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    1 s2.0 0304885395011137 Main

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    Ayush Verma
    High coercivity N d - f e - b powder with Hcj up to 14 kOe was achieved after optimisation of the two latest phases of the HDDR process. The best conditions are defined by the couples 60 min-720degC and 20 min-860degC for the two main operations, respectively.

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    1 s2.0 0304885395011137 Main

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    Ayush Verma
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    High coercivity N d - f e - b powder with Hcj up to 14 kOe was achieved after optimisation of the two latest phases of the HDDR process. The best conditions are defined by the couples 60 min-720degC and 20 min-860degC for the two main operations, respectively.

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    High coercivity N d - f e - b powder with Hcj up to 14 kOe was achieved after optimisation of the two latest phases of the HDDR process. The best conditions are defined by the couples 60 min-720degC and 20 min-860degC for the two main operations, respectively.

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    34 views2 pages

    1 s2.0 0304885395011137 Main

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    Ayush Verma
    High coercivity N d - f e - b powder with Hcj up to 14 kOe was achieved after optimisation of the two latest phases of the HDDR process. The best conditions are defined by the couples 60 min-720degC and 20 min-860degC for the two main operations, respectively.

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    cZz:

    ELSEVIER

    Journal of Magnetism and Magnetic Materials 157/158 (1996) 57-58

    journal Of i ~ . magnetism J I M and magnetic


    materials

    Anisotropic and coercive HDDR Nd-Fe-B powders prepared under magnetic field
    S. Liesert a p. de Rango a,* J.L. Soubeyroux R. Perrier de la Bfithie b
    a

    D. Fruchart a

    " Laboratoire de Cristallographie du CNRS, BP 166, 38042 Grenoble Cedex 9, France b EPM-MATFORMAG, CNRS, BP I66, 38042 Grenoble Cedex 9, France

    Abstract High coercivity N d - F e - B powder with Hcj up to 14 kOe was achieved after optimisation of the two latest phases of the Hydrogen-Disproportionation-Desorption-Recrystallisation (HDDR) process. The progression of the solid gas reaction ( N d - F e - B / H 2) as analysed by a thermomagnetic balance, has given the possibility to monitor the disproportionation reaction. The first step was to define favourable conditions to develop a controlled but uncompleted disproportionation reaction. The second step was the application of an high magnetic field o f / x o H = 7 T during the DR process. Anisotropic N d - F e - B powder was crystallised.
    Keywords: Rare earth magnets; Hydrides; Texture

    A highly coercive isotropic powder was prepared by the HDDR method from a starting material of composition Nd32.1Dyl.6Fe64.TNb0.6B1.0 . Optimisation of the disproportionation (HD) and the recrystallisation (DR) of the HDDR process was achieved after a large series of experiments, where the disproportion temperature, the recrystaltisation time and temperature were adjusted respectively [1]. The best conditions are defined by the couples 60 min-720C and 20 min-860C for the two main operations, respectively. For the latter, high vacuum conditions were required. A coercive field Hcj of 14 kOe has been achieved, but the powder was still isotropic. The control of the texture by solidification under an high magnetic field, already successfully applied to the high Tc superconductor YBa2Cu30 7 [2], puts into evidence new possibilities for the development of anisotropic magnetic powders. Contrarily to the reported 'chemical' route, where addition of elements (Zr, Ga,...) was used to give rise to an anisotropic crystallisation [3], we propose to develop a 'physical' route in order to induce a high degree of texturation in the sample. A dedicated furnace was designed and developed specially to apply either a high magnetic field (up to 8 T) or a high field gradient during the thermal process [4]. The temperature range from RT to

    * Corresponding author. Fax: +33-7688-1038; rango@labs.polycnrs-gre.fr.

