Sei sulla pagina 1di 10

Journal Pre-proofs

Selective laser melting vitrification of amorphous soft magnetic alloys with help
of double-scanning-induced compositional homogeneity

Yeong Gyun Nam, Bonuk Koo, Mise Chang, Sangsun Yang, Jihun Yu, Yong
Ho Park, Jae Won Jeong

PII: S0167-577X(19)31700-8
DOI: https://doi.org/10.1016/j.matlet.2019.127068
Reference: MLBLUE 127068

To appear in: Materials Letters

Received Date: 3 October 2019


Accepted Date: 20 November 2019

Please cite this article as: Y. Gyun Nam, B. Koo, M. Chang, S. Yang, J. Yu, Y. Ho Park, J. Won Jeong, Selective
laser melting vitrification of amorphous soft magnetic alloys with help of double-scanning-induced compositional
homogeneity, Materials Letters (2019), doi: https://doi.org/10.1016/j.matlet.2019.127068

This is a PDF file of an article that has undergone enhancements after acceptance, such as the addition of a cover
page and metadata, and formatting for readability, but it is not yet the definitive version of record. This version will
undergo additional copyediting, typesetting and review before it is published in its final form, but we are providing
this version to give early visibility of the article. Please note that, during the production process, errors may be
discovered which could affect the content, and all legal disclaimers that apply to the journal pertain.

© 2019 Published by Elsevier B.V.


Selective laser melting vitrification of amorphous soft magnetic alloys

with help of double-scanning-induced compositional homogeneity

Yeong Gyun Nam1, Bonuk Koo1,2, Mise Chang1, Sangsun Yang1, Jihun Yu1, Yong Ho Park2, and Jae

Won Jeong1,*
1Powder/Ceramic Research Division, Korea Institute of Materials Science, 797 Changwondae-ro,

Seongsan-gu, Changwon, 51508, Korea


2School of Materials Science and Engineering, Pusan National University, Busandaehak-ro 63beon-gil,

Geumjeong-gu, Busan, 46241, Korea

*Correspondence: Dr. Jae Won Jeong and Prof. Yong Ho Park

E-mail: jeongjw1204@kims.re.kr

Y. G. Nam and B. Koo equally contributed to this work.

Abstract

Recently, selective laser melting (SLM) of Fe-based soft magnetic bulk metallic glass (BMG) is

garnering great attention because it can yield both superior magnetic properties such as high permeability

and low core loss and near-net shaping of 3-dimensial complex components. However, full vitrification of

BMGs with high saturation magnetization above 1.2 T has never been realized because cooling rates are

limited and compositional inhomogeneity induced by rapid laser processing causes severe undesirable

crystallization. In this work, a double scan strategy has been employed with the aim of amorphous phase

fraction enhancement as well as densification. We have shown that double scanning effectively fills voids

generated due to partial melting of powders, and leads to relative density of up to 96% and corresponding

saturated magnetization of 1.22 T. More importantly, the double scan strategy stimulates reflow in the

melt pool, securing compositional uniformity, and eventually enhances amorphous phase fraction to as

much as 47%. As a consequence, coercivity has been significantly decreased, which in turn reduces core

loss and increases permeability.


Keywords: amorphous soft magnetic; selective laser melting; additive manufacturing; bulk metallic glass;

laser vitrification

1. Introduction

Soft-magnetic bulk metallic glass (BMG) has been extensively studied because it exhibits superior

magnetic properties such as low core loss and high permeability, originating from its disordered atomic

arrangement.[1, 2] However, actual applications of BMGs have been restricted because glass forming

ability (GFA) is limited and conventional fabrication methods such as suction casting and spark plasma

sintering can only produce fully-amorphous BMG at thicknesses of several millimeters.[3]

As an alternative, selective laser melting (SLM) of metal powder can be a promising solution.[4] SLM is

a kind of rapid melting/quenching process with quenching rate at a level of 103~105,[5, 6] which is

sufficient for BMG alloys with moderate saturated magnetization (Ms) (<1.2 T).[7] The SLM process

can also be used to realize 3-dimensional near net shaping of 3-dimensional components with optimized

magnetic path, leading to small, lightweight, and highly efficient devices

Nevertheless, there have been only a few works that have considered SLM of soft magnetic amorphous

alloys.[7, 8] In particular, full vitrification of BMGs with high Ms above 1.2 T has never been realized

because cooling rates are limited and compositional inhomogeneity induced by rapid laser processing

causes severe undesirable crystallization,[9] which will eventually degrade the magnetic properties.

Recently, X.P. Li et al.,[9] have shown that a multiple scan strategy was effective in the stable formation

of amorphous phase because it can induce re-circulation in the melt pool leading to enhanced chemical

homogeneity. And, while that study was tentatively conducted for high-GFA Zr-based BMG alloys, such

methods may also be effective for Fe-based BMG alloys.

Here we present a study on the microstructure and magnetic properties of Fe-based soft magnetic

amorphous alloys prepared by SLM. In particular, a double scan strategy was employed for amorphous

phase fraction (fam) enhancement as well as densification.

