Trans. Nonferrous Met. Soc.

China 23(2013) 2874−2881

Microstructure optimization of
directionally solidified hypereutectic Nb−Si alloy

Jia-yi WANG1, Li-na JIA1, Li-min MA1, Sai-nan YUAN1, Xiao-li ZHANG2, Hu ZHANG1
1. School of Materials Science and Engineering, Beihang University, Beijing 100191, China;
2. Department of Military Logistics, Military Transportation University, Tianjin 300161, China
Received 19 September 2012; accepted 7 January 2013

Abstract: Nb−16Si−24Ti−10Cr−2Al−2Hf alloy was directionally solidified with withdrawal rates of 1.2, 6, 18, 36 and 50 mm/min
and then heat treated at 1400, 1450 and 1500 °C with withdrawal rate of 50 mm/min for 10 h. The effects of withdrawal rate and heat
treatment temperature on the microstructure were studied. The microstructure of directionally solidified alloy was composed of the
primary Nb5Si3, Nbss/Nb5Si3 eutectic cells and Cr2Nb, which distribute paralleled to the growth direction. The microstructure
becomes more refined with the increasing withdrawal rate, accompany with the evolution of eutectic cells morphology. After heat
treatment, Nbss phase connects and forms a continuous matrix, and the Cr2Nb phase becomes smaller and distributes more
dispersedly. After heat treatment at 1450 °C for 10 h, the alloy achieves balance between the optimization of microstructure and
alleviation of solute segregation.
Key words: Nb−Si alloy; directional solidification; eutectic; withdrawal rate; microstructure; heat treatment

segregation and also eliminate meta-stable phases in the

1 Introduction alloy [15,16]. Until now, the effect of withdrawal rate
and heat treatment temperature on the microstructure
With high melting points, low densities and evolution and composition homogenizing of directionally
attractive high temperature strength and excellent creep solidified (DS) Nb−Si based alloys is still unclear.
resistance, the Nb−Si based ultrahigh temperature alloys Therefore, it is instructive to study the microstructure
are expected to be promising candidate materials for optimizing of Nb−Si based alloys.
employment at 1200−1400 °C [1−4]. Current studies In this study, Nb−16Si−24Ti−10Cr−2Al−2Hf alloy
focus on the Nb−Ti−Si−Cr−Al−Hf in situ composites was directionally solidified by liquid-metal-cooled
which consist of the ductile niobium solid solution Nbss method (LMC) and then heat treated (HT). The purpose
phase, creep resistant but brittle phase Nb5Si3, and with of the present work was to investigate the effects of
or without Cr2Nb phase (C14 Laves phase) which withdrawal rate and heat treatment temperature on the
improves the oxidation resistance [5−8]. A balanced solidification behavior and optimize the microstructure
effect of ductile and brittle phases can be achieved by of the alloy.
appropriate volume fractions of composition phases [3,9].
Moreover, morphological characteristics of component 2 Experimental
phases play an important role in the mechanical
properties of structural materials [10,11]. SEKIDO and A master alloy button, with the nominal
KIMURA [12] reported that directional solidification composition of Nb−16Si−24Ti−10Cr−2Al−2Hf (mole
could produce well-aligned regular structures and fraction, %), was prepared by vacuum non-consumable
improve fracture toughness and high temperature arc-melting (VCAM). Master alloy rods with 13 mm in
strength. However, high withdrawal rate during diameter and 90 mm in length were prepared by the
directional solidification may result in the decrease of electro-discharge machining (EDM). The directional
composition homogenizing [13,14]. Appropriate heat solidification was performed using a laboratory-scale
treatment is an effective way to alleviate solute Bridgman LMC furnace, equipped with a self-contributed

