Metals and Materials International

, Volume 24, Issue 2, pp 241–247 | Cite as

Development of High Strength Ni–Cu–Zr–Ti–Si–Sn In-Situ Bulk Metallic Glass Composites Reinforced by Hard B2 Phase

  • Hyo Jin Park
  • Sung Hwan Hong
  • Hae Jin Park
  • Young Seok Kim
  • Jeong Tae Kim
  • Young Sang Na
  • Ka Ram Lim
  • Wei-Min Wang
  • Ki Buem Kim


In the present study, the influence of atomic ratio of Zr to Ti on the microstructure and mechanical properties of Ni–Cu–Zr–Ti–Si–Sn alloys is investigated. The alloys were designed by fine replacement of Ti for Zr from Ni39Cu20Zr36−xTixSi2Sn3. The increase of Ti content enhances glass forming ability of the alloy by suppression of formation of (Ni, Cu)10(Zr, Ti)7 phase during solidification. With further increasing Ti content up to 24 at.%, the B2 phase is introduced in the amorphous matrix with a small amount of B19′ phase from alloy melt. The bulk metallic glass composite containing B2 phase with a volume fraction of ~ 10 vol% exhibits higher fracture strength (~ 2.5 GPa) than that of monolithic bulk metallic glass (~ 2.3 GPa). This improvement is associated to the individual mechanical characteristics of the B2 phase and amorphous matrix. The B2 phase exhibits higher hardness and modulus than those of amorphous matrix as well as effective stress accommodation up to the higher stress level than the yield strength of amorphous matrix. The large stress accommodation capacity of the hard B2 phase plays an important factor to improve the mechanical properties of in situ Ni-based bulk metallic glass composites.


Amorphous materials Composites Microstructure Mechanical properties Strength 

1 Introduction

Bulk metallic glasses (BMGs) with unique properties, such as high strength, large elasticity and excellent corrosion resistance have been developed in various multi-component alloy systems [1, 2]. The excellent physical and chemical properties are associated with their unique atomic structure [2, 3]. However, the BMGs usually undergo catastrophic failure due to the formation and propagation of a few shear bands introduced by inhomogeneous plastic deformation at room temperatures [3], which have limited use of BMGs for engineering applications. In order to overcome this critical drawback of BMGs, many researchers have attempted to improve plasticity by introducing a second phase in the amorphous matrix. The formation of second phases in the amorphous matrix leads to a new class of materials, which is called the bulk metallic glass composites (BMGCs) [4]. The manufacturing methods for BMGCs can be generally divided into two categories according to how the second phase is introduced in the materials: ex situ and in situ methods. The ex situ BMGCs have been fabricated using the reinforcements with high melting temperature, such as W, Ta, and ceramic particles. The homogeneously dispersed ex situ reinforcements in amorphous matrix induce the formation of multiple shear bands by homogeneous plastic deformation in the BMGCs [5, 6, 7]. The second one is an in situ method that forms the ductile crystalline phases in the amorphous matrix during solidification. Especially, the relatively low interface energy between amorphous matrix and second phases in the in situ BMGCs produces more stable interface than that of ex situ BMGCs, which leads to excellent mechanical properties [8, 9, 10]. Moreover, the volume fraction and size of in situ crystalline phases can be easily controlled by fine compositional tuning in the alloy systems [11, 12].

Recently, a new strategy for the in situ BMGCs has been proposed to form B2 crystalline phase in TiCu- [12, 13, 14] and CuZr-based alloys [15, 16, 17]. It has been reported that the formation of B2 phase in the amorphous matrix contributes to significantly improvement in plasticity as well as strong work-hardening behavior [18, 19, 20]. These outstanding mechanical properties of B2 phase-reinforced BMGCs strongly are connected with the volume fraction, strain accommodation capacity and stress-induced martensitic transformation behavior of B2 phase during deformation [21, 22, 23]. Moreover, a suitable elastic mismatch between B2 phase and amorphous matrix is also regarded as a crucial factor that leads to the occurrence of stress-induced martensitic transformation of B2 phase and formation multiple shear bands from the interface of amorphous matrix and B2 phase [14]. Based on these effective mechanisms to improve the mechanical properties of B2 phase-reinforced BMGCs, the researchers have attempted to develop the BMGC containing in situ B2 phase in other element-based glass forming alloys, such as Ni-based alloy systems. However, the in situ B2 phase-reinforced BMGCs have been reported just in the CuZr- and TiCu-based glass forming alloys. Therefore, it is noteworthy to develop the B2 phase-reinforced in situ BMGC by systemic compositional investigation in the Ni-based alloy systems.

