Characteristics of urea under high pressure and high temperature

The properties of urea under high pressure and high temperature(HPHT) are studied using a China-type large volume cubic high-presentation apparatus(CHPA)(SPD-6 × 600).The samples are characterized by scanning electron microscopy(SEM), x-ray diffraction(XRD), and Raman spectroscopy.By directly observing the macroscopic morphology of urea with SEM, it is confirmed that the melting point of urea rises with the increase of pressure.The XRD patterns of urea residues derived under different pressures show that the thermal stability of urea also increases with the increase of pressure.The XRD pattern of the urea residue confirms the presence of C3H5N5O(ammeline) in the residue.A new peak emerges at 21.80°, which is different from any peak of all urea pyrolysis products under normal pressure.A more pronounced peak appears at 708 cm^-1 in the Raman spectrum, which is produced by C-H off-plane bending.It is determined that the urea will produce a new substance with a C-H bond under HPHT, and the assessment of this substance requires further experiments.

Effects of Mg on diamond growth and properties in Fe–C system under high pressure and high temperature condition

Diamond crystal crystallized in Fe–Mg–C system with Archimedes buoyancy as a driving force is established under high pressure and high temperature conditions. The experimental results indicate that the addition of the Mg element results in the nitrogen concentration increasing from 87 ppm to 271 ppm in the diamond structure. The occurrence of the {100}plane reveals that the surface character is remarkably changed due to the addition of Mg. Micro-Raman spectra indicate that the half width of full maximum is in a range of 3.01 cm^-1–3.26 cm^-1, implying an extremely good quality of diamond specimens in crystallization.

Pressure-Induced Metallization and Electrical Phase Diagram for Polycrystalline CaB_6 under High Pressure and Low Temperature

The electrical properties of polycrystaltine CaB6 are revealed by in-situ resistance measurements under high pressure and low temperature. Due to the existence of grain boundaries, polycrystalline CaB6 behaves with semiconducting transport properties, which is different from the semimetallic CaB6 single crystals. The temperaturedependent resistance measurement results show that before the structural phase transition at 12.3 GPa the high pressure first induces the metallization at 6.5 GPa for CAB6. Moreover, the phase diagram for CaB6 is drawn based on the investigated electric conducting properties and at least three different conducting phases are found even at moderate high pressure and low temperature, indicating that the electric nature of CaB6 is very sensitive to the environment.

Experimental study on liquid immiscibility of lamprophyre-sulfide melt at high temperature and high pressure and its geological significance

With lamprophyre and pyrite from the Laowangzhai gold deposit, Yunnan Province, China, as starting materials, and at pressures from 1.5 to 3.0 GPa and temperatures from 1160 to 1560℃ , an experimental study was carried out on the liquid immiscibility of lamprophyre-sulfide melt at high temperature and ultra-high pressure in the DS-29A cubic 3600T/6-type high pressure apparatus. Results showed that the liquid immiscibility of lampro-pyre-sulfide melt in the magmatic system would happen during the early magmatic evolution (high temperature and high pressure conditions) and was controlled by temperature and pressure. The sulfide melt which was separated from the lamprophyric melt would make directional movement in the temperature and pressure field and assemble in the low-temperature and low-pressure region. Because the density of SM is higher than that of the lamprophyric melt, the former would gather together at the bottom of the magma chamber and there would exist a striking boundary between the two melts. On the other hand, the results also suggested that there would be little possibility for lampro-phyric magma to carry massive gold, and lamprophyres can't provide many of oreforming materials (Au) in the processes of gold mineralization.

Molecular Dynamics Simulation of MgO Melting at High Pressure

分子的动力学模拟被用来学习在高压力融化 MgO。MgO 的融化的温度精确地基于融化的现代理论在修正以后在提高的温度和高压力被获得。计算融化曲线在 0-135 GPa 的压力范围与可得到的试验性的数据和另外的理论结果相比。MgO 的改正的融化的温度在对从在 15 GPa 下面融化方程和二阶段的模仿的结果的 Lindemann 的结果的好同意。

固体氢在极端压强下的超导性能

氢元素在常压下具有最简单的晶体结构和物理性质。随着压强增加,氢单质发生相变,由绝缘体转变为金属,被称为金属氢。数值模拟表明,金属氢具有高温超导电性,因此,金属氢研究也被称为高压物理领域的“圣杯”课题。利用基于密度泛函理论的第一性原理计算方法,对固体氢在极端高压(0.5~5.0 TPa)下的结构和超导电性开展了系统研究。研究结果表明:固体氢的高压相变序列为I4_(1)/amd→oC12→cI16;对于同一种结构,随着压强增加,电声耦合系数减小,费米面处电子态密度减小,特征振动频率增加,超导转变温度发生小幅变化;在2.0 TPa压强下,固体氢的超导转变温度高达418 K(库伦赝势经验值μ^(*)=0.10)。研究工作将为金属氢及其超导电性的后续理论和实验研究提供参考。

