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1 s2.0 S0272884219313264 Main
1 s2.0 S0272884219313264 Main
1 s2.0 S0272884219313264 Main
Ceramics International
journal homepage: www.elsevier.com/locate/ceramint
A R T I C LE I N FO A B S T R A C T
Keywords: The Si–Y eutectic alloy has been prepared by Bridgeman method where the high temperature gradient (GE) can
Si–Y alloy be obtained by means of double heating combining with liquid metal cooling. The microstructures of long-
Directional solidification itudinal section and cross section at different GE have been observed. It can be seen clearly that the YSi2 phase
Temperature gradient GE presents the evolution process of thick banded shape, island shape, reticular shape and fine strip shape as GE
Interface growth temperature
increases from 90 K/cm to 200 K/cm. Based on the interface growth temperature model, it can be concluded that
Competitive growth
the interface growth temperatures of Si phase and YSi2 phase both will decrease linearly with increasing GE
while that of eutectic structure will keep a constant of 1485.6 K. Two critical temperature gradients
GEC1 = 52 K/cm and GEC2 = 111 K/cm have been calculated. Eutectic coupling growth will take the dominant
position when the actual GE is greater than GEC2. The primary Si phase will begin to form as GE is smaller than
GEC2 and will be thicker as GE is smaller than GEC1. The coupling effect of withdrawal rate and GE on the
microstructures of the Si–Y alloy also has been analyzed comprehensively.
∗
Corresponding author. State Key Laboratory of Solidification Processing, Northwestern Polytechnical University, Xi'an, 710072, Shaanxi Province, PR China.
E-mail address: rhu@nwpu.edu.cn (R. Hu).
https://doi.org/10.1016/j.ceramint.2019.05.213
Received 11 April 2019; Received in revised form 9 May 2019; Accepted 20 May 2019
Available online 21 May 2019
0272-8842/ © 2019 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
J. Li, et al. Ceramics International 45 (2019) 16776–16783
A Si-18at. %Y alloy master ingot was prepared which was melted this paper)and appropriately increasing the temperature T of direc-
three times in order to ensure a homogeneous composition by vacuum tional solidification all will be conducive to obtain a high GE.
arc melting using 99.999% polysilicon powder and 99.9% Y powder. Through adjusting the heating power, the temperature of solid
Then the alloy ingot was cut into cubes by electric spark cutting ma- phase TS, the temperature of liquid phase TL have been measured by
chine and was filled in a 7 mm × 110 mm thin-walled alundum tube. two thermocouples respectively and the GE can be calculated as shown
The directional solidification experiment was carried out in the in Fig. 2. The results have shown that the GE can reach 90 K/cm, 120 K/
Bridgman furnace with a high purity argon atmosphere. In order to cm, 160 K/cm and 200 K/cm respectively when the liquid phase tem-
obtain a higher GE, double heating method was adopted in this paper, peratures are 1703 K, 1768 K, 1850K, 1943K.
as shown in Fig. 1. At the location near the Ga-In-Sn liquid metal
cooling bath, an additional high purity graphite heating element, 3.2. Directionally solidified microstructures
Heater 2, was added. In addition, two thermocouples were placed ad-
jacent to the solid-liquid interface in order to obtain the GE. One was The Si–Y eutectic alloy has been prepared by Bridgeman method
next to the liquid phase and the other was next to the solid phase. Both with GE of 90 K/cm, 120 K/cm, 160 K/cm and 200 K/cm respectively.
two thermocouples were attached to the outer wall of the thin-walled The microstructure morphology has been observed by SEM. It can be
alundum tube, so as to measure the temperature in each region more seen the directional solidified microstructure has been more regular and
accurately. The molten alloy was pulled down into the cooling bath more orderly than that of master alloy, as shown in Fig. 3(a)–b.
with four different GE of 90 K/cm, 120 K/cm, 160 K/cm and 200 K/cm The phase and composition have been detected by XRD and EDS
respectively at a constant withdrawal rate 1.5 mm/min. The cylindrical respectively. According to the XRD detection results, there are only Si
bars of Si–Y eutectic alloy with 7 mm diameter and 80 mm length were phase and YSi2 phase in Si–Y eutectic alloy. Combining with EDS
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J. Li, et al. Ceramics International 45 (2019) 16776–16783
Fig. 2. The relation curve of the GE with the directional solidification heating
power P.
composition detection results, it can be determined that the black area Fig. 4. Microstructures of longitudinal sections at different GE: (a) 90 K/cm, (b)
is Si phase and white area is YSi2 phase, as shown in Fig. 3(c)–d. The 120 K/cm, (c) 160 K/cm and (d) 200 K/cm.
interface between Si phase and YSi2 phase is curved and irregular just
like Al2O3/Y3Al5O12/ZrO2 composites fabricated by directional solidi-
shape distributed along the thick primary Si phase to island shape and
fication which belongs to faceted system [19]. The actual composition
finally to fine, long strip shape in Si–Y eutectic alloy with a constant GE
of alloy measured by EDS is Si-18.02 at. %Y which is close to the
of 47 K/cm but different withdrawal rates [10].
nominal composition Si-18 at. %Y. Hence, the effect of element vola-
When the GE is 90 K/cm, a large number of primary Si phases exist
tilization on alloy composition during directional solidification could be
in the microstructure whose average diameter is 50 μm approximately,
negligible.
as shown in Fig. 4(a). The growth direction of primary Si phases is
The microstructure of directional solidification Si–Y alloy samples
highly parallel to the opposite direction of withdrawal in directional
has been observed by SEM, and obvious differences in microstructure
solidification. At the boundary of primary Si phase, Y element is en-
morphology can be found. The microstructure in longitudinal section is
riched due to the poor fluidity of alloy melt, which can result in the
shown in Fig. 4. It can be seen clearly that the YSi2 phase presents the
formation of thick banded YSi2 phase where the study by F. W. Dynys
evolution process of thick banded shape, island shape, reticular shape
also confirmed the existence of thick blocky YSi2 phase [20]. More than
and strip shape successively as GE increases from 90 K/cm to 200 K/cm,
10 μm away from the primary Si phase, there is a large amount of
which is consistent with the evolution process of YSi2 phase from blocks
Fig. 3. Analysis results for Si–YSi2 eutectic alloy: (a) microstructure of master alloy, (b) directional solidified microstructure, (c) the chemical composition, (d) the
XRD spectrum.
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Fig. 9. Relationship between interface growth temperature of Si/YSi2 and solidification conditions: (a)(c) The relationship curves of interfacial growth temperature
and withdrawal rate under different GE, (b)(d) The relationship curves of interfacial growth temperature and GE under different withdrawal rates.
(4) The uniform eutectic microstructure could be obtained by faster of components in Ge–Si bulk single crystals grown under the continuous feeding of
withdrawal rate under the condition of high GE. When the GE is the melt with the second component (Si), J. Cryst. Growth 226 (2001) 437–442.
[9] E. Çadirli, M. Gündüz, The dependence of lamellar spacing on growth rate and
greater than 200 K/cm, as long as the actual withdrawal rate is less temperature gradient in the lead–tin eutectic alloy, J. Mater. Process. Technol. 97
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The authors acknowledge the sponsor of Creative Research
microstructure of directionally solidified NiAl–Cr(Mo) hypereutectic alloy,
Foundation of Science and Technology on Thermostructural Composite Intermetallics 22 (2012) 99–105.
Materials Laboratory (614291102010417). [13] Z. Shang, J. Shen, J.F. Zhang, L. Wang, L. Qin, H.Z. Fu, Effects of withdrawal rate
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