Experimental Study on the Electrical Conductivity of Orthopyroxene at High Temperature and High Pressure under Different Oxygen Fugacities

At presure 1.0-4.0 GPa and temperature 1073-1423 K and under oxygen partial pressure conditions, a YJ-3000t multi-anvil solid high-pressure apparatus and Sarltron-1260 Impedance/Gain-Phase analyzer were employed to conduct an in-situ measurement of the electrical conductivity of orthopyroxene. The buffering reagents consist of Ni＋NiO, Fe＋Fe3O4, Fe＋FeO and Mo＋MoO2 in order to control the environmental oxygen fugacity. Experimental results made clear that： （1） within the measuring frequency range from 10-1 to 106 Hz, the complex impedance （R） is of intensive dependence on the frequency; （2） The electrical conductivity （a） tends to increase along to the rise of temperature （T）, and Log a vs. 1/ T fit the Arrenhius linear relations; （3） Under the control of oxygen buffer Fe＋Fe3O4, with the rise of pressure, the activation enthalpy tends to increase whereas the electrical conductivity tends to decrease. The activation energy and activation volume of the main current carders of orthopyroxene have been obtained, which are （1.715±0.035） eV and （0.03±0.01） cm^3/mol, respectively; （4） Under given pressure and temperature, the electrical conductivity tends to increase with increasing oxygen fugacity, while under given pressure the activation enthalpy tends to decrease with increasing oxygen fugacity; and （5） The sample＇s small polarons mechanism has provided a reasonable explanations to the conduction behavior at high temperature and high pressure.

The Research Status and Major Problems of High Temperature and High Pressure Experiment on Petrogenesis and mineralization

1 Introduction In contrast,1experimental geochemistry is a young subject,but in recent years,the research on experiment of high temperature and high pressure has become an important branch in the parallel subjects of traditional mineralogy,petrology,geochemistry and geophysics.It is not only an important and essential way and window to understand geological processes in depth and geological

Prospect of HDR geothermal energy exploitation in Yangbajing,Tibet,China,and experimental investigation of granite under high temperature and high pressure

Hot dry rock （HDR） geothermal energy, almost inexhaustible green energy, was first put forward in the 1970s. The development and testing of HDR geothermal energy are well reported in USA, Japan, UK, France and other countries or regions. In this paper, the geological characters of Yangbajing basin were first analyzed, including the continental dynamic environments to form HDR geothermal fields in Tibet, the tectonic characteristics of south slope of Nyainqentanglha and Dangxiong-Yangbajing basin, and the in-situ stresses based on the investigations conducted, and then the site-specific mining scheme of HDR geothermal resources was proposed. For the potential development of HDR geothermal energy, a series of experiments were conducted on large-scale granite samples, 200 mm in diameter and 400 mm in length, at high temperature and high triaxial pressure for cutting fragmentation and borehole stability. For the borehole stability test, a hole of 40 mm in diameter and 400 mm in length was aforehand drilled in the prepared intact granite sample. The results indicate that the cutting velocity obviously increases with temperature when bit pressure is over a certain value, while the unit rock-breaking energy consumption decreases and the rock-breaking efficiency increases with temperature at the triaxial pressure of 100 MPa. The critical temperature and pressure that can result in intensive damage to granite are 400-500℃ and 100-125 MPa, respectively.

Development of a High Temperature and High Pressure Oil-Based Drilling Fluid Emulsion Stability Tester