低熔点合金高低温循环浸渍杨木的性能及机理研究

利用气-液相变自驱动原理,选用Sn-Bi-Pb低熔点合金(LMPA),通过木材含水率的调控及采用高低温交替循环浸渍法,在不破坏木材本身结构的条件下制备了金属化杨木,探讨了低熔点合金在木材中的渗透机理,并分析了金属化杨木的增重率、吸水率、顺纹抗压强度及导热性能。结果表明:提高木材的含水率并在高低温循环条件下浸渍有助于LMPA渗透到木材导管中,当杨木的含水率为60%时,其增重率高达52.47%;浸泡144 h后的吸水率比对照样减小了78.4%,顺纹抗压强度提高了33.75%,导热系数是对照样的2.6倍,在地暖地板领域显示出较好的应用前景。

电容器用金属化高温电介质薄膜的自愈性能研究

现代电力电子系统的高温应用迫切需要耐高温的金属化膜电容器(MFC)。虽然已有大量研究表明高温电介质膜具有令人满意的储能性能,但其自愈性能尚不清楚,而该性能是决定高温电介质膜能否应用到MFC中的关键。本文主要研究了聚萘二甲酸乙二醇酯(PEN)、聚醚醚酮(PEEK)和聚酰亚胺(PI)三种金属化高温电介质膜在直流高电压下的自愈性能,具体分析了层间压强、卷绕张力和温度等外部因素对自愈性能的影响。结果表明,PI由于碳含量高,在实验中很容易击穿短路导致自愈失败,不适合应用到MFC中。PEEK的自愈性能受层间压强和卷绕张力的影响较大,应用到MFC后需重点考虑卷绕张力和卷绕层数。PEN具有较低的碳含量和优异的脂肪族-芳香族交替结构,且在各项研究中均表现出较为优异的自愈性能。从自愈角度来看,PEN适合成为高温强电场MFC用的绝缘电介质材料。

海洋超高温高压油气钻井关键设备技术研究

为了提升我国海洋超高温高压钻井设备的国产化水平,对海洋超高温高压钻井主要设备进行了简要介绍,分析了海洋超高温高压钻井设备的国内外技术现状,重点阐述了海洋超高温高压钻井设备的关键技术及其研发思路。分析结果表明:钻井防喷器及控制系统、井口装置、泥线悬挂装置及井下工具等为当前急需攻关突破的超高温高压钻井关键设备;我国在这些关键设备的设计、制造和试验等多方面与国外存在差距,主要体现在高强度金属材料开发、密封设计制造、控制元器件开发和系统设备海试等4项关键技术方面。就这些关键技术提出了比较详细的研发思路,以期推动超高温高压钻井关键装备的国产化进程,增强我国海洋超高温高压油气田的勘探开发能力。

高温高压非金属元素掺杂金刚石的研究进展

金刚石因其优越的极限特性,使得其应用领域非常广泛。金刚石的功能特性往往由其内部所含杂质元素决定,包括非金属元素如硼(B)、氮(N)、硫(S)和磷(P)等。掺杂这些单元素以合成金刚石一直是国内外研究课题的热点。本文首先介绍了金刚石单晶在高温高压条件下的合成方法及其研究发展现状,随后分析了硼(B)、氮(N)、硫(S)、磷(P)等单元素掺杂对金刚石晶体生长和电学等性能的影响。同时对金刚石在半导体中的应用以及金刚石中的含氮色心进行了分析。最后展望了掺杂后金刚石的光学和电学性能研究前景,并指出进一步探索多元素共掺杂的理论和实验方法对提升掺杂金刚石的性能具有重要意义。

