镁热还原-酸洗制备钽粉工艺中粉体的演变规律

doi:10.19976/j.cnki.43-1448/TF.2024085

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Abstract Currently, the tantalum powders prepared by sodium reduction of potassium fluorotantalate cannot meet the requirements of high-end capacitors for the morphology uniformity and oxygen content of tantalum powders. This paper prepared tantalum powders by magnesium reduction of tantalum oxide-acid leaching process. The phase composition, micro-morphology, element content, and particle size distribution of tantalum powders before and after the acid leaching were studied using X-ray diffractometer, scanning electron microscope, energy spectrometer, laser particle size analyzer, oxygen/nitrogen/hydrogen analyzer, and inductively coupled plasma emission spectrometer. The results indicate that the tantalum powder particles inherit the morphology of the raw material. When n(Mg)∶n(Ta₂O₅)=5∶1, a few of the tantalum powders absorb hydrogen forming Ta₂H during acid leaching owing to the fine grain and high activity of the tantalum, the insufficient magnesium led to the formation of Mg₄Ta₂O₉ resulting from the reaction of unreacted Ta₂O₅ and MgO at this moment, which is difficult to separate from tantalum powders; when n(Mg)∶n(Ta₂O₅)=7.5∶1, the tantalum oxides are completely reduced to tantalum; when n(Mg)∶n(Ta₂O₅)=10∶1, the oxygen content of tantalum powders decreases to 0.58%, and the morphology uniformity is obviously improved.

Key words： tantalum magnesiothermic reduction powder morphology oxygen content capacitor

Received: 11 October 2024 Published: 08 April 2025

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	Articles by authors
	CHENG Yuewei
	CHEN Yi
	WANG Ruifang
	XING Yichen
	HAN Zhenghao
	CHE Yusi
	HE Jilin

Cite this article:

CHENG Yuewei,CHEN Yi,WANG Ruifang, et al. Evolution rule of powders during preparation of tantalum powders by magnesiothermic reduction-acid leaching[J]. Materials Science and Engineering of Powder Metallurgy, 2025, 30(1): 35-41.

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http://pmbjb.csu.edu.cn/EN/10.19976/j.cnki.43-1448/TF.2024085 OR http://pmbjb.csu.edu.cn/EN/Y2025/V30/I1/35

