CN110092663B - 一种(Y1-xHox)2Si2O7固溶体材料及其制备方法 - Google Patents
一种(Y1-xHox)2Si2O7固溶体材料及其制备方法 Download PDFInfo
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Abstract
本发明涉及低热导率和难熔材料领域，具体为一种(Y1‑xHox)2Si2O7固溶体材料及其制备方法。所合成的(Y1‑xHox)2Si2O7固溶体为从室温到1450℃可稳定存在的γ相，其中x的取值范围为0<x<1。首先，以氧化钇、氧化钬和二氧化硅混合粉末作为原料，以乙醇为介质，进行球磨混合8～24h，形成浆料；接着，浆料烘干后筛成粉末，然后在马弗炉中烧结，烧结温度为1500～1600℃，烧结时间为0.5～1.5小时，最后得到(Y1‑xHox)2Si2O7固溶体粉体。将固溶体粉体装入石墨磨具中冷压成型，在通有保护气氛的热压炉内烧结，制备出(Y1‑xHox)2Si2O7固溶体块体。本发明在简单的工艺下制备出具有耐高温、相稳定性好、高纯度、低热导率以及力学性能良好的(Y1‑xHox)2Si2O7固溶体材料。
Description
技术领域
本发明涉及低热导率和难熔材料领域，具体为一种(Y1-xHox)2Si2O7固溶体材料及其制备方法，通过无压-固相反应法制备(Y1-xHox)2Si2O7固溶体陶瓷粉体或者通过热压/固-液相反应制备(Y1-xHox)2Si2O7固溶体陶瓷块体。
背景技术
随着航空事业的快速发展，高温部件面临着更极端环境的挑战。氮化硅和碳化硅等高温结构陶瓷及其复合材料具有高温强度优、耐热冲击性好、抗高温蠕变强的特点，是在1200℃以上航空发动机应用的候选高温结构材料。但是硅基陶瓷在涡轮发动机的高温燃气环境中快速失效，需要在部件表面覆盖“环境障涂层”来保护。稀土硅酸盐是下一代环境障涂层的首选材料，但仍需要优化这类材料的力学、热学和抗高温腐蚀性能，实现综合性能优化。
γ-Y2Si2O7是从室温到1450℃可稳定存在的高温相，具有诸多优异的性能，如：较高的抗损伤容限、较高的化学和热学稳定性，较好的抗高温腐蚀性，非常低的热导率(<2W/(m·K)，1000℃以上)和与硅基陶瓷匹配的热膨胀系数(3.9×10-6/K， 25～1400℃)，是科学家们广泛关注的环境障涂层体系(Z.Q.Sun,et al.Inter.Mater. Rev.(国际材料评论),2014(59)357–383.)。但是γ-Y2Si2O7的室温热导率偏高，约 6.5W/(m·K)，高温力学性能稍偏低，限制其应用前景。
研究发现：含Y硅酸盐中固溶其它稀土元素时，可以得到性能更加优异的固溶体材料(如：(YxYb1-x)2SiO5)，具有更高杨氏模量和更低热导率等。因此，通过固溶方法是改善稀土硅酸盐材料性能的重要方法(田志林，几种稀土硅酸盐陶瓷的预测、制备和性能研究，中国科学院大学博士学位论文，2016)。可以预计，将具有更大原子量和4f电子层的Ho来取代Y2Si2O7中原子量较小以及没有4f电子层的Y，可制备出具有更优综合性能的固溶体材料。例如，由于固溶产生的晶格畸变和强烈的声子散射，可明显降低材料的热导率。而且，含Ho硅酸盐具有非常优良的高温力学性能，Ho的固溶也可提高γ-Y2Si2O7的高温强度。
发明内容
本发明的目的在于提供一种(Y1-xHox)2Si2O7固溶体陶瓷材料及其制备方法，该材料耐高温、相稳定性好、高纯度、低热导率、力学性能良好。
本发明的技术方案如下：
一种(Y1-xHox)2Si2O7固溶体材料，(Y1-xHox)2Si2O7固溶体为从室温到1450℃可稳定存在的γ相(Y1-xHox)2Si2O7固溶体陶瓷材料，Ho取代Y的原子摩尔量x的取值范围为0<x<1。
所述的(Y1-xHox)2Si2O7固溶体材料的制备方法，首先，以氧化钇、氧化钬和二氧化硅混合粉末作为原料，(Y1-xHox)：Si：O的摩尔比为2：2：7，其中Ho取代Y的原子摩尔量x的取值范围为0<x<1；以乙醇为介质，进行球磨混合8～24h，形成浆料；接着，将浆料烘干后筛成粉末，倒入坩埚中；然后，在马弗炉中进行高温无压烧结，升温速率为5～10℃/min，烧结温度为1500～1600℃，烧结时间为0.5～1.5小时，最后得到(Y1-xHox)2Si2O7固溶体粉体。
