CN113105238A CN202110387501.XA CN202110387501A CN113105238A CN 113105238 A CN113105238 A CN 113105238A CN 202110387501 A CN202110387501 A CN 202110387501A CN 113105238 A CN113105238 A CN 113105238A
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姜伯晨
曹将栋
王建涛
陈涵麟
姚达
孙萍
黄健
王金龙
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Jiangsu Vocational and Technical Shipping College
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Abstract

本发明公开了一种SiC掺杂Gd2Zr2O7热障涂层陶瓷层材料及其制备方法，所述SiC掺杂Gd2Zr2O7热障涂层陶瓷层材料化学式Gd2Zr2O7‑XTiSi2‑YC(X＝0‑5wt％,Y＝0‑1.7wt％),Gd2Zr2O7‑XTiSi2‑YC(X＝0‑5wt％,Y＝0‑1.7wt％)系列热障涂层陶瓷层材料，具有以下显著优点：掺杂不同含量的原位生成的第二相物质SiC后，在1500℃下仍然能够保持良好的高温相稳定性和较好的抗烧结性，与传统的Gd2Zr2O7热障涂层陶瓷材料相比，本发明在1000℃高温下热膨胀系数可达到11W/m.K，其1000℃热导率可达到0.6‑0.7W·m‑1·k‑1，断裂韧性提高至1.5‑1.6MPa·m1/2，完全有潜力作为耐高温的热障涂层陶瓷层材料。

Description

一种原位生成SiC掺杂Gd2Zr2O7热障涂层陶瓷材料及其制备 方法
技术领域
本发明属于高温隔热防护材料领域，特别涉及一种耐高温、低热导率、高热膨胀系数、高断裂韧性的热障涂层陶瓷材料及其制备方法。
背景技术
随着现代航空科技的不断发展，以燃气涡轮发动机为代表的航空发动机正朝着高推重比、高热效率、高流量比的方向发展着，因此发动机内部的热端部件所经受的温度和压力也在不断提高。而现有的高温合金和冷却技术并不能满足当前的状况要求，在这种情况下，具有隔热、耐腐蚀和抗高温氧化等性能的热障涂层技术逐渐发展成为解决发动机热端部件高温使用难题的有效途径之一，并且逐步成为研究的热点。
典型的热障涂层的结构分为三部分：基体、粘结层、陶瓷层，陶瓷层起着隔热的作用，粘结层起到抗氧化腐蚀、增强陶瓷层和基体的结合力以及缓和热失配的作用，粘结层的成分主要是MCrAlY，陶瓷层主要有以下几种体系：1、部分稳定的氧化锆体系：就是在ZrO2中加入Y2+、Ca2+、Mg2+、Ce4+等离子半径与Zr4+离子半径相差小于12％的阳离子(通常以相应的氧化物形式加入)以一种或者多种共渗的方式进行ZrO2稳定。2、稀土焦绿石或萤石结构化合物体系：这是一大类具有相似结构的化合物，其化学通式可写作A2B2O7，其中A为稀土元素，B为某种四价元素。从晶体学角度，焦绿石结构亦可看作是一种存在“有序缺陷”的萤石结构。它具有比YSZ陶瓷更低的杨氏模量、更低的热导率和更好的高温相稳定性，因此可以在更高的温度进行使用，符合高温材料的发展趋势。3、其他结构化合物体系：稀土磷酸盐体系、磁铅石结构化合物、石榴石结构化合物以及钙钛矿结构锆酸盐等。
现役部分航空发动机的热端部件工作环境已达到1500℃，而传统的YSZ热障涂层在超过1200℃的工作环境下会过快产生烧结并且导致相变使得涂层剥落失效，现已无法满足如今高性能燃气发动机的使用需求了。所以如今陶瓷层的研究重点在于稀土焦绿石或萤石结构的A2B2O7化合物体系，该结构主要有Gd2Zr2O7、Sm2Zr2O7、La2Zr2O7等，如文献发表在《Surface&Coatings Technology》上的《Microstructure and lifetime of EB-PVD TBCswith Hf-doped bond coat and Gd-zirconate ceramic top coat on CMSX-4substrates》。不过该体系仍然存在几个缺陷，较低的热膨胀系数和较差的断裂韧性以及与 TGO层材料Al2O3的化学稳定性差，此外其抗热震性能比较差。研究发现，对A位或者B位进行一种元素或者多种元素的掺杂可以显著改变该体系的热物理性能，提高热膨胀系数、改善断裂韧性等，如文献发表在《Acta Materialia》上的《Influence of B sitesubstituent Ti on the structure and thermophysical properties of A2B2O7 typepyrochlore Gd2Zr2O7》。