In the present study, we attempt to develop the B2 phase-reinforced in situ BMGCs in the Ni–Cu–Zr–Ti–Si–Sn glass forming alloy system via of the compositional tuning in constituent elements without additional element. To understand the influence of atomic ratio between constituent elements on the microstructural evolution and formation of in situ B2 phase in amorphous matrix, the alloys were designed by controlling the atomic ratio between Ti and Zr elements. In addition, the individual mechanical characteristic of B2 phase and amorphous matrix were investigated to understand the influence of B2 phase on the mechanical properties of present Ni-based BMGCs.

2 Experimental Procedures

Ni39Cu20Zr36−xTixSi2Sn3 alloy ingots with different ratio of Zr to Ti (x = 9, 12, 16, 20, 24 and 27 at.%) were prepared by arc-melting with high-purity elements (> 99.9% purity) in an Ar atmosphere. The ingots were re-melted at least five times to achieve chemical homogeneity. The as-cast sample was fabricated by injection casting into a cylindrical rod-shape Cu mold with diameter of 2 mm and lengths of 50 mm. The phase identification was carried out by X-ray diffraction (XRD, SHIMADZU XRD-6100) with Cu Kα1 radiation (λ = 1.5406 Å). The microstructure of the as-cast samples was investigated using scanning electron microscopy (SEM, JEOL JSM-6390) and transmission electron microscopy (TEM, Tecnai F-20) coupled with energy dispersive spectroscopy (EDS). Thin foil samples for TEM analysis were prepared by conventional ion milling in a liquid nitrogen atmosphere. Thermal properties associated with the glass transition temperature (T g ) and the onset of crystallization temperature (T x ) were measured by a differential scanning calorimeter (DSC, Perkin-Elmer DSC-8500) under constant heating rate of 20 K min−1. Cylindrical specimens with a 2:1 aspect ratio for compression tests were prepared and the mechanical properties of the specimens were examined by uniaxial compressive test with initial strain rate of 1 × 10−3 s−1 at room temperature. Nano-indentation experiments were conducted to measure the hardness and elastic modulus of amorphous matrix and second phase in a load-control mode with a maximum load of 50 mN at a constant loading/unloading rate 100 mN min−1 using a Nano-indentation tester (CSM, NHT-X).

3 Results and Discussion

Figure 1 shows the XRD traces and DSC curves of the as-cast Ni39Cu20Zr36−xTixSi2Sn3 (x = 9, 12, 16, 20, 24 and 27 at.%) alloys with the diameter of 2 mm. As depicted in Fig. 1a, the XRD patterns of as-cast alloys with low Ti content (x = 9 and 12 at.%) exhibit sharp crystalline peaks corresponding to oC68 (Ni, Cu)10(Zr, Ti)7 phase without other crystalline peaks. As Ti content increases to 16 at.%, the crystalline peaks corresponding to (Ni, Cu)10(Zr, Ti)7 phase suddenly disappear and only the broad diffraction of amorphous phase is detected. The amorphous phase still maintains until the Ti content increases to 24 at.%. This result suggests that an increase of Ti above 16 at.% suppresses the precipitation of the (Ni, Cu)10(Zr, Ti)7 phase, and thus enhances glass forming ability. With increase of Ti content up to 27 at.%, the alloy exhibits the intense diffraction peaks of B2 phase with weak diffraction peaks of B19′ phase, while the broad diffraction corresponding the amorphous phase becomes invisible [24, 25, 26]. This result indicates that the Ti addition over 24 at.% deteriorates the glass forming ability of Ni39Cu20Zr36−xTixSi2Sn3 alloys; meanwhile, it is believed that the substitution of Ti for Zr is effective for the formation of B2 phase in present alloy system. Figure 1b shows the DSC curves of the as-cast alloys. The 9 at.%Ti alloy shows no event corresponding to the crystallization of amorphous phase, indicating fully crystalline alloy. With addition of 12 at.%Ti, the shallow exothermic crystallization event is detected. One the other hands, the alloys containing Ti content of 16, 20 and 24 at.% clearly display the endothermic events corresponding glass transition of amorphous, followed by a couple of strong exothermic events corresponding to the crystallization of metastable supercooled liquid phase. However, the 27 at.%Ti alloy reveals a sudden decrease of exothermic peak, indicating the drastic increase of volume fraction of crystalline phase. These observations confirm that the amorphous phase forms in present alloys without 9 at.%Ti alloy and the glass forming ability of the alloys strongly depends on atomic ratio of Ti and Zr elements. Based on XRD and DSC results, it is believed that the proper substitution of Ti for Zr enhances glass forming ability by suppressing formation (Ni, Cu)10(Zr, Ti)7 phase and leads to formation of B2 phase as an stable phase in the Ni39Cu20Zr36−xTixSi2Sn3 alloys.
Fig. 1

