共沉淀法制备镁基六铝酸镧粉体的性能研究

doi:10.11900/0412.1961.2018.00448

金属学报

2019, Vol. 55

Issue (5): 657-663 DOI: 10.11900/0412.1961.2018.00448

本期目录 | 过刊浏览

共沉淀法制备镁基六铝酸镧粉体的性能研究

李㼆^1,²,孙超¹,宫骏¹(

)

1. 中国科学院金属研究所沈阳 110016
2. 中国科学院大学北京 100049

Performance Research of Magnesium Base Lanthanum Hexaaluminate Prepared by Co-Precipitation

Ying LI^1,²,Chao SUN¹,Jun GONG¹(

)

1. Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China
2. University of Chinese Academy of Sciences, Beijing 100049, China

引用本文:

李㼆,孙超,宫骏. 共沉淀法制备镁基六铝酸镧粉体的性能研究[J]. 金属学报, 2019, 55(5): 657-663.
Ying LI, Chao SUN, Jun GONG. Performance Research of Magnesium Base Lanthanum Hexaaluminate Prepared by Co-Precipitation[J]. Acta Metall Sin, 2019, 55(5): 657-663.

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摘要:

用共沉淀法，选取沉淀温度60 ℃，沉淀pH值11.5制备的镁基六铝酸镧前驱粉体，在1500 ℃煅烧5 h后制备出热障涂层陶瓷层材料LaMgAl₁₁O₁₉。采用XRD、TEM、SAED和XPS分析了反应产物的相结构、形貌、半峰全宽和谱强。结果表明，提高沉淀温度制备的前驱粉体磁铅石相生成效率提高；LaMgAl₁₁O₁₉晶体发育良好，晶粒呈六角片方状；前驱粉体煅烧温度在1500 ℃左右，La、Mg、Al、O 4种原子的电子结合能增大，动能减小，反应物趋于稳定；LaMgAl₁₁O₁₉晶胞结晶过程中先生成尖晶石层，后形成镜面层。生成纯磁铅石相粉体的过程中，LaAlO₃、MgAl₂O₄键的半峰宽度有增大，晶体结构无序度增加，有利于提高陶瓷层的抗烧结能力及热稳定性。关键词磁铅石相，六铝酸镧，晶体结构，原子成键

Abstract：

Thermal barrier coatings are widely used on turbine blades to provide high temperature insulation, oxidation and corrosion protection. Thermal barrier coatings are composed of matrix, oxide layer, bonding layer and ceramic layer. The lanthanum magnesium hexaaluminate with magnetoplumbite structure have a high aspect ratio, large specific surface area and strong resistance to high temperature sintering, and it can be used as ceramic layer of thermal barrier coatings. In this work, the former powders of lanthanum magnesium hexaaluminate was prepared at synthesized temperature of 60 ℃, pH=11.5. Comparing with the conventional chemical co-preparation synthesis, the synthesized temperature was raised and the pH value for synthesizing was reduced, which resulted in improving production efficiency of former powders. And the lanthanum magnesium hexaaluminate powders for ceramic layer of thermal barrier coating was prepared after the precursor powders were calcinated at 1500 ℃ for 5 h. The phase structure of reaction products, morphology of the powders, full width at half maximum and spectral intensity were analyzed by XRD, SEM, TEM and XPS. The results showed that the magnetoplumbite structured formation generation was elevated much more efficiency if the former powders were precipitated at higher temperature. Since the bonding energy of La, Mg, Al and O atoms increased, the kinetic energy of electrons decreased, therefore, chemical composition of the reaction products were steady near 1500 ℃. During the crystallization process of lanthanum magnesium hexaaluminate, the spinel layer was generated firstly and mirror layer was consequently produced. In the process of producing pure magnetoplumbite phase powders, the full width at half maximum of LaAlO₃ formula and MgAl₂O₄ formula were increased and the activation energy of the crystal structure was higher than that before reaction, which was beneficial to improve anti-sintering performance and thermal stability of the ceramic coating.

Key words： magnetoplumbite phase lanthanum hexaaluminate crystal structure atomic bonding

收稿日期: 2018-09-19

ZTFLH:

TG174.442

基金资助:国家自然科学基金项目(51301180)

作者简介: 李㼆, 女，1988年生，博士生

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链接本文:

https://www.ams.org.cn/CN/10.11900/0412.1961.2018.00448 或 https://www.ams.org.cn/CN/Y2019/V55/I5/657

图1 前驱粉体在不同温度煅烧后的XRD谱

图2 沉淀pH=11.5、沉淀温度为60 ℃下制备的前驱粉体在1500 ℃煅烧5 h后得到的LaMgAl11O19粉体的SEM像及TEM明场像

表1 不同温度下煅烧后的粉体原子结合能

图3 沉淀pH=11.5、沉淀温度为60 ℃下制备的前驱粉体在1500 ℃煅烧5 h得到的LaMgAl11O19粉体的XPS全谱图

图4 沉淀pH=11.5、沉淀温度为60 ℃下制备的前驱粉体在1500 ℃煅烧5 h得到的LaMgAl11O19粉体中La3d、Al2p、Mg2p、O1s峰的XPS拟合谱

图5 La2O3、LaAlO3、MgAl2O4的半峰全宽及LaAlO3与La2O3键含量

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