When drilling deep wells and ultra-deep wells, the downhole high temperature and high pressure environment will affect the emulsion stability of oil-based drilling fluids. Moreover, neither the demulsification voltage method nor the centrifugal method currently used to evaluate the stability of oil-based drilling fluids can reflect the emulsification stability of drilling fluids under high temperature and high pressure on site. Therefore, a high-temperature and high-pressure oil-based drilling fluid emulsion stability evaluation instrument is studied, which is mainly composed of a high-temperature autoclave body, a test electrode, a temperature control system, a pressure control system, and a test system. The stability test results of the instrument show that the instrument can achieve stable testing and the test data has high reliability. This instrument is used to analyze the factors affecting the emulsion stability of oil-based drilling fluids. The experimental results show that under the same conditions, the higher the stirring speed, the better the emulsion stability of the drilling fluid;the longer the stirring time, the better the emulsion stability of the drilling fluid;the greater the oil-water ratio, the better the emulsion stability of the drilling fluid. And the test results of the emulsification stability of oil-based drilling fluids at high temperature and high pressure show that under the same pressure, as the temperature rises, the emulsion stability of oil-based drilling fluids is significantly reduced;at the same temperature, the With the increase in pressure, the emulsion stability of oil-based drilling fluids is in a downward trend, but the decline is not large. Relatively speaking, the influence of temperature on the emulsion stability of oil-based drilling fluids is greater than that of pressure.

Influence of annealing treatment on as-grown Ib-type diamond crystal at a high temperature and high pressure

In this paper,we report on the influence of annealing treatment on as-grown Ib-type diamond crystal under high pressure and high temperature in a china-type cubic anvil high-pressure apparatus.Experiments are carried out at a pressure of 7.0 GPa and temperatures ranging from 1700 C to 1900 C for 1 h.Annealing treatment of the diamond crystal shows that the aggregation rate constant of nitrogen atoms in the as-grown Ib-type diamond crystal strongly depends on diamond morphology and annealing temperature.The aggregation rate constant of nitrogen remarkably increases with the increase of annealing temperature and its value in octahedral diamond is much higher than that in cubic diamond annealed at the same temperature.The colour of octahedral diamond crystal is obviously reduced from yellow to nearly colorless after annealing treatment for 1 h at 1900 C,which is induced by nitrogen aggregation in a diamond lattice.The extent of nitrogen aggregation in an annealed diamond could approach approximately 98% indicated from the infrared absorption spectra.The micro-Raman spectrum reveals that the annealing treatment can improve the crystalline quality of Ib-type diamond characterized by a half width at full maximum at first order Raman peak,and therefore the annealed diamond crystals exhibit nearly the same properties as the natural IaA-type diamond stones of high quality in the Raman measurements.

A Comprehensive Method for the Optimization of Cement Slurry and to Avoid Air Channeling in High Temperature and High-Pressure Conditions

Air channeling in the annulus between the casing and the cement sheath and/or between the cement sheath and formation is the main factor affecting the safe operation of natural gas wells at high temperatures and pressures.Prevention of this problem requires,in general,excellent anti-channeling performances of the cement sheath.Three methods to predict such anti-channeling performances are proposed here,which use the weightless pressure of cement slurry,the permeability of cement stone and the volume expansion rate of cement sheath as input parameters.Guided by this approach,the anti-channeling performances of the cement slurry are evaluated by means of indoor experiments,and the cement slurry is optimized accordingly.The results show that the dangerous transition time of the cement slurry with optimized dosage of admixture is only 76 min,the permeability of cement stone is 0.005 md,the volume shrinkage at final setting is only 0.72%,and the anti-channeling performances are therefore maximized.The effective utilization of the optimized cement slurry in some representative wells(LD10–1-A1 and LD10–1-A2 in LD10–1 gas field)is also discussed.

Mechanical Analysis of a Multi-Test String in High-Temperature and High-Pressure Deep Wells

The mechanical behavior of the test string in deep wells is generally relatively complex as a result of the high temperature and high pressure,severe dogleg and buckling effects,which in some circumstances can even lead to string failure.Traditional computational methods for the analysis of these behaviors are often inaccurate.For this reason,here a more accurate mechanical model of the test string is introduced by considering variables such as temperature,pressure,wellbore trajectory,and buckling,as well as combining them with the deformation and string constraint conditions brought in by changes in temperature and pressure during the tripping,setting,and test operations.The model is validated by applying it to a specific high-pressure gas well(located in Northeast Sichuan).

