Investigation of Optimized Process Parameters on Densification of Samarium Cobalt 2:17 Series (SM2CO17) Magnets

International Journal of Electromagnetic ( IJEL ),Vol 2, No 1
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INVESTIGATION OF OPTIMIZED PROCESS
PARAMETERS ON DENSIFICATION OF
SAMARIUM COBALT 2:17 SERIES (SM2CO17)
MAGNETS
Alireza Taherizadeh1
, Sirus. Javadpour1
and Habibollah Alikhani2
1
School of Materials Science and Engineering, Shiraz University, Shiraz, Iran
2
School of Material Science and Engineering, Sahand University of Technology. Iran
ABSTRACT
Samarium Cobalt 2:17 series (Sm2Co17) magnet is prepared by powder metallurgy technique. Different
parameters for sintering and heat treatment process such as sintering time, temperature, furnace
atmosphere and heating rate were tested in order to achieve the highest density for Samarium Cobalt 2:17
series that could be obtained. To analyze and evaluate the microstructure and particle size of fabricated
magnets, scanning electron microscopy (SEM) and X-ray diffraction (XRD) tests were used. Results show
that sintering temperatures and furnace atmosphere are among the most important parameters that
affecting on the density of the samples and consequently the magnetic properties. It is showed that the
highest density of 7.98 g/cm3
(%95 of theoretical density) has been obtained from initial particles with the
size of 3 to 6 µm and sintering temperature of 11950
C with a rate of 17˚C/min for 1 hr in vacuum condition.
KEYWORDS
Samarium Cobalt, rare earth permanent magnet, powder metallurgy, heat treatment.
1. INTRODUCTION
Samarium Cobalt (Sm2Co17) magnets are ideal materials for applications such as microwave
tubes, sensors and servo motors because of their high magnetic properties, thermal stability and
appropriate corrosion resistance. Among all the rare earth permanent magnets, Samarium Cobalt
2:17 series have the highest Curie temperature and the maximum value of saturation
magnetization at high temperatures [1-8]. Samarium Cobalt magnets are usually manufactured by
powder metallurgy technique. They are brittle and show a high thermal and corrosion resistance
[10-13]. They are also relatively expensive because of the rarity of the elements in their
composition. Manufacturing process of Samarium Cobalt by powder metallurgy is as following:
Preparing initial alloy, powder milling, mixing powder, pressing and magnetic orientation,
sintering and homogenization process, heat treatment, machining operation and finally
magnetization [9,10,14,15]. Adding Iron to a limit extent to this composition by replacing Cobalt
atoms increases the maximum energy BH)max, magnetic saturation (Ms) and magnetic remanence
(Br), and it is because of Iron atoms have higher magnetic moments than the Cobalt atoms.
However, if the limit is exceeded, magnetic coercivity would be decreased. The Curie
temperature reduction is one of the problems that happen when Iron is added to the main
composition [18-23]. Copper in the composition makes it more difficult for domain walls to move
thus increases the magnetic saturation. Copper also decreases the eutectic temperature of the
composition [10,24,25]. Adding Zirconium increases anisotropy and magnetic coercivity,
however adding too much will also reduce the magnetic properties [26,27].