Foundation item: Project (51101005) supported by the National Natural Science Foundation of China
Corresponding author: Hu ZHANG; Tel: +86-10-82316958; E-mail: zhanghu@[Link]
DOI: 10.1016/S1003-6326(13)62809-5
 Jia-yi WANG, et al/Trans. Nonferrous Met. Soc. China 23(2013) 2874−2881 2875
Y2O3 crucible (18 mm in outer diameter, 15 mm in Nbss/Nb5Si3 eutectic clusters or cells, and black Cr2Nb
inner diameter and 200 mm in length), as described in phase. Besides, dark grey Ti-rich Nbss phase was found
our previous work [17,18]. After holding for 20 min at surrounding Nbss/Nb5Si3 eutectic clusters or cells.
1850 °C in the atmosphere of argon, the assembled From the longitudinal sections of the DS specimens
crucibles were withdrawn at 1.2 mm/min (DS1.2), 6 (Fig. 2), it can be seen that the growth direction of the
mm/min (DS6), 18 mm/min (DS18), 36 mm/min (DS36) component phases was parallel to the withdrawal
and 50 mm/min (DS50), respectively. Then the DS50 direction. Primary Nb5Si3 laths, with straight boundary,
samples were heat treated at 1400 °C (HT1400), 1450 °C were 1 mm or longer in length and possessed
(HT1450) and 1500 °C (HT1500) for 10 h, respectively, quadrilateral morphology in transversal sections (Fig. 3).
in a high vacuum heat treatment furnace. Microstructure The Nbss presented the morphology of dendrites and the
analysis was performed by a scanning electron secondary dendrite arms were fully developed. The
microscope (SEM, JXA−8100) equipped with an energy Nbss/Nb5Si3 eutectic clusters or cells were found to
dispersive X-ray spectroscope (EDS, INCA PentaFETx3). present three types of morphologies. The first one,
The phases were identified by micro-area X-ray marked as eutectic I, was an irregular lamellar eutectic
diffraction (XRD, D/max2550HB+/PC Cu Kα). morphology aligning along the growth direction on
longitudinal section (see Figs. 2(a) and (b)) and
3 Results and discussion presented irregular quadrilateral petaloid morphology on
transversal-section (see Figs. 3(a) and (b)). In the center
3.1 Microstructure and composition of directionally of the eutectic cells, fine Nbss and Nb5Si3 were arranged
solidified alloy alternately and in the exterior margin of most eutectic
Figure 1 shows the XRD patterns of DS alloy with cells, Nbss became coarser and some dendrite Nbss
withdrawal rates (Rw) of 1.2, 6, 18, 36 and 50 mm/min, formed. The second one, marked as eutectic II, was a
respectively. The DS alloy with withdrawal rates of 1.2, complex and regular eutectic structure. It was composed
6, 18 and 36 mm/min was composed of the same phases: of eutectic cells which coupled arranged along the
Nbss, α-Nb5Si3, γ-Nb5Si3 and Cr2Nb. However, it is growth direction, and presented as fishbone, fibrous and
interesting that the γ-Nb5Si3 disappears in the alloy with cluster shaped morphology (see Figs. 2(c)−(f)). On
50 mm/min. γ-Nb5Si3 (hexagonal structure) is considered transversal section, the eutectic cells consisted of sub-
a meta-stable phase, while β-Nb5Si3 (tetragonal structure) spherical Nbss and Nb5Si3 which distributed alternatively
is the stable phase at a lower temperature and α-Nb5Si3 with a petaloid morphology. And granular Nbss did not
(tetragonal structure) is the stable phase at high become coarser in the exterior margin (see Fig. 3(c)−(f)).
temperatures. This indicates that the meta-stable phase The third one, marked as eutectic III, was a quasi-regular
can be eliminated by the increase of withdrawal rate. structure of eutectic morphology, whose microstructure
was the rod-like Nb5Si3 inside and the lamellar-like
Nbss/Nb5Si3 eutectic cells in the periphery (see Figs. 2(g)
and (h)). The small faceted phase Nb5Si3 connected and
formed a continuous matrix, and the rod-like structure
was perpendicular to the lamellar-like Nbss/Nb5Si3
eutectic cells. On the transversal section, it was found
that the fine Nbss/Nb5Si3 eutectic cells were arranged
surrounding the quadrilateral Nb5Si3, with divorced Nbss
dendrites in the exterior margin (see Figs. 3(g) and (h)).
With the increase of withdrawal rate，the microstructure
of the DS alloy became more oriented and homogeneous.
The morphology of the eutectic cells varied from eutectic
I to eutectic III.
Table 1 shows the quantitative metallographic
Fig. 1 XRD patterns of directionally solidified Nb−16Si− analysis of directional solidification microstructures
24Ti−10Cr−2Al−2Hf alloy with different withdrawal rates under different withdrawing rates. It can be found that
with the increase of the withdrawing rates, the volume
Figures 2 and 3 show the longitudinal and fraction of primary Nb5Si3 phase, Ti-rich Nbss,
transversal microstructures of the steady-state zones of Nbss/Nb5Si3 eutectic and Nb5Si3 in the eutectic cell
the alloy with withdrawal rates of 1.2, 6, 18, 36 and 50 decreased, the width of Nb5Si3 laths and the size of
mm/min, respectively. The microstructures of all DS eutectic cells reduced, and the Nbss dendrites
specimens were composed of gray primary Nb5Si3 laths, were refined. Based on the above analysis, it could be
2876 Jia-yi WANG, et al/Trans. Nonferrous Met. Soc. China 23(2013) 2874−2881