a XRD patterns and b DSC traces obtained from the as-cast Ni39Cu20Zr36−xTixSi2Sn3 (x = 9, 12, 16, 20, 24 and 27 at.%) alloys

Figure 2 shows the cross sectional SEM back-scattered electron (BSE) micrographs of Ni39Cu20Zr36−xTiySi2Sn3 (x = 16, 20, 24 and 27 at.%) alloys together with inset low magnified micrographs corresponding to the each alloy. The BSE image of 16 at.%Ti alloy in Fig. 2a displays a homogeneous contrast, indicating the formation of monolithic amorphous alloy. The result is consistent with the XRD result shown in Fig. 1a. On the contrary, the BSE image of the 20 at.%Ti alloy in Fig. 2b reveals homogeneously distributed black particles with a size of 1–5 μm on the bright amorphous matrix. Furthermore, the volume fraction of the particles is measured to be ~ 5 vol%. The BSE image obtained from the 24 at.%Ti alloy shown in Fig. 2c represents an additional dark contrast phase with the black particles embedded in bright amorphous matrix. The volume fraction of black particles and dark phase is ~ 5 and ~ 10 vol%, respectively. In both alloys, the black and dark phases embedded in amorphous matrix did not detected in XRD results shown in Fig. 1a, which is caused by their imperceptibly low volume fraction and size. The detailed investigation on phase identification of these particles will be described in Fig. 3 with systematic TEM analysis. On the one hand, when the Ti content increases to 27 at.% (BSE image in Fig. 2d), the volume fraction of the crystalline phases drastically increases and much smaller black particles are precipitated in gray contrast matrix. From the XRD result in Fig. 1a, the black particles and gray matrix in the alloy are identified as B19′ and B2 phases, respectively. By combining the results in XRD traces, DSC curves in Fig. 1 and SEM observation in Fig. 2, it is possible to conclude that only the 16 at.%Ti alloy forms monolithic BMG upon solidification, whereas the 20 and 24 at.%Ti alloys form BMG composites containing the different crystalline phases in amorphous matrix. From these results, it is believed that the increase of Ti content above 16 at.% by substitution of Ti for Zr in Ni39Cu20Zr36−xTixSi2Sn3 alloys deteriorates the glass forming ability, but induces the precipitation of homogeneously distributed second phases in amorphous matrix.
Fig. 2

SEM BSE micrographs obtained from cross sectional area of the as-cast Ni39Cu20Zr36−xTixSi2Sn3 alloys with inset low magnified micrographs: a x = 16, b x = 20, c x = 24 and d x = 27 at.%

Fig. 3

a A TEM BF image of 24 at.%Ti alloy, b though d SAED patterns obtained from (i) to (iii) areas in (a), the e EDS line profile carried out the direction of black allow in (a)