Metal-free Optical Pressure Sensor with High Sensitivity and Extensive Range

Pressure monitoring of a transformer oil tank can grasp the pressure change process caused by gas production when severe internal defects occur and take timely measures to ensure the safe operation of the transformer.Existing pressure sensors generally use metal encapsulation or have an air cavity structure,threatening the transformer’s insulation if it is directly used inside the transformer.To this end,this paper proposes a method for developing a high-sensitivity,large-range,and metallizationfree optical pressure sensing device with temperature compensation.Fiber grating is encapsulated by fluorosilicone rubber and supplemented by an epoxy resin shielding shell on the outside.At the same time,a double-grating vertical arrangement is adopted to improve pressure measurement sensitivity,further avoiding the influence of temperature rise caused by a defect of the transformer on the measurement result of the sensor.In addition,by optimizing the geometric structure of the internal sensitizing element,pre-stretching length of the fiber grating,gap distance,and other parameters,probe size can be reduced while ensuring the sensor’s performance.Results show the proposed method can meet the requirements of sensor fabrication with different sensitivities and ranges,and to a certain extent,both high sensitivity and extensive ranges can be taken into account.The sensitivity of the fabricated prototype is 15 pm/kPa,and the range is about 0.2 MPa.At the same time,the metal-free feature of the sensor makes it suitable for use in various oil-immersed power equipment.It records oil pressure changes caused by oil discharge breakdown,making it sensitive to small pressure changes in early failures.

Pb系简单钙钛矿氧化物PbMO_(3)(M=3d过渡族金属)的高温高压制备及物性研究

系统总结了近十几年利用高压技术制备简单钙钛矿功能氧化物材料PbMO_(3)(M=3d过渡族金属)及其物性研究方面的进展,重点关注M元素变化过程中的晶体结构、电子结构、磁性和电输运性质的演化,以及高压调控下的结构相变、电荷转移和绝缘体金属化等行为,同时也对该领域中一些亟需解决的问题做了展望。

金属合金高温环境下的耐腐蚀性能与化工设备选材优化

文章探讨了金属合金在高温高压环境下的耐腐蚀性能以及化工设备选材的优化问题,分析了金属合金的制造要素和要求,强调了合金制备的关键因素,讨论了高温高压环境对金属合金抗腐蚀性能的影响以及金属合金在高温高压环境下化工设备选材的难点和问题,提出了金属合金在高温高压环境下化工设备选材优化的有效策略。通过这些策略的综合实施,可以提高金属合金在高温高压环境下的耐腐蚀性能,确保化工设备的可靠运行和长期稳定性。

Nb-Ti-Al基合金的防护涂层研究及其抗氧化性能机理分析

利用真空电子束熔炼与电弧炉技术合成了Nb-Ti-Al基合金,利用料浆熔烧技术在合金表面制备了Si-Cr-W防护涂层,并对1250℃条件下的涂层抗氧化性能进行了评估,同时采用扫描电子显微镜和能量散射光谱研究分析了氧化前后的涂层微观形态和元素分布。研究结果表明:防护涂层的主要成分包括Nb、Ti、Cr、W等金属硅化物,其在高温下抗氧化机制为通过金属硅化物的氧化分解,生成SiO2和复合金属氧化物层,从而有效阻挡氧气的渗透。在经历了100 h的氧化测试后,涂层的外部结构因氧化而呈现出疏松的状态,但内部结构仍然保持着致密的特性,验证了该涂层在高温条件下具有出色的抗氧化性能。

工艺参数对高温高压合成Ⅱa型培育钻石的影响

针对国内采用六面顶压机利用高温高压法合成Ⅱa型培育钻石存在成核晶种粒数少、优晶占比小、生长缺陷多等问题,对合成前期和合成结束后的工艺参数曲线进行了优化。通过调控合成腔体内部的压力和温度,使其在合成腔体中的生长环境稳定,从而提高晶种形核生长数和优晶率。结果表明,最优工艺方案为:培育钻石生长阶段的前20h,在低温高压环境下缓慢升温并采取一段时间的保温措施,然后恒功率升温至设定温度,在高温高压下生长3d;在合成结束的2h内,采取分阶段带加热功率低速卸压,能够有效控制裂纹、金属包裹体等缺陷的产生,提高合成晶体品质。最终晶种形核生长数为25颗,优晶占比为92%。

Partial Melting and Its Implications for Understanding the Seismic Velocity Structure within the Southern Tibetan Crust

In order to constrain the crustal wave velocity structure in the southernTibetan crust and provide insight into the contribution of crustal composition, geothermal gradientand partial melting to the velocity structure, which is characterized by low average crustalvelocities and widespread presence of low-velocity zone(s), the authors model the crustal velocityand density as functions of depth corresponding to various heat flow values in light of velocitymeasurements at high temperature and high pressure. The modeled velocity and density are regarded ascomparison standards. The comparison of the standards with seismic observations in southern Tibetimplies that the predominantly felsic composition at high heat flow cannot explain the observedvelocity structure there. Hence, the authors are in favor of attributing low average crustalvelocities and low-velocity zone(s) observed in southern Tibet mainly to partial melting. Modelingbased on the experimental results suggests that a melting percentage of 7-12 could account for thelow-velocity zone(s).