Various admixtures to mitigate the long-term strength retrogression of Portland cement cured under high pressure and high temperature conditions

In order to investigate the problem of long-term strength retrogression in oil well cement systems exposed to high pressure and high temperature(HPHT)curing conditions,various influencing factors,including cement sources,particle sizes of silica flour,and additions of silica fume,alumina,colloidal iron oxide and nano-graphene,were investigated.To simulate the environment of cementing geothermal wells and deep wells,cement slurries were directly cured at 50 MPa and 200?C.Mineral compositions(as determined by X-ray diffraction Rietveld refinement),water permeability,compressive strength and Young’s modulus were used to evaluate the qualities of the set cement.Short-term curing(2e30 d)test results indicated that the adoption of 6 m m ultrafine crystalline silica played the most important role in stabilizing the mechanical properties of oil well cement systems,while the addition of silica fume had a detrimental effect on strength stability.Long-term curing(2e180 d)test results indicated that nano-graphene could stabilize the Young’s modulus of oil well cement systems.However,none of the ad-mixtures studied here can completely prevent the strength retrogression phenomenon due to their inability to stop the conversion of amorphous to crystalline phases.

High-pressure and high-temperature sintering of pure cubic silicon carbide:A study on stress-strain and densification

Silicon carbide(SiC)is a high-performance structural ceramic material with excellent comprehensive properties,and is unmatched by metals and other structural materials.In this paper,raw SiC powder with an average grain size of 5μm was sintered by an isothermal-compression process at 5.0 GPa and 1500?C;the maximum hardness of the sintered samples was31.3 GPa.Subsequently,scanning electron microscopy was used to observe the microscopic morphology of the recovered SiC samples treated in a temperature and extended pressure range of 0-1500?C and 0-16.0 GPa,respectively.Defects and plastic deformation in the SiC grains were further analyzed by transmission electron microscopy.Further,high-pressure in situ synchrotron radiation x-ray diffraction was used to study the intergranular stress distribution and yield strength under non-hydrostatic compression.This study provides a new viewpoint for the sintering of pure phase micron-sized SiC particles.

Polycrystalline cubic boron nitride prepared with cubic-hexagonal boron nitride under high pressure and high temperature

Polycrystalline cubic boron nitride（Pc BN） compacts, using the mixture of submicron cubic boron nitride（c BN） powder and hexagonal BN（h BN） powder as starting materials, were sintered at pressures of 6.5–10.0 GPa and temperature of1750℃ without additives. In this paper, the sintering behavior and mechanical properties of samples were investigated.The XRD patterns of samples reveal that single cubic phase was observed when the sintering pressure exceeded 7.5 GPa and h BN contents ranged from 20 vol.% to 24 vol.%, which is ascribed to like-internal pressure generated at grain-to-grain contact under high pressure. Transmission electron microscopy（TEM） analysis shows that after high pressure and high temperature（HPHT） treatments, the submicron c BN grains abounded with high-density nanotwins and stacking faults, and this contributed to the outstanding mechanical properties of Pc BN. The pure bulk Pc BN that was obtained at 7.7 GPa/1750℃ possessed the outstanding properties, including a high Vickers hardness（～ 61.5 GPa）, thermal stability（～ 1290℃ in air）,and high density（～ 3.46 g/cm^3）.