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Grain size and dislocation density are two important microstructural factors which affect the
magnetic properties. It has been proved experimentally that magnetic coercivity has a direct
relation with 0.5
(where is dislocation density) [28,29]. However, when the grain size is small,
grain boundaries increase and it greatly improves coercivity due to the fact that grain boundaries
lock magnetic domain walls. Therefore by reducing the size of particles, single domains are
produced and consequently the magnetic coercivity decreases to zero. In this case a
superparamagnetic material is made [30,31].
In Samarium Cobalt 2:17 series the main matrix is the Sm2(CoFe)17, a phase with rhombohedral
unit cell. The matrix increases the magnetic saturation of the system which is surrounded by
Sm(CoFe)5, a Cu-rich phase with hexagonal unit cell. This grain boundary phase increases the
magnetic coercivity of the system which works by domain boundaries pinning mechanism.
Nevertheless, both cellular and lamellar phases with hexagonal unit cell also exist at phase
boundaries. A Zr-rich phase is precipitated on cellular phase. This phase also makes an easy
diffusion path for Copper atoms motion [32-39].
It has been reported that density of a sample has direct proportion to magnetic properties.
Achieving a high dense body requires some factors such as apparent density, particle size, particle
size distribution, particle shape, powder purity and etc [40]. In this paper the effective parameters
such as size of the powders, pressing load, furnace atmosphere, heating rate, sintering time and
temperature and heat treatment cycles on developing a full dense Samarium Cobalt 2:17 series
magnet were investigated. The theoretical density of SmCo magnets have been reported 8.2-8.4
gr/cm3
[42]. In each step of fabrication, the density was measured by Archimedes method
precisely.
2. EXPERIMENTAL
2.1. Analyzing the powders
X-ray fluorescence (XRF) analysis (BRUKER, S4PIONEER, Germany) using Rhodium anode
was used to determine the elements and the weight percent of them which are existing in primary
material. Results are shown in table 1.
Table1. Result of element analysis of initial compound 2:17 series
Phases available in the powders and samples were determined by X- ray diffraction (XRD)
analysis (Bruker, D8 advance, Germany) using Cu Kα radiation (λ=1.5406 Å), equipped with
X'Pert HighScore for data analyzing.

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Size and shape of particles were examined by scanning electron microscopy (SEM; stereo SCAN,
S360 version V03.03, England). The powders were sputtered by gold in order to improve the
quality of SEM micrographs.
2.2. Development of the samples
To make a single domain Samarium Cobalt magnet by powder metallurgy technique, initial size
of powders should be at least less than 10 µm. Ball milling was performed in a planetary mill
having steel balls with diameter 10 and 20 mm. This process was done under the Argon
atmosphere with purity of 99.9% and velocity of 350-450 rpm for 1-2 hours. The powder/ball
weight ratio was set from 1 to 20. Then, samples were formed with a hydraulic uniaxial press
with the pressure of 40 to 60 kg/cm2
in the presence of magnetic field with intensity of 1.5 to 2
Tesla to align the magnetic particles [18,27,32,42-44]. Afterward, samples were encapsulated in
the vacuumed high purity quartz tubes for sintering and homogenization process.
2.3 Sintering, homogenization and heat treatment processes of the samples
Sintering process of Samarium Cobalt 2:17 series magnet took place at a temperature range of
1180-1250 ˚C for different time intervals. After sintering, homogenization process took placed in
order to form the secondary phases with composition of SmCo5 throughout the matrix phase of
the Sm2Co17. The temperature of this process was about 15-25˚C lower than sintering
temperature. Immediately after homogenization process, quenching was performed in a cold
water to prevent the decomposition of secondary phase. Next, Samples were heated up to 850˚C
and kept at this temperature for 8 hours, finally the temperature reduced to 400˚C during 11
hours. These heat treatments were done for precipitating the Cu-rich phase on matrix grain
boundaries enhancing the magnetic remanence [45-47].
3. RESULTS AND DISCUSSION
3.1. Effect of particle size on final density
Size of initial powder and size distributions are two effective factors on densification. The coarse
particles increase porosity size; therefore, density would be decreased. Achieving a single domain
particle is desirable. Since the particles with average size of 5 µm have single domain behavior
[44,50], milling was done on the powders to reach to this particle size. Image Analyzer software
was used to obtain the particle size distribution of the initial powders. The results from SEM
micrographs Fig. 1 and 2 show that most of the green powder size were between 20 to 40 µm.
Milling process was continued to obtain single domain grains with size of 3 to 6 µm [18].
Afterward, pressing was performed in the presence of a magnetic field. It aligned all the particles
that their easy axis had the same direction of applied magnetic field in a specific direction. Then,
sintering was done at 1200˚C with 15ºC/min heating rate and 1 hr soaking time. After pressing
and sintering process density of the samples were measured. Table 2 shows the effects of particle
size on final density of the samples. The results show that the 2:17 series powders, milling for 2
hours at 400 rpm have the best result. SEM micrographs show that the shapes of particles were
changed to spherical during milling process. Spherical shape is more suitable for pressing and has
less and smaller porosities, hence better density would be obtained.

