In-situ crystallization study of amorphous Ni-P nanoparticles with high P content

Y. Tan, D. Sun, B. Yang, Y. Gong, S. Yan, R. Du, H. L. Guo, W. Chen, X. Xing, G. Mo, Z. J. Chen, Q. Cai, Z. H. Wu, H. Y. Yu
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引用次数: 1

Abstract

The crystallization behavior of amorphous Ni-P nanoparticles produced by liquid pulsed-discharge was studied by using in situ high temperature XRD at beamline 4B9A of Beijing Synchrotron Radiation Facility. Transmission electron microscope (TEM) was used to observe the morphology and Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) was used to analyze the chemical composition of the as-prepared Ni-P nanoparticles. TEM results show that the average size of the as-prepared nanoparticles is about 13.5 nm. ICP-AES identifies the Ni-P nanoparticles contain 13.16 wt. % (21.85 at. %) of P and 86.84 wt. % (78.15% at. %) of Ni. Eight XRD patterns were, respectively, collected at 300, 373, 473, 573, 673, 773, 873 and 973K under low-vacuum condition (0.1 Pa). XRD results show that the as-prepared Ni-P nanoparticles are amorphous, no peaks of crystalline phases can be observed until 573K. Afterwards, the crystallization of the amorphous phase undergoes the formation and decomposition of some metastable phases. Finally, the obtained stable phases are the bct Ni3P and fcc Ni cryatalline phases. Both are randomly distributed in the sample. The crystallization mechanisms of the as-prepared amorphous Ni-P nanoparticles has also been discussed at the end of this paper.
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高磷非晶Ni-P纳米颗粒原位结晶研究
在北京同步辐射装置4B9A束线上,利用原位高温XRD研究了液体脉冲放电制备的非晶态Ni-P纳米颗粒的结晶行为。采用透射电镜(TEM)观察形貌,电感耦合等离子体原子发射光谱(ICP-AES)分析制备的Ni-P纳米颗粒的化学成分。TEM结果表明,制备的纳米颗粒的平均尺寸约为13.5 nm。ICP-AES鉴定出Ni-P纳米颗粒含有13.16 wt. % (21.85 at。%)和86.84 %(78.15%)。%)的Ni。在低真空(0.1 Pa)条件下,分别在300、373、473、573、673、773、873、973K处采集了8种XRD图谱。XRD结果表明,制备的Ni-P纳米颗粒为非晶态,在573K温度下均未出现晶相峰。之后,非晶相的结晶经历了一些亚稳相的形成和分解。最后,得到的稳定相是bct Ni3P和fcc Ni结晶相。两者都是随机分布在样本中的。本文最后还对制备的非晶Ni-P纳米粒子的结晶机理进行了讨论。
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