发明人在先文章(Enhanced physical properties of TiSi2 doped Gd2ZrO7ceramic for thermal barrier coatings，Yingqun Hua等，Mater. Res.Express，第6卷)公开了TiSi2掺杂的Gd2ZrO7，其导热率约为 0.9W·m-1·k-1，导热效果依旧存在提高空间。
但国内外有关对A2B2O7，特别是Gd2Zr2O7这种结构材料进行两相、三相甚至更多相元素掺杂的研究尚属空白。
发明内容
本发明要解决的技术问题是提供一种具有较高热膨胀系数、较低热导率以及较好的断裂韧性的掺杂改性的Gd2Zr2O7热障涂层陶瓷层材料及其制备方法，以此来寻求解决Gd2Zr2O7的相关缺陷的问题。
本发明的技术方案是：
一种原位生成元素掺杂Gd2Zr2O7热障涂层陶瓷材料，其特征在于：所述掺杂元素包括Si和C；
进一步优选为，一种原位生成SiC掺杂Gd2Zr2O7热障涂层陶瓷材料，其化学式为Gd2Zr2O7-XTiSi2-YC(X＝0-5wt％,Y＝0-1.7wt％)，掺杂产物SiC通过TiSi2和石墨(C)按照化学反应进行，TiSi2和石墨的摩尔比为1:9-9:1。
进一步优选为，X、Y分别代表相应物料在陶瓷材料中的重量占比；
进一步优选为，X＝0.1-5wt％,Y＝0.1-1.7wt％，TiSi2和石墨的摩尔比为1:9-1:1。
进一步优选为，X＝1-5wt％,Y＝0.34-1.7wt％，TiSi2和石墨的摩尔比为1:5-1:2。
进一步优选为，一种原位生成SiC掺杂Gd2Zr2O7热障涂层陶瓷材料，其化学式为Gd2Zr2O7-XTiSi2-YC(X＝0.1-5wt％,Y＝0.1-1.7wt％), 掺杂产物SiC通过TiSi2和石墨按照化学反应进行，TiSi2和石墨的摩尔比为1:3，掺杂产物原位生成其以SiC为主。
所述原位生成SiC掺杂Gd2Zr2O7热障涂层陶瓷材料的制备方法，其制备方法包括如下步骤：
(1)将Gd2O3和ZrO2加热，然后进行干燥处理；
(2)将TiSi2和石墨以及干燥过的Gd2O3和ZrO2进行球磨处理，得到混合粉末；
(3)对粉末进行烘干、筛分；
(4)制胚后进行高温处理，随炉冷却。
进一步优选为，步骤(1)中Gd2O3和ZrO2的摩尔比为1：4-4:1；加热温度为200-800℃。
进一步优选为，步骤(2)中Gd2O3、ZrO2、TiSi2和石墨摩尔比例为(1-4):(1-8):(0-0.305):(0-0.42),球磨时间为1-20小时。
进一步优选为，步骤(3)中筛分所用筛网目数为100-500目。
进一步优选为，步骤(4)中高温处理条件为1000-2000℃，并常压下保温4-20小时。
进一步优选为，所述原位生成SiC掺杂Gd2Zr2O7热障涂层陶瓷材料的制备方法，其包括如下步骤：
(1)将摩尔比为1：2的Gd2O3和ZrO2加热至500℃，保温5 小时做干燥处理；
(2)用湿法高能球磨法混合干燥处理过后的x摩尔Gd2O3、2x 摩尔ZrO2，以及(1％wt、2.5％wt、5％wt)TiSi2和石墨(分别为0.34wt％、 0.85wt％、1.7wt％)，球磨10小时；
(3)取出混合的粉末在120℃干燥箱中保温10小时烘干，过300 目标准分样筛；
(4)将上述烘干粉末放入模具中，将模具放入压力机(压片直径1.5cm)下进行压制，压强250MPa，压制完成后将样品放入坩埚中，置于高温炉中在1500℃中保温12小时，然后随炉冷却，制得上述热障涂层陶瓷材料。
同时如上所述的原位生成SiC掺杂Gd2Zr2O7热障涂层陶瓷材料，其特征在于：所述Gd2O3、ZrO2、TiSi2、石墨的粉末纯度质量分数>99.9％。
本发明制备的原位生成SiC掺杂Gd2Zr2O7热障涂层陶瓷材料的技术优势如下：
