欢迎访问沈阳真空杂志社 Email Alert    RSS服务

VACUUM ›› 2025, Vol. 62 ›› Issue (5): 91-97.doi: 10.13385/j.cnki.vacuum.2025.05.14

• Vacuum Metallurgy and Thermal Engineering • Previous Articles     Next Articles

Research on High Specific Capacity Tantalum Powder Passivation Device and Process

GUI Yuping1,2, LUO Guoqing1,2, DU Zhe1,2, LI Shaojun1,2, DU Wei1,2   

  1. 1. Ningxia Orient Tantalum Industry Co., Ltd., Shizuishan 753000, China;
    2. National Engineering Research Center of Tantalum and Niobium, Shizuishan 753000, China
  • Received:2024-08-19 Published:2025-09-29

Abstract: A passivation method for high specific volume tantalum powder with a specific volume of 100 000 μF·V/g and above after high temperature heat treatment and the design of a strong cooling device were introduced. Through rapid cooling technology, the strong cooling device significantly improves the production efficiency of tantalum powder, and avoids potential pollution of tantalum powder by volatiles in the furnace, ensuring the purity of the product. In addition, a three-step passivation technology was proposed, including primary passivation, secondary passivation and final passivation. This method can effectively solve the problem of heat retention caused by the reaction of oxygen-containing gas with tantalum powder in the passivation process, avoid the high oxygen caused by the temperature rise of tantalum metal powder, realize the fully stable passivation of tantalum powder, shorten the processing time, and do not introduce additional pollution. It has high practical value.

Key words: tantalum powder, heat treatment, passivation, forced cooling device, process optimization

