Synthesis experiments on in-Sb and B-Sb systems in a laser heated diamond-anvil cell

Abstract

High pressure and high temperature synthesis experiments were carried out on In-Sb and B-Sb systems with a laser heated diamond-anvil cell. InSb was synthesized starting from In and Sb at various pressures ranging from 0.2 to 10 GPa. The cubic as well as the high pressure phases were successfully synthesized. Experiments above 8 GPa, wherein antimony exists in the tetragonal phase, have revealed no new phases of InSb. Trials of synthesizing a compound from B and Sb gave negative result to at least 30 GPa.     

Synthesis of Ge-Sn at high pressure and high temperature in a laser-heated diamond anvil cell

Ge–Sn compound is predicted to be a direct band gap semiconductor with a tunable band gap. However, the bulk synthesis of this material by conventional methods at ambient pressure is unsuccessful due to the poor solubility of Sn in Ge. We report the successful synthesis of Ge–Sn in a laser-heated diamond anvil cell (LHDAC) at ~7.6 GPa &; ~2000 K. In situ Raman spectroscopy of the sample showed, apart from the characteristic Raman modes of Ge TO (Г) and β-Sn TO (Г), two additional Raman modes at ~225 cm^?1 (named Ge–Sn₁) and ~133 cm^?1 (named Ge–Sn₂). When the sample was quenched, the Ge–Sn₁ mode remained stable at ~215 cm^?1, whereas the Ge–Sn₂ mode had diminished in intensity. Comparing the Ge–Sn Raman mode at ~225 cm^?1 with the one observed in thin film studies, we interpret that the observed phonon mode may be formed due to Sn-rich Ge–Sn system. The additional Raman mode seen at ~133 cm^?1 suggested the formation of low symmetry phase under high P–T conditions. The results are compared with Ge–Si binary system.     

硼氢协同掺杂Ib型金刚石大单晶的高温高压合成与电学性能研究

在压力6.0 GPa和温度1600 K条件下, 利用温度梯度法研究了(111)晶面硼氢协同掺杂Ib型金刚石的合成. 傅里叶红外光谱测试表明: 氢以sp³杂化的形式存在于所合成的金刚石中, 其对应的红外特征吸收峰位分别位于2850 cm^-1和2920 cm^-1处. 此外, 霍尔效应测试结果表明: 所合成的硼氢协同掺杂金刚石具有p型半导体材料特性. 相对于硼掺杂金刚石而言, 由于氢的引入导致硼氢协同掺杂金刚石电导率显著提高. 为了揭示硼氢协同掺杂金刚石电导率提高的原因, 对不同体系进行了第一性原理理论计算, 计算结果表明其与实验结果符合. 该研究对金刚石在半导体领域的应用有重要的现实意义.     

La0.3Sr0.7CrO3钙钛矿化合物高压合成和物性

 采用高压高温方法合成了单相的带宽调控型La_0.3Sr_0.7CrO₃ Mott化合物,对其晶体结构和磁学性质进行了研究。结果表明：La_0.3Sr_0.7CrO₃化合物具有立方钙钛矿晶体结构,温度在170 K以上其磁性为顺磁性,满足居里-外斯定律,温度低于20.7 K发生了自旋玻璃转变。     

In situ characterization of liquid network structures at high pressure and temperature using X-ray absorption spectroscopy coupled with the Paris-Edinburgh press

ABSTRACT

We review recent progress in studying structural properties of liquids using X-ray absorption spectroscopy coupled with the Paris-Edinburgh press at third-generation synchrotron facilities. This experimental method allows for detecting subtle changes in atomic arrangements of melts over a wide pressure–temperature range. It has been also employed to monitor variations of the local coordination environment of diluted species contained in glasses, liquids and crystalline phases as a function of the pressure and temperature. Such information is of great importance for gaining deeper insights into the physico-chemical properties of liquids at extreme condition, including the understanding of such phenomena as liquid–liquid phase transitions, viscosity drops and various transport properties of geological melts. Here, we describe the experimental approach and discuss its potential in structural characterization on selected scientific highlights. Finally, the current ongoing instrumental developments and future scientific opportunities are discussed.     

二维Rh-C60聚合相的制备和表征

 利用高压合成装置在6 GPa压力、700 ℃温度条件下合成了二维C₆₀聚合相,并用X射线衍射（XRD）和高分辨核磁共振（NMR）等方法对样品进行了表征。XRD分析结果表明,C₆₀分子在高温高压下发生了聚合反应,晶体结构由面心立方结构变为菱形结构,通过［2+2］加环反应在邻近分子间形成sp³杂化共价键。¹³C核磁共振魔角谱 （¹³C MAS NMR）在δ145和δ72处出现了两个共振峰,其中在δ145附近的峰展宽并有两个边带。δ145附近的峰的展宽与分裂主要是由于C₆₀分子上出现了不等价的sp²杂化碳和高温高压条件下产生的结构无序,边带的形成说明了其结构的各向异性;位置为δ72附近的峰证明了聚合物内C₆₀分子之间出现了sp³杂化键。     

大块钙钛矿MgSiO3和镁方铁矿(Mg,Fe)O的高压合成

 钙钛矿相MgSiO₃和镁方铁矿(Mg,Fe)O作为地球下地幔含量最丰富的候选矿物，其高温高压实验数据通常用来与地震学探测数据做对比，对限定下地幔的真实矿物学组分具有决定性的作用。但天然的钙钛矿相MgSiO₃和镁方铁矿(Mg,Fe)O很难得到，给这两种矿物的高温高压实验研究工作带来不便。介绍了应用活塞圆筒（Piston-Cylinder）压机和大腔体二级压砧（Mutli-Anvil）压机高温高压合成大块钙钛矿相MgSiO₃和不同Fe/Mg比的镁方铁矿(Mg,Fe)O样品的实验技术和实验方法，对所得到的样品进行了微区电子探针、拉曼光谱和X射线衍射分析。所得样品可以作为高压实验特别是冲击压缩实验的初始样品。     

New soft porous frameworks based on lambda-zirconium phosphate and aliphatic dicarboxylates: Synthesis and structural characterization

New dicarboxylate-functionalized pillared materials with a general formula of λ-ZrPO₄(OH)_1-x(OOC(CH₂)_nCOO)_x/2(dmso) (n=6, 8 and 10) have been prepared by post-synthesis modification of the inorganic layers of λ-zirconium phosphate (λ-ZrP), where the superficial Chloride monovalent anionic ligands of λ-layer are partially exchanged with the divalent anionic ligands of a series of long-chain aliphatic dicarboxylic acids, namely octanedioic acid, decanedioic acid and dodecanedioic acid. The synthesized materials are characterized by X-ray diffractometry, FT-IR spectrophotometry, elemental and thermogravimetric analyses. The X-ray diffraction patterns show that the obtained solid phases are pure. Furthermore, the interlayer distance of λ-ZrP systematically increases from 1.02 to 1.59 nm as a result of the incorporation of the mentioned acids inside the interlayer gallery.