掺杂不同含量的原位生成的SiC后在1500℃下仍然能够保持良好的高温相稳定性和较好的抗烧结性，与传统的YSZ热障涂层陶瓷材料相比，本发明在高温下具有更高的热膨胀系数以及更低的热导率，同时具有更好的断裂韧性。在室温-1000℃之间，其热导率在0.6-0.8 W·m-1·k-1之间，好于纯Gd2Zr2O7热障涂层陶瓷材料，也好于TiSi2掺杂的Gd2ZrO7，证明TiSi2和石墨的共同掺杂，能够协同降低导热率。此外，在1000℃，其热膨胀系数可以达到11×10-6K-1以上，掺杂过后其室温断裂韧性最高可以达1.6MPa·m1/2，其具有良好的高温相稳定性以及很好的高温抗烧结性，适合作为耐高温的热障涂层陶瓷层材料。
附图说明
图1：掺杂不同含量的TiSi2和石墨(TiSi2含量分别为1％wt、2.5％wt、 5％wt，石墨与之对应的含量分别为0.34wt％、0.85wt％、1.7wt％)的 Gd2Zr2O7的成型结构形貌。
图2：掺杂不同含量的TiSi2和石墨(TiSi2含量分别为1％wt、 2.5％wt、5％wt,石墨与之对应的含量分别为0.34wt％、0.85wt％、1.7wt％)的Gd2Zr2O7的1000℃的热导率。
图3：掺杂不同含量的TiSi2和石墨(TiSi2含量分别为1％wt、 2.5％wt、5％wt,石墨与之对应的含量分别为0.34wt％、0.85wt％、1.7wt％)的Gd2Zr2O7的断裂韧性。
图4：掺杂不同含量的TiSi2和石墨(TiSi2含量分别为1wt％、 2.5wt％、5wt％,石墨与之对应的含量分别为0.34wt％、0.85wt％、1.7wt％)的Gd2Zr2O7的硬度。
图5：掺杂不同含量的TiSi2和石墨(TiSi2含量分别为1wt％、2.5wt％、5wt％,石墨与之对应的含量分别为0.34wt％、0.85wt％、1.7wt％)的Gd2Zr2O7的XRD图谱。
具体实施方式
实施例1
一种纯Gd2Zr2O7热障涂层陶瓷材料。
所述纯Gd2Zr2O7热障涂层陶瓷材料的制备方法如下：
(1)将0.039摩尔的Gd2O3和0.078摩尔的ZrO2加热至500℃，保温5小时做干燥处理；
(2)用湿法高能球磨法混合干燥处理过后的0.039摩尔的Gd2O3、 0.078摩尔的ZrO2，球磨10小时；
(3)取出混合的粉末在120℃干燥箱中保温10小时烘干，过300 目标准分样筛；
(4)将上述烘干粉末放入模具中，将模具放入压力机(压片直径1.5cm)下进行压制，压强250MPa，压制完成后将样品放入坩埚中，置于高温炉中在1500℃中保温12小时，然后随炉冷却，制得上述热障涂层陶瓷材料。
纯Gd2Zr2O7的1000摄氏度热导率为1.44176W·m-1·k-1，其断裂韧性为1.22968MPa·m1/2，其硬度为6.863GPa。
实施例2
一种原位生成SiC掺杂Gd2Zr2O7热障涂层陶瓷材料。
所述原位生成SiC掺杂Gd2Zr2O7热障涂层陶瓷材料的制备方法(TiSi2和石墨的含量分别为1wt％和0.34％)：
(1)将0.024摩尔的Gd2O3和0.048摩尔的ZrO2加热至500℃，保温5小时做干燥处理；
(2)用湿法高能球磨法混合干燥处理过后的0.024摩尔的Gd2O3、0.048摩尔的ZrO2，以及0.0015摩尔TiSi2和0.004摩尔石墨，球磨 10小时；
(3)取出混合的粉末在120℃干燥箱中保温10小时烘干，过300 目标准分样筛；
(4)将上述烘干粉末放入模具中，将模具放入压力机(压片直径1.5cm)下进行压制，压强250MPa，压制完成后将样品放入坩埚中，置于高温炉中在1500℃中保温12小时，然后随炉冷却，制得上述热障涂层陶瓷材料。
该种组分掺杂过后的1000摄氏度热导率可低至0.60039 W·m-1·k-1，其断裂韧性可高达1.52376MPa·m1/2，其硬度降低至 5.73GPa。
实施例3
一种原位生成SiC掺杂Gd2Zr2O7热障涂层陶瓷材料。
所述原位生成SiC掺杂Gd2Zr2O7热障涂层陶瓷材料的制备方法(TiSi2和石墨的含量分别为2.5wt％和0.85wt％)：
(1)将0.024摩尔的Gd2O3和0.048摩尔的ZrO2加热至500℃，保温5小时做干燥处理；
(2)用湿法高能球磨法混合干燥处理过后的0.024摩尔的Gd2O3、 0.048摩尔的ZrO2，以及0.0036摩尔的TiSi2和0.01摩尔的石墨，球磨10小时；
