传压介质对晶格振动和相变压力的影响——α-Bi2O3的高压拉曼光谱研究

 本文分别使用4∶1的甲醇-乙醇混合溶液和固态氩做传压介质测量α-Bi₂O₃的高压拉曼光谱。实验结果表明，传压介质对样品的谱线频移速率及相变压力有明显的影响。通过对拉曼光谱的分析认定，α-Bi₂O₃在高压下可能经历了一次结构相变，在准静水压和非静水压条件下的相变压力分别为23.1 GPa和20.4 GPa。     

90 GPa（准）静水压力的产生及压力分布的测量

 本文使用固态氩做传压介质，在自制的Mao-Bell型金刚石对顶砧装置中获得了90 GPa的准静水压。通过测量样品室内不同位置上红宝石荧光R₁线的频移来确定压力分布。实验结果表明在80 GPa以下，样品室内不同位置上的压力与平均压力（p）的差Δp很小，最大的Δp/p不超过1.5%。在90 GPa时，红宝石的荧光R线与常压的很相似。这表明利用固态氩做传压介质可以获得接近100 GPa的准静水压。此外，对红宝石荧光光谱中位置在14 938 cm^-1和14 431 cm^-1两条谱线随压力的变化情况也作了讨论，并由此得出结论，14 938 cm^-1这条线也可用来标定压力。     

超高压下红宝石荧光R线的猝灭压力与入射激发线波长的关系

 分别使用固态氩和体积比为4∶1的甲醇-乙醇混合溶液做传压介质，测量红宝石在这两种介质中的荧光光谱随压力的变化。首先发现在超高压下红宝石荧光R线的压致猝灭与入射激发线波长以及高压样品室内的静水压程度有关。实验结果表明：入射激发线的波长越长，荧光R线的猝灭压力越低；对同一激发线波长，静水压程度差，猝灭压力高。这一现象归因于红宝石吸收谱中U带和Y带随压力的蓝移。     

甲醇作为压标的拉曼研究

 利用立方氧化锆压腔研究了甲醇在温度301 K、压力169.2~713.8 MPa下C—H伸缩振动ν_{2 835}的拉曼特征,实验结果表明：在试验的压力范围内甲醇稳定,其拉曼位移和压力具有很好的线性关系。加上常压下的数据,拟合后得出压力与甲醇2 835 cm^-1拉曼线频率位移的关系为：p= -3.508 9[(Δν_p)_{2 835}]²+135.17 (Δν_p)_{2 835}+54.397(0.1~713.8 MPa)。因此在实验的压力范围内甲醇作为压标非常合适。     

Ba3Bi3Ti4NbO18的压致结构相变

 利用Mao-Bell型金刚石对顶砧装置（DAC）,使用4∶1的甲醇-乙醇混合液作传压介质,研究了层状铁电固溶体Ba₃Bi₃Ti₄NbO₁₈的在位高压拉曼光谱和压致结构相变（0~8.87 GPa）。观测到了Ba₃Bi₃Ti₄NbO₁₈的一个典型的压致结构相变。发现了赝钙钛矿结构A₄B₅O₁₆的A位和B位联合置换对Ba₃Bi₃Ti₄NbO₁₈的拉曼振动模式及压致相变点的调制作用。并使用内模方法对Ba₃Bi₃Ti₄NbO₁₈的内模进行了指认。通过对加压下的拉曼光谱的分析,得到了压力作用下样品中BO₆八面体的结构畸变的演化方向。     

名义成分为La1.0Ca2.0Mn2O7锰氧化物的压阻效应

 利用低温高压电阻原位测量装置（自箝铍青铜活塞-圆筒式压砧），在0~1.05 GPa静水压力范围内，对以层状钙钛矿结构为主相、名义成分为La_1.0Ca_2.0Mn₂O₇的锰氧化物样品进行了压阻效应研究。实验观测到异常的压阻效应。在低温5~150 K范围内，压力为0.55 GPa时，样品呈现出高达40%的压阻效应，而且，金属-绝缘体相变温度在低压范围内随压力的增加而增加，但随着压力的进一步增加而减小。     

