Journal of Magnetism and Magnetic Materials 157/158 (1996) 45-46

journal of
magnetism
and
magnetic
~li materials
ELSEVIER

Irreversible losses of magnetisation in F e - N d - B type magnets

M. Leonowicz a, *, W. K a s z u w a r a a, S. Wojciechowski a, H.A. Davies b
a Faculty of Materials Science and Engineering, Warsaw University of Technology, Narbutta 85, 02-524 Warsaw, Poland
b Department of Engineering Materials, University of Sheffield, Sheffield, UK

Abstract
Irreversible losses of magnetisation for magnets, based on F e - N d - B alloys processed by melt spinning, HDDR, and
sintering and on F e - N d - C - B ingot material, have been evaluated. Magnets having the same intrinsic properties and
coercivity but different compositions and processed by different routes exhibit the same losses. Thus, optimization of the
alloy composition, phase constitution and microstructure of the magnets, leading to high coercivity, appears to be crucial for
minimisation of the irreversible losses of magnetisation.

Keywords: Irreversible losses; Nd-Fe-B magnets

One of the most important limitations in application of Mir are the remanent magnetisations immediately after
F e - N d - B magnets is their behaviour at elevated tempera- magnetisation to saturation and after thermal ageing, re-
tures. In addition to the reversible changes, irreversible spectively.
losses of magnetisation (ILM) occur in the course of The variation of the ILM with time for hot pressed
ageing. The ILM are due to the fluctuations of thermal isotropic magnets processed f r o m melt-spun ribbon was
energy sufficient to cause irreversible rotation or wall investigated for Fe94_xNdxB 6 ( x = 11-14) alloys having
displacement in small volumes of the material. The range different coercivities. A strong dependence of the ILM on
of the ILM depends on several parameters, such as: coer- coercivity ( j H c) was observed (Fig. 1). The magnets hav-
civity, working point, ageing temperature and Curie tem- ing j H c = 1470 k A / m exhibited only a few percent loss
perature [1-3]. Thus, it is difficult to give a general answer after 1000 h annealing, whereas those having j H c = 300
to the question of ageing behaviour and, rather, compari- k A / m showed ~ 20% losses.
son of different materials under constant test conditions The ILM for the magnets prepared by different process-
should be considered. In this study ageing behaviour is ing routes are shown in Fig. 2. The time dependence of:the
compared and discussed for F e - N d - B type magnets pro- ILM reported for bonded melt spun, melt spun hot pressed,
cessed by different methods and having totally different sintered and HDDR F e - N d - B magnets, and cast F e - N d -
microstructures, compositions and, possibly, coercivity C - B alloys varied for materials having different m i -
mechanisms. crostructures and coercivities. Both F e - N d - B and F e -
The following specimens were prepared: (a) rapidly N d - C - B - t y p e magnets have similar intrinsic magnetic
solidified resin bonded MQ1 magnets; (b) rapidly solidi-
fied hot pressed isotropic Fe94_xNdxB6 ( x = 11-14) mag-
nets; (c) sintered anisotropic Fe77NdlsB8 magnets; (d)
0
HDDR (hydrogenation, disproportionation, desorption and R
t
[]
#
C
t
-
~< * ~ *
recombination) and hot pressed Fe76Nd16B8 magnets; and 10
(e) cast Fe68Nd20C9.sCu2B0. 5 alloys. The cylindrical spec- o
imens of 7 mm diameter and 7 mm long were annealed at 20.
temperatures ranging from room temperature to 200°C for 41 [] 1470 kA/m

1
* 1460 kA/m
times up to 1000 h. The magnetic flux for completely 30- o 7.50kA/m
magnetized specimens was monitored in each case at room ,L 300 kA/m
temperature using a vibrating sample magnetometer. The 40
0.1 100 I000
ILM were expressed by ( M r - M i r ) / M r, where M r and
Ageing "lime [Hours]

Fig. 1. Variation of the ILM with ageing time at 125°C for

* Corresponding author. Email: mkl@inmat.pw.edu.pl; fax: isotropic melt spun and hot pressed magnets Fe94_xNdxB 6 (x =
+ 48-22-484875. 11-14) of different coercivities.

