Formation of In Situ Particle Composite Solidification Microstructure of Gd-Co-Ti Alloy Under Microgravity Conditions

doi:10.11900/0412.1961.2024.00174

Acta Metall Sin

2025, Vol. 61

Issue (12): 1933-1944 DOI: 10.11900/0412.1961.2024.00174

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Formation of In Situ Particle Composite Solidification Microstructure of Gd-Co-Ti Alloy Under Microgravity Conditions

SUN Hao¹^,², JIANG Hongxiang¹^,²(

), ZHAO Jiuzhou¹^,²(

), ZHANG Lili¹^,², HE Jie¹^,²

1 Shi-changxu Innovation Center for Advanced Materials, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China
2 School of Materials Science and Engineering, University of Science and Technology of China, Shenyang 110016, China

Cite this article:

SUN Hao, JIANG Hongxiang, ZHAO Jiuzhou, ZHANG Lili, HE Jie. Formation of In Situ Particle Composite Solidification Microstructure of Gd-Co-Ti Alloy Under Microgravity Conditions. Acta Metall Sin, 2025, 61(12): 1933-1944.

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Abstract

Gd and its alloys are good magnetic materials, and the addition of the transition metal Co to Gd-Ti alloy can facilitate the formation of thermally stable magnetic compounds. The Gd-Co-Ti alloy exhibits significant potential for the development of magnetic in situ composite materials. However, because of the large positive mixing enthalpy between Gd and Ti, the Gd-Co-Ti alloy is a typical monotectic alloy, exhibiting a miscibility gap in the liquid state. Under the ground gravity conditions, the alloy tends to form a phase-segregated solidification microstructure resulting from liquid-liquid phase transformation. Strong convection in the melt during solidification aggravates this process, rendering it difficult for various influencing factors to interact. However, research on solidification theory for these alloys is limited. Microgravity environments can effectively weaken or even eliminate natural convection in alloy melts, which is beneficial for studying the solidification process and microstructure formation in monotectic alloys. Previous studies have focused on the phase structures, material properties, and thermodynamic behavior of Gd-Co-Ti ternary monotectic alloys. However, research on their solidification process is sparse. In this study, rapid and sub-rapid solidification experiments under drop-tube microgravity conditions were performed using Gd-Co-Ti ternary monotectic alloys. The effects of cooling rates on the solidification microstructure of the alloy were investigated. The resulting samples exhibited a composite microstructure comprising homogeneously dispersed subspherical TiCo-rich particles in the Gd matrix. These particles include: (i) TiCo-rich phase particles formed via liquid-liquid phase transformation, and (ii) TiCo-rich nanoparticles formed through desolventizing precipitation during the cooling process after solidification. To elucidate the microstructure evolution in Gd-Co-Ti alloys solidified under drop-tube conditions, a population dynamics model was established. The model comprehensively considers the thermal and mass transfer characteristics during solidification, as well as the nucleation, growth, and spatial motions of TiCo-rich phase droplets. The algorithm for solving the controlling equations in this model was developed based on the finite volume method. The microstructure formation was simulated, and the results were consistent with the experimental data, thus validating the accuracy of the model. The numerical results demonstrated that the nucleation of the TiCo-rich phase droplets occurred during the liquid-liquid phase transformation under drop-tube microgravity conditions. The number density of these TiCo-rich phase droplets remained unchanged after nucleation, indicating that the Ostwald coarsening of the TiCo-rich droplets was weak during the cooling of the alloy melt. Thus, nucleation and diffusion growth were the primary factors influencing the size of TiCo-rich phase droplets formed during the liquid-liquid phase transformation. With the increase in the sample sizes, the cooling rate of the alloy melt and the number density of the TiCo-rich particles decreased; thus, the average radius of the TiCo-rich particles in the solidification microstructure increased. Furthermore, the maximum nucleation rate (I_DMax) and the number density (N_D) of the TiCo-rich phase droplets/particles exhibited an exponential dependence on the cooling rate ( $T ˙ n u c$ ) during the nucleation period as per the following expression: $I D M a x$ = 7.202 × 10^-5 $T ˙ n u c 2.2$ and $N D$ = 3.385 × 10^-4 $T ˙ n u c 1.3$ .

Key words: Gd-Co-Ti alloy microgravity liquid-liquid phase separation solidification modeling and simulation

Received: 20 May 2024

ZTFLH:

TG111.4

Fund: Space Utilization System of China Manned Space Engineering(KJZ-YY-NCL-1-06);National Key Research and Development Program of China(2021YFA0716303);National Natural Science Foundation of China(52174380);Natural Science Foundation of Liaoning Province(2023-MS-023)

Corresponding Authors: JIANG Hongxiang, associate professor, Tel: (024)23971905, E-mail: hxjiang@imr.ac.cn; ZHAO Jiuzhou, professor, Tel: (024)23971918, E-mail: jzzhao@imr.ac.cn

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	JIANG Hongxiang
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	ZHANG Lili
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https://www.ams.org.cn/EN/10.11900/0412.1961.2024.00174 OR https://www.ams.org.cn/EN/Y2025/V61/I12/1933