    email: de-

    1000C, gas pressure and vacuum level are strictly controlled by dedicated sensors. The cryogenic device used to apply a magnetic field is described in Ref. [5]. In a first series of experiments, we have applied a magnetic field or field gradient during the previously optimised steps of the HDDR process. No significant anisotropic growth was developed at such high temperature. In fact, in the paramagnetic state, the magnetocrystalline anisotropy is either too weak or has lost its axial character. No texturation can be achieved. In the second series of experiments, we have applied a high magnetic field on Nd2FelgB nuclei. Orientation of these fine crystallites was effective when the sample was cooled down to the Curie temperature. Simultaneously, we have built a new type of magnetic torque, allowing us to control and analyse the magnetic characteristics of the sample under reaction in an autoclave under gas flow or gas pressure. A best control of the disproportionation reaction where the characteristics of Nd2Fe14 B, Nd2Fe14BH x, a-Fe .... are clearly observed, is made possible. Fig. 1 gives an example of a diagram recorded during a disproportionation process. The sample was flowed under a hydrogen atmosphere at normal pressure and the temperature was monitored up to 630C. During the temperature increase (5C/rain, step 1 to 3) one can observe a slight increase in magnetisation (200C) corresponding to the hydrogenation of Nd2Fe14B grains, the Curie temperatures of nonhydrogenated (minor part) and hydrogenated

    0304-8853/96/$15.00 Copyright 1996 Elsevier Science B.V. All rights reserved.


    SSDI 0304-8853(95)011 13-7

    58
    i

    S. Liesert et al. / Journal of Magnetism and Magnetic Materials 157/158 (1996) 57-58
    t i i i

    150

    0 6 ~ - 2 ~ 5 .~ -10 := -20 -30 -40 I 100 I 200 I 300


    -

    10050 :[ ~
    v 12 h 4

    2 _ ---7perpendicularI
    l

    "

    '

    N "
    400 500 600

    50

    3
    700

    -lo0

    -150

    T (oc) Fig. 1. Variation of the magnetisation versus temperature during an incomplete disproportionation reaction. (major part = step 2) N d - F e - B are clearly perceived. Up to 400C some increase in magnetisation corresponds to the beginning of the disproportionation process of intergranular matter. This phenomenon is amplified at T > 550C, and it takes place mainly during a plateau temperature at Tp = 630C (step 3 to 4). A complete disproportionation is achieved when the time elapsed at Tp is long enough. However, if the sample is cooled down before the end of this process (step 4 to 6), the resulting sample is a mixture of disproportionated and non-disproportionated particles. Therefore an increase in magnetisation corresponding to the Curie temperature of Nd2Fel4B slightly hydrogenated can again be observed (step 5). In Fig. 2 we
    120
    lOO 80

    -20 -15 -10

    -5

    0 5 H(kOe)

    115

    20

    Fig. 3. Hysteresis loops measured at 300 K, along the magnetic field applied to orient the powder parallel and perpendicular to this direction.

    i.

    show the rate of disproportionation versus temperature (Tp) for a one hour and a five hour temperature plateau. Hence, we have adapted these parameters on finely divided monocrystalline N d - F e - B powders in order to maintain very small and numerous particles, yet exhibiting a good crystallinity. Such a material was processed under a 7 T magnetic field in our specially dedicated furnace. The rest of the nondisproportionated N d - F e - B fine nuclei was oriented and then a recrystallisation process was applied. Fig. 3 shows the parallel and perpendicular magnetisation curves recorded versus the applied field. It is clear that a high degree of anisotropy was achieved. Crystallographic alignment has been confirmed by X-ray diffraction analysis performed on two perpendicular surfaces. Today, the different steps of this new 'physical' route for the synthesis of texturing anisotropic N d - F e - B powders are under optimisation.
    References

    6o
    40
    20

    ,,,,I,,,,I,,,,
    100 200 300

    ,,,,I,,,,I,,,,[,r,

    T(oc)

    400

    500

    600

    700

    Fig. 2. Disproportionation rate versus temperature during one hour and five hour temperature plateaus. The rate has been evaluated by comparing the height of the transition at To before and after disproportionation.

    [1] D. Fruchart, S. Miraglia, L. Pontonnier, P. de Rango, J.L. Soubeyroux, R. Fruchart, P. Mollard and R. Perrier de la Bgthie, Proc. 1lth Workshop on Rare Earth Magnets and their Applications, 11-14 September 1994, p. 511. [2] P. de Rango, M. Lees, P. Lejay, A. Sulpice, R. Tournier, M. Ingold, P. Germi and M. Pernet, Nature 349 (1991) 770. [3] R. Nakayama and T. Takeshita, J. Alloys Comp. 193 (1993) 259. [4] S. Rakotoarison, Thesis, University of Grenoble:(1995). [5] P. de Rango, Thesis, University of Grenoble (1992).

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