Fig. 2 Back scattered electron (BSE) images of microstructure on longitudinal-section of steady-state zones of directionally solidified
Nb−16Si−24Ti−10Cr−2Al−2Hf alloy with withdrawal rates of 1.2 mm/min (a, b), 6 mm/min (c, d), 18 mm/min (e, f), 36 mm/min (g)
and 50 mm/min (h)
 Jia-yi WANG, et al/Trans. Nonferrous Met. Soc. China 23(2013) 2874−2881 2877

Fig. 3 Back scattered electron (BSE) images of microstructure on transversal-sections of steady-state zones of directionally solidified
Nb−16Si−24Ti−10Cr−2Al−2Hf alloy with withdrawal rates of 1.2 mm/min (a, b), 6 mm/min (c, d), 18 mm/min (e, f), 36 mm/min (g)
and 50mm/min (h)
2878 Jia-yi WANG, et al/Trans. Nonferrous Met. Soc. China 23(2013) 2874−2881
Table 1 Quantitative metallographic analysis of directional Table 2 Compositions of constituent phases of directionally
solidification microstructures under different withdrawing rates solidified Nb−16Si−24Ti−10Cr−2Al−2Hf alloy with different
Rw/ (v2/v1)/ v3/ v4/ withdrawing rates
d1/μm d2/μm
(mm·min−1) % % % Rw/ x/%
Phase
100.16−235.79 250.63−300.72 (mm·min−1) Nb Ti Si Cr Al Hf
1.2 19.3 25.7 3.6
(139.44) (278.67) Nb5Si3
70.16−100.38 111.49−137.69 48.36 13.90 35.67 0.32 1.69
6 28.6 21.5 3.3 blocks
(84.79) (105.80)
Nbss 61.30 24.37 11.50 1.96 0.87
46.39−63.15 67.89−88.23
18 32.5 17.6 3.2 Nb5Si3
(55.65) (76.15) 1.2 45.92 16.15 35.72 0.39 1.84
in EU
30.72−37.33 42.21−60.38
36 40.8 13.8 2.9 Ti-rich
(34.27) (50.69) 45.55 40.82 7.17 0.98 6.40
Nbss
17.13−28.15 30.05−40.30
50 41.6 10.9 2.8 Cr2Nb 26.80 16.17 54.04 2.98
(21.15) (34.71)
d1: Size of primary Nb5Si3; d2: Average diameter of eutectic cells; v1: Nb5Si3
Volume fraction of eutectic clusters or cells; v2: Volume fraction of Nb5Si3
48.49 13.60 35.81 0.43 1.67
blocks
in eutectic cluster or cells; v3: Volume fraction of primary Nb5Si3; v4:
Volume fraction of Ti-rich Nbss Nbss 64.91 23.33 10.15 0.91 0.67
Nb5Si3
18 44.04 17.29 35.38 0.87 1.92
concluded that the alloy directionally solidified with the in EU
50 mm/min possessed optimal microstructure. Ti-rich
40.20 34.52 22.35 0.44 2.48
Table 2 illustrates the compositions of constituent Nbss
phases of DS alloys with different withdrawing rates (1.2, Cr2Nb 22.74 18.99 54.14 3.15
18, 50 mm/min). From Table 2, it was clear that the Nb5Si3
48.18 14.04 35.63 0.52 1.63
content of refractory element Nb in primary Nb5Si3 blocks
phase was 2%−4% (mole fraction) higher than that in the Nbss 64.10 23.69 10.23 1.27 0.72
Nb5Si3 phase in eutectics and the content of low melting Nb5Si3
50 46.21 16.73 34.35 1.25 1.48
point elements (Ti and Cr) was 2%−4% (mole fraction) in EU
lower than that in the Nb5Si3 phase in eutectics. This was Ti-rich
28.93 47.47 18.76 1.99
due to the fact that primary Nb5Si3 phase formed first, Nbss
which contained more refractory elements, and at the Cr2Nb 23.98 17.54 55.81 2.67
same time it excluded low melting point elements to the EU represents the abbreviation for eutectic cells; Ti-rich Nbss regions were
observed in boundaries of eutectic cells.
surrounding liquid phase, leading to the later formed
Nb5Si3 phase in eutectic contained more Ti and Cr. For distribution and volume fraction of Cr2Nb were not
the above reason, the content of low melting point different from those of the DS alloy. After heat treatment
elements in Nbss in eutectics was also lower than that in at 1450 °C for 10 h, primary Nb5Si3 blocks with sharp
Ti-rich Nbss, which was observed at boundaries of interfaces converted into relatively small size particles
eutectic cells and formed after the eutectics. Thus, with blunted and round interfaces, and the volume
necessary measures need to be taken to alleviate severer fraction of Cr2Nb phase decreased and the Cr2Nb phase
micro-segregation. became smaller and distributed more dispersedly. After
heat treatment at 1500 °C for 10 h, a lot of eutectic cells
3.2 Microstructure and composition after heat in the DS specimens lost their lamellar morphologies. A
treatment semi-solid microstructure was generated with sub
In order to homogenize the composition of DS50 spherical Nbss and small faceted Nb5Si3 blocks arranging
alloy, heat treatments were preceded at 1400, 1450 and alternately. The formation of Nbss/Cr2Nb eutectic cells
1500 °C for 10 h. Figure 4 illustrates the microstructures (as marked by the rectangle in Fig. 4(e)) suggested that
after heat treatment and the phases present were the incipient melting temperature of Nbss/Cr2Nb
confirmed to be Nbss, α-Nb5Si3 and Cr2Nb, the same eutectics was between 1450 °C and 1500 °C.
phases as directionally solidified alloy. From Fig. 4, it Table 3 shows the compositions of constituent
can be found that after heat treatment at 1400 °C for 10 h, phases of DS50 alloy after heat treatments. It could be
Nbss connected and formed a continuous matrix while found that the Ti-rich Nbss regions disappeared and the
the boundaries of primary Nb5Si3 were still smooth. Ti content increased by 5%−6% (mole fraction) in Nbss
Eutectic cells changed into fine Nb5Si3 fibers distributed than the DS alloy. The disappearance of Ti-rich
uniformly in Nbss matrix. However, the morphology, Nbss regions suggested the diminishment of micro-
 Jia-yi WANG, et al/Trans. Nonferrous Met. Soc. China 23(2013) 2874−2881 2879

