Evidence for the transition from primary to peritectic phase growth during solidification of undercooled ni-zr alloy levitated by electromagnetic field

ABSTRACT The Ni83.25Zr16.75 peritectic alloy was undercooled by electromagnetic levitation method up to 198 K. The measured dendritic growth velocity shows a steep acceleration at a critical

undercooling of Δ_T_crit = 124 K, which provides an evidence of the transition of the primary growth mode from Ni7Zr2 phase to peritectic phase Ni5Zr. This is ascertained by combining the

temperature-time profile and the evolution of the solidified microstructures. Below the critical undercooling, the solidified microstructure is composed of coarse Ni7Zr2 dendrites,

peritectic phase Ni5Zr and eutectic structure. However, beyond the critical undercooling, only a small amount of Ni7Zr2 phase appears in the solidified microstructure. The dendritic growth

mechanism of Ni7Zr2 phase is mainly governed by solute diffusion. While, the dendritic growth mechanism of Ni5Zr phase is mainly controlled by thermal diffusion and liquid-solid interface

atomic attachment kinetics. SIMILAR CONTENT BEING VIEWED BY OTHERS IN SITU SYNCHROTRON DIFFRACTION AND MODELING OF NON-EQUILIBRIUM SOLIDIFICATION OF A MNFECONICU ALLOY Article Open access 15

March 2021 THE EFFECT OF PHOSPHORUS ON SOLIDIFICATION BEHAVIOUR OF UNDERCOOLED AL–70 WT.%SI ALLOYS Article Open access 26 October 2020 STUDY ON ISOTHERMAL CRYSTALLIZATION KINETICS OF

ZR55.7CU22.4NI7.2AL14.7 BULK AMORPHOUS ALLOY Article Open access 24 March 2022 INTRODUCTION Peritectic solidification is frequently encountered among metallic alloy systems, such as Fe-Ni,

Fe-Al, Al-Ni, Ni-Zr, etc.1,2,3,4,5, which is of great importance in preparing various commercial component materials. Recently, a transition of the primary growth mode from primary phase to

peritectic phase during the solidification of undercooled peritectic alloys has been paid considerable attention6,7,8,9,10. The underlying reason is that the transition of the primary growth

mode may result in the formation of phase-pure peritectic phase in the final solidified microstructure, and thus improve the performance of peritectic alloys7. Tourret _et al_.4,5

investigated the multiple phase transformations of Al-Ni peritectic alloys by electromagnetic levitation and gas atomization methods, and found that peritectic phase Al3Ni preferentially

grows when the droplet diameter is 10 μm for gas atomized Ni-80 at% Al hyperperitectic alloy, which is attributed to the competition between the cooling kinetics and the diffusion kinetics.

Phanikumar _et al_.11 found that once the undercooling (unless stated otherwise, any mention of undercooling in the paper refers to nucleation undercooling) exceeds a critical value of about

110 K, the solidified microstructure consists of only peritectic phase in Fe-25%Ge peritectic alloy processed by an electromagnetic levitator. Leonhardt _et al_.12 reported that a

transition of the primary growth mode from primary bcc-Mo to peritectic σ-phase was revealed if the undercooling of Fe47Mo53 alloy is beyond 345 K. However, although some significant

progresses have been reported, direct experimental evidence of the transition of the primary growth mode from the primary phase to peritectic phase is rather limited. Previous studies

revealed this transition of primary growth mode mainly by the evolution of solidified microstructures. Actually, dendritic growth is the major growth mode in undercooled melts, the velocity

of which can provide valuable insight into the transition of primary growth mode. Nevertheless, few investigations of dendritic growth kinetics in undercooled peritectic alloys have been

reported. As a typical peritectic alloy system, Ni-Zr binary alloy system has aroused particular interests due to its good glass forming ability in a wide compositional range13,14,15 as well

as its abundant intermetallic compounds16,17,18. Ni83.25Zr16.75 is a peritectic composition in Ni-Zr alloy system, whose primary phase and peritectic phase are both intermetallic compounds.