In order to obtain deep insight into the microstructural features of the present Ni-based BMGC, we performed the TEM analysis for 24 at.%Ti alloy consisting of black, gray particles and amorphous matrix as shown in Fig. 2c. Figure 3 shows TEM bright field (BF) image of as-cast 24 at.%Ti alloy, together with the corresponding selected area electron diffraction (SAED) patterns and the EDS composition profile of the alloy components. The TEM BF image in Fig. 3a displays the typical microstructure of BMGC containing the gray particles with a size of ~ 5 μm and dark particles with a size of ~ 0.5 μm in amorphous matrix. The SAED pattern in Fig. 3b obtained from (i) area (marked by white dotted square in matrix) in Fig. 3a presents a typical hallow diffraction intensity, indicating an amorphous structure, as demonstrated in the XRD and SEM results in Figs. 1 and 2. The SAED pattern in Fig. 3c obtained from (ii) area (marked by white dotted square in dark particle) in Fig. 3a shows the spotty diffraction intensity and is indexed as the [101] zone axis of the NiTi-type B19′ compound. The SAED pattern obtained from (iii) area (marked by white dotted square in gray particle) in Fig. 3a can be identified as [001] zone axis of the CsCl-type B2 compound. Furthermore, the superlattice of the {100} plane of the B2 compound is clearly visible, indicating the ordered structure of the B2 compound. Partitioning of each element in amorphous matrix, B19′ and B2 compounds are illustrated in Fig. 3e, showing EDS composition profiles of Ni, Cu, Zr, Ti, Sn and Si across the three phases. All elements exhibit similar contents between amorphous matrix and B2 compound. On the other hand, Ti and Si elements are enriched in B19′ compound while the Zr, Cu, and Sn content are higher in amorphous and B2 phases. This result intimates that the B19′ NiTi-rich compound containing high Si contents can be precipitated by solute partitioning of Ti and Si in liquid state [27]. On the other hand, the B2 compound with similar composition compared with an amorphous matrix can possibly form due to the small chemical fluctuation in the undercooled melts similar to the case of TiCu-based BMGC containing B2 compound [12]. Based on these results, it can be concluded that the 24 at.%Ti alloy is a BMGC containing B19′ and B2 intermetallic compounds. Moreover, these results also imply that the black particles in 20 and 27 at.%Ti alloys as shown in Fig. 2b, d can be considered as NiTi-type B19′ compound.

Figure 4 shows the compressive stress–strain curves of as-cast Ni39Cu20Zr36−xTixSi2Sn3 (x = 16, 20, 24 and 27 at.%) alloys and the nano-indentation results of as-cast Ni39Cu20Zr36−xTixSi2Sn3 (x = 16 and 24 at.%) alloys. From the compressive stress–strain curves in Fig. 4a, it can be seen that all alloys are fractured catastrophically with no plasticity. However, the alloys including different phases and volume fraction of crystalline phases exposes the difference in fracture strength. The fracture strength of monolithic BMG (x = 16 at.%) is about 2.3 GPa, which is similar to the other monolithic Ni-based BMGs (2.2–2.34 GPa) [28]. When the B19′ particles with a volume fraction of ~ 5 vol% are formed in the amorphous matrix in 20 at.%Ti alloy, the fracture strength slightly decreases to ~ 2.2 GPa. On the other hand, the 24 at.%Ti alloy containing B2 phase with ~ 10 vol% together with B19′ particles with ~ 5 vol% in amorphous matrix exhibits an increase in fracture strength to ~ 2.5 GPa. Moreover, the 27 at.%Ti alloy consisting of B19′ particles with ~ 5 vol% and B2 matrix shows further enhanced fracture strength of 2.6 GPa. These changes in fracture strength of present alloys are mainly related to the microstructural evolution depending on Ti content. In general, the formation of B2 phase in the CuZr- and TiCu-based BMGCs is effective to improve the plasticity and work-hardenability, whereas the yield strength decreased due to early deformation of softer B2 and B19′ phases with lower elastic modulus and hardness than those of amorphous matrix [12, 21, 22]. In contrast, present Ni-based BMGCs including the different amounts of the B2 phase exhibits a tendency to increase in fracture strength with an increase of volume fraction of B2 phase. This result implies that the mechanical relationship between the B2 and amorphous phases in the present alloys have a difference in comparison with that of the CuZr- and the TiCu-based BMGCs. Therefore, in order to investigate the influence of mechanical characteristics of B2 phase on the fracture strength of these alloys, the nano-indentation test on the amorphous matrix and B2 phase were conducted in 16 at.%Ti and 24 at.%Ti alloys, and the corresponding results are displayed in Fig. 4b, c. As shown in Fig. 4b, c, the modulus and average hardness values of the amorphous phase in both alloys are 158.8 ± 1.7 and 14.31 ± 0.2 GPa for 16 at.%Ti alloy and 160.4 ± 0.8 and 14.15 ± 0.2 GPa for 24 at.%Ti alloy, respectively. There is no significant difference in mechanical characteristic of amorphous phase in both alloys. However, the modulus and hardness of B2 phase in 24 at.%Ti alloy are 164.3 ± 3.3 and 15.13 ± 0.1 GPa, respectively. This result indicates that the B2 phase embedded in amorphous phase is harder phase with higher elastic modulus than amorphous matrix. Therefore, it can be inferred that the strengthening of the present alloys results from the formation of B2 phase with higher hardness than amorphous matrix.
Fig. 4

a The compressive stress–strain curves of the as-cast Ni39Cu20Zr36−xTixSi2Sn3 (x = 16, 20, 24 and 27 at.%) alloys, b modulus and c micro-hardness of 16 and 24 at.%Ti alloys