Fig. 4 BES images of longitudinal-section (a, c, e) and transversal-section (b, d, f) of directionally solidified Nb−16Si−
24Ti−10Cr−2Al−2Hf alloy with withdrawal rate of 50 mm/min after high temperature heat treatments: (a, b) 1400 °C for 10 h; (c, d)
1450 °C for 10 h; (e, f) 1500 °C for 10 h

Table 3 Compositions of constituent phases of Nb−16Si−24Ti−10Cr−2Al−2Hf alloy after different heat treatment (mole fraction, %)
Temperature/°C Phase x(Nb)/% x(Ti)/% x(Si)/% x(Cr)/% x(Al)/% x(Hf)/%
Nb5Si3 blocks 48.25 14.05 35.71 0.38 1.61
Nbss 53.93 30.47 12.98 1.84 0.68
1400
Nb5Si3 in EU 44.10 17.61 35.89 0.68 1.72
Cr2Nb 27.78 13.87 54.97 3.38
Nb5Si3 blocks 47.80 14.25 35.72 0.68 1.55
Nbss 52.96 30.29 0.49 13.36 1.99 0.91
1450
Nb5Si3 in EU 44.46 17.12 36.11 0.59 1.72
Cr2Nb 25.61 15.76 55.68 2.95
Nb5Si3 45.05 16.27 35.97 0.75 1.96
1500 Nbss 53.36 31.68 12.92 1.56 0.48
Cr2Nb 25.96 16.31 54.78 2.95
2880 Jia-yi WANG, et al/Trans. Nonferrous Met. Soc. China 23(2013) 2874−2881
segregation after heat treatment. The composition of temperature, thus leads to the decrease of DCr. The
Nb5Si3 in HT1500 was obviously different for the reason micro-segregation is also alleviated.
of the disappearance of the Nbss/Nb5Si3 eutectics.
Moreover, the HT1450 alloy possessed the highest
average Cr content in Nbss due to the solution of part
Cr2Nb, which resulted in the minimum volume fraction
of Cr2Nb in the alloy.
From above results, it could be concluded that the
HT1450 alloy possessed optimal microstructure and
homogeneous compositions of component phases.

