静态超高压容器中温度、压力等参数的测试

本文对以叶蜡石为固体压力介质,石墨为发热体的立方体型超高压容器进行了温度、压力测定.给出了高温下的压力标定曲线和求解腔内温度的经验公式;对热电偶热电势的压力效应也进行了测定.并给出了近似的计算公式.实验中压力测至 61.5千巴,温度测至1600℃. 一、高温下的压力标定 本实验用金的熔融曲线对立方体型的超高压容器进行了高温下的压力标定.实验是在DS-29A型铰链式液压机上进行的. 实验方法是把套有氮化硼绝缘保护管的热电偶丝和黄金丝从叶蜡石(传压介质)的对角边插入.并垂直穿过合金片,使热结点在腔体中心部位.用电桥观察黄金丝熔融…     

金刚石压腔高温高压实验的压力标定方法及其现状

 介绍和评论了金刚石压腔中进行高温高压实验时的压力标定方法及其应用条件。其中红宝石和石英压标具有较高的准确度和精度,但前者不适合于高温和含饱和水条件下的标定,且在较低压力下误差较大,后者可用于高温且含水体系的压力标定,但仅适于低于2.0 GPa时的压力标定。矿物状态方程是较可靠的方法,但不方便且受条件限制。采用水的状态方程进行压力标定,可以解决压腔中不允许有压标矿物的问题,但在实验过程中要求压腔的体积保持恒定。因此,在采用金刚石压腔进行高温高压实验时,应根据研究需要决定合适的压力标定方法,而且寻找新的压力标定方法仍是金刚石压腔高压实验的基础工作。     

静态超高压高温技术的若干问题

本文简要阐述了准围压的超高压的测量方法与结果,测定并讨论了封垫摩擦镀层,叶蜡石尺寸对压力产生的影响,以及高压下传压介质的热学、力学性质与压力的关系。     

3 GPa熔融盐固体介质高温高压三轴压力容器的围压标定

 新研制的3 GPa熔融盐固体介质高温高压三轴实验系统,改进了高压容器的装样方式以及样品的尺寸,由于装样部件之间摩擦以及克服传压介质本身的强度,视载围压和真实围压具有较大差异,在完成压力容器温度标定的基础上,采用部分熔融法在不同温度和压力条件下进行围压标定实验研究。实验使用LiCl-KCl混合氯化盐样品,分别在300~1 400 MPa视载围压的条件下,对样品进行缓慢加温,成功观测到实验力学数据和温度数据的同时响应,确定了混合氯化盐的初熔温度,通过已知熔融曲线方程计算得出真实围压。通过比较不同的实验条件和观察实验后装样结构,给出了摩擦力的变化规律：在300~500 MPa压力条件下,摩擦力百分比呈现降低趋势,从52%降低到31.2%;在700~1 200 MPa压力条件下,摩擦力约占11.4%;在1 400 MPa压力条件下,摩擦百分比从11.4%上升到15.5%。通过对比国内外同类实验设备摩擦力认为,该设备真实围压的精度达到了国际同类设备的水平。     

叶蜡石高温高压相变的荧光光谱研究

 对合成金刚石过程中，叶蜡石经高温高压淬火后的不同部位进行了研究。发现叶蜡石的两条荧光线14 428 cm^-1和14 398 cm^-1在高温和高压作用下均发生蓝移，温度压力共同作用比温度压力分别作用时两峰的蓝移明显减小。通过合成金刚石的温度、压力条件的共同作用，仅在靠近合成样品位置的叶蜡石发生了相变。本文认为造成蓝移的原因是温度压力的作用使电子能级或成键电子能级发生改变。     

YJ-3000t型紧装式六面顶大腔体高温高压实验装置样品室的压力标定

 在温度为389~1 245 ℃和砧面压力为1.0~5.0 GPa的条件下,利用金属高压熔融标定法,采用Cu、Al、Zn和Pb四种金属,对YJ-3000t型紧装式六面顶大腔体高温高压实验装置样品室内的实际压力进行了标定。通过对由四种金属所获得的标定结果的多项式三维模拟,获得了以叶蜡石为外传压介质、氧化铝为内传压介质的情况下,由砧面压力和样品室温度估算样品室内实际压力的定量表达式。该结果可为今后该设备上类似实验组装中样品腔内实际压力的估算提供方便准确的压力标。     