SiO_2 Solubility in Rutile at High Temperature and High Pressure

Silicon-bearing rutile has been found in chromitite from the Luobusa （罗布莎） ophiolite, Tibet. However, the extent of SiO2 solubility in rutile and the nature of its origin are still unclear. At high pressure, SiO2 takes a rutile structure with Si in 6-fold coordination. Thus, high pressures may enhance its solubility in rutile because of possible isovalent exchange in the octahedral site. In this study, we report new experimental results on SiO2 solubility in rutile up to 23 GPa and 2 000℃. Starting materials were mixtures of powdered pure rutile and pure quartz, with compositions of （Ti0.5Si0.5）O2, （Ti0.93Si0.07）O2, and （Ti0.75Si0.25）O2. The mixtures were loaded into either platinum capsules （for a 10/5 assembly） or rhenium capsules （for an 8/3 assembly）. The experiments were carried out using multi-anvil high-pressure apparatus with a rhenium resistance heater. Sample temperatures were measured with a W5%Re-W26%Re thermocouple and were controlled within ±1 ℃ of the set temperature. TiO2-rich and SiO2-rich phases were produced in all the quenched samples. Microprobe analyses of the phases show that the solubility of SiO2 in rutile increases with increasing pressure, from 1.5 wt.% SiO2 at 10 GPa to 3.8 wt.% SiO2 at 23 GPa at a temperature of 1 800 ℃. The solubility also increases with increasing temperature from 0.5 wt.% SiO2 at 1 500 ℃ to 4.5 wt.% SiO2 at 2 000 ℃ at a pressure of 18 GPa. On the other hand, the solubility of TiO2 in coesite or stishovite is very limited, with an average of 0.6 wt.% TiO2 over the experimental P-T ranges. Temperature has a much larger effect on the solubility of SiO2 in ruffle than pressure. At high pressure, the melting point of SiO2 is definitely higher than that of TiO2 and the eutectic point moves towards SiO2 in the TiO2-SiO2 system. Lower oxygen fugacity decreases the solubility of SiO2 in ruffle, whereas water has little effect on the solubility. Our experimental data are extremely useful for determining the depth of origin of the SiO2-bearing rutfle found in nature.

Synthesis of large diamond crystals containing high-nitrogen concentration at high pressure and high temperature using Ni-based solvent by temperature gradient method

This paper reprots that with Ni-based catalyst/solvent and with a dopant of NAN3, large green single crystal diamonds with perfect shape are successfully synthesized by temperature gradient method under high pressure and high temperature in a China-type cubic anvil high-pressure apparatus （SPD-6 × 1200）, and the highest nitrogen concentration reaches approximately 121-1257 ppm calculated by infrared absorption spectra. The synthesis conditions are about 5.5 CPa and 1240-1300 ℃. The growth behaviour of diamond with high-nitrogen concentration is investigated in detail. The results show that, with increasing the content of NaN3 added in synthesis system, the width of synthesis temperature region for growth high-quality diamonds becomes narrower, and the morphology of diamond crystal is changed from cube-octahedral to octahedral at same temperature and pressure, the crystal growth rate is slowed down, nevertheless, the nitrogen concentration doped in synthetic diamond increases.

Anti-allergic Effects of Ginsenosides Extracted by High Temperature and High Pressure Method

Ginseng（Panax ginseng C. A. Mey.） is a traditional medicinal herb in Asia. Studies have shown that ginsenosides significantly affect immnnoregulation and rare ginsenosides have anti-allergic effects. In this research, a high temperature and high pressure method was utilized to increase the contents of rare ginsenosides in the ginseng extract（GE）. The anti-allergic effects of this extract were investigated in vivo. Water was used as the extraction solvent in extracting the rare ginsenosides via the high temperature and high pressure method. Extraction time and temperature were investigated in order to increase the contents of rare ginsenosides. Rare ginsenosides were qualitatively analyzed by HPLC-ESI-MS and quantitatively analyzed by HPLC-UV. Anti-allergic effects of the extracts were assessed using the ovalbumin（OVA）-induced allergic asthma model in vivo. An extraction temperature of 145 ℃ and extraction time of 2.0 h were chosen as the optimal conditions. Compared with traditional method, the contents of total rare ginsenosides extracted were considerably higher using the new method, that is, 14.74 times that extracted by the traditional method. In our in vivo experiments, treatment with high concentration GE may have anti-allergic erects in decreasing the total amount of IgE in serum and IL-4 in bronchoalveolar lavage fluid（BALF）, aud in improving the ratio of CD4^＋ to CD8^＋ T cells. The high temperature and high pressure method was an effective method to obtain GE containing more rare ginsenosides, which maybe become anti-allergic agents.