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

SSDI 0 3 0 4 - 8 8 5 3 ( 9 5 ) 0 1 1 2 8 - 5
46 M. Leonowicz et al. / Journal of Magnetism and Magnetic Materials 157/158 (1996) 45-46

/
o 0 ]..
u}
8 o o (~ q o£/
] i
10 10-
.,J
G) zx

20 ~ t ~
,- 3O D mot
o slnt~ed 1080 kA/m z~ cast Fe-Nd-C 728 kA/m
* bonded 7 9 ~ D R - H P - 667 kA/m
40
0.1 I 10 100
Ageing Time ]Hours]
Fig. 2. Variation of the ILM with ageing time at 125°C for
magnets prepared by different processing routes.
properties such as anisotropy field, saturation magnetisa-
tion and Curie temperature which enables the comparison
of their behaviour at elevated temperatures. The differ-
ences in the microstructure and composition are reflected
in the value of coercivity which, irrespective of the mate-
rial, appears to be a decisive parameter which determines
the ILM. These observations are further confirmed and
shown in Fig. 3 where the effect of phase structure on the
1LM is presented. The ILM for the Fe76Nd~6.zBT. 8 mag-
nets having a ternary phase structure (@-Fe14Nd2B , ~7-
NdFe4B 4 and Nd-rich) ( j H c = 560 k A / m ) are greater
than those for Fe74.sNdI8.6B6.sA10.1 magnets containing
only the qb and Nd-rich phases (jH~ = 720 k A / m ) [4].
Elimination of the ~7 phase reduces the number of nucle-
ation sites for reverse domains and thus increases the
coercivity and reduces the ILM. A higher Nd content also
improves the magnetic isolation of the q~ grains.
Finally, in Fig. 4 the ILM for magnets of different type
but having similar coercivities are presented. All these
magnets showed similar losses, approaching 15%, after
annealing at 125°C for 1000 h, emphasising that the key
parameter is the coercivity.
Exposure time 0.5 h
20"
_0 40-
.Q
3e~
20-
* bonded melt spun - 797 kA/m
-~ a melt spun h.p. - 751 kA/m
30-
I " o slntered - 728 kA/m
J zx cast - 728 kA/m
1000
4O
0.1 1 1; 1~ 1~0
Ageing Time [Hours]
Fig. 4. Variation of the ILM with ageing time at 125°C for
magnets prepared by different processing routes and having com-
parable initial (before ageing) coercivities.
No effect of texture on the ILM was found. This
behaviour can be explained on the basis that, in each
crystallite, the magnetisation and its related demagnetizing
field lie parallel to the easy direction giving, for magneti-
cally isolated grains, the same losses, irrespective of tex-
ture.
We conclude that the irreversible losses of magnetisa-
tion result from demagnetization of small volumes of the
material under the influence of the magnet's own demag-
netizing field. Due to the energy fluctuations the mutual
relations between anisotropy and exchange energies alter
and this affects the domain structure and reduces the
magnetisation of the material. The magnets having higher
coercivities have higher resistance to demagnetization. All
the microstructural elements which can stabilize the do-
main structure and retard domain wail propagation are
very effective in reducing the losses. Assuming constant
intrinsic properties (saturation magnetisation, anisotropy
field, Curie temperature) and permeance coefficients, the
coercivity of a magnet is practically the only parameter
controlling the magnitude of the ILM. Thus, the ILM
appear to correlate closely with jHc, irrespective of the
alloy microstructure and apparently of the detailed mecha-
nism of domain reversal.
Acknowledgement: Financial support from the Polish
Committee for Scientific Research (KBN) (grants 3P407
005 05 and D Z / 2 6 3 1 / J P ) and British Council is grate-
fully acknowledged.

~, so- References

80- ~ 2-phase magnet [1] N. Yoshikawa, Y. Kasai, T. Watanabe and S. Shibata, J. Appl.
Phys. 69 (1991) 6049.
100
20 60 100 1~10 180 220 [2] Wei Gong, Qingsheng Li and Lin Yin, J. Appl. Phys. 69
(1991) 5512.
Exposure Temperature [~C]
[3] W. Rodewald and B. Wall, J. Magn. Magn. Mater. 101 (1991)
Fig. 3. Temperature dependence of the ILM for three-phase 338.
Fe76Nd16.2BT.8 and two-phase Fe74.8Ndls.6B6.5A10.1 magnets for [4] G. Schneider, E.-Th. Henig, P.F. Missell and G. Petzow, Z.
a constant exposure time of 0.5 h. Metallk. 81 (1990) 322.