The solidification behavior for this type of peritectic alloy is complicated but also considerably important for deep and comprehensive understanding of peritectic solidification under

highly undercooled condition. Therefore, the objective of this work is to investigate the transition of the primary growth mode from Ni7Zr2 phase to peritectic phase Ni5Zr during the

solidification of undercooled Ni83.25Zr16.75 peritectic alloy by the measured dendritic growth velocity and solidified microstructures. Meanwhile, the dendritic growth kinetics of Ni7Zr2

phase and Ni5Zr phase is also studied to reveal the evolution of solidified microstructure. RESULTS AND DISCUSSION The high-speed camera technique can allow the visualization of the

propagation front, which is a feasible approach to investigate the rapid solidification process. Figure 1 shows a few snapshots of rapid solidification front in undercooled Ni83.25Zr16.75

peritectic melts at different undercoolings, which were captured by a Red-lake HG 100 K high-speed camera with the resolution of 24 bits (color) pixel depth. The yellow area corresponds to

the solid due to the released heat, and the red area corresponds to the undercooled liquid. Noticeably, solidification starts at the upper surface of the sample and proceeds to the lower

part. The propagating front appears ambiguous for low undercooling, and gives distinct feature of dendritic structure for high undercooling. The dendritic growth velocity can be determined

from the sequence of projected images captured by the high-speed camera, which is coincident with the value measured by a photoelectric detector. The results of dendritic growth velocity

with different undercoolings in Ni83.25Zr16.75 melts are presented in Fig. 2(a), which was measured by a photoelectric detector. The maximum undercooling obtained in the present work is

about 198 K. It is obvious that the measured dendritic growth velocity continuously increases with the enhancement of the undercooling. When the undercooling is smaller than a critical value

of Δ_T_crit = 124 K, the growth velocity appears sluggishly. Once the undercooling exceeds the critical value of Δ_T_crit = 124 K, the growth velocity increases rapidly. More importantly, a

steep rise of the growth velocity is observed at the critical undercooling of Δ_T_crit = 124 K, which jumps from 61 mm/s to 88 mm/s. Such a phenomenon implies that a transition of the

primary growth mode from Ni7Zr2 phase to peritectic phase Ni5Zr occurs. The equilibrium solidification of Ni7Zr2 phase is replaced by the direct growth of peritectic phase Ni5Zr if the

undercooling exceeds the critical value of Δ_T_crit = 124 K. As for Ni83.25Zr16.75 peritectic alloy, the liquidus temperature of Ni7Zr2 phase is just higher than that of Ni5Zr phase by about

39 K. If the undercooling of the melt goes through the peritectic temperature _T_p, the peritectic phase Ni5Zr becomes a metastable phase and may form directly from the undercooled melt

despite the low thermodynamic driving force. Our previous study3 has revealed that the peritectic phase Ni5Zr can form directly from the undercooled melt by completely suppressing the growth

of Ni7Zr2 phase if the droplet diameter is less than a critical value in the drop tube experiments. To verify the transition of the primary growth mode, the temperature-time curves during

undercooling and rapid solidification of Ni83.25Zr16.75 peritectic melts at two different undercoolings are illustrated in Fig. 2(b). The recalescence behavior is characterized by a steep

temperature rise detected by the pyrometer. For low undercooling of 58 K, the temperature of the melt after recalescence rises nearly to the liquidus temperature _T_L, which gives an

indication of growth of primary Ni7Zr2 dendrites. However, for high undercooling of 160 K, the recalescence process is observed to stop below the peritectic temperature _T_P. This may give

an evidence for a change of growth mode that the growth of Ni7Zr2 phase is replaced by the growth of peritectic phase Ni5Zr if the undercooling exceeds the critical value of 124 K. The

microstructures of Ni83.25Zr16.75 peritectic samples solidified at different undercoolings are shown in Fig. 3, in which both the Ni7Zr2 phase and Ni5Zr phase have been marked. The

solidified microstructure consists of Ni7Zr2 dendrites, peritectic phase Ni5Zr and inter-dendritic eutectic microstructure for low undercooling of Δ_T_ = 9 K, as illustrated in Fig. 3(a).