From the previous investigations [13], one can notice that the crystalline phase with much higher hardness and modulus than those of amorphous matrix can be hardly deformed by stress concentration at the interface between crystalline and amorphous phase, which eventually leads to the creation of cracks before yielding of amorphous matrix. Thus, the BMGC fractures without any plasticity at lower stress level than yield strength of monolithic BMG. In present study, the B2 phase embedded in amorphous matrix exhibits the higher hardness and modulus than that of amorphous. This elastic modulus mismatch in both phases also induces the stress concentration at the interface between B2 phase and amorphous matrix [13, 14]. Nevertheless, the present BMGC including B2 phase reveals much higher fracture strength in comparison with a monolithic BMG. This implies that the hard B2 phase in present BMGCs can accommodate the stress concentrated at the interface up to the higher stress level than the yield strength of amorphous matrix without early crack creation. In case of Cu60Zr30Ti10 BMGC reinforced by hard ZrC particle [29], moreover, the formation of micro-sized brittle ZrC particles with suitable volume fraction enhances simultaneously both strength and plasticity by disturbing quick development of the shear band. Based on this understanding, it is suggested that when the micro-sized hard B2 phase homogenously disperses with a proper volume fraction in the Ni39Cu20Zr36−xTiySi2Sn3 BMGCs, it might be possible to improve macroscopic plasticity without typical tradeoff between plasticity and strength which have generally observed on the ductile or soft phase-reinforced BMGCs [8, 9, 10, 12, 22].

4 Conclusion

In the present investigation, we found the in situ crystalline dispersed Ni-based BMGCs by modulating the atomic ratio between Zr and Ti from the Ni39Cu20Zr36−xTiySi2Sn3 glass forming alloys. The detailed investigation in microstructural evolutions depending on Ti content revealed that an increase of Ti content enhanced glass forming ability by suppression of the precipitation of the (Ni, Cu)10(Zr, Ti)7 phase and induced the formation of monolithic BMG without any crystalline phase. Moreover, further increase of Ti content up to 24 at.% led to the formation of BMGCs, consisted of the B2 phase embedded amorphous matrix with the small amount of B19′ particles. The BMGC containing B2 phase with a volume fraction of ~ 10 vol% exhibited higher fracture strength (~ 2.5 GPa) than that of monolithic BMG (~ 2.3 GPa). This improvement in fracture strength is mainly related to the individual mechanical characteristics of the B2 phase. The B2 phase with higher hardness and modulus values than those of amorphous matrix can effectively accommodate the stress concentrated at interface between amorphous matrix and B2 phase up to the higher stress level than the yield strength of amorphous matrix. This large stress accommodation capacity of the hard B2 phase can play an important factor to develop the Ni-based in situ BMGCs with further enhanced mechanical properties.



This work was supported by the National Research Foundation (NRF) of Korea grant funded by the Korea government (Ministry of Science, ICT & Future Planning) (No. 2017R1C1B5017092), the Industrial Infrastructure Program for fundamental technologies (Project No. N0000846) and the Energy Efficiency & Resources Core Technology Program of the Korea Institute of Energy Technology Evaluation and Planning (KETEP) (No. 20142020103910) funded By Ministry of Trade, Industry and Energy (MOTIE, Korea).


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Copyright information

© The Korean Institute of Metals and Materials 2018

Authors and Affiliations

  • Hyo Jin Park
    • 1
  • Sung Hwan Hong
    • 1
  • Hae Jin Park
    • 1
  • Young Seok Kim
    • 1
  • Jeong Tae Kim
    • 1
  • Young Sang Na
    • 2
  • Ka Ram Lim
    • 2
  • Wei-Min Wang
    • 3
  • Ki Buem Kim
    • 1
  1. 1.Department of Nanotechnology and Advanced Materials EngineeringSejong UniversitySeoulRepublic of Korea
  2. 2.Light Metal DivisionKorea Institute of Materials Science (KIMS)ChangwonRepublic of Korea
  3. 3.Key Laboratory for Liquid–Solid Structural Evolution and Processing of Materials, Ministry of EducationShandong UniversityJinanChina

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