所述的(Y1-xHox)2Si2O7固溶体材料的制备方法，将无压烧结后的固溶体粉体放入球磨罐中球磨然后干燥，并将干燥好的固溶体粉体装入石墨磨具中进行冷压成型，施加压强为5～15MPa；在通有保护气氛的热压炉内进行热压烧结，升温速率为5～30℃/min，烧结温度为1550～1700℃，烧结时间为0.5～3小时，烧结压强为15～45MPa，制备出(Y1-xHox)2Si2O7固溶体块体陶瓷。
所述的(Y1-xHox)2Si2O7固溶体材料的制备方法，热压烧结采用的保护气氛为氩气或氮气。
所述的(Y1-xHox)2Si2O7固溶体材料的制备方法，氧化钇、氧化钬和二氧化硅粉末的原始粒度范围在100～600目。
所述的(Y1-xHox)2Si2O7固溶体材料的制备方法，无压烧结采用常压在空气气氛下进行。
本发明的优点及有益效果是：
1.纯度高，耐腐蚀，高温性能优良。采用本发明制备的(Y1-xHox)2Si2O7固溶体材料是将钬(Ho)元素原位固溶到Y2Si2O7陶瓷的晶格中，几乎不含Y2SiO5或者磷灰石等杂质相。Y2Si2O7陶瓷良好的耐腐蚀性能和钬硅酸盐陶瓷优异的低热导、良好的抗热震性能和高温力学性能相结合，获得综合性能良好的固溶体材料。
2.本发明的操作方便，工艺简单，成本低。
3.本发明中，粉体的制备是通过无压烧结直接制备。块体材料的制备是通过热压/固-液相反应，由于在烧结过程中有液相的出现，而且液相的传质过程较快，所以反应时间明显缩短，又更容易使材料致密化。
附图说明
图1为实施例1中Ho取代0.2Y的(Y0.8Ho0.2)2Si2O7固溶体的X射线衍射图。
图2为实施例1中Ho取代0.2Y的(Y0.8Ho0.2)2Si2O7固溶体粉体的扫描照片。
图3为实施例2中Ho取代0.5Y的(Y0.5Ho0.5)2Si2O7固溶体的热导率图。
图4为实施例3中Ho取代0.33Y的(Y0.67Ho0.33)2Si2O7固溶体的X射线衍射图。
图5为实施例3中Ho取代0.33Y的(Y0.67Ho0.33)2Si2O7固溶体的热导率图。
具体实施方式
在具体实施过程中，本发明一种(Y1-xHox)2Si2O7固溶体材料及其制备方法，具体步骤如下：
1.固溶体粉体的制备：以氧化钇、氧化钬和二氧化硅混合粉末作为原料，以乙醇为介质，进行球磨混合8～24h，形成浆料；接着，浆料烘干后筛成粉末，倒入坩埚中，然后在马弗炉中高温烧结，升温速率为5～10℃/min，烧结温度为 1500～1600℃，烧结时间为0.5～1.5小时，最后得到(Y1-xHox)2Si2O7固溶体粉体。
2.固溶体块体的制备：将无压烧结后的固溶体粉体放入球磨罐中球磨然后干燥，并将干燥好的固溶体粉体装入石墨磨具中进行冷压成型，施加压强为5～ 15MPa，在通有保护气氛的热压炉内烧结，升温速率为5～30℃/min，烧结温度为 1550～1700℃，烧结时间为0.5～3小时，烧结压强为15～45MPa，制备出 (Y1-xHox)2Si2O7固溶体块体陶瓷。
从而，可以在简单的工艺下制备出具有耐高温(1550℃)、相稳定性好(室温到1450℃可稳定存在)、高纯度(>99％)、低热导率(1.5～4W/(m·K))以及力学性能良好 (室温和高温强度优良)的(Y1-xHox)2Si2O7固溶体陶瓷材料。
下面，通过实施例进一步详述本发明。
实施例1
原料氧化钇、氧化钬和二氧化硅粉末的原始粒度为600目，将氧化钇8克、氧化钬3.35克和二氧化硅5.32克(摩尔比为(Y0..8Ho0.2)2Si2O7)，以乙醇为介质，进行球磨混合24h，形成浆料；接着，浆料烘干后筛成粉末，倒入坩埚中，然后在马弗炉中进行高温无压烧结，升温速率为5℃/min，烧结温度为1550℃，烧结时间为0.5小时，制备出(Y0..8Ho0.2)2Si2O7固溶体粉体，其XRD图谱见图1，可看出为γ-(Y0.8Ho0.2)2Si2O7相，形貌见图2。
实施例2
原料氧化钇、氧化钬和二氧化硅粉末的原始粒度为300目，将氧化钇10克、氧化钬16.73克和二氧化硅10.65克(摩尔比为(Y0.5Ho0.5)2Si2O7)，以乙醇为介质，进行球磨混合8h，形成浆料；接着，浆料烘干后筛成粉末，倒入坩埚中，然后在马弗炉中进行高温无压烧结，升温速率为10℃/min，烧结温度为1580℃，烧结时间为1小时，制备出(Y0.5Ho0.5)2Si2O7固溶体粉体。