Fig.1 Macromorphology of Gd-2%Co-2%Ti alloy sample (a) and SEM images showing the microstructures at the center region of the samples with diameters of 285 μm (b), 355 μm (c), 420 μm (d), 445 μm (e), and 710 μm (f)

Fig.2 SEM image of Gd-2%Co-2%Ti alloy sample with a diameter of 445 μm (a), and corresponding EDS element mappings of Gd (b), Co (c), and Ti (d) at the center region

Fig.3 SEM image of shell/core TiCo-rich particle and the EDS point scanning results (inset) for the shell and core (a) and element line scanning results for Gd, Co, and Ti along line I in Fig.3a (b) of the Gd-2%Co-2%Ti alloy sample with a diameter of 445 μm (Shell and core represent the outer shell and inner core of TiCo-rich particle, respectively)

Fig.4 2D size distributions of the TiCo-rich particles in the Gd-2%Co-2%Ti alloy samples with diameters of 285 μm (a), 355 μm (b), 420 μm (c), 445 μm (d), and 710 μm (e)

Fig.5 Number density (N_D) of the TiCo-rich particles in the Gd-2%Co-2%Ti alloy sample vs sample size (D)

Fig.6 Verical section of w_Co∶w_Ti = 1∶1 for the phase diagram of the Gd-Co-Ti system (a) and schematic of the solidification process of the Gd-2%Co-2%Ti alloy under equilibrium conditions (b) (w_Co and w_Ti—mass fractions of solutes Co and Ti, respectively. L₁ + L₂ represents liquid-liquid phase transformation region. T—temperature. T₁, T₂, T₃, and T₄ represent the equilibrium binodal line temperature, onset temperature of liquid-liquid-solid phase transformation, and temperatures of the invariant reactions 1 and 2, respectively)

Parameter	Symbol	Value	Unit
Thermal conductivity of liquid Gd	$λ l G d$	16.0	W·K^-1·m^-1
Thermal conductivity of liquid Co	$λ l C o$	42.42	W·K^-1·m^-1
Thermal conductivity of liquid Ti	$λ l T i$	36.82	W·K^-1·m^-1
Thermal conductivity of solid Gd	$λ s G d$	8.0	W·K^-1·m^-1
Thermal conductivity of solid Co	$λ s C o$	69.04	W·K^-1·m^-1
Thermal conductivity of solid Ti	$λ s T i$	21.8	W·K^-1·m^-1
Density of liquid Gd	$ρ l G d$	7410 - 0.46(T - 1585)	kg·m^-3
Density of liquid Co	$ρ l C o$	7750 - 1.09(T - 1768)	kg·m^-3
Density of liquid Ti	$ρ l T i$	4130 - 0.23(T - 1941)	kg·m^-3
Density of solid Gd	$ρ s G d$	7900	kg·m^-3
Density of solid Co	$ρ s C o$	8860	kg·m^-3
Density of solid Ti	$ρ s T i$	4510	kg·m^-3
Specific heat capacity of liquid Gd	$c p l, G d$	213	J·kg^-1·K^-1
Specific heat capacity of liquid Co	$c p l, C o$	590	J·kg^-1·K^-1
Specific heat capacity of liquid Ti	$c p l, T i$	700	J·kg^-1·K^-1
Specific heat capacity of solid Gd	$c p s, G d$	116	J·kg^-1·K^-1
Specific heat capacity of solid Co	$c p s, C o$	427	J·kg^-1·K^-1
Specific heat capacity of solid Ti	$c p s, T i$	500	J·kg^-1·K^-1
Latent heat of solidification of pure Gd	$L G d$	9.87 × 10⁴	J·kg^-1
Latent heat of solidification of pure Co	$L C o$	2.63 × 10⁵	J·kg^-1
Latent heat of solidification of pure Ti	$L T i$	3.66 × 10⁵	J·kg^-1

Table 1 Thermo-physical parameters of Gd-Co-Ti system^[43]

Fig.7 Dependence of temperature at the center of the Gd-2%Co-2%Ti alloy samples with different diameters on time (t)

Fig.8 Supersaturation of the matrix liquid (S), nucleation rate (I_D) and number density (N_D) of the TiCo-rich droplets (a), equilibrium volume fraction (φ $l e$ ) and actual volume fraction (φ_l) of the TiCo-rich droplets, equilibrium volume fraction (φ $s m$ ) of the primary Gd-rich solid phase (b) at the center region of the Gd-2%Co-2%Ti alloy sample with a diameter of 445 μm as a function of t

Fig.9 Average radius (<R_D>) of the TiCo-rich droplets at the center region (a) and N_D of the TiCo-rich droplets at different positions (r) from the center (b) of the alloy sample with a diameter of 445 μm as a function of t (L₁ + L₂ + S represents liquid-liquid-solid three-phase region)

Fig.10 T₁, melt temperature (T_Melt), I_D (a) and N_D (b) of the TiCo-rich droplets at the center region of the Gd-2%Co-2%Ti alloy samples with diameters of 285 and 710 μm as a function of t

Fig.11 Maximum nucleation rate (I_DMax) of the TiCo-rich droplets and N_D of the TiCo-rich particles at the center region of the Gd-2%Co-2%Ti alloy samples as a function of the local cooling rate ( $T ˙ n u c$ ) during the nucleation period

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