Dispersant-assisted preparation of ultra-fine HfB2 powder

Various HfB2 powders were prepared by coprecipitation method combined with carbothermal reduction method, and were characterized by XRD, SEM, TEM, XPS, NMR, FTIR, TGA-DSC, etc. using the instrument platform of the Chinese Academy of Sciences to obtain the original experimental data. Philips X’Pert powder X-ray diffractometer using CuKα (PANalytiacl X’Pert-Pro MPD,USA, λ = 0.15419 nm) radiation. Field emission scanning electron microscope (FESEM, Hitachi SU8020, Japan) and field emission transmission electron microscope (FETEM, Tecnai G2 F20, USA) were used to study the microscopic morphology and structure of samples. An X-ray photoelectron spectrometer (XPS, KRATOS AXIS SURPRA+, Japan) was performed to investigate the valence bonds and surface chemical status of the samples. Thermogravimetric-differential thermal analysis (TGADSC) was performed in an argon atmosphere at a heating rate of 5 ◦C/ min (METTLER-TOLEDO, TGA/DSC 3+, Switzerland). Fourier transform infrared (FTIR, Thermo Nicolet Corporation, NEXUS G2192, USA) analysis was performed in the range of 500–4000 cm- 1 using the KBr pellet method. Nitrogen and oxygen analyzer (LECO, ON836 series elements analyzer, USA) was used to determine the oxygen content of the samples. 1H Nuclear Magnetic Resonance (1H NMR) spectra were taken on Avance 400 spectrometer (Bruker, AVANCE 400, USA) with Methanol-D4 as the solvent and chemical shift references for 1H NMR.The experiment was completed from September 2021 to August 2022.

本数据集通过共沉淀法结合碳热还原法制备了多种二硼化铪（HfB2）粉末，依托中国科学院的仪器平台，采用X射线衍射（XRD）、扫描电子显微镜（SEM）、透射电子显微镜（TEM）、X射线光电子能谱（XPS）、核磁共振（NMR）、傅里叶变换红外光谱（FTIR）、热重-差示扫描量热法（TGA-DSC）等多种表征手段获取原始实验数据。采用PANalytical X’Pert-Pro MPD型粉末X射线衍射仪（使用CuKα辐射，波长λ=0.15419 nm，美国）完成物相表征。借助场发射扫描电子显微镜（FESEM，日立SU8020，日本）与场发射透射电子显微镜（FETEM，Tecnai G2 F20，美国）分析样品的微观形貌与微观结构。通过X射线光电子能谱仪（XPS，KRATOS AXIS SURPRA+，日本）探究样品的价键状态与表面化学状况。热重-差示扫描量热分析（TG-DSC）在氩气气氛下进行，升温速率为5 ℃/min，所用仪器为METTLER-TOLEDO TGA/DSC 3+（瑞士）。傅里叶变换红外光谱（FTIR，赛默飞世尔Nicolet公司NEXUS G2192，美国）测试采用溴化钾压片法，测试波数范围为500~4000 cm⁻¹。使用氮氧元素分析仪（LECO ON836系列元素分析仪，美国）测定样品的氧含量。氢核磁共振（¹H NMR）谱图在Avance 400光谱仪（布鲁克AVANCE 400，美国）上采集，以氘代甲醇（Methanol-D4）为溶剂，并以其作为¹H NMR的化学位移参考物。本实验于2021年9月至2022年8月间完成。