Molecular dynamics of MgSiO3 perovskite melting

The melting curve of MgSiO3 perovskite is simulated using molecular dynamics simulations method at high pressure. It is shown that the simulated equation of state of MgSiO3 perovskite is very successful in reproducing accurately the experimental data. The pressure dependence of the simulated melting temperature of MgSiO3 perovskite reproduces the stability of the orthorhombic perovskite phase up to high pressure of 130GPa at ambient temperature, consistent with the theoretical data of the other calculations. It is shown that its transformation to the cubic phase and melting at high pressure and high temperature are in agreement with recent experiments.

Congruent melting of tungsten phosphide at 5 GPa and 3200℃ for growing its large single crystals

As one of important members of refractory materials,tungsten phosphide(WP)holds great potential for fundamental study and industrial applications in many fields of science and technology,due to its excellent properties such as superconductivity and as-predicted topological band structure.However,synthesis of high-quality WP crystals is still a challenge by using tradition synthetic methods,because the synthesis temperature for growing its large crystals is very stringently required to be as high as 3000℃,which is far beyond the temperature capability of most laboratory-based devices for crystal growth.In addition,high temperature often induces the decomposition of metal phosphides,leading to off-stoichiometric samples based on which the materials'intrinsic properties cannot be explored.In this work,we report a high-pressure synthesis of single-crystal WP through a direct crystallization from cooling the congruent W-P melts at 5 GPa and^3200℃.In combination of x-ray diffraction,electron microscope,and thermal analysis,the crystal structure,morphology,and stability of recovered sample are well investigated.The final product is phase-pure and nearly stoichiometric WP in a single-crystal form with a large grain size,in excess of one millimeter,thus making it feasible to implement most experimental measurements,especially,for the case where a large crystal is required.Success in synthesis of high-quality WP crystals at high pressure can offer great opportunities for determining their intrinsic properties and also making more efforts to study the family of transition-metal phosphides.

Development of Zr/ZrO_2 high temperature and high pressure sensors for in-situ measuring chemical parameters of deep-sea water

In order to in situ measure chemical parameters of deep-sea water and hydrothermal fluids at midocean ridge(MOR), it is necessary to use high temperature and high pressure chemical sensors.Developing new sensors is essential to measure in-situ pH and other chemical parameters(dissolved H2, dissolved H2S) of deep-sea water and hydrothermal fluids in a wide temperature range(2℃―400℃) at MOR vents.The YSZ(Yttria Stabilized Zirconia, 9%Y2O3) ceramic-based(HgO/Hg) chemical sensors possess excellent electrochemical properties at high temperatures, which have been used to measure chemical parameters of hydrothermal fluids above 200℃.A novel Zr/ZrO2 oxidation/reduction electrode was constructed by oxidation of Zr wire in Na2CO3 melt.This Zr/ZrO2 electrode has good chemical stability while measuring pH of high-temperature aqueous solutions, combined with a Ag/AgCl reference electrode.Potentials of the Zr/ZrO2 sensor in association with a Ag/AgCl reference electrode vary linearly with pH over a wide pH range, as tested by various NaCl-HCl-H2O solutions(NaOH-NaCl-H2O for basic solutions), at temperatures in the range of 20℃―200℃.Thus, the Zr/ZrO2 sensors can be utilized in monitoring the fluids over the temperature range of 2℃―200℃.The Zr/ZrO2 electrode combined with Ag/AgCl, Ag/Ag2S, and Au electrodes has been used to measure pH and other chemical parameters(dissolved H2, dissolved H2S) of aqueous fluids from low to high temperatures and high pressures in the laboratory and to monitor those parameters of deep-sea water in South China Sea.

80 MPa保压取心工具的研制与应用

为充分认识深井、高温井区块原始地层条件下岩心的油气组分物性和结构构造,真实评价该区块油气储量,文章以现有保压取心技术为基础,通过优化设计、技术创新成功研制出80 MPa保压取心技术。该技术设计的氟素橡胶密封件可以长时工作在井下150℃高温环境中并保持良好的橡胶性能,满足高温环境中静、动高压差密封;球端活塞承高压金属密封、承低压胶环的双密封设计;优选7075型硬质铝合金内筒,优化设计工具壁厚及增强丝扣强度实现内筒总成承压差80 MPa;通过表面镀层及涂层处理应对井下长时间高温、高循环压耗的工作环境,提高保压取心工具安全性。现场应用表明,80 MPa保压取心技术可以满足深井、高温井保压取心的技术需求,对于深井、高温井地质勘探开发及储量评价具有重要意义。