CLC Number:  TG146.4+16

[1] 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.
[2] 潘伦桃. 钽金属表面钝化方法及装置:CN201110097815.2[P]. 2011-09-14.
[3] ORLOV V M,PROKHOROVA T Y,SEMUSHIN V V.Features of segregation of the oxide phase during sintering of tantalum powders with a large specific surface[J].Protection of Metals and Physical Chemistry of Surfaces, 2023,59(3):428-433.
[4] VENIGALLA S.Passivation of tantalum and other metal powders using oxygen:US7803235B2[P].2010-09-28.
[5] 王时光. 一种钽粉受控钝化镁处理降氧方法:CN200810032195.2[P].2009-01-21.
[6] 郑浩宇,廖志刚,朱德忠. 一种钽粉的热处理方法:CN201710354165.2[P].2019-08-23.
[7] 郑爱国,马跃忠,郑世萍,等. 钽金属表面钝化方法及装置:CN201180069256.2[P].2011-03-23.
[8] HWANG S M, PARK S J,WANG J P, et al.Preparation of tantalum metal powder by magnesium gas reduction of tantalum pentoxide with different initial particle size[J].International Journal of Refractory Metals & Hard Materials, 2021,100:105620.
[9] 帅柱军,余琨,何坤池.电容器钽粉镁处理降氧工艺探究[J].硬质合金, 2013,30(2):86-90.
[10] KOLOSOV V N,MIROSHNICHENKO M N,PROKHOROVA T Y,et al.Preparation of tantalum powders by the reduction of complex oxyfluoride compounds with sodium[J].Russian Journal of Non-Ferrous Metals, 2016,57(6):599-603.
[11] 赵军,张兴凯,王云海. 硫铁矿的比表面积、孔体积及其对硫铁矿吸附能力的影响研究[J]. 中国安全生产科学技术, 2008,4(4):119-121.
[12] 陈林,冒海红,董学成,等. 钽粉的热处理方法:CN201110039272.9[P].2011-02-14.
[13] 郭青蔚,王肇信.现代铌钽冶金[M].北京:冶金工业出版社.2009.
[14] 桂愉平,王彦杰,李少军,等. 真空热处理炉绝缘陶瓷对钽粉杂质的影响[J]. 热处理技术与装备, 2023,44(2):64-67.
[15] XU J Z,ZHANG T A,LI X L.Study on the condensation behaviour of magnesium vapour by the condensing flow field under relative vacuum conditions[J].Chemical Engineering and Processing, 2024,200:109785.
[16] 吴道雄,史鑫尧,张雁祥. 真空热处理炉的隔热屏设计及传热学分析[J]. 热处理技术与装备, 2015,36(5):73-76.
[17] 孙坤,李坤,汪森辉,等.“双碳”愿景下螺杆真空泵的设计与对策[J].真空, 2023,60(1):57-61.
[18] HE J L,PAN L T,LU Z D,et al.Observations on the morphology of sodium-reduced tantalum powders and modification to their physical properties[C]//International Symposium on Tantalum & Niobium:Production,Processing,Applications,Electronics and Ceramics. San Francisco,CA, US,2000:255-271.
[19] SONG C,DENG Z,CHEN J,et al.Study on the influence of oxygen content evolution on the mechanical properties of tantalum powder fabricated by laser powder bed fusion[J].Materials Characterization, 2023,205:113235.
[20] 潘伦桃. 钽粉降氧工艺研究与应用[J]. 稀有金属, 1990(4):259-263.
[21] PIROOZ M,WENDELL C H.A simple method for accurate determination of porosity using ideal gas law[J].Journal of Porous Materials, 2013,20(2):441-445.
[1] LIU Yihui, JIA Guocheng, WANG Weichao, MA Yi, QIAO Haibin, ZHAN Chunming. Failure Analysis of Pressure Leakage of Vacuum Melting ZTA15 Titanium Alloy Casting [J]. VACUUM, 2025, 62(3): 27-32.
[2] CHEN Bolong, LI Zhongren, WANG Ying, WU Yifei, SU Ning, SONG Jiaxing, CHE Enlin, LIU Jun. Study on Temperature Uniformity of Heat Treatment System for Large Superconducting Coils [J]. VACUUM, 2025, 62(3): 33-37.
[3] WANG Zhenhong, WANG Benlong, CHE Enlin, SU Ning, LIU Jun. Safety Analysis of the Hydrogenation and Dehydrogenation Process of Zirconium-2 Powder [J]. VACUUM, 2025, 62(3): 38-41.
[4] WANG Jie, ZHANG Jinglun, ZHANG Zenghai, E Dongmei, WANG Lingling, LIU Shimeng, ZHAN Chunming, ZHANG Pixian, SONG Qingzhu, WU Siwei. Research Progress on Process and Standardization of Additive Manufacturing Superalloys [J]. VACUUM, 2025, 62(2): 12-21.
[5] XIONG Qing-hai, LÜ Wei, LIN Wen-sen, ZHAN Chun-ming. Study on Forging Technology of Duplex Stainless Steel for Single Point Liquid Slip Ring in Vacuum Oxygen Argon Decarbonization Converter [J]. VACUUM, 2024, 61(6): 73-78.
[6] WANG Bao-lai, SU Ning, CHEN Ding, CHE En-lin, LIU Jun, WANG Zhen. Design Analysis of External Mechanized Chamber Heat Treatment Furnace [J]. VACUUM, 2024, 61(3): 79-83.
[7] WU Li-ying, QU Min-ni, FU Xue-cheng, TIAN Miao, MA Ling, CHENG Xiu-lan. Study on Atomic Layer Deposition of Al2O3 Protective Film of Cu Electrode [J]. VACUUM, 2023, 60(1): 30-35.
[8] WANG Gui-peng, HUANG Yu-xing, QU Shao-fen, GAO Guang-wei, XIE Yuan-hua, LIU Kun, BA De-chun. Study on Influence of the Change of Inlet and Outlet Angle of Impeller Blade of Vacuum Heat Treatment Furnace on Cooling Efficiency [J]. VACUUM, 2022, 59(5): 63-68.
[9] DUAN Shan-Shan, SHI Chang-yong, YANG Li-Zhen, LIU Zhong-wei, ZHANG Hai-bao, CHEN Qiang. The Recent Development and Future of Atomic Layer Deposition of Alumina Thin Films [J]. VACUUM, 2021, 58(6): 13-20.
[10] ZHANG Xin-hui, LI Qing-xiao. Effect of Vacuum Heat Treatment on Structure and Photoelectric Properties of AZO Film [J]. VACUUM, 2021, 58(3): 45-50.
[11] E Dong-mei. Application of Vacuum Technology in Aerospace [J]. VACUUM, 2021, 58(3): 77-81.
[12] WANG Ying, MING Yue, DAI Yu-bo, CHE En-lin, WANG Biao. Structure Optimization of Graphite Furnace for Vacuum High Temperature Heat Treatment Furnace [J]. VACUUM, 2020, 57(6): 27-30.
[13] WANG Fu-zhen. Heat Treatment and Vacuum Coating Towards Integration [J]. VACUUM, 2020, 57(5): 1-6.
[14] WANG Zhi-rong, MA Qiang, LONG Guo-liang, LI Xue-feng, LIU Cheng. Development and Application of Multi-Chamber Tunnel Continuous Vacuum Sintering Furnace and Heat Treatment Furnace [J]. VACUUM, 2019, 56(5): 6-11.
[15] WANG Bo, ZHANG Zhong-he, WANG Fei-yu, WANG Shuai, YAN Shuai, CUI Tian-long, ZHANG Zhong-xin. Study on Vacuum Heat Treatment Distortions of Martensite Precipitation Hardening Stainless Steel [J]. VACUUM, 2019, 56(4): 49-52.
Viewed
Full text


