• 한국분말재료학회지
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• 제23권6호
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• pp.447-452
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• 2016

Neodymium-iron-boron (Nd-Fe-B) sintered magnets have excellent magnetic properties such as the remanence, coercive force, and the maximum energy product compared to other hard magnetic materials. The coercive force of Nd-Fe-B sintered magnets is improved by the addition of heavy rare earth elements such as dysprosium and terbium instead of neodymium. Then, the magnetocrystalline anisotropy of Nd-Fe-B sintered magnets increases. However, additional elements have increased the production cost of Nd-Fe-B sintered magnets. Hence, a study on the control of the microstructure of Nd-Fe-B magnets is being conducted. As the coercive force of magnets improves, the grain size of the $Nd_2Fe_{14}B$ grain is close to 300 nm because they are nucleation-type magnets. In this study, fine particles of Nd-Fe-B are prepared with various grinding energies in the pulverization process used for preparing sintered magnets, and the microstructure and magnetic properties of the magnets are investigated.

• 한국분말재료학회지
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• 제20권5호
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• pp.359-365
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• 2013

In this study, we fabricated $Nd_2Fe_{14}B$ hard magnetic powders with various sizes via spray drying combined with reduction-diffusion process. Spray drying is widely used to produce nearly spherical particles that are relatively homogeneous. Thus, the precursor particles were prepared by spray drying using the aqueous solution containing Nd salts, Fe salts and boric acid with the target stoichiometric composition of $Nd_2Fe_{14}B$. The mean particle sizes of the spray-dried powders are in the range from one to seven micrometer, which are adjusted by controlling the concentrations of precursor solutions. After debinding the as-prepared precursor particles, ball milling was also conducted to control the particle sizes of Nd-Fe-B oxide powders. The resulting particles with different sizes were subjected to subsequent treatments including hydrogen reduction, Ca reduction and washing for CaO removal. The size effect of Nd-Fe-B oxide particles on the formation of $Nd_2Fe_{14}B$ phase and magnetic properties was investigated.

• Journal of Magnetics
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• 제17권3호
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• pp.185-189
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• 2012

The coercivity of near single domain size $Nd_2Fe_{14}B$-type particles prepared by ball milling of HDDR-treated $Nd_{12.5}Fe_{80.6}B_{6.4}Ga_{0.3}Nb_{0.2}$ alloy was investigated. The feasibility of a surface nitrogenation for improving the coercivity stability of the fine $Nd_2Fe_{14}B$-type particles was also studied. The near single domain size $Nd_2Fe_{14}B$-type particles had a high coercivity of over 9 kOe. However, the coercivity radically deteriorated as the temperature increased in air (< 2 kOe at $200^{\circ}C$). This coercivity reduction was attributed to the soft magnetic phases, ${\alpha}$-Fe and $Fe_3B$, which formed on the surface of the fine particle due to oxidation. Surface nitrogenation of the fine particles significantly improved the stability of their coercivity. The improvement in coercivity stability was attributed to the formation of a thin nitrogenated layer on the surface of the fine $Nd_2Fe_{14}B$-type particles, which enhanced the anisotropy field and gave improved resistance to oxidation (dissociation).

• Journal of Magnetics
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• 제10권4호
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• pp.152-156
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• 2005

Effects of the disproportionating hydrogen pressure and alloy composition on the texture in the HDDR-treated Nd-Fe-B particles were examined using the $Nd_{12.6}Fe_{81.4}B_6$ and $Nd_{12.6}Fe_{68.7}B_6Co_{11.0}Ga_{1.0}Zr_{0.l}$ alloys. Disproportionation kinetics of the $Nd_2Fe_{14}B$ phase in the Nd-Fe-B alloy was retarded significantly by the addition of Co, Ga and Zr. The retarded disproportionation kinetics of the $Nd_2Fe_{14}B$ phase ensured a wider processing win­dow in terms of disproportionating hydrogen pressure for achieving a texture in the HDDR-treated Nd-Fe-B alloy particles.

• Journal of Magnetics
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• 제13권3호
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• pp.102-105
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• 2008

This study examined the feasibility of the combining HDDR-process (hydrogenation, disproportionation, desorption and recombination) with mechanical milling to prepare single domain $Nd_2Fe_{14}B$ particles from a Nd-Fe-B alloy ingot. The $Nd_{15}Fe_{77}B_8$ alloy was HDDR-treated and then subjected to a roller-milling. In the HDDR-treated $Nd_{15}Fe_{77}B_8$ alloy, very small $Nd_2Fe_{14}B$ grains comparable to their critical single domain size(0.3 ${\mu}m$) were observed. These fine individual grains were separated successfully along the grain boundaries by a roller-milling. The separated $Nd_2Fe_{14}B$ grains were found to be single domain particles. These results suggest that single domain particles of the $Nd_2Fe_{14}B$ phase can be prepared from a Nd-Fe-B ingot alloy by combining a HDDR-process with mechanical milling.

• Journal of Magnetics
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• 제20권1호
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• pp.21-25
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• 2015

Fine Nd-Fe-B-type particles were prepared by ball milling of different types of Nd-Fe-B precursor materials, such as die-upset magnet, HDDR-treated material, and sintered magnets. Coercivity dependence on the grain and particle size of the powder was investigated. Coercivity of the milled particles was reduced as the particle size decreased, and the extent of coercivity loss was dependent upon the precursor material. Coercivity loss in the finely milled particles was attributed to the surface oxidation. The extent of coercivity loss in the fine particles was closely linked to grain size of the precursor materials. Coercivity loss was more profound for the fine particles with larger grain size. Contrary to the fine particles from the sintered magnets with larger grain size the fine particles (~10 um) from the die-upset magnet and HDDR-treated material with much finer grain size still retained high coercivity (> 10 kOe for die-upset magnet, > 4 kOe for HDDR-treated material).