[1] 何季麟, 张宗国. 中国钽铌工业的现状与发展[J].中国金属通报, 2006, 14(48): 2-8.
HE Jilin, ZHANG Zongguo.Current status and development of tantalum niobium industry in China[J].China Metal Bulletin, 2006, 14(48): 2-8.
[2] 杨国启, 何季麟, 郑爱国, 等. 电容器级高比容钽粉制备工艺研究进展[J].湖南有色金属, 2014, 30(1): 48-52.
YANG Guoqi, HE Jilin, ZHNEG Aiguo, et al.Research progress of capacitor grade high capacitance tantalum powder preparation new technology[J].Hunan Nonferrous Metals, 2014, 30(1): 48-52.
[3] 程越伟, 郑爱国, 潘伦桃, 等. 电容器用钽粉的高比容化[J].宁夏工程技术, 2006, 5(1): 99-101.
CHENG Yuewei, ZHENG Aiguo, PAN Luntao, et al.Trend of high capacitance tantalum powder[J].Ningxia Engineering Technology, 2006, 5(1): 99-101.
[4] 梁雅丽, 王英红. 高比容钽粉在电容器中的应用[J].电子元件与材料, 2006, 25(5): 46-48.
LIANG Yali, WANG Yinghong.Application of high CV tantalum powder in tantalum capacitors[J].Electronic Components & Materials, 2006, 25(5): 46-48.
[5] 李福成. 钠还原高比容钽粉湿法提纯过程中酸洗新工艺[J].河南理工大学学报(自然科学版), 2022, 41(4): 176-180.
LI Fucheng.Pickling technology in the wet purification process of sodium reduction high specific capacity tantalum powder[J].Journal of Henan Polytechnic University (Natural Science), 2022, 41(4): 176-180.
[6] 李福成, 杨雨, 包富贵. 高比容钽粉湿法新工艺提纯过程中物化性能的研究[J].宁夏大学学报(自然科学版), 2022, 43(3): 1-5.
LI Fucheng, YANG Yu, BAO Fugui.High specific capacity metal tantalum powder wet new technology purification and chemical properties research[J].Journal of Ningxia University (Natural Science Edition), 2022, 43(3): 1-5.
[7] 包玺方, 谢永旭, 李仲香, 等. 气流粉碎机在高压高比容钽粉中的应用研究[J].有色金属(冶炼部分), 2017(3): 44-48.
BAO Xifang, XIE Yongxu, LI Zhongxiang, et al.Study on application of air jet mill in high voltage high capacitance tantalum powder[J].Nonferrous Metals (Extractive Metallurgy), 2017(3): 44-48.
[8] 刘银元. 高压电解电容器用钽粉的制备[D].长沙: 中南大学, 2011.
LIU Yinyuan.Preparation of tantalum powder for high voltage electrolytic capacitors[D].Changsha: Central South University, 2011.
[9] 胡小锋. 熔盐电脱氧法制备金属Ta及Nb-Ta合金[D].沈阳: 东北大学, 2006.
HU Xiaofeng.Preparation of tantalum and Nb-Ta alloy by electro-deoxidation in a eutectic CaCl₂-NaCl melt[D].Shenyang: Northeastern University, 2006.
[10] ZHU H M, SADOWAY D R.Synthesis of nanoscale particles of Ta and Nb₃Al by homogeneous reduction in liquid ammonia[J].Journal of Materials Research, 2001, 16: 2544-2549.
[11] 何季麟, 潘伦桃, 郑爱国, 等. 氧化钽(铌)还原制取钽(铌)粉的新方法[J].矿业研究与开发, 2003, 8(S1): 15-17.
HE Jilin, PAN Luntao, ZHENG Aiguo, et al.A new method for making tantalum/niobium powder by reducing Ta/Ta oxide[J].Mining Research and Development, 2003, 8(S1): 15-17.
[12] CHAI L Y, ZHONG H Y.Influence of alkali halide additions on tantalum powder production[J].Transactions of Nonferrous Metals Society of China, 1996, 6(3): 36-39.
[13] 宋金磊. 多级深度还原法制备钽粉的基础研究[D].沈阳: 东北大学, 2019.
SONG Jinlei.Basic research on preparation of tantalum powder by multistage depth reduction process[D].Shenyang: Northeastern University, 2019.
[14] 雒国清, 李慧, 陈学清, 等. 氟钽酸钾还原制备工艺对钽粉性能的影响[J].有色金属(冶炼部分), 2022(11): 85-88.
LUO Guoqing, LI Hui, CHEN Xueqing, et al.Effeet of potassium fluotantalate reduction condition on properties of tantalum powder[J].Nonferrous Metals (Extractive Metallurgy), 2022(11): 85-88.
[15] 王东新, 李军义, 孙本双, 等. 还原氧化钽制备钽粉工艺研究进展[J].中国材料进展, 2011, 30(10): 54-58.
WANG Dongxin, LI Junyi, SUN Benshuang, et al.Research progress on tantalum powder production technology by reducing Ta₂O₅[J].Materials China, 2011, 30(10): 54-58.
[16] 马海燕, 王浩亮, 程越伟, 等. 氟钽酸钾钠还原搅拌釜中的搅拌流场数值模拟[J].有色金属(冶炼部分), 2022(12): 92-100.
MA Haiyan, WANG Haoliang, CHENG Yuewei, et al.Numerical simulation of stirring flow field in stirred tank for potassium fluotantalate sodium reduction[J].Nonferrous Metals (Extractive Metallurgy), 2022(12): 92-100.
[17] YUAN B Y, OKABE T H.Production of fine tantalum powder by preform reduction process using Mg-Ag alloy reductant[J].Journal of Alloys and Compounds, 2007, 443(1/2): 71-80.
[18] OKABE T H, SATO N, MITSUDA Y, et al.Production of tantalum powder by magnesiothermic reduction of feed preform[J].Materials Transactions, 2003, 44(12): 2646-2653.
[19] LEE Y K, SIM J J, BYEON J S, et al.Production of high-purity tantalum metal powder for capacitors using self-propagating high-temperature synthesis[J].Archives of Metallurgy and Materials, 2021, 66(4): 935-939.
[20] ORLOV V M, KRYZHANOV M V.Magnesium-thermic reduction of tantalum oxide by self-propagating high-temperature synthesis[J].Russian Metallurgy (Metally), 2010, 2010(5): 384-388.
[21] ORLOV V M, KRYZHANOV M V.Magnesiothermic reduction of Mg₄Ta₂O₉ in the combustion regime[J].Inorganic Materials, 2018, 54: 910-914.