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Table2. Effect of particle size on final density of 2:17 series
Fig1. SEM micrographs of green powder of 2:17 series before milling (magnification:1000)
Fig 2. SEM micrographs of green powder of 2:17 series after two hours milling (magnification:1000)
3.2. Effect of pressing pressure
Pressing pressure is one of the important parameters affecting the green and final density of the
sample. Low pressing pressure decreases the density and high pressing pressure makes problems
such as rapid degradation of the mold, misaligning of the powder and cracking the sample.
Therefore, choosing the optimum pressure is necessary. In this way, different pressures were
tested to determine the optimum pressure and results are showed in table 3 versus final density of
the samples. Results show that the appropriate pressure is 50 kg/cm2
. Pressures above 50 kg/cm2
would make crack in the sample or decreases the final density and pressures less than 50 kg/cm2
may prevent densification in particles and reduce the final density of the samples.

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Table3. Relation of pressing pressure versus final density of 2:17 series
3.3. Effect of furnace atmosphere on final density
Diffusion in solids significantly increases at high temperature; therefore, unwanted phases may be
formed or the formation of desired phases may be prevented. This phenomenon is very important
for Samarium Cobalt magnets due to the high chemical activity of elements in their composition
[9,10]. For this purpose, samples were sintered at 1200˚C for 60 minutes under four different
atmospheric conditions. In the first case, sintering process took place under air atmosphere and
then quenched in cold water. In this case, the measured density was 5.20 g/cm3
. In the next case,
sample was sintered under hydrogen atmosphere. Since there was no possibility of quenching
owing to hydrogen atmosphere, sample was cooled in the furnace. The sample appearance was
good at first but within a few days sample was fully destroyed because of the formation of cracks.
The final density was decreased to 4.63 g/cm3
. In the third case, sample was placed in quartz tube
and sintered under argon atmosphere with purity of 99.999%. In this case, the measured density
was 7.67 g/cm3
. In the last case, sample was placed in quartz tube with vacuum conditions. The
density was increased to 7.95 g/cm3
. Because of the high reactivity of elements in the
composition such as Samarium and Zirconium, in the first case the surface was completely
oxidized. Surface oxidation can be considered as important cause for the coercive force loss of
powders. Due to the presence of open pores or microcracks, the oxidation rate of massive bodies
can be increased. In the second case because of high tendency of rare earth elements to absorb
hydrogen at high temperature and releasing hydrogen from pores during cooling [45], sample was
bloated and eventually destroyed. For the third case sublimation of slight percentage of alloying
elements such as Samarium and accumulation of water vapor in the powders as well as argon gas
at high temperature increases vapor pressure in quartz tube so that high pressure gases penetrated
into the pores of sample and prevent fully densification. Therefore, the vacuum is the best choice
for high temperature process.
3.4. Effect of heating rate on final density
Thermal shock, thermal expansion and outgassing process mainly have been discussed elsewhere,
when studying heating rate of Samarium Cobalt magnet [44]. Apart from these parameters, grain
growth with increasing time and temperature are two other important issues. In permanent
magnets based on rare earth elements which magnetic properties are based on domain walls
pinning mechanism, grain growth should be prevented through reducing time and temperature of
sintering process [51]. In order to obtain appropriate heating rate, the thermal process of
Samarium Cobalt 2:17 series was conducted in three different conditions. The temperature of the
samples A, B and C was raised from room temperature to 1200˚C in 190, 130 and 70 minutes
respectively. They were kept at this temperature for 1 hour. Figure 3 showed that the samples can
be reached to appropriate density by rapid heating. If heating rate would be too slow, desired
density could not be obtained. Higher heating rate would prevent Samarium sublimation and
decreases inner pressure of the tube so that makes it possible to reach higher density.

