Recension of boron nitride phase diagram based on high-pressure and high-temperature experiments

Cubic boron nitride and hexagonal boron nitride are the two predominant crystalline structures of boron nitride.They can interconvert under varying pressure and temperature conditions.However,this transformation requires overcoming significant potential barriers in dynamics,which poses great difficulty in determining the c-BN/h-BN phase boundary.This study used high-pressure in situ differential thermal measurements to ascertain the temperature of h-BN/c-BN conversion within the commonly used pressure range(3-6 GPa)for the industrial synthesis of c-BN to constrain the P-T phase boundary of h-BN/c-BN in the pressure-temperature range as much as possible.Based on the analysis of the experimental data,it is determined that the relationship between pressure and temperature conforms to the following equation:P=a+1/bT.Here,P denotes the pressure(GPa)and T is the temperature(K).The coefficients are a=-3.8±0.8 GPa and b=229.8±17.1 GPa/K.These findings call into question existing high-pressure and high-temperature phase diagrams of boron nitride,which seem to overstate the phase boundary temperature between c-BN and h-BN.The BN phase diagram obtained from this study can provide critical temperature and pressure condition guidance for the industrial synthesis of c-BN,thus optimizing synthesis efficiency and product performance.

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.

Advanced high-pressure transport measurement system integrated with low temperature and magnetic field

We briefly introduce a new high-pressure transport measurement system integrated with low temperature and magnetic field that is being established as one of the user experimental stations of the Synergetic Extreme Condition User Facilities in the Huairou District of Beijing, China. To demonstrate the capabilities of the system for condensed matter research, the emergence of some pressure-induced phenomena and physics related to superconductivity found previously is also introduced, and then a perspective for such an advanced high-pressure system is presented.

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.

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.

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).

Effects of FeNi-phosphorus-carbon system on crystal growth of diamond under high pressure and high temperature conditions

This paper reports the crystal growth of diamond from the Fe Ni–Carbon system with additive phosphorus at high pressures and high temperatures of 5.4–5.8 GPa and 1280–1360°C. Attributed to the presence of additive phosphorus,the pressure and temperature condition, morphology, and color of diamond crystals change obviously. The pressure and temperature condition of diamond growth increases evidently with the increase of additive phosphorus content and results in the moving up of the V-shape region. The surfaces of the diamonds also become coarse as the additive phosphorus added in the growth system. Raman spectra indicate that diamonds grown from the Fe Ni-phosphorus-carbon system have more crystal defects and impurities. This work provides a new way to enrich the doping of diamond and improve the experimental exploration for future material applications.

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)).

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.

Experimental Study on Water-rock Reactions with CO2 Fluid in a Deep Sandstone Formation under High Temperature and Pressure

Qiongdongnan Basin has a tectonic geological background of high temperature and high pressure in a deep reservoir setting,with mantle-derived CO2.A water-rock reaction device was used under high temperature and high pressure conditions,in conjunction with scanning electron microscope(SEM)observations,to carry out an experimental study of the diagenetic reaction between sandstone at depth and CO2-rich fluid,which is of great significance for revealing the dissolution of deep clastic rock reservoirs and the developmental mechanism of secondary pores,promoting deep oil and gas exploration.In this study,the experimental scheme of the water-rock reaction system was designed according to the parameters of the diagenetic background of the deep sandstone reservoir in the Qiongdongnan Basin.Three groups of single mineral samples were prepared in this experiment,including K-feldspar samples,albite samples and calcite samples.Using CO2 as a reaction solution,a series of diagenetic reaction simulation experiments were carried out in a semi-closed high temperature and high pressure simulation system.A field emission scanning electron microscope(SEM)was used to observe the microscopic appearance of the mineral samples after the water-rock reaction,the characteristics of dissolution under high temperature and high pressure,as well as the development of secondary pores.The experimental results showed that the CO2-rich fluid has an obvious dissolution effect on K-feldspar,albite and calcite under high temperature and high pressure.For the three minerals,the main temperature and pressure window for dissolution ranged from 150℃to 300℃and 45 MPa to 60 MPa.Scanning electron microscope observations revealed that the dissolution effect of K-feldspar is most obvious under conditions of 150℃and 45 MPa,in contrast to conditions of200℃and 50 MPa for albite and calcite.Through the comparative analysis of experimental conditions and procedures,a coupling effect occurred between the temperature and pressure change and the dissolution strength and calcite.Under high temperature and high pressure,pressure changed the solubility of CO2,furthermore,the dissolution effect and strength of the sandstone components were also affected.The experiment revealed that high temperature and high pressure conditions with CO2-rich fluid has a significant dissolution effect on aluminosilicate minerals and is conducive to the formation of secondary pores and effective reservoirs.Going forward with the above understanding has important implications for the promotion of deep oil and gas exploration.

