硅酸盐学报

液相前驱体法合成纳米AlN及钇助剂作用机制

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沈强 ¹ , 姜亦夏 ¹ , 李美娟 ¹ , 徐志刚 ¹ , 梁明川 ²

硅酸盐学报 | 研究论文 2026,54(9): 3185-3193

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硅酸盐学报 |研究论文 2026 , 54 (9) : 3185 -3193

液相前驱体法合成纳米AlN及钇助剂作用机制

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沈强¹, 姜亦夏¹, 李美娟¹, 徐志刚¹, 梁明川²

作者信息

^1．武汉理工大学，材料复合新技术全国重点实验室，武汉 430070

^2．南充三环电子有限公司，四川南充 637100

通讯作者:

李美娟（1969—），女，博士，副教授。

作者简介:

沈强（1970—），男，博士，研究员。

Synthesis of Nano-Sized AlN via Liquid-Phase Precursor Method with Yttrium Additives

Qiang SHEN¹, Yixia JIANG¹, Meijuan LI¹, Zhigang XU¹, Mingchuan LIANG²

Affiliations

^1.State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070, China

^2.Nanchong Sanhuan Electronic Co., Ltd., Nanchong 637100, Sichuan, China

Corresponding Author:

{LI} Meijuan (1969-), female, Ph.D., Associate Professor. E-mail: meijuanli@whut.edu.cn

SHEN Qiang (1970-), male, Ph.D., Researcher. E-mail: 2864207430@qq.com

出版时间: 2026-08-18 doi: 10.14062/j.issn.0454-5648.20250645

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摘要

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高品质氮化铝（AlN）粉末是制备高性能氮化铝陶瓷的关键技术环节之一。本工作采用液相分散和低温氮化工艺，在1100 ℃低温下还原煅烧合成了钇助剂分布均匀的纳米AlN粉体，探讨了钇助剂对合成AlN粉末物相组成、形貌、粒径、元素分布的影响。结果表明，合成的AlN粉末颗粒呈类球形，晶粒尺寸小于80 nm，且随着钇助剂含量的增大，晶粒尺寸从74 nm减小至40 nm，不同钇添加量下AlN的晶胞参数与晶面间距均保持不变，未发现AlN晶格畸变现象。研究发现：通过液相法引入钇助剂可在低温下得到均匀分散的纳米AlN粉体，且引入的钇助剂处于AlN晶界处，调控AlN晶粒的尺寸、颗粒的微观形貌等。

关键词

氮化铝 / 钇助剂 / 纳米球形粉末 / 晶粒细化

Abstract

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Introduction

With the rapid development of new thermal management materials, a demand for high quality AlN powders becomes increasingly urgent. The liquid phase precursor method is regarded as a crucial approach for producing high purity AlN nano-powder due to its advantage of homogeneous mixing in molecular level. Therefore, a study on the liquid phase precursor method and the effect of additives within the system on the precursor pyrolysis, liquid phase regulation, and nitridation kinetics is essential for improving the purity, reaction efficiency, and structural uniformity of sized AlN nano-powder. In this study, AlN nano-powder was synthesized by a liquid phase precursor method at low temperatures, and the role, reaction pathways, and regulatory mechanisms of yttrium additives in the precursor system were systematically investigated. This work could provide significant insights toward enhancing powder purity, achieving controlled crystal growth, and optimizing structural homogeneity.

Methods

Aluminum chloride hexahydrate was used as an aluminum source and dicyandiamide and melamine as nitrogen sources. Yttrium acetate tetrahydrate acted as a soluble yttrium additive, and methanol was selected as a solvent. The aluminum and nitrogen sources were dissolved in methanol at an N/Al molar ratio of 4, and yttrium was added at 0-3% (calculated as Y₂O₃ in the final AlN). After magnetic stirring for 30 min, a uniform precursor solution was obtained. The solution was dried at 85 ℃ for 12 h, and then ground into a white precursor powder. The precursor powders were placed in covered alumina crucibles and heated in a tube furnace under flowing N₂ to 1100 ℃ at 10 ℃/min, followed by a 3h dwell, to synthesize AlN powders with different yttrium contents. The thermal behavior of yttrium acetate and precursor powders was determined in N₂ by thermogravimetric analysis-differential scanning calorimetry (TG-DSC) from room temperature to 1200 ℃. The phase compositions were examined by X-ray diffraction (XRD, Cu K_α, 20°-80°). The particle morphology of the synthesized powder was determined by field-emission scanning electron microscopy, using an accelerating voltage of 20 kV. The microstructure of the particles in the powder was analyzed by transmission electron microscopy (TEM). The elemental composition and distribution were characterized by energy dispersive spectroscopy (EDS), while the crystalline phase and crystal structure were determined by selected area electron diffraction (SAED).