Abstract

Cited
  Shared   
  Discussed   
[1] LI De-tian, CHENG Yong-jun, ZHANG Hu-zhong, SUN Wen-jun, WANG Yong-jun, SUN Jian, LI Gang, . Preparations and applications of carbon nanotube field emitters[J]. VACUUM, 2018, 55(5): 1 -9 .
[2] ZHOU Bin-bin, ZHANG jian, HE Jian-feng, DONG Chang-kun. Carbon nanotube field emission cathode based on direct growth technique[J]. VACUUM, 2018, 55(5): 10 -14 .
[3] CHAI Xiao-tong, WANG Liang, WANG Yong-qing, LIU Ming-kun, LIU Xing-zhou, GAN Shu-yi. Operating parameter data acquisition system for single vacuum pump based on STM32F103 microcomputer[J]. VACUUM, 2018, 55(5): 15 -18 .
[4] LI Min-jiu, XIONG Tao, JIANG Ya-lan, HE Yan-bin, CHEN Qing-chuan. 20kV high voltage based on double transistor forward converter pulse power supply for metal deburring[J]. VACUUM, 2018, 55(5): 19 -24 .
[5] LIU Yan-wen, MENG Xian-zhan, TIAN Hong, LI Fen, SHI Wen-qi, ZHU Hong, GU Bing. Test of ultra high vacuum in space traveling-wave tube[J]. VACUUM, 2018, 55(5): 25 -28 .
[6] XU Fa-jian, WANG Hai-lei, ZHAO Cai-xia, HUANG Zhi-ting. Application of chemical gases vacuum-compression recovery system in environmental engineering[J]. VACUUM, 2018, 55(5): 29 -33 .
[7] XIE Yuan-hua, HAN Jin, ZHANG Zhi-jun, XU Cheng-hai. Discussion on present situation and development trend of vacuum conveying[J]. VACUUM, 2018, 55(5): 34 -37 .
[8] SUN Li-zhi, YAN Rong-xin, LI Tian-ye, JIA Rui-jin, LI Zheng, SUN Li-chen, WANG Yong, WANG Jian, . Research on distributing law of Xenon in big accumulation chamber[J]. VACUUM, 2018, 55(5): 38 -41 .
[9] HUANG Si, WANG Xue-qian, MO Yu-shi, ZHANG Zhan-fa, YING Bing. Experimental study on similarity law of liquid ring compressor performances[J]. VACUUM, 2018, 55(5): 42 -45 .
[10] CHANG Zhen-dong, MU Ren-de, HE Li-min, HUANG Guang-hong, LI Jian-ping. Reflectance spectroscopy study on TBCs prepared by EB-PVD[J]. VACUUM, 2018, 55(5): 46 -50 .
辽ICP备06004570号-4
Copyright © VACUUM, All Rights Reserved.
Tel: （024）24134406 24110136 24121929　Fax: （024） 24121929　E-mail: zkzk1964@126.com
Powered by Beijing Magtech Co. Ltd