高压腔内叶蜡石相变对发热石墨管电阻的影响

 在高温高压实验中，发现叶蜡石相变过程引起旁热式合成腔的加热石墨管电阻异常变化现象。对这一现象的若干规律及与叶蜡石相变的内在联系，进行了测试研究。本实验现象为在高温高压过程中实时地观察与研究叶蜡石相变规律，提供了可能性。     

Bridgman压砧上叶蜡石封垫预烧工艺与内加热方式的改进北大核心CSCD

在Bridgman压砧上研究了不同预烧工艺对叶蜡石封垫高压性能的影响,发现提高焙烧温度有助于提高叶蜡石封垫的临界厚度和中心弹性区面积,能有效扩大样品腔尺寸,并对高温焙烧(最高900℃)的叶蜡石封垫进行了压力标定。在此基础上,对叶蜡石封垫的内加热组装方式进行了改进,并在常压和高压下分别测试了新组装方式的加热性能,实现了4.0GPa高压下1 300℃温度范围内的加热。这些实验工作为进一步开展在Bridgman压砧上制备大尺寸亚稳材料提供了实验条件。     

活塞-圆筒型高温高压容器的端面保护和加温方法的改进

活塞-圆筒型高温高压容器在原理上是自由活塞压力计的变型,其工作压力可由外加载荷中扣除摩擦损耗后直接定出,故在高温高压研究中得到广泛的应用[1].但是这种容器的端面保护很不完善,容易使容器内衬出现横向开裂. 早期的活塞-圆筒容器使用时只有径向保护并无端面保护[2].Hall指出,要进一步提高工作压力,容器内衬的所有自由面均须加保护.Boyd与 England曾采用固定的端面保护[3].接着Kennedy等提出另一种端面保护力可变的设计[4].但是这两种设计的不足之处,在于端面保护力不能随工作压力的升降按某一定的比例而增减. 我们的新设计(称作“差…     

Bridgman压砧上叶蜡石封垫预烧工艺与内加热方式的改进

在Bridgman压砧上研究了不同预烧工艺对叶蜡石封垫高压性能的影响,发现提高焙烧温度有助于提高叶蜡石封垫的临界厚度和中心弹性区面积,能有效扩大样品腔尺寸,并对高温焙烧(最高900℃)的叶蜡石封垫进行了压力标定。在此基础上,对叶蜡石封垫的内加热组装方式进行了改进,并在常压和高压下分别测试了新组装方式的加热性能,实现了4.0GPa高压下1 300℃温度范围内的加热。这些实验工作为进一步开展在Bridgman压砧上制备大尺寸亚稳材料提供了实验条件。     

六面顶压机立方压腔内压强的定量测量及受力分析

将六面顶压机立方压腔内置入电路,采用原位电阻测量确定Bi,Tl,Ba相变的方法,标定了压腔内不同位置的压力(强).通过标定立方压腔顶锤表面的压力并结合计算,分别得到了外部加载与压腔密封边受力以及合成腔体受力的对应关系.实验分析结果表明,随着外部加载的增加,当腔体压力达到5 GPa时,消耗在压腔密封边上的加载急剧上升,消耗在合成腔体的加载趋于不变,从而导致立方压腔压力达到上限.利用实验结果,分析了立方压腔在高压下的受力状态,解释了立方压腔的压力难以超过7 GPa的原因.结合立方压腔的几何结构,通过理论分析,提出了采用高体弹模量的物质作为传压介质,同时采用低体弹模量的物质作为密封边提高立方压腔压力上限的可行方案.通过定量标定叶腊石压腔轴向的压力梯度,给出了压腔内沿对称轴不同位置压力值的计算方法,此方法可为高压实验提供更精确的压力数据.     