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Fig3. Effect of heating rate on final density of Samarium Cobalt 2:17 series, sample A, B and C
3.5. Effect of sintering temperature on final density
Sintering helps to homogenize the microstructure and increase the densification of samples.
Sintering time and temperature have many effects on grain size [51]. In order to analyze effects of
sintering temperature on final density and also choosing the most appropriate temperature,
samples were sintered at 5 different temperatures between 1180 to 1250˚C for 1 hour at same
conditions.
In the first case, sintering process took place by heating the sample to 1250˚C. The sample lost its
shape totally and the density was 7.05 g/cm3
. In the second case, sintering took place by heating
the sample to 1220˚C. The sample deformed from its original shape and the density was 7.75
g/cm3
. In the next case, sintering took place by heating the sample to 1205˚C. In addition, only
the edge of sample lost their original shape and the density measured 7.90 g/cm3
. Afterward, for
the next one, sintering took place by heating the sample to 1195˚C. The sample retained its
original shape and the density increased to 7.97 g/cm3
. Finally, for the last case, sintering took
place by heating the sample to 1180˚ C. In this sense, the sample also retained its original shape
but the density decreased to 7.91 g/cm3
. One can see from fig. 4 that in low sintering
temperatures, high density has been obtained. By increasing sintering time and temperature, grain
size increases more than the single domain size. The sample which sintered at 1195˚C had higher
density than all samples, so it can be concluded that the best sintering temperature for Samarium
Cobalt 2:17 series is 1195˚C.
Fig4. Final density of Samarium Cobalt 2:17 series based on sintering temperature

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3.6. Effect of homogenization temperature on final density
The purpose of homogenization is to produce highly supersaturated single phase alloy. The
solution temperature has a main effect on coercivity of Samarium Cobalt magnets. The
relationship between diffusion coefficient D and temperature T can be described as in Eq.(1):
D=D0e-Q/RT
(1)
Where, D0 is a constant, Q is activation energy and R is gas constant. With the same solution
time, higher T leads to higher D, which is beneficial for the solution of different phases and is
easier to obtain a highly supersaturated single phase.
Homogenization process took place in order to make a fully Sm2(CoFe)17 matrix in the sample.
Homogenization temperature is usually 15 to 25˚C lower than sintering temperature [45]. To
study the effect of homogenization temperature on final density and choosing the best
temperature, samples were sintered at 1195˚C for 1hour and kept at five different homogenizing
temperatures between 1165 to 1180˚C for another 1 hour.
First sample, homogenized at 1185˚C. In this case density was 7.80 g/cm3
. For the second one,
sample homogenized at 1180˚C and the density reached to 7.80 g/cm3
. In the next case, sample
was homogenized at 1175˚C and the density increased to 7.93 g/cm3
. In the fourth case, sample
homogenized at 1170˚C and the density decreased to 7.83 g/cm3
. Finally, the last sample was
homogenized at 1165˚C and the density reached to its minimum at 7.76 g/cm3
. Consequently, a
temperature of 1175˚C was found to be the best homogenizing temperature.
3.7. Heat treatments
Sintering and heat treatment are the most important steps in the production of sintered Samarium
Cobalt magnets. The aim of sintering is, on one side, achievement of a high density without
opened connecting pores whereas, on the other hand, the growth of crystal grains should be
avoided. Open pores cause intrinsic oxidation and, therefore, reduce the magnetic remanence. The
growth of crystal grains directly reduces the coercivity, making the nucleation of reversed
domains easier. The heat treatment after sintering must be chosen to correspond to the chemical
composition of the alloy, and its purpose is to obtain a microstructure that improves coercivity.
Magnetic remanence at the end of homogenization process reaches to its required value. In
addition, heat treatments should be done in order to increase the coercivity of the samples. In fact
before quenching the solid is composed of single 2:17 phase which has low value of coercivity
and energy product, so that a heat treatment of 850˚C for 8 hours was employed on the quenched
sample to form a multiphase solid with cellular microstructure around the grain boundaries [46].
Afterward, the temperature reduced to 400˚C for 11 hours. Slow cooling may form some deposits
around domain walls [47]. Figure 5 represents the whole procedure for heat treatment of
Samarium Cobalt 2:17 series magnets.
Fig5. Typical temperature profile for sintering and heat treatment for Sm2Co17 [27].