2. Experimental

Commercially available amorphous soft magnetic powder (KUAMENT 6B2) with nominal composition

of Fe73.7Si11B11C2Cr2.28 (at%) was purchased from Epson Atmix, Japan, and used as received. The powder
has almost spherical shape, with average diameter of 25 µm, and has values of Ms and coercivity of 1.27

T and 7 Oe, respectively. SLM processing was conducted using a Mlab machine (Conceptlaser, Germany).

Cubic (10X10X5 mm3) and toroid (ID: 10 mm, OD: 20 mm, and H: 5 mm) samples were fabricated with

linear scan method (Figure 1a). Hatch space and layer thickness were fixed at 80 and 25 µm, respectively.

In the double-scan strategy, before the coating of second powder layer, a laser with the same power and

scan speed was used to re-scan in a manner perpendicular to the trace of the previous scan.

Microstructural, magnetic, and mechanical properties were examined using XRD, optical microscopy,

SEM, TEM, DSC, VSM, B-H analysis, and transverse rupture strength (TRS) measurement.

3. Results and discussion

The energy that the powder layer receives is usually expressed by energy density (Ed), as in the

following equation.[10]

𝑝
𝐸𝑑 =
ℎ𝑠𝑑

, where P, h, s, and d are the laser power, hatch space, scan speed, and powder layer thickness,

respectively. From relative density plot as a function of Ed shown in Figure 1b, it can be clearly seen that

double scanning had a positive effect on densification. Even though multiple scans do not increase the

volume fraction of the melted part of the powder, increases of the duration to which the powders are

exposed to the laser can lead to shrinkage of voids. Figure 1d shows optical microscopy images of

surface-polished SLMed alloys prepared though double-scan strategy. Large pores, visible as black dots,

originated from removal of partially-melted (so loosely bound) powders during surface polishing; these

almost disappeared at high power of 90 W. With the highest Ed of 37.5 J/mm3, in combination with the

double scanning strategy, a highest relative density of 96% was obtained. Under this condition,

mechanical strength (TRS) also reached its maximum of 75 MPa due to minimal inclusion of pores,

which act as ignition points of crack, as shown in Figure 1c.[11]


Figure 1. (a) Digital photograph of cubic-shaped SLMed alloys. (b) Relative density and (c) TRS plot as
a function of energy density. (d) Optical microscopy images of double-scanned alloys.

From the XRD patterns presented in Figure 2a, it can be seen that all samples show broad halo patterns

with small crystal peaks corresponding to α-Fe. Presumably the alloys were partially crystallized due to

insufficient cooling rate. However, the intensity of the peak is significantly reduced for double-scanned

samples, implying lower fraction of crystalline phases.

From the DSC results shown in Figure 2b, all samples can be seen to have exothermic peak near 550 oC,

which correlates with the formation of the α-Fe phase. Crystallization enthalpy (ΔHcry) was calculated and

is also depicted in Figure 2b. As Ed increases, the cooling rate decreases, and vice versa;[5] the

descending trend of fam (=ΔHcry of SLMed alloy/ ΔHcry of original powder) with respect to Ed can be

reasonably understood.

On the other hand, double-scanned alloys showed ΔHcry higher than those of single-scanned alloys under

the same process condition. In the case of Ed of 29.2 J/mm3, the relative enhancement of fam was 47%.

From the high resolution TEM images shown in Figure 2c, the alloys can be seen to be composed of

mixed amorphous and nanocrystalline phase. The average size of nanocrystallites was 65 nm, which was

too large to induce exchange interaction between crystallites; other than that, this size of nanocrystallite

induced magnetocrystalline anisotropy, resulting in increased coercivity.


The positive effect of double scanning on vitrification can be explained by the enhanced compositional

homogeneity. Chemical inhomogeneity induced during the melting of the original powders needs to be

eliminated by subsequent capillary flow in the melt pool before solidification. In linear-scan SLM, the

average displacement of a liquid particle (ln) in the melt pool is proportional to the laser power, and

inversely proportional to the square of the scan speed.[9]

𝑝
𝑙𝑛 ~
𝑠2

In this experiment, s was kept to >1000 mm/s to maximize cooling rate; this is disadvantageous for

flow-induced homogenization. In addition, the laser energy has a Gaussian distribution,[12] and so even

thermocapillary flow within the melt pool is inhomogeneous.

However, in the double scanning process, the perpendicularly applied second scan induces melt pool

reflow and Gaussian-distributional inhomogeneity is compensated. As a result, compositional uniformity

was enhanced, and undesirable formation of large α-Fe or intermetallic crystallites was notably prevented.

From the EPMA analysis results shown in Figure 2d, segregated precipitates with sizes of several tens of

micrometers are present in the single-scanned alloys, while they have mostly disappeared from the

double-scanned alloys.

Figure 2. (a) XRD patterns of SLMed alloys. (b) DSC curve and crystallization enthalpy plot as function
of energy density. (c) High-resolution TEM images obtained from double-scanned alloys. (d) EPMA
surface compositional mapping of SLMed alloys.
Enhancement of fam has a positive effect on the magnetic properties. In Figure 3a and 3b, we plotted Ms,

and coercivity as a function of Ed. Ms has a linear dependence on the density, and maximum Ms of 1.22 T

was obtained with double scanning. Coercivity shows an upward tendency with Ed, as opposed to fam.