铝的等温状态方程

 采用原位高压同步辐射X射线衍射技术,利用金刚石对顶砧（DAC）装置产生高压,选用高纯NaCl粉末作为传压介质与标压物质,在室温下、21.5 GPa的压力范围内,测定了铝的等温状态方程。利用Murnaghan方程对实验结果进行了数值拟合,得到铝的零压体弹模量及其一级压力导数分别为B₀=(77±2) GPa,B₀′=4.8±0.3。该结果同相关文献资料报导的值在误差范围内符合得很好,略显得较大,这是由于传压介质NaCl的非静水压效应所致。在实验所达到的压力范围内,未发现明显的相变迹象。     

非金属晶体导热系数与压力和温度相关性

 讨论了非金属晶体的导热系数k与压力p和温度T的相互关系。从理论上导出了低压和低温下的两个实验拟合关系式，即K_T=A+Bp和k_p＝A₁+B₁/T，其中A、B、A₁、B₁为拟合常数。计算结果与实验结果符合得非常好。此外，还讨论了k在高压、高温及冲击压缩下的响应。     

钙钛矿（GaTiO3）高压相变及等温压缩

 高温高压条件下对钙钛矿（Perovstsite）多晶进行了研究，在金刚石压砧设备上压力条件最高达38 GPa，YAG莱塞加热温度近1 000 ℃以上，用红宝石荧光校压系统进行压力标定。实验结果表明静水压条件X射线就位测量，GaTiO₃(Ⅰ)由斜方晶系在10 GPa时直接向六方GaTiO₃(Ⅱ)结构相变，体积变化为1.6％；1 000 ℃加热及其非静水压条件下GaTiO₃(Ⅰ)由斜方晶系首先转变为四方晶系GaTiO₃(Ⅲ)转变压力为8.5 GPa，体积变化为0％，继续增加压力导15 GPa，GaTiO₃(Ⅲ)向GaTiO₃(Ⅱ')转化成六方晶系，体积变化亦为1.6％。三种高压相，在压力降到一个大气压时都会消失，所以是逆转化的非淬火相。等温压缩在标准静水压条件下进行，压力应小于10.4 GPa，K₀'=5.6时，K₀=(210±7)GPa，此数据是根据Birch-Murnaghan状态方程求得的体模量。     

百吉帕压力下固态氩的状态方程

 利用最新的X光衍射实验数据和Ar原子的弹性散射实验结果，得到了Ar原子间的相互作用和350 GPa下的固态氩的状态方程。这个状态方程可以作为超高压力下的压标。在150 GPa以上的压标，是目前高压研究中急需的。固态氩既可作为准静水压传压介质，又可作为高压X光衍射中的压标使用。本文计算了固态氩的Grüneisen参数、Debye特征参数、定容比热和等温体模量随压力的变化，压力范围为0~150 GPa。     

Dependence of the annihilation pressure of ruby R-line fluorescence on the laser exciting wavelength

Abstract

Using solid argon as pressure medium, quasi-hydrostatic pressure was obtained at room temperature in the diamond cell up to 90 GPa. The mechanism of the disappearance of ruby R lines and the applicability of ruby pressure scale under quasi-hydrostatic pressure above 100 GPa was discussed. The deviation of every pressure measured at nine positions in the cell per mean pressure was less than 1.5% at pressure below 80 GPa.     

On the phase-transition in anthracene induced by high pressure

The crystallographic structure of anthracene is studied under high pressure up to 27 GPa using diamond anvil cells. Different pressure-transmitting media (helium, a methanol-ethanol mixture, a normal- and iso-pentane mixture and no medium) were used up to specific critical pressures where the hydrostatic conditions are lost. It is clearly observed that the loss of hydrostaticity is associated with a crystallographic phase-transition in anthracene. The phase-transition is observed as reversible, and it is accompanied by a large hysteresis. These observations clarify conflicting reports in the literature on the high-pressure phase-transition of anthracene.     