之后，将无压烧结后的固溶体粉体放入球磨罐中球磨然后干燥，并将干燥好的固溶体粉体装入石墨磨具中进行冷压成型，施加压强为5MPa，冷压时间为 15min，在通有氩气气氛的热压炉内烧结，升温速率为5℃/min，烧结温度为1600 ℃，烧结时间为1小时，保温时烧结压强一直保持45MPa，最后获得(Y0.5Ho0.5)2Si2O7固溶体块体。所制备样品的密度为4.75g/cm3，为理论密度的96.9％。从室温到1200 ℃的热导率见图3，从图中可以看出，γ-(Y0.5Ho0.5)2Si2O7固溶体的热导率明显低于γ-Y2Si2O7和γ-Ho2Si2O7相。
实施例3
原料氧化钇、氧化钬和二氧化硅粉末的原始粒度为100目，将氧化钇9克、氧化钬7.53克和二氧化硅7.18克(摩尔比为(Y0.67Ho0.33)2Si2O7)，以乙醇为介质，进行球磨混合12h，形成浆料；接着，浆料烘干后筛成粉末，倒入坩埚中，然后在马弗炉中进行高温无压烧结，升温速率为5℃/min，烧结温度为1510℃，烧结时间为1.5小时，制备出(Y0.67Ho0.33)2Si2O7固溶体粉体。
之后，将无压烧结后的固溶体粉体放入球磨罐中球磨然后干燥，并将干燥好的固溶体粉体装入石墨磨具中进行冷压成型，施加压强为15MPa，冷压时间为 10min，在通有氮气气氛的热压炉内烧结，升温速率为10℃/min，烧结温度为1700 ℃，烧结时间为2小时，保温时烧结压强一直保持15MPa，最后获得 (Y0.67Ho0.33)2Si2O7固溶体块体。所制备样品的密度为4.39g/cm3，为理论密度的96％，其XRD图谱见图4，可看出为(Y0.67Ho0.33)2Si2O7相。而且从图5的热导率图中能直观的看到，固溶体的热导率低于两种单相陶瓷的热导率，尤其在室温时，热导率显著降低。
由实施例1、实施例2和实施例3可见，本发明方法制备的(Y1-xHox)2Si2O7固溶体材料具有纯度高、块体致密度高和热导率低等优点，此外还具有耐高温、相稳定性好、以及力学性能良好的特点。而且本发明成本低廉、生产工艺简单且可操作性强，便于转化为生产力。
Claims (6)
1.一种(Y1-xHox)2Si2O7固溶体材料，其特征在于，(Y1-xHox)2Si2O7固溶体为从室温到1450℃可稳定存在的γ相(Y1-xHox)2Si2O7固溶体陶瓷材料，Ho取代Y的原子摩尔量x的取值范围为0<x<1。
2.一种权利要求1所述的(Y1-xHox)2Si2O7固溶体材料的制备方法，其特征在于，首先，以氧化钇、氧化钬和二氧化硅混合粉末作为原料，(Y1-xHox)：Si：O的摩尔比为2：2：7，其中Ho取代Y的原子摩尔量x的取值范围为0<x<1；以乙醇为介质，进行球磨混合8～24h，形成浆料；接着，将浆料烘干后筛成粉末，倒入坩埚中；然后，在马弗炉中进行高温无压烧结，升温速率为5～10℃/min，烧结温度为1500～1600℃，烧结时间为0.5～1.5小时，最后得到(Y1-xHox)2Si2O7固溶体粉体。
3.按照权利要求2所述的(Y1-xHox)2Si2O7固溶体材料的制备方法，其特征在于，将无压烧结后的固溶体粉体放入球磨罐中球磨然后干燥，并将干燥好的固溶体粉体装入石墨磨具中进行冷压成型，施加压强为5～15MPa；在通有保护气氛的热压炉内进行热压烧结，升温速率为5～30℃/min，烧结温度为1550～1700℃，烧结时间为0.5～3小时，烧结压强为15～45MPa，制备出(Y1-xHox)2Si2O7固溶体块体陶瓷。
4.按照权利要求3所述的(Y1-xHox)2Si2O7固溶体材料的制备方法，其特征在于，热压烧结采用的保护气氛为氩气或氮气。
5.按照权利要求2所述的(Y1-xHox)2Si2O7固溶体材料的制备方法，其特征在于，氧化钇、氧化钬和二氧化硅粉末的原始粒度范围在100～600目。
6.按照权利要求2所述的(Y1-xHox)2Si2O7固溶体材料的制备方法，其特征在于，无压烧结采用常压在空气气氛下进行。
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