• 한국자기학회지
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• 제12권2호
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• pp.57-63
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• 2002

Nd-Fe-B계 소결자석의 특성을 향상시키기 위해서는 Nd-Fe-B계 합금의 조성 및 제조공정을 조절하여 자성분말의 입도 및 입도분포, 강자성상인 N $d_2$F $e_{14}$B상의 분율, 자성분말의 배향도, 산소 함량, grain size 등과 같은 factor들을 최적화 하여야 한다. 본 연구에서는 실험실 규모로 Nd-Fe-B계 합금 조성 및 공정 조절을 통하여 Nd-Fe-B계 소결자석을 제조하는 연구를 수행하였으며, 분쇄매체 분쇄시간 및 ball size에 따른 Nd-Fe-B계 소결자석의 자기적특성을 분석하여 최적의 분쇄조건을 조사하였다. 또한 분쇄공정 중 FeGa합금을 첨가하여 잔류자속밀도의 감소없이 Nd-Fe-B계 소결자석의 보자력을 향상시킬 수 있었다. 이와 같은 분쇄 조건의 연구, FeGa 합금에 의한 보자력 향상, 건식분쇄 방법 및 powder blending 공정을 적용하여 잔류자속밀도( $B_{r}$,) : 14.4kG, 보자력($_{i}$ $H_{c}$) : 9.4kOe, 최대자기에너지적((BH)$_{\max}$) : 47 MGOe의 자기적 특성을 갖는 Nd-Fe-B계 소결자석을 제조하였다.

• 한국자기학회지
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• 제11권1호
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• pp.8-13
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• 2001

Axial pressing process를 이용하여 31RE-68TM-1B(RE : 희토류원소, TM: 3d천이금속) 조성을 갖는 소결자석을 제조함에 있어서 Casting process와 Lubricant 변화에 따른 잔류자속밀도 변화를 조사하였다. 출발합금 제조방법으로서 Strip casting process는 $\alpha$-Fe 편석없이 미세하고, 균일한 microstructure를 얻기에 용이한 잇점이 있었으며, Jet mill 이후 균일한 입도의 분말을 얻을 수 있었다. 또한, Jet mill 전후에 적절한 분말 혹은 무수알콜과 같은 Lubricant를 첨가함으로써 잔류자속밀도를 향상시킬 수 있었다. 본 실험에서는 Strip casting 및 분말 Lubrican인 Zn-st(Zinc stearate)에 첨가에 의한 분말입도분포 개선효과와 무수알콜에 의한 배향율 향상효과를 접목하여 잔류자속밀도, 보자력 및 최대자기에너지적이 각각 13.1 kG, 13.5 kOe 및 39.5 MGOe인 경자기특성이 얻어졌다.

• 한국자기학회지
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• 제25권4호
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• pp.111-116
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• 2015

Nd-Fe-B계 합금에 대한 HDDR(hydrogenation : 수소화 - disproportionation : 분해 - desorption : 탈가스 - recombination : 재결합) 공정에서 실질적인 어려움은 제조된 분말의 자기적 특성, 특히 보자력의 재현성이 대단히 낮다는 점이다. 본 연구에서는 수소파쇄 시 입자 내에 미세균열을 최대한 도입하고 이것이 HDDR 처리한 $Nd_{12.5}Fe_{80.6}B_{6.4}Ga_{0.3}Nb_{0.2}$ 합금 분말의 보자력의 재현성에 미치는 영향을 조사하였다. 수소파쇄된 분말 입자 내에 미세균열을 최대한 많이 도입하기 위하여 분해반응 전 고온에서 충분히 수소방출 처리를 실시하였다. 추가 수소방출처리를 실시하고 HDDR 처리하여 제조한 분말은 보자력 및 그 재현성이 향상되었다. 추가 수소방출로 결정격자가 수축하면서 입자 내에 더욱 더 많은 미세균열이 도입되고, 이로 인하여 분말의 HDDR 반응 시 입자 전체에 걸쳐서 HDDR 반응이 균일하게 진행 되어 보자력의 재현성이 향상되었다.

• Journal of Magnetics
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• 제20권2호
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• pp.97-102
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• 2015

The waste of sintered Nd-Fe-B magnets was recycled using the method of dopingPrNd nanoparticles. The effect of PrNd nanoparticle doping on the magnetic properties of the regenerated magnets has been studied. As the content of the PrNd nanoparticles increases, the coercivity increases monotonically, whereas both the remanence and the maximum energy products reach the maximum values for 4 wt% PrNd doping. Microstructural observation reveals that the appropriate addition of PrNd nanoparticles improves the magnetic properties and refines the grain. Domain investigation shows that the self-pinning effect of the rare earth (Re)-rich phase is enhanced by PrNd nano-particle doping. Compared to the magnet with 4 wt% PrNd alloy prepared using the dual-alloy method, the regenerated magnet doped with the same number of PrNd nanoparticles exhibits better magnetic properties and a more homogeneous microstructure. Therefore, it is concluded that PrNd nanoparticle doping is an efficient method for recycling the leftover scraps of Nd-Fe-B magnets.