(3)取出混合的粉末在120℃干燥箱中保温10小时烘干，过300 目标准分样筛；
(4)将上述烘干粉末放入模具中，将模具放入压力机(压片直径1.5cm)下进行压制，压强250MPa，压制完成后将样品放入坩埚中，置于高温炉中在1500℃中保温12小时，然后随炉冷却，制得上述热障涂层陶瓷材料。
该种组分掺杂过后的1000摄氏度热导率可低至0.6111W·m-1·k-1，其断裂韧性可高达1.60164MPa·m1/2，其硬度降低至4.76GPa。
实施例4
一种原位生成SiC掺杂Gd2Zr2O7热障涂层陶瓷材料。
所述原位生成SiC掺杂Gd2Zr2O7热障涂层陶瓷材料的制备方法(TiSi2和石墨的含量分别为5wt％和1.7wt％)：
(1)将0.024摩尔的Gd2O3和0.048摩尔的ZrO2加热至500℃，保温5小时做干燥处理；
(2)用湿法高能球磨法混合干燥处理过后的0.024摩尔的Gd2O3、 0.048摩尔的ZrO2，以及0.0072摩尔的TiSi2和0.02摩尔的石墨，球磨10小时；
(3)取出混合的粉末在120℃干燥箱中保温10小时烘干，过300 目标准分样筛；
(4)将上述烘干粉末放入模具中，将模具放入压力机(压片直径1.5cm)下进行压制，压强250MPa，压制完成后将样品放入坩埚中，置于高温炉中在1500℃中保温12小时，然后随炉冷却，制得上述热障涂层陶瓷材料。
该种组分掺杂过后的1000摄氏度热导率可低至0.79338W·m-1·k-1，其断裂韧性可高达1.58692MPa·m1/2，其硬度降低至4.56GPa。
以上所述仅为本发明的较佳实施例，对本发明而言仅仅是说明性的，而非限制性的。本专业技术人员理解，在本发明权利要求所限定的精神和范围内可对其进行许多改变，修改，甚至等效，但都将落入本发明的保护范围内。

Claims (10)

1.一种原位生成元素掺杂Gd2Zr2O7热障涂层陶瓷材料，其特征在于：所述掺杂元素包括Si和C。
2.一种如权利要求1所述陶瓷材料，其特征在于：该材料为原位生成SiC掺杂Gd2Zr2O7热障涂层陶瓷材料，化学式为Gd2Zr2O7-XTiSi2-YC(X＝0-5wt％,Y＝0-1.7wt％),掺杂产物SiC通过TiSi2和石墨按照化学反应进行，TiSi2和石墨的摩尔比为1:9-9:1。
3.如权利要求2所述陶瓷材料，其特征在于：X＝0.1-5wt％,Y＝0.1-1.7wt％，TiSi2和石墨的摩尔比为1:9-1:1。
4.如权利要求2所述陶瓷材料，其特征在于：X＝1-5wt％,Y＝0.34-1.7wt％，TiSi2和石墨的摩尔比为1:5-1:2。
5.一种如权利要求1-4中任一项所述陶瓷材料的制备方法，其特征在于，包括如下步骤：
(1)将Gd2O3和ZrO2加热，然后进行干燥处理；
(2)将TiSi2和石墨以及干燥过的Gd2O3和ZrO2进行球磨处理，得到混合粉末；
(3)对粉末进行烘干、筛分；
(4)制胚后进行高温处理，随炉冷却。
6.如权利要求5所述制备方法，其特征在于：步骤(1)中Gd2O3和ZrO2的摩尔比为1：4-4:1；加热温度为200-800℃。
7.如权利要求6所述制备方法，其特征在于：步骤(2)中Gd2O3、ZrO2、TiSi2和石墨摩尔比例为(1-4):(1-8):(0-0.305):(0-0.42),球磨时间为1-20小时。
8.如权利要求7所述制备方法，其特征在于：步骤(3)中筛分所用筛网目数为100-500目。
9.如权利要求8所述制备方法，其特征在于：步骤(4)中高温处理条件为1000-2000℃，并常压下保温4-20小时。
10.如权利要求5所述制备方法，其特征在于，包括如下步骤：
(1)将摩尔比为1：2的Gd2O3和ZrO2加热至500℃，保温5小时做干燥处理；
(2)用湿法高能球磨法混合干燥处理过后的Gd2O3、ZrO2，以及TiSi2和石墨，其摩尔比例为1:2:(0.1-0.305):(0.1-0.42)，球磨10小时；
(3)取出混合的粉末在120℃干燥箱中保温10小时烘干,过300目标准分样筛；
(4)将上述烘干粉末在模具中压制成预制胚体，放在氧化锆坩埚中，再放入高温炉中在1500℃中常压保温12小时，然后随炉冷却，制得上述热障涂层陶瓷材料。
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