3 GPa熔融盐固体介质三轴高温压力容器的轴压摩擦力标定

 在温度标定和围压标定的基础上,采用轴压循环方法,对3 GPa固体介质三轴高温高压实验系统的轴压摩擦力进行了标定,分析了围压、温度、轴向位移速率、装样方式（盐套类型）等实验条件对轴压摩擦力的影响。结果表明：静摩擦力、挤压摩擦力和滑动摩擦力3种轴压摩擦力对轴向应力的影响不同,其中静摩擦力和挤压摩擦力对轴向应力的影响很小,影响应力精度的主要是滑动摩擦力。静摩擦力及滑动摩擦力与围压正相关;静摩擦力与轴向位移速率正相关,但受其影响较小,滑动摩擦力不受其影响;静摩擦力和滑动摩擦力与温度负相关,并且受其影响较显著;盐套类型对轴压摩擦力的影响较大,当实验条件接近盐套熔点时,轴压摩擦力显著降低,当样品周围的盐套处于熔融状态时,轴压摩擦力最小。基于此,确定了标定轴压摩擦力的具体步骤,并对角闪岩的应力-应变曲线进行了轴压摩擦力标定。对比轴压摩擦力校正前、后的应力-应变曲线发现,经过轴压摩擦力校正的应力-应变曲线能更好地反映样品的实际变形情况。     

Effect of precompression on pressure-transmitting efficiency of pyrophyllite gaskets

Pyrophyllite is widely used both as a gasket material and as a pressure-transmitting medium, especially for a large-volume press. Its pressure-transmitting efficiency mainly depends on the following factors: geometry of anvil and pyrophyllite block, chemical composition, density and strength. For a long time, most studies have been devoted to the first two factors, whereas the third one has been studied less. In this work, we report that the pressure-transmitting efficiency of pyrophyllite is improved by precompressing. The results show that pyrophyllite was fully densified when the pressure reached about 1 GPa. The press load for Ba I–II transition in the cubic large-volume pressure cell is reduced more than 8×10⁵ N by using the densified pyrophyllite, compared with the unprecompressed pyrophyllite. Namely, the press-load utilization efficiency was improved above 15% when the precompressed pyrophyllite is used as a pressure-transmitting medium.     

Simulation of pressure distribution in a pyrophyllite high-pressure cell by finite-element analysis

The pressure-transmitting behavior and pressure distribution of a pyrophyllite cell in a cubic-anvil large volume high-pressure apparatus is investigated by finite-element analysis (FEA). The mechanical equations describing pyrophyllite under high pressure are given, which are composed of the Drucker–Prager criterion and a linear equation of state. The related material parameters such as cohesive strength, angle of internal friction etc. are experimentally measured. The FEA simulation includes the non-uniformity deviatoric stress caused by plastic deformation and the isotropy hydrostatic pressure of the pyrophyllite cell caused by volume compression. The results demonstrate that, in such a pyrophyllite cell, almost 90{%} of the pressure is isotropy hydrostatic pressure, and the pressure gradient mainly arise from non-uniform deviatoric stresses. Simulated data are displayed using the contour and the path plots.     