Result and discussion

The liquid phase dispersion combined with a low temperature calcination effectively reduces the synthesis temperature. Compared with the conventional carbothermal reduction method, the Al—Cl bond exhibits a bond strength of approximately 174 kJ/mol, which is lower than that of the Al—O bond, resulting in a reduced activation energy for the reaction. As high nitrogen solid molecules, cyanamide species can release high concentrations of highly reactive nitrogen in-situ on the surface and inside the aluminum precursor, facilitating the completion of the nitridation reaction at a lower temperature for a shorter time. The aluminum source, nitrogen sources, and yttrium additives are mixed and contacted more uniformly due to the excellent dispersibility of the liquid phase, thereby further enhancing both the nitridation rate and its uniformity. The results indicate that the introduction of a small amount of yttrium additive promotes the refinement and uniformity of AlN particles. As the yttrium content increases from 0% to 3%, the AlN particles gradually evolve toward a quasi-spherical morphology, accompanied by improved sphericity and reduced particle size. The average AlN grain size decreases from 74 nm without yttrium addition to 40 nm at 3% yttrium addition. A similar grain-size reduction trend is also obtained based on calculations using the Scherrer equation from the XRD results. The added yttrium additive is uniformly distributed throughout the AlN samples and does not compromise the lattice purity of AlN. No lattice expansion associated with impurity incorporation or solid solution formation occurrs in either the lattice parameters or interplanar spacings.

Conclusions

At the synthesis temperature of 1100 ℃ that could be lower than that required for the carbothermal reduction method, the precursor effectively transformed into crystalline AlN regardless of whether yttrium additives introduced. The addition of a small amount of yttrium effectively promoted the refinement and uniformity of AlN particles, resulting in synthesized AlN powders with relatively uniform particle size and morphology. Yttrium containing compounds had an inhibitory effect on the AlN grain growth, leading to a further refinement of AlN grains in nanoscale. The average grain size of AlN decreased from 74 nm without yttrium addition to 62 nm at 1% yttrium content, and further to 40 nm at 3% yttrium content. The incorporation of yttrium additives did not compromise the lattice purity of AlN during synthesis. The interplanar spacing of AlN nanocrystals remained consistently at 0.270 nm at all yttrium concentrations, corresponding to the plane (100) of hexagonal AlN. In addition, no significant increase occurred in the a-axis, c-axis, c/a ratio, or unit cell volume of AlN nanocrystals with different yttrium contents, confirming the absence of lattice expansion due to the impurity incorporation or the solid-solution formation.

Key words

aluminum nitride / yttrium additives / nanometer spherical powder / grain refinement

引用本文

沈强, 姜亦夏, 李美娟, 徐志刚, 梁明川. 液相前驱体法合成纳米AlN及钇助剂作用机制. 硅酸盐学报, 2026 , 54 (9) : 3185 -3193 . DOI: 10.14062/j.issn.0454-5648.20250645

Qiang SHEN, Yixia JIANG, Meijuan LI, Zhigang XU, Mingchuan LIANG. Synthesis of Nano-Sized AlN via Liquid-Phase Precursor Method with Yttrium Additives[J]. Journal of the Chinese Ceramic Society, 2026 , 54 (9) : 3185 -3193 . DOI: 10.14062/j.issn.0454-5648.20250645

基金

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国家重点研发计划(2023YFB3507200)

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2026年第54卷第9期

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文章信息

doi: 10.14062/j.issn.0454-5648.20250645

接收时间：2025-09-01
首发时间：2026-10-22
出版时间：2026-08-18

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收稿日期：2025-09-01
修回日期：2025-09-21

基金

国家重点研发计划(2023YFB3507200)

作者信息

^1．武汉理工大学，材料复合新技术全国重点实验室，武汉 430070

^2．南充三环电子有限公司，四川南充 637100

通讯作者:

李美娟（1969—），女，博士，副教授。

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https://castjournals.cast.org.cn/joweb/gsyxb/CN/10.14062/j.issn.0454-5648.20250645

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2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
				栓菌属 Trametes	5	2.39

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