Apparently, the Ni7Zr2 phase exhibits coarse and developed dendrites, which is enwrapped by peritectic phase Ni5Zr. Figure 3(b) is an enlarged view of the inter-dendritic eutectic

microstructure. It can be seen that the morphology is characterized by rod-like eutectic structure, which is the mixture of (Ni) and Ni5Zr phases. With the enhancement of undercooling, the

fragment of Ni7Zr2 dendrites occurs which seems like the primary Ni7Zr2 dendrite trunks have partially been transformed to peritectic phase, and the fragmented zone is marked as a box, as

shown in Fig. 3(c). However, when the undercooling is beyond the critical value of Δ_T_crit = 124 K, a significant change of microstructure takes place. The solidified microstructure for a

high undercooling of Δ_T_ = 160 K is composed of a small amount of Ni7Zr2 phase, predominant Ni5Zr phase and eutectic microstructure, as presented in Fig. 3(d). It is evident that the amount

of Ni7Zr2 phase is very low, and the Ni7Zr2 phase seems to be decomposed and nearly disappears. To further confirm the variation of phase constitution, X-ray diffraction (XRD) patterns of

samples solidified at two different undercoolings of 77 K and 160 K are shown in Fig. 4. It can be seen that the main peaks of Ni7Zr2 phase decrease sharply with the increasing undercooling.

On the contrary, the peaks of Ni5Zr phase increase with the enhancement of undercooling. This indicates that the volume fraction of Ni5Zr phase at high undercooling is larger than that at

low undercooling. According to the above microstructures presented in Fig. 3, two growth modes can be concluded. If the undercooling is smaller than the critical value of Δ_T_crit = 124 K,

the Ni7Zr2 phase is preferred to primarily nucleate and grow into the manner of dendrites during the rapid solidification of the undercooled melt, which results in a sudden temperature rise

due to the released heat of crystallization. Subsequently, with the decrease of temperature, the peritectic phase Ni5Zr starts to nucleate at the surface of the Ni7Zr2 dendrites when the

temperature drops below the peritectic temperature _T_P. In this case, the primary Ni7Zr2 dendrites, peritectic phase Ni5Zr and liquid phase will contact with each other at a triple

junction, which is the requirement of peritectic reaction. Then, peritectic reaction of Ni7Zr2 + L → Ni5Zr takes place and peritectic phase Ni5Zr grows along the surface of Ni7Zr2 dendrites

to form a thin peritectic layer. Peritectic reaction, which is governed by local short range diffusion of the solute in the melt ahead of the primary Ni7Zr2 dendrites and peritectic phase

Ni5Zr, can proceed rapidly at the initial stage of the peritectic growth process. Whereas, once the primary Ni7Zr2 dendrites are enwrapped by peritectic phase Ni5Zr, peritectic phase Ni5Zr

will separate the primary phase Ni7Zr2 and liquid phase, leading to the disappearance of the triple junction and the cease of peritectic reaction. After which, the peritectic phase Ni5Zr

grows into the primary Ni7Zr2 dendrites by peritectic transformation. Since the peritectic transformation is controlled by long range solid-state diffusion, it proceeds sluggishly.

Unfortunately, the cooling rate in the experiments is about 15 K/s, which results in that peritectic transformation could not proceed completely11 and only a small amount of primary

dendrites could transform to peritectic phase by peritectic transformation. Therefore, the primary phase is always retained in the final microstructures after peritectic solidification, as

shown in Fig. 3(a–c). Due to the existence of the Ni7Zr2 phase, the composition of residual liquid deviates from the initial composition of the melt and moves to eutectic zone according to

the phase diagram in Fig. 2(c). Hence, the residual liquid solidifies as eutectic when the temperature drops below the eutectic temperature, which is presented in Fig. 3(b). Once the

undercooling exceeds the critical value of Δ_T_crit = 124 K, there exists only a small amount of Ni7Zr2 phase in the solidified microstructure, as illustrated in Fig. 3(d). There are two

possible solidification paths for the formation of such a microstructure. The first possibility is that only a small amount of Ni7Zr2 phase forms first but peritectic phase Ni5Zr prefers to

grow from the undercooled melts. Thus, the microstructure is composed of predominant peritectic phase Ni5Zr and a small amount of Ni7Zr2 phase. The second possibility is that Ni5Zr phase

primarily grows in the undercooled melt. Since the atoms of different species have to sort themselves onto proper lattice place during the growth of intermetallic compounds, the growth

velocity of Ni5Zr phase is sluggish. The released heat of crystallization results in a steep rise of temperature and a decrease of interface undercooling. Thus, the growth of peritectic