Increasing Ed will lower the cooling rate, and crystals will grow larger, resulting in increased coercivity.

Double scanning is helpful for fam, and coercivity has been significantly decreased.

Evaluation of the loss characteristics of soft magnets has significant importance because it is directly

related to device efficiency. To the best of our knowledge, this is the first report of core loss

measurements of SLMed soft magnetic BMG alloys. For simplicity, core loss relativity (𝑟𝑃𝑐), defined as

the core loss of SLMed samples divided by that of compacted amorphous powder core, is presented in

Figure 3c. In can be clearly seen that 𝑟𝑃𝑐 was significantly reduced by application of double scanning;

this reduction is attributable to the decreased hysteresis loss. Because permeability (µr) is inversely

proportional to coercivity,[13] enhancement of µr was also observed (Figure 3d).

Figure 3. (a) Saturated magnetization (Ms), (b) coercivity, (c) core loss relativity, and (d) relative
permeability as a function of energy density for the SLMed alloys.

4. Conclusion

Selective laser melting processing of soft magnetic amorphous alloys with high Ms above 1.2 T with the

help of double scanning strategy has been demonstrated. The following conclusions have been drawn

from this work.

(1) Double scan strategy is advantageous for densification and for enhancing Ms. Double

scan increases the duration at which the powders are exposed to the laser; increased exposure
leads to shrinkage of voids, and density dramatically increases. Double scanning combined with

high Ed can lead to the highest density of 96% and corresponding Ms of 1.22 T.

(2) More importantly, double scanning induces reflow in the melt pool, securing

compositional uniformity, and eventually enhances fam to a level as high as 47%. As a

consequence, coercivity has been significantly decreased, which in turn reduces core loss and

increases permeability.

Acknowledgements

This study was supported financially by the Fundamental Research Program (PNK6050) of the Korea

Institute of Materials Science (KIMS), and by the Civil-Military Technology Cooperation Program (18-

CM-MA-15).

References

[1] H.X. Li, Z.C. Lu, S.L. Wang, et al., Prog. Mater. Sci., 103, (2019), 235-318.
[2] S.Y. Meng, H.B. Ling, Q. Li, et al., Scr. Mater., 81, (2014), 24-27.
[3] Z.W. Yu, Y. Liu, J. Li, et al., Rare Metal Mat Eng, 38, (2009), 44-47.
[4] L. Wang, H. Wang, Y.K. Liu, et al., J. Alloy. Compd., 808, (2019).
[5] S. Pauly, P. Wang, U. Kuhn, et al., Addit. Manuf., 22, (2018), 753-757.
[6] J. Song, Y.X. Chew, L.S. Jiao, et al., Addit. Manuf., 24, (2018), 543-551.
[7] H.Y. Jung, S.J. Choi, K.G. Prashanth, et al., Mater. Des., 86, (2015), 703-708.
[8] S. Pauly, L. Lober, R. Petters, et al., Mater. Today, 16, (2013), 37-41.
[9] X.P. Li, M.P. Roberts, S. O'Keeffe, et al., Mater. Des., 112, (2016), 217-226.
[10] A. Simchi, H. Pohl, Mater. Sci. Eng. A-Struct. Mater. Prop., 359, (2003), 119-128.
[11] F. Xie, Q.J. Chen, J.W. Gao, et al., J Mater Eng Perform, 28, (2019), 3478-3486.
[12] S. Katakam, J.Y. Hwang, S. Paital, et al., Metall. Mater. Trans. A-Phys. Metall. Mater. Sci., 43a,
(2012), 4957-4966.
[13] G. Herzer, IEEE Trans. Magn., 26, (1990), 1397-1402.
Figure Captions

Figure 1. (a) Digital photograph of cubic-shaped SLMed alloys. (b) Relative density and (c) TRS plot as

a function of energy density. (d) Optical microscopy images of double-scanned alloys.

Figure 2. (a) XRD patterns of SLMed alloys. (b) DSC curve and crystallization enthalpy plot as function

of energy density. (c) High-resolution TEM images obtained from double-scanned alloys. (d) EPMA

surface compositional mapping of SLMed alloys.

Figure 3. (a) Saturated magnetization (Ms), (b) coercivity, (c) core loss relativity, and (d) relative

permeability as a function of energy density for the SLMed alloys.

Declaration of Competing Interest

The authors declare that they have no known competing financial interests or personal relationships that

could have appeared to influence the work reported in this paper.


Highlights
 Selective laser melting of amorphous soft magnetic alloy has been demonstrated.

 Double scanning densifies alloys leading saturated magnetization of up to 1.22 T.

 Double scanning induces reflow in the melt pool and secures compositional uniformity

 Amorphous phase fraction has been enhanced to a level as high as 47%.

 Double-scanned alloys show improved magnetic properties.

Potrebbero piacerti anche