Porosity, permeability and rock mechanics of Lower Silurian Longmaxi Formation deep shale under temperature-pressure coupling in the Sichuan Basin, SW China

To investigate the porosity, permeability and rock mechanics of deep shale under temperature-pressure coupling, we selected the core samples of deep shale from the Lower Silurian Longmaxi Formation in the Weirong and Yongchuan areas of the Sichuan Basin for porosity and permeability experiments and a triaxial compression and sound wave integration experiment at the maximum temperature and pressure of 120 ℃ and 70 MPa. The results show that the microscopic porosity and permeability change and the macroscopic rock deformation are mutually constrained, both showing the trend of steep and then gentle variation. At the maximum temperature and pressure, the porosity reduces by 34%–71%, and the permeability decreases by 85%–97%. With the rising temperature and pressure, deep shale undergoes plastic deformation in which organic pores and clay mineral pores are compressed and microfractures are closed, and elastic deformation in which brittle mineral pores and rock skeleton particles are compacted. Compared with previous experiments under high confining pressure and normal temperature,the experiment under high temperature and high pressure coupling reveals the effect of high temperature on stress sensitivity of porosity and permeability. High temperature can increase the plasticity of the rock, intensify the compression of pores due to high confining pressure, and induce thermal stress between the rock skeleton particles, allowing the reopening of shale bedding or the creation of new fractures along weak planes such as bedding, which inhibits the decrease of permeability with the increase of temperature and confining pressure. Compared with the triaxial mechanical experiment at normal temperature, the triaxial compression experiment at high temperature and high pressure demonstrates that the compressive strength and peak strain of deep shale increase significantly due to the coupling of temperature and pressure. The compressive strength is up to 435 MPa and the peak strain exceeds 2%, indicating that high temperature is not conducive to fracture initiation and expansion by increasing rock plasticity. Lithofacies and mineral composition have great impacts on the porosity, permeability and rock mechanics of deep shale. Shales with different lithologies are different in the difficulty and extent of brittle failure. The stress-strain characteristics of rocks under actual geological conditions are key support to the optimization of reservoir stimulation program.

Large single crystal diamond grown in FeNiMnCo-S-C system under high pressure and high temperature conditions

大钻石成功地在 1255-1393 敤瑮漠 ? 摀畲的温度从 FeNiMnCo-S-C 系统被综合了吗？

Growth and annealing study of hydrogen-doped single diamond crystals under high pressure and high temperature

A series of diamond crystals doped with hydrogen is successfully synthesized using LiH as the hydrogen source in a catalyst-carbon system at a pressure of 6.0 GPa and temperature ranging from 1255 C to 1350 C.It is shown that the high temperature plays a key role in the incorporation of hydrogen atoms during diamond crystallization.Fourier transform infrared micro-spectroscopy reveals that most of the hydrogen atoms in the synthesized diamond are incorporated into the crystal structure as sp 3-CH 2-symmetric（2850 cm-1） and sp 3 CH 2-antisymmetric vibrations（2920 cm-1）.The intensities of these peaks increase gradually with an increase in the content of the hydrogen source in the catalyst.The incorporation of hydrogen impurity leads to a significant shift towards higher frequencies of the Raman peak from 1332.06 cm-1 to 1333.05 cm-1 and gives rise to some compressive stress in the diamond crystal lattice.Furthermore,hydrogen to carbon bonds are evident in the annealed diamond,indicating that the bonds that remain throughout the annealing process and the vibration frequencies centred at 2850 and 2920 cm-1 have no observable shift.Therefore,we suggest that the sp 3 C-H bond is rather stable in diamond crystals.