Al-0.5%Cu合金中表现反常振幅效应的低频位错内耗

用低频扭摆的方法,系统地研究了能够较有把握地观测到在Al-0.5％Cu合金中所出现的反常位错内耗的实验程序。结果指出,把试样在拉力试验机上预先拉伸到某一适当的形变量后,立即测量它在某一适当温度下时效的过程中的内耗,可以在内耗-时效时间曲线上观察到一个表现反常振幅效应(即内耗-振幅曲线上出现一个峯值)的时效内耗峯。用经过充分时效而内耗已经达到稳定值的试样,逐渐增加振幅,测量内耗,也可以观察到一个应变振幅内耗峯(当内耗表示为应变振幅的函数时)。此外,用一定的应变振幅在较高温度下,测量经过充分时效的试样的内耗时,也可以观察到一个表现反常振幅效应的温度内耗峯(当内耗表示为温度的函数时)。这些实验结果肯定地指出,在一定测量温度下的振幅内耗峯和表现反常振幅效应的温度内耗峯是存在的。为了找出以前在Al-0.5％Cu中所观察到的反常内耗现象重复性不好的原因,系统地研究了测量内耗所用的应变振幅对于出现振幅内耗峯的影响以及预形变量对于出现时效内耗峯和温度内耗峯的影响。对于出现反常内耗现象的实验条件进行了分析。所观察到的关于反常内耗现象的实验结果,都可用位错拖着溶质原子气团运动的模型来作定性的解释。具体的模型和理论分析将另行报导。     

A hybrid pressure cell of pyrophyllite and magnesium oxide to extend the pressure range for large volume cubic presses

A hybrid pressure cell of pyrophyllite and magnesium oxide (HPCPM) used in large volume cubic presses is presented. In the HPCPM, a cubic frame which is made of pyrophyllite with face-centered square holes works as gaskets, and a heteromorphosis magnesium oxide works as the pressure-transmitting medium. Our experimental results indicated that the pressure-generation efficiency using the HPCPM was improved by about 40% than that using the traditional pyrophyllite pressure cell without decreasing the anvil truncation size (without sacrificing the sample volume). The HPCPM could pressurize samples of 1000 mm³ volume up to about 8 GPa, which is significantly higher than that available using the traditional pressure cell, which reports a highest pressure of about 6 GPa.     

Φ42 mm腔体高岭石-白云石质传压密封介质金刚石合成扩大试验

 高岭石具有良好的流动密封、固体传压及机械加工等物理性能,是传统传压密封介质原料叶蜡石的替代品。采用比纯高岭石更适合作为传压密封介质原料的某地高岭石矿物,经过配料、混料、装模、压制成型以及焙烧等工序,制成了高岭石-白云石质传压密封介质,并对其进行金刚石合成扩大试验。试验结果表明：高岭石-白云石质传压密封介质能够达到与叶蜡石质传压密封介质相当的效果;合成金刚石的单产为19 g,抗压强度不小于160 N的晶粒占32%,晶粒尺寸大于或等于0.30 mm的占82%,合成1 g金刚石的顶锤消耗小于0.5 g,合成过程稳定。     

Finite-element analysis on pressure transfer mechanism in large-volume cubic press

Pressure transmission inside a large-volume cubic press was examined using finite-element (FE) simulations. Calculations were carried out for the pyrophyllite P-transmitting mediums (32.5?×?32.5?×?32.5?mm³). The cell pressures of the simulations were chosen as representative values, including 3.75 and 5.5?GPa. A modified constitutive model for pyrophyllite and more realistic modelling were proposed. The global pressure fields were displayed using the contour plots. The results reveal that (1) at the centre of the pyrophyllite cube exists a region of constant quasi-hydrostatic pressure (RoCQHyP) where the pressure drop is less than 50?MPa; (2) how mechanical property (e.g. bulk modulus) of the P-transmitting medium affects cubic press P-transmitting performance. The simulated results were corroborated by high pressure experiments.     

A method to retrieve blackbody temperature errors in the two points radiometric calibration

Measurements of the atmospheric thermal emission using an infrared Fourier transform spectrometer need to be radiometrically calibrated. As for several existing instruments (IASI-MetOp, IASI-balloon, NAST-I, AERI, etc.), the two points radiometric calibration is generally performed using two well-characterized blackbodies at two different temperatures (or one blackbody and the cold space), which allow to determine the response and the self-emission of the instrument. To perform an accurate radiometric calibration, the emissivity and the temperature of each blackbody should be known accurately. The blackbody temperatures are chosen to fit the characteristics of the instrument. The measurement of these temperatures is essential. This paper proposes a method to perform an accurate radiometric calibration even when one of the two blackbodies temperatures is not perfectly measured, by numerically retrieving this erroneous temperature.