Microstructures of the phase transition of nano-magnesium hydroxide to nano-magnesium oxide by positron annihilation lifetime spectroscopy

Chunlong YAO; Zhejie ZHU; Jianjian SHI; Xuehui XU; Yichu WU

doi:10.11889/j.0253-3219.2018.hjs.41.090201

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Microstructures of the phase transition of nano-magnesium hydroxide to nano-magnesium oxide by positron annihilation lifetime spectroscopy

LOW ENERGY ACCELERATOR, RAY AND APPLICATIONS | 更新时间：2021-05-19

- Microstructures of the phase transition of nano-magnesium hydroxide to nano-magnesium oxide by positron annihilation lifetime spectroscopy
- NUCLEAR TECHNIQUES Vol. 41, Issue 9, Article number: 090201(2018)
- 作者机构：
  
  武汉大学物理科学与技术学院物理国家级实验教学示范中心(武汉大学) 湖北省核固体物理重点实验室武汉 430072
- 作者简介：
- 基金信息：
  
  National Natural Science Foundation of China
- DOI：10.11889/j.0253-3219.2018.hjs.41.090201
  CLC： TL99
- Received：13 April 2018，
  
  Revised：05 May 2018，
  
  Published：2018-09
- 稿件说明：
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Chunlong YAO, Zhejie ZHU, Jianjian SHI, et al. Microstructures of the phase transition of nano-magnesium hydroxide to nano-magnesium oxide by positron annihilation lifetime spectroscopy[J]. Nuclear techniques, 2018, 41(9): 090201
DOI：

Chunlong YAO, Zhejie ZHU, Jianjian SHI, et al. Microstructures of the phase transition of nano-magnesium hydroxide to nano-magnesium oxide by positron annihilation lifetime spectroscopy[J]. Nuclear techniques, 2018, 41(9): 090201 DOI： 10.11889/j.0253-3219.2018.hjs.41.090201.

摘要

用添加聚乙二醇（Polyethylene Glycol，PEG）表面活性剂的直接沉淀法合成氢氧化镁纳米粉末，将其在不同温度下煅烧得到的纳米氢氧化镁和纳米氧化镁，采用正电子湮没寿命谱（Positron Annihilation Lifetime Spectroscopy，PALS）、X射线衍射（X-ray Diffraction，XRD）、热重分析（Thermal Gravimetric Analysis，TGA）、场发射扫描电子显微镜（Field Emission Scanning Electron Microscope，FESEM）和氮气吸附脱附实验（N

adsorption-desorption）等方法研究了纳米氢氧化镁转变为氧化镁过程中的微观变化机制。研究结果表明：实验制得的纳米氢氧化镁为厚度15 nm左右的片状形貌，在300℃左右热分解为直径30 nm左右的纳米球状氧化镁，颗粒大小均匀，分散性较好。正电子寿命测量发现两个长寿命分量

、

分别反映样品内部微孔和介孔的信息，在250~300℃的相转变温度区间，

显著升高，同时

却迅速减小，说明纳米氢氧化镁转变氧化镁时介孔数量突然增大，而微孔的数量迅速减少。由改进的Tao-Eldrup模型计算得到的孔径尺寸与氮气吸附脱附实验测量孔径分布的最可几孔径（2~4 nm）基本吻合，有理由推测在片状氢氧化镁转变球状的氧化镁时因晶粒长大、重组导致大量微孔发生迁移聚集成了较大的介孔；另一方面，水分子的脱离促进了晶粒内空位团和微孔不断产生、迁移和聚集。

Abstract

Background

Magnesium hydroxide and magnesium oxide are both important metal compounds with many excellent properties which make them have great application prospects in various fields of industry and environmental protection

such as flame-retardant

antibacterial agents

water/gas treatment

catalysts.

Purpose

This paper focus on analysis of the microstructure of magnesium hydroxide at different calcining temperatures

especially the changes of vacancy clusters and pores before and after phase transition temperature.

Methods

Nano-magnesium hydroxide was prepared by direct precipitation method with the addition of polyethylene glycol (PEG) surfactant and nano-magnesium oxide was obtained by calcining nano-magnesium hydroxide. The microstructure and defects of both magnesium hydroxide and magnesium oxide were investigated by positron annihilation lifetime spectroscopy (PALS)

X-ray diffraction (XRD)

thermal gravimetric analysis (TGA)

field emission scanning electron microscopy (FESEM) and nitrogen adsorption-desorption experiment.

Results

The original magnesium hydroxide particle prepared by direct precipitation method has flake -like morphology with about 15 nm thickness. Corresponding magnesium oxide is a sphere-like particle with a size of about 30 nm and good dispersivity. The positron lifetime measurement found that two long lifetime components

and

reflect the information of micropores and mesopores in the samples

respectively. When the nano-magnesium hydroxide transformed to nano-magnesium oxide in the temperature range of 250~300℃

relative intensity

increases significantly and

decreases rapidly

indicating that the number of mesopores increases suddenly

while the number of micropores decreases rapidly. The pore size calculated by the improved Tao-Eldrup model is consistent with the pore size (2~4 nm) measured by nitrogen adsorption-desorption experiment.

Conclusion

Flake-like nano-magnesium hydroxide was synthesized by precipitation method with the addition of PEG surfactant. Sphere-like nano-magnesium oxide was obtained by calcining nano-magnesium hydroxide in the temperature range of 300~700℃. During the phase transition from nano-magnesium hydroxide to nano-magnesium oxide

a large number of micropores are migrated and integrated into larger mesoporous pores because of growth and recombination of the grain. On the other hand

the removement of water molecules promotes formation

migration and aggregation of the vacancy clusters and microvoids.

关键词

Keywords

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