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3.8. Phase analysis of Samarium Cobalt 2:17 series
Figure 6 represented the result of XRD patterns of Samarium Cobalt 2:17 series initial
composition. It shows that SmCo5 and Sm2Co17 phases exist in the powders.
Fig6. XRD analysis of initial composition of Samarium Cobalt 2:17 series magnet
Sintering of Samarium Cobalt permanent magnets was applied for integrating and densification of
green bodies. After sintering, homogenization is needed to uniform the microstructure. As can be
seen in fig. 7, after sintering and homogenization process represents that Sm2Co17 phase has
formed in samples [45]. Fig 8 represents that after heat treating in addition to Sm2Co17 phase,
SmCo5 phase also has been formed. The combination of these two phases causes the pinning
mechanism of magnetic domain walls and increases the magnetic properties [52].
Fig7. X-ray diffraction analysis of Samarium Cobalt 2:17 series after sintering at 1190˚C and
homogenization at 1175˚ C before heat treatment

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Fig8. XRD analysis of Samarium Cobalt 2:17 series after heat treatments at 850˚C for 8 hours and reducing
to 400˚ C for 11 hours. SmCo5 phase has been formed in Sm2Co17 phase
Finally for magnetizing the samples, an external magnetic field which is 2 to 3 times stronger
than the residual field with a magnitude of 2.5 to 3.5 Tesla was applied throughout the ring.
Hystograph model MESSTECHIK BROCKAUS was used to measure the magnetic properties of
sintered samples. Fig 9 is hysteresis curve for a Samarium Cobalt 2:17 series which is first
sintered at 1190˚C and homogenization at 1175˚ C and then heat treated at 850˚C for 8 hours and
finally its temperature is reduced to 400˚ C for 11 hours.
Fig9. Hysteresis curve for a sintered Samarium Cobalt 2:17 series after heat treatments at 850˚C for 8 hours
and reducing to 400˚ C for 11 hours.
4. CONCLUSIONS
The density of Sm2(Co0.67Fe0.23Cu0.07Zr0.03)17 compound varied by controlling the grain size and
the highest density was obtained by using a 3-6 µm green powder. SEM micrographs showed that
the shapes of particles were changed to spherical which was found to be more suitable for
obtaining high density. The highest density achieved by sintering at 1195˚C with a rate of
17˚C/min under the vacuum conditions. Meanwhile, the sample reached to the appropriate density

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by rapid heating at the shortest time. Consequently, a temperature of 1175˚C was found to be the
best homogenizing temperature. Heat treatment process in 850˚C kept for 8 hours to form 1:5
phase at grain boundaries and then reduced to 400˚C in the course of 11 hours was done to
increase the coercivity. Deposits around magnetic domain walls were formed by applying slow
cooling rates.
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AUTHORS
Sirus Javadpour is a Professor at Materials Science and Engineering Department,
Shiraz University, Iran. He received the Ph.D. in Maryland University, USA. His
current research interests include development of fibrous and nanocomposites, bio-
materials, electro-ceramics and the advanced materials.
Alireza Taherizadeh has received his M.Sc. degree in Materials Science and
Engineering (Ceramics and Electroceramics) from Shiraz University, where he
completed his thesis entitled “Manufacturing, investigation and improvement on
magnetic properties of Sm2Co17 and SmCo5 magnets” which was mainly carried
out in the Electroceramics lab at the Department of Materials Engineering, under the
supervision of Prof. Dr. Sirus Javadpour. Since his master's graduation in February
2013, He has been employed as full-time research assistant in Steel Institute of
Isfahan University of Technology, Isfahan, Iran. ‘His field of expertise includes
synthesis and characterization of materials and nanomaterials by novel methods,
ceramics, composites and magnetic materials.

13
Habibollah Alikhani has received his MSc. Degree degree in Nanotechnology from
Sahand University of Technology. He completed his thesis entitled “The effect of
surface roughness of Inconel 738 superalloy substrate on nano- structured yttria-
stabilized zirconia coating by electrophoretic deposition (EPD)”. He has a good
corporation with Dr Javadpour and his research group. His interesting fields
includes: electromagnetic materials, Zirconia ceramics, nanoparticle and nano-
fabrication.

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