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真空 ›› 2026, Vol. 63 ›› Issue (4): 52-57.doi: 10.13385/j.cnki.vacuum.2026.04.08

• 测量与控制 • 上一篇    下一篇

一种基于钽阳极块体积收缩的高真空热处理炉校温方法研究*

李少军1,2, 李仲香1,2, 陈学清1,2, 杜威1, 桂愉平1, 李琦凡1   

  1. 1.宁夏东方钽业股份有限公司,宁夏 石嘴山 753000;
    2.稀有金属特种材料全国重点实验室,宁夏 石嘴山 753000
  • 收稿日期:2025-09-18 发布日期:2026-07-27
  • 通讯作者: 李仲香,硕士,正高级工程师。
  • 作者简介:李少军(1974-),男,本科,中级职称。
  • 基金资助:
    *宁夏自然科学基金资助项目(2025AAC031063)

Study on Temperature Calibration Method for High-Vacuum Heat Treatment Furnace Based on Volume Shrinkage of Tantalum Anode Blocks

LI Shaojun1,2, LI Zhongxiang1,2, CHEN Xueqing1,2, DU Wei1, GUI Yuping1, LI Qifan1   

  1. 1. Ningxia Orient Tantalum Industry Co., Ltd., Shizuishan 753000, China;
    2. National Key Laboratory of Rare Metal Special Materials, Shizuishan 753000, China
  • Received:2025-09-18 Published:2026-07-27

摘要: 针对高温高真空热处理炉在钽粉烧结过程中存在的温度稳定性与均温性问题,本研究提出了一种基于钽电解电容器阳极块体积收缩特性的新型校温方法。通过压制特定规格的钽阳极块(1 g钽粉,直径6 mm,压制密度5.5 g/cm³),在1 500~2 000℃烧结条件下,结合高斯分布3σ原则建立体积收缩比控制模型。实验结果表明:该方法能有效监测炉膛前、中、后区域温度偏差,当体积收缩比超出置信区间时,提示热电偶衰减需及时更换。与传统测温环校温法相比,该方法具有温度适应力强、精度高(±5℃)的特点,可为钽粉电容器级物料的烧结工艺优化提供可靠依据。

关键词: 钽粉, 高真空热处理, 体积收缩率

Abstract: Aiming at the problems of temperature stability and uniformity existing in the sintering process of tantalum powder in high-temperature and high-vacuum heat treatment furnace, this study proposes a new temperature calibration method based on the volume shrinkage characteristics of the anode block of tantalum electrolytic capacitors. By pressing tantalum anode blocks of specific specifications (1 g tantalum powder, with a diameter of 6 mm and a pressing density of 5.5 g/cm³), under the sintering conditions of 1 500~2 000℃, a volume shrinkage ratio control model was established in combination with the 3σ principle of the Gaussian distribution. The experimental results show that this method can effectively monitor the temperature deviation in the front, middle and rear areas of the furnace. When the volume shrinkage ratio exceeds the confidence interval, it indicates that the thermocouple is attenuated and needs to be replaced in a timely manner. Compared with the traditional temperature calibration method using temperature measuring rings, this method has the characteristics of strong temperature adaptability and high precision (within ±5℃), and can provide a reliable basis for the optimization of the sintering process of capacitor-grade materials of tantalum powder.

Key words: tantalum powder, vacuum heat treatment, volume shrinkage rate

中图分类号:  TF841.6

[1] 夏耀勤,王敬生.钽电容器的应用现状和展望[J].电子原件与材料,1999(2):34-36,54.
[2] 陈学清,李仲香,李慧,等. 一种金属粉末及其制备方法和应用:CN201611239557.6[P].2019-08-16.
[3] 鄂东梅. 真空技术在航空航天中的应用[J]. 真空, 2021, 58(3):77-81.
[4] 李仲香, 程越伟, 陈学清, 等. 一种高纯钽粉及其制备方法:CN201480016668.3[P].2018-02-06.
[5] 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
[6] Song Changhui, Deng Zhengtai, Chen Jiaqi, 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.
[7] 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 and Hard Materials, 2021, 100:105620.
[8] 徐卫, 叶高英, 萧锋. 一种高压电容器用球形钽粉的制备方法:CN201610720889.X[P].2016-08-25.
[9] 月日辉, 周丽. 添加细化剂对FTB-48电容器钽粉粒度及电性能的影响[J]. 稀有金属及硬质合金, 2020, 48(2):20.
[10] 李少军, 王志勇, 桂玉平. 一种高真空热处理炉的校温方法极其装置:2023110979031[P].2024-01-02.
[11] 刘易刚, 易金峰. 成形烧结过程对固体电解质钽电容器电性能的影响[J]. 稀有金属与硬质合金, 2008, 36(4):17-19, 67.
[12] 赵春霞, 雒国清, 杨国启, 等. 氧含量对钽粉电性能影响的研究[J]. 湖南有色金属, 2016, 32(5):39-40,59.
[13] 刘蓬云, 马春红, 黄凯, 等. 热处理时间和压制密度对氮化钽粉电性能的影响[J]. 有色金属冶炼部分, 2012(10):34-37,41.
[14] Gonzales G.How green rot affects Type K thermocouples[EB/OL].[2025-07-22].https://blog.wika.com/us/products/temperature-products/green-rot-affects-type-k-thermoc-ouples/.
[15] Tan Qiulin, Li Chen, Xiong Jijun, et al.A high temperature capacitive pressure sensor based on alumina ceramic for in situ measurement at 600℃[J]. Sensors, 2014, 14(2):2417-2430.
[16] Rakshan Kumar J K, Bhattacharjee D, Dsilva P, et al. Creep cavitation damage of K-type thermocouples[J]. Engineering Failure Analysis, 2023, 143(Part A):106846.
[17] Wang Yuefei, Liu Zhen.Development of numerical modeling and temperature controller optimization for internal heating vacuum furnace[J]. IEEE Access, 2021, 9:126765-126773.
[18] Akikubo K, Kurahashi T, Kawaguchi S, et al.Thermal expansion measurements of nano-graphite using high-temperature X-ray diffraction[J]. Carbon, 2020, 169:307-311.
[19] 王小明,赵春霞,王晓明, 等.钽粉中碳的来源及其对电性能的影响研究[J],湖南有色金属,2019,35(6):49-50,66.
[20] 崔京华, 王惠贞, 苗旭辉. 高真空退火炉模糊自适应温度控制器的研究[J]. 价值工程, 2010, 29(25):131-132.
[21] 王昊杰. 一种真空热处理炉加热器的结构优化方法:CN108170897A[P].2018-06-15.
[22] 石月娥, 聂英兰. 燃气热处理炉温度均匀性测试结果影响因素分析[J]. 中国计量, 2016(9):98-100.
[23] 周军勇, 俞能君, 金向阳, 等. 基于ANSYS的真空热处理炉的温度场分析[J]. 热加工工艺, 2024, 53(8):31-37.
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