Mechanochemical preparation of a modified NiAl2O4 structure,Faraday Discussions

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Mechanochemical preparation of a modified NiAl2O4 structure
Faraday Discussions ( IF 3.3 ) Pub Date : 2022-07-14 , DOI: 10.1039/d2fd00099g
Maria Elena Rivas ₁ , Charlotte Blakiston ₁ , Riho T Seljamäe-Green ₁ , Trung Dung Tran ₁ , David Thompsett ₁ , Stephen Day ₁ , Edward Bilbe ₁ , Janet Fisher ₁

Affiliation

Mechanochemical synthesis routes offer a sustainable, simple method for preparing materials. In this work, NiAl₂O₄ was synthesised by a mechanically activated method using a high-energy planetary mill and a calcination step. This study aims to identify the effect of different milling energies on the phases, chemical environments and surface composition of the material. In addition, it explores the thermal impact on the decomposition and structure of the materials. The materials were characterised by X-ray phosphorescence (XPS), solid-state UV-VIS (SS-UV-VIS), X-ray diffraction (XRD), nuclear magnetic resonance (NMR), high-resolution transmission electron microscopy (HR-TEM) and thermal gravimetry differential scanning calorimetry (TGA-DSC). A co-precipitated material is used as a reference along with the ground reagents which were used as a baseline. From this in-depth analysis of the material, a good understanding of the disordered partially inverse spinel structure is provided. This study has found that with calcination temperatures of 750 °C and 900 °C a mixed NiAl₂O₄ : NiO phase is produced with a Ni enriched surface. The surface is found to be relatively stable with the increase from 750 °C to 900 °C.

中文翻译：

改性NiAl2O4结构的机械化学制备

机械化学合成路线提供了一种可持续的、简单的材料制备方法。在这项工作中，NiAl ₂ O ₄是通过使用高能行星磨和煅烧步骤的机械活化方法合成的。本研究旨在确定不同研磨能量对材料的相、化学环境和表面组成的影响。此外，它还探讨了热对材料分解和结构的影响。通过X射线磷光（XPS）、固态紫外-可见（SS-UV-VIS）、X射线衍射（XRD）、核磁共振（NMR）、高分辨率透射电子显微镜（HR）对材料进行了表征。 -TEM）和热重差示扫描量热法（TGA-DSC）。共沉淀材料与用作基线的研磨试剂一起用作参考。通过对材料的深入分析，提供了对无序部分反尖晶石结构的良好理解。这项研究发现，在 750 °C 和 900 °C 的煅烧温度下，混合的 NiAl₂ O₄ ：NiO相产生具有富含Ni的表面。随着温度从 750 °C 升高到 900 °C，发现表面相对稳定。

更新日期：2022-07-14

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