B-C Bond in Diamond Single Crystal Synthesized with h-BN Additive at High Pressure and High Temperature

The synthesis of diamond single crystal in the Fe64Ni36-C system with h-BN additive is investigated at pressure 6.5 GPa and temperature range of 1300-1400℃. The color of the obtained diamond crystals translates from yellow to dark green with increasing the h-BN addition. Fourier-transform infrared （FTIR） results indicate that sp2 hybridization B-N-B and B-N structures generate when the additive content reaches a certain value in the system. The two peaks are located at 745 and 1425cm-1, respectively. Fhrthermore, the FTIR characteristic peak resulting from nitrogen pairs is noticed and it tends to vanish when the h-BN addition reaches 1.1 wt%. Furthermore, Raman peak of the synthesized diamond shifts down to a lower wavenumber with increasing the h-BN ~ddition content in the synthesis system.

Synthesis and characterizations of boron and nitrogen co-doped high pressure and high temperature large single-crystal diamonds with increased mobility

We synthesized and investigated the boron-doped and boron/nitrogen co-doped large single-crystal diamonds grown under high pressure and high temperature(HPHT) conditions(5.9 GPa and 1290℃). The optical and electrical properties and surface characterization of the synthetic diamonds were observed and studied. Incorporation of nitrogen significantly changed the growth trace on surface of boron-containing diamonds. X-ray photoelectron spectroscopy(XPS) measurements showed good evident that nitrogen atoms successfully incorporate into the boron-rich diamond lattice and bond with carbon atoms. Raman spectra showed differences on the as-grown surfaces and interior between boron-doped and boron/nitrogen co-doped diamonds. Fourier transform infrared spectroscopy(FTIR) measurements indicated that the nitrogen incorporation significantly decreases the boron acceptor concentration in diamonds. Hall measurements at room temperature showed that the carriers concentration of the co-doped diamonds decreases, and the mobility increases obviously. The highest hole mobility of sample BNDD-1 reached 980 cm^(2)·V^(-1)·s^(-1), possible reasons were discussed in the paper.

Stability of Titanium-aluminium Nitride (Ti_2AlN) at High Pressure and High Temperatures

The stability of Ti2AlN at high pressure of 5 GPa and different temperatures of 700-1 600 ℃ was investigated using X-ray diffraction （XRD）,scanning electron microscopy （SEM） equipped with an energy dispersive spectrometer （EDS）.Ti2AlN was found to be stable at temperatures as high as 1 400 ℃under 5 GPa for 20 min,and was proved that it held better structure stability than Ti2AlC under 5 GPa through comparative experiments of Ti2AlN and Ti2AlC （representative compounds of M2AX phases （211 phase））.The reaction process at high pressure had some difference from that at ambient pressure/vacuum,and Ti2AlN directly decomposed to TiN and TiAl at 5 GPa and 1 500 ℃ for 20 min.Moreover,the mechanism of phase segregation was discussed.In addition,the behavior of Ti2AlN contacting with Zr at high pressure and high temperature （HPHT） was also studied.

Fretting Wear Characteristics of Nuclear Fuel Cladding in High-Temperature Pressurized Water

In pressurized water reactor(PWR),fretting wear is one of the main causes of fuel assembly failure.Moreover,the operation condition of cladding is complex and harsh.A unique fretting damage test equipment was developed and tested to simulate the fretting damage evolution process of cladding in the PWR environment.It can simulate the fretting wear experiment of PWR under different temperatures(maximum temperature is 350℃),displacement amplitude,vibration frequency,and normal force.The fretting wear behavior of Zr-4 alloy under different temperature environments was tested.In addition,the evolution of wear scar morphology,profile,and wear volume was studied using an optical microscope(OM),scanning electron microscopy(SEM),and a 3D white light interferometer.Results show that higher water temperature evidently decreased the cladding wear volume,the wear mechanism of Zr-4 cladding changed from abrasive wear to adhesive wear and the formation of an oxide layer on the wear scar reduced the wear volume and maximum wear depth.