Ni5Zr phase cannot proceed to completion and a small amount of liquid remains in the inter-dendritic region. The undercooling of residual liquid after recalescence is smaller than 124 K

according to the temperature data in Fig. 2(b). In this case, Ni7Zr2 is preferred to grow from the residual undercooled liquid. Actually, due to less released heat and high cooling rate

during the solidification of Ni7Zr2 phase, the second recalescence is difficult to distinguish from the undulations in the pyrometer signal in Fig. 2(b). The second possibility is more

likely to occur according to our previous study3. We suggest that peritectic phase Ni5Zr preferentially grows when the undercooling is larger than 124 K. It is verified again that the

equilibrium solidification of Ni7Zr2 phase is replaced by the direct growth of peritectic phase Ni5Zr when the undercooling is beyond the critical value of 124 K. A heat flux from the melt

to the surrounding is necessary during the solidification, which is dominated by cooling rate. If the cooling rate of undercooled Ni83.25Zr16.75 melt is sufficiently high, the

crystallization heat would be rapidly transferred to the surrounding during the growth of peritectic phase Ni5Zr. This will result in the continuous growth of peritectic phase Ni5Zr and the

formation of phase-pure peritectic phase Ni5Zr microstructure. In the case of electromagnetic levitation, heat is mainly transferred by flowing helium gas. To obtain high cooling rate and

verify the speculation, a Ni83.25Zr16.75 sample was undercooled up to 160 K and then quenched on a Cu-substrate. The cross-sectional micrographs of different zones in the quenched sample are

shown in Fig. 5. Figure 5(b) presents the microstructure away from the Cu-substrate, which consists of Ni7Zr2 dendrites, peritectic phase Ni5Zr and eutectic. The microstructures on the

Cu-substrate side are illustrated in Fig. 5(c,d). Obviously, the microstructure is composed of two regions. The upper one is characterized by the primary Ni7Zr2 dendrites enveloped by

peritectic phase Ni5Zr. The below one adjacent to the Cu-substrate consists of only peritectic phase Ni5Zr with no primary phase Ni7Zr2 because high cooling rate is obtained at the interface

between the Cu-substrate and melt. To check the reproducibility of the observation, the quench experiments were performed on two samples and the results agree well. This suggests that

peritectic phase Ni5Zr directly solidifies by completely suppressing the growth of the primary Ni7Zr2 dendrites. Furthermore, this is an evident proof for the transition of the primary

growth mode from Ni7Zr2 phase to peritectic Ni5Zr phase when the undercooling exceeds the critical value of 124 K. Dendritic growth is the major growth mode in undercooled melts, which

determines the evolution of the solidified microstructure. Meanwhile, dendritic growth is controlled by the temperature and concentration gradients, resulting from the heat and solute

transport around the solid-liquid interface. To analyze the dendrites growth kinetics of Ni7Zr2 and Ni5Zr, a LKT/BCT model19,20,21 is adopted to describe the dendritic growth as a function

of undercooling. The physical parameters used in the calculations are obtained by molecular dynamics simulation and linearly fitting the values of pure metals22, which are listed in Table 1.

The calculated dendritic growth velocities of Ni7Zr2 and Ni5Zr phase are shown in Fig. 2(a). Evidently, the calculated results of Ni7Zr2 phase are in good agreement with the experimental

results when the undercooling is smaller than 80 K. The dendritic growth mechanism of Ni7Zr2 phase is mainly governed by solute diffusion. Similarly, the calculated dendritic growth velocity

of Ni5Zr phase is also close to the experimental values. The initial composition of the melts is the same as that of peritectic phase Ni5Zr. Hence, if peritectic phase Ni5Zr preferentially

grows, mass transport by segregation and constitutional effects can be neglected23, thus, the constitutional undercooling Δ_T_c = 0. The curvature undercooling is usually small due to the

large curvature radius of dendrites, which also can be neglected. Therefore, the dendritic growth of Ni5Zr phase is controlled by thermal undercooling and kinetic undercooling. In other

words, thermal diffusion and liquid-solid interface atomic attachment kinetics play a vital role in determining the growth velocity of Ni5Zr phase. CONCLUSION In summary, the dendritic

growth in undercooled Ni83.25Zr16.75 peritectic alloy was investigated by electromagnetic levitation method. The maximum undercooling achieved in the experiment is 198 K. The dendritic

growth velocity shows a steep acceleration around a critical undercooling of Δ_T_crit = 124 K, which gives the evidence of the transition of the primary growth mode from Ni7Zr2 phase to