富硼稀土硼化物NdB6的高温高压合成

 提出了一种在高温高压极端条件下合成富硼稀土硼化物NdB₆的新方法，即以稀土氧化物Nd₂O₃为钕源与单质硼反应的方法获得了稀土六硼化物NdB₆。并对合成产物进行了粉末X射线衍射分析。结果表明在配比为Nd：B＝1：6时，压力为4.0 GPa、温度为1 600 ℃、反应时间为15 min的条件下，获得了单相性非常好的NdB₆。高温高压合成NdB₆方法具有反应条件易达到、合成时间短、反应产物单相性好等优点。其XRD结果表明该合成产物为立方结构，晶格常数为a＝0.417 nm。     

Measurement of improved pressure dependence of superconducting transition temperature

We describe a technique for making electrical transport measurements in a diamond anvil cell at liquid helium temperature having in situ pressure measurement option, permitting accurate pressure determination at any low temperature during the resistance measurement scan. In general, for four-probe resistivity measurements on a polycrystalline sample, four fine gold wires are kept in contact with the sample with the help of the compression from the soft solid (usually alkali halides such as NaCl, KCl, etc.) acting as a pressure-transmitting medium. The actual pressure on the sample is underestimated if not measured from a ruby sphere placed adjacent to the sample and at that very low temperature. Here, we demonstrate the technique with a quasi-four-probe resistance measurement on an Fe-based superconductor in the temperature range 1.2–300 K and pressures up to 8 GPa to find an improved pressure dependence of the superconducting transition temperature.     

The difference between hydrostatic and nonhydrostatic compression of gold and iron

Abstract

We have measured the compression of gold to 300 kbar in NaCl, methanol-ethanol, argon, and to 1.1 Mbar in diamond powder as pressure transmitting media and of α-iron to 150 kbar under hydrostatic conditions using synchrotron radiation. Diamond powder as pressure medium yields the same results as in hydro-static experiments. For hydrostatic pressure conditions the bulk modulus of gold and iron is about 10% higher than from non-hydrostatic x-ray, ultrasonic, and shock experiments.     

Cobalt-doped magnesium oxide pressure-transmitting medium for high pressure and high-temperature apparatus

ABSTRACT

Magnesium oxide (MgO) doped with cobalt (Co) semi-sintered pressure-transmitting medium (MCOPM) was prepared at 1200°C in air, starting with a pre-compressed mixture of MgO and cobalt oxide (CoO). The samples were characterized using powder X-ray diffraction, scanning electron microscopy, and thermal conductivity measurements. The results demonstrate that during the sintering process, the exchange of metal ions between the mixture powders introduced lattice defects into the MgO lattice structure, and an MgO–CoO solid solution was formed. Compared to commercial semi-sintered MgO pressure-transmitting medium (SSMPM), the temperature-generation efficiency of MCOPM-17 (MgO?+?17?mol% CoO) improved by about 220% at the high pressure of 12?GPa with a cell assembly in a two-stage multi-anvil large volume press. Moreover, the thermal conductivity of CoO-doped MgO decreased with increasing CoO doping.     

细菌纤维素菌株超高压诱变选育及其发酵培养基的优化

 为了获得高产细菌纤维素菌株,对初选的细菌纤维素菌株J₂进行超高压诱变,运用Plackett-Burman设计对影响高压诱变菌株生产细菌纤维素的因素效应进行评价,采用Box-Behnken试验优化发酵培养基组成。试验结果表明,超高压诱变压力、时间对细菌纤维素菌株有显著或极显著影响。细菌纤维素菌株高压诱变条件为压力250 MPa、时间15 min、温度25 ℃。经超高压诱变,获得产纤维素能力高、遗传稳定性好的诱变菌株M₄₃₈。影响诱变菌株M₄₃₈发酵生产细菌纤维素的关键因子是酵母浸出汁、MgSO₄和无水乙醇。优化的发酵培养基为碳源5%（葡萄糖∶蔗糖为4∶1）、酵母浸出汁1.25%、CaCl₂0 15%、ZnSO₄ 0.20%、K₂HPO₄ 0.20%、MgSO₄ 0.93%、富马酸0.30%、无水乙醇0.50%。利用此培养基培养诱变细菌纤维素菌株M₄₃₈,其纤维素产量是优化前的1.84倍,是超高压诱变之前的2.69倍。超高压技术用于细菌纤维素菌株的诱变育种是可行的。发酵培养基的优化可显著提高菌株M₄₃₈发酵生产细菌纤维素的能力。