R-D & HDDR Process에 의한 Nd-Fe-B계 희토류 이방성 본드자석재료의 제조에 관한 기초연구 (I)

조선미; 송창빈; 조통래; Sun Mi Cho; Chang Bin Song; Tong Rae Cho

Korean Journal of Materials Research, Vol.11, No.7, 609-614, July, 2001

Basic Study on the Production of Nd-Fe-B System Rare Earth Anisotropic bonded Magnet Materials by the R-D & HDDR Process(I)

조선미, 송창빈 , 조통래¹

공주대학교 공과대학 신소재공학부
¹충남대학교 공과대학 재료공학부

Sun Mi Cho, Chang Bin Song , and Tong Rae Cho¹

Department of Materials Engineering, Kongju National University, Kongju, Korea
¹School of Materials Engineering, Chungnam National University, Taejon, Korea

초록

본 연구는 R-B & HDDR process를 적용해서 Nd-Fe-B계 회토류 이방성 본드자석의 제조를 위한 기초 데이터를 확보할 목적으로. 환원확산법을 사용해서 Nd-Fe-B계 자석합금분말을 제조하는 데 필요한 금속 Ca에 의한 Nd 2 O 3 의 환원반응과 Fe-B합금분말중에서의 Nd확산반응을 조사하였다. 그 결과 Nd 2 O 3 의 환원시 필요한 최적의 Ca첨가량은 100 0 ? C 에서 1h동안 R-D 반응후 Nd 및 B원소의 수율관계로부터 이론당량의 1.3배정도가 적량인 것으로 나타났다. 또한 Fe-B합금분말중에 Nd의 확산과 관련된 XRD의 분석결과에 따라 완전한 균질화를 위해서는 110 0 ? C 에서 45min정도의 R-D반응이 필요하였으며, R-D반응에 대한 Nd의 수율도 그 조건에서 최대로 얻어졌다. 그리고 수세후의 최종 분말시료중에 잔류하는 Ca 및 O 2 량을 ICP발광분석 및 산소분석기에 의해 분석한 결과, 각각의 함유량은 0.17 및 0.42wt%정도가 검출되었다.

This study was carried out to obtain a basic data on the production of the Nd-Fe-B system rare earth anisotropic bonded magnet by R-D & HDDR process. The reduction reaction of Nd 2 O 3 by metallic Ca and the diffusion reaction of Nd into Fe-B alloy powder were investigated for the production the Nd-Fe-B alloy powder. We concluded that a proper quantity of metallic Ca was about 1.3 times of theoretical equivalent from the yields of Nd and B after the R-D reaction at 100 0 ? C for 1h. In the XRD analysis the diffusion reaction of Nd into the center of Fe-B alloy powder for the completed homogenization was required through about 45min at 110 0 ? C for the R-D reaction, and also the maximum efficiency on the yield of Nd was obtained with such a condition. Residual Ca and oxygen contents of the final powder sample after washing were detected in 0.17wt% and 0.42wt% by ICP and oxygen analyzer, respectively.

Keywords:reduction and diffusion process . hydrogenation . disproportiontion;desorption and recombination;transition metal;rare earth;metal calcium;neodymium oxide

[References]

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Qi G, Hino M, Yazawa Y, Materials Trans., 31(6), 463 (1990)
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김현철, 전동민, 노재철, 서수정, 대한금속학회 학술발표강연회발표요지, 236 (1996)
송창빈, 조통래, 한국재료학회지, 8(8) (1998)
김근용, 조선미, 이준형, 강병민, 김용복, 송창빈, 한국재료학회춘계학술강연회, E-12, 94 (1999)
Massalski TB : Binary Alloy Phase Diagrams, ASM, Metals Park, Ohio. Vol.1, p.467 for B-Ca System (1986) (1986)

[Related Articles]

[1] 工業材料 : 日刊工業新聞社, 10, 1996 (1996)

[2] Cech RE, : USP 3, 748, 193, granted for general Electric Co., 24, 7, 1973 (1973)

[3] Li D, Liu JL, Xu ED, : Paper No.X-1, Presented at the 5th International Workshop on Rare Earth-Cobalt Permanent Magnets and their Application, Roanoke, Virginia, U.S.A., 571-581, (1981) (1981)

[4] Herget C, : Proc. 8th International Workshop on Rare Earth Permaenet Magnets and their Applications, 407-422, Dayton, USA, (1985) (1985)

[5] 昌彬, 小川修 : 資源 . 素材學會誌, Vol.106, No.12, 761-767, (1990) (1990)

[6] 田邊晃生;務中達也;朝木善次郞 : 資源 · 素材學會誌, Vol.106, No.14, 867-872, (1990) (1990)

[7] Qi G, Hino M, Yazawa Y, Materials Trans., 31(6), 463 (1990)

[8] Tanabe T, Hirose S, Asaki Z : Proc. Int. Sympo. on Processing of Rare metals, 307-310, Kokura, Japan

[9] 宋昌彬, 小川修 : 資源 . 素材學會平成3年度春季大會講演槪要集, P.265, (1991) (1991)

[10] 田邊晃生 . 務中達也 . 朝木善次郞 : 資源 . 素材學會誌, Vol.108, No.2, 95-101, (1992) (1992)

[11] 安田淸隆 . 李自强. 析垣乙未生 : 資源 . 素材學會誌, Vol.108, No.2, 103-109, (1992) (1992)

[12] 宋昌彬 . 小川修 : 資源 . 素材學會誌, Vol.108, No.5, 407-411, (1992) (1992)

[13] Liu TY, Chang WC, Chen CJ, Chu TY, Wu CD, IEEE Trans. Magn., 28(5), 2593 (1992)

[14] 宋昌彬 . 小川修 : 資源 . 素材學會誌, Vol.110, No.14, 1145-1150, (1994) (1994)

[15] 김현철, 전동민, 노재철, 서수정, 대한금속학회 학술발표강연회발표요지, 236 (1996)

[16] 송창빈, 조통래, 한국재료학회지, 8(8) (1998)

[17] 김근용, 조선미, 이준형, 강병민, 김용복, 송창빈, 한국재료학회춘계학술강연회, E-12, 94 (1999)

[18] Massalski TB : Binary Alloy Phase Diagrams, ASM, Metals Park, Ohio. Vol.1, p.467 for B-Ca System (1986) (1986)