Ni5Zr phase. This is ascertained by combining the temperature-time profile and the evolution of the microstructures. The solidified microstructure is composed of coarse Ni7Zr2 dendrites,

peritectic phase Ni5Zr and eutectic structure when the undercooling is less than the critical undercooling of Δ_T_crit = 124 K. However, only a small amount of Ni7Zr2 phase appears in the

solidified microstructure once the undercooling exceeds the critical value of 124 K, which indicates that the peritectic phase Ni5Zr primarily solidifies. Furthermore, In the case of

dropping the undercooled sample of 160 K onto a Cu-substrate, the microstructure of the quenched sample adjacent to the Cu-substrate consists of only peritectic phase Ni5Zr with no primary

phase Ni7Zr2, which suggests that peritectic phase Ni5Zr directly solidifies by completely suppressing the growth of the primary phase Ni7Zr2. The dendritic growth mechanism of Ni7Zr2 phase

is mainly governed by solute diffusion. However, thermal diffusion and liquid-solid interface atomic attachment kinetics play a vital role in determining the growth velocity of Ni5Zr phase.

EXPERIMENTAL DETAILS Master alloys of Ni83.25Zr16.75 peritectic alloy were prepared by 99.99% pure Ni and 99.9% pure Zr mixtures in an arc melting furnace. The samples of about 0.6 g were

levitated and melted by an electromagnetic levitation facility, which was evacuated to 10−5 Pa and backfilled with argon gas to 1 atm. The sample was cooled with flowing helium gas to

achieve substantial undercooling. Its temperature was measured using a one-color Raytek Marathon MR1SCSF infrared pyrometer, which was calibrated by a PtRh30-PtRh6 thermocouple. The

dendritic growth velocity was determined from the recalescence time measured by a photoelectric detector. The solidified samples and phase constitution were analyzed by a Phenom Pro SEM and

a Rigaku D/max 2500 X-ray diffractometer (XRD). ADDITIONAL INFORMATION HOW TO CITE THIS ARTICLE: Lü, P. _et al_. Evidence for the transition from primary to peritectic phase growth during

solidification of undercooled Ni-Zr alloy levitated by electromagnetic field. _Sci. Rep._ 6, 39042; doi: 10.1038/srep39042 (2016). PUBLISHER'S NOTE: Springer Nature remains neutral with

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Binary alloy phase diagram Vol. 3, 1249 (ASM international, 1990). Download references ACKNOWLEDGEMENTS This work is financially supported by National Natural Science Foundation of China

(Grant No. 51474175, 51506182 and 51522102) and Shaanxi Industrial Science and Technology Project (Grant No. 2015GY138). We would like to thank the director of LMSS, Prof. B. Wei, for his

consistent support. The authors are grateful to Dr. J. Chang, Dr. L. Hu, Mr. S. J. Yang and Mr. X. Cai for their help with the experiments. AUTHOR INFORMATION AUTHORS AND AFFILIATIONS *

Department of Applied Physics, MOE Key Laboratory of Space Applied Physics and Chemistry, Northwestern Polytechnical University, Xi’an, 710072, P.R. China P. Lü, K. Zhou & H. P. Wang

Authors * P. Lü View author publications You can also search for this author inPubMed Google Scholar * K. Zhou View author publications You can also search for this author inPubMed Google

Scholar * H. P. Wang View author publications You can also search for this author inPubMed Google Scholar CONTRIBUTIONS P. Lü and H.P. Wang designed the experiments. P. Lü carried out the

experiments and wrote the paper. H.P. Wang and K. Zhou revised this paper. ETHICS DECLARATIONS COMPETING INTERESTS The authors declare no competing financial interests. RIGHTS AND

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P., Zhou, K. & Wang, H. Evidence for the transition from primary to peritectic phase growth during solidification of undercooled Ni-Zr alloy levitated by electromagnetic field. _Sci Rep_

6, 39042 (2016). https://doi.org/10.1038/srep39042 Download citation * Received: 14 June 2016 * Accepted: 17 November 2016 * Published: 13 December 2016 * DOI:

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