4 Discussion

4.1 Mechanism of effects of withdrawal rate on

morphology of eutectic cells
With the increase of withdrawal rate, the
microstructure of the DS alloy becomes more oriented Fig. 5 Distribution ratio of Cr between Nbss and Nb5Si3 at
and homogeneous. The morphology of the eutectic cells different heat treatment temperatures
varies from eutectic I to eutectic III. As mentioned in
Ref. [19], it can be concluded that the growth trend of 5 Conclusions
small faceted phase could be weakened or transformed to
non-small faceted trend with increasing growth rate, and 1) In the withdrawal rate range between 1.2 and 36
the volume fraction of small faceted phase in the mm/min, the DS alloys are composed of the same phases:
eutectics (φf) exerts a great influence on the eutectic Nbss, α-Nb5Si3, γ-Nb5Si3 and Cr2Nb. However, the
morphology. Since Nb5Si3 is a small faceted phase and γ-Nb5Si3 disappears in the DS50 alloy. The
the growth of Nbss/Nb5Si3 eutectics is irregular, the microstructures of all DS specimens are composed of
increase of volume fraction of Nb5Si3 in eutectic cluster primary Nb5Si3 laths, Nbss/Nb5Si3 eutectic clusters or
or cells (v2/v1, shown in Table 1) which increased cells, Cr2Nb and Ti-rich Nbss phase around Nbss/Nb5Si3
proportionally with the withdrawal rate, results in the eutectics.
transformation of eutectic morphology. 2) The Nbss/Nb5Si3 eutectics present three types of
morphologies which change from eutectic I to eutectic
4.2 Mechanism of effects of heat treatment on III with the increase of withdrawal rate. In the DS50
compositions of constituent phases alloy, the microstructure is refined; however, the higher
With the increase of heat treatment temperature, the withdrawing rate results in the severer
content of Ti in Nb5Si3 increases while the content of Nb micro-segregation.
decreases, which may be caused by the diffusion of Ti 3) As the heat treatment temperature increases, the
and Nb driven by the concentration difference between compositions of component phases are more
Nbss and Nb5Si3. The Ti atom is more active and diffuses homogeneous and the microstructure of the alloy
more easily than Nb due to its smaller radius. However, becomes further smooth and rounded, but lost lamellar
the sum of the mole fraction of Ti and Nb is almost morphologies totally at 1500 °C. Heat treatment at 1450
consistent. During high temperature heat treatment, the °C for 10 h possesses optimal microstructure for the
distribution ratio of alloying elements between Nbss and alloy.
Nb5Si3 changes for the alloying elements diffusing in
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定向凝固过共晶 Nb−Si 基合金的组织优化

王嘉宜 1，贾丽娜 1，马立敏 1，原赛男 1，张晓丽 2，张 虎 1

1. 北京航空航天大学 材料科学与工程学院，北京 100191；

2. 军事交通学院 军事物流系，天津 300161

摘 要：采用液态金属冷却定向凝固炉制备 Nb−16Si−24Ti−10Cr−2Al-2Hf 合金，凝固速率分别为 1.2、6、18、36、

50 mm/min，随后对定向凝固速率为 50 mm/min 的合金进行(1400 °C，10 h), (1450 °C，10 h)和(1500 °C，10 h)的
热处理。研究了定向凝固速率和热处理温度对合金微观组织的影响。结果表明：合金的定向凝固组织主要由沿着
试棒轴向生长的初生 Nb5Si3 相和耦合生长的 Nbss/Nb5Si3 共晶胞组成，在共晶胞边缘，有少量的 Cr2Nb 存在。横
截面上共晶胞边界明显，随着凝固速率的增加，定向凝固组织明显细化，Nbss/Nb5Si3 共晶胞形貌也发生变化。合
金经过热处理，Nbss 连成基体，部分 Cr2Nb 相熔解，微观成分偏析减小。经过(1450 °C，10 h)热处理，实现了对
过共晶 Nb−Si 基合金的组织优化。
关键词：Nb−Si 合金；定向凝固；共晶；抽拉速率；组织；热处理
(Edited by Xiang-qun LI)