Thermodynamic Study on the Compositions of Fluid Phases in the C-O-H System Under High Temperature and Pressure

Based on the fluid phase equilibrium of the C-O-H system, the compositions of var-ious fluid phases under high temperatures and pressures have been calculated in terms of the available thermodynamic data and new P-V-T data and on the assumption of PT = ΣPi in this paper. The results indicate that in this system there are 5 major fluid phases in different pro-portions at various T and P. CH4 is the dominant phase (about 70% ) under relatively lower T and P. Its proportion obviously decreases with increasing T, P and fo2. The results pro-vide sufficient theoretical grounds for discussing the possibility of CH4 formation and the physical-chemical conditions of its stable occurrence and proportion in the geological environment.

A Study of High-Temperature and High-Pressure Experiment of Correlativity between Deformational System of Au-Bearing Rocks and Element Adjustment

Modelling of migration and accumulation of elements Au and Ag in rocks under temperatures of 350–450°C and a confining pressure of 300 MPa and axial pressure of 100–150 MPa is conducted. It is found that the contents of gold and silver get higher in metallic sulphides such as pyrite, chalcopyrite and sphalerite as well as in quartz and muscovite, and get lower in chlorite, biotite, seriate, albite and calcite, showing that tectono-dynamics is one of the important factors for petrogenesis and metallogenesis.

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.

Crystallization and characteristics of {100}-oriented diamond with CH4N2S additive under high pressure and high temperature

Diamond crystallization was carried out with CH4N2S additive in the FeNiCo-C system at pressure 6.0 GPa and temperature ranging from 1290 ℃ to 1300 ℃. The crystallization qualities of the synthetic crystals were characterized by Raman spectra and the Raman peaks located at 1331 cm-1. Fourier transform infrared (FTIR) results showed that the hydrogen-related absorption peak of the as-grown diamond was at 2920 cm-1, respectively. Interestingly, A-center nitrogen was observed in the obtained diamond and the characteristic absorption peaks located at 1095 cm-1 and 1282 cm-1. Especially, the absorption peak at 1426 cm-1 attributing to the aggregation B-center nitrogen defect was distinctly found when the CH4N2S content reached 0.3 mg in the synthesis system, which was extremely rare in synthetic diamond. Furthermore, optical color centers in the synthesized crystals were investigated by photoluminescence (PL).

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.

Novel Methodologies for Preventing Crack Propagation in Steel Gas Pipelines Considering the Temperature Effect

Using the software ANSYS-19.2/Explicit Dynamics,this study performedfinite-element modeling of the large-diameter steel pipeline cross-section for the Beineu-Bozoy-Shymkent gas pipeline with a non-through straight crack,strengthened by steel wire wrapping.The effects of the thread tensile force of the steel winding in the form of single rings at the crack edges and the wires with different winding diameters and pitches were also studied.The results showed that the strengthening was preferably executed at a minimum value of the thread tensile force,which was 6.4%more effective than that at its maximum value.The analysis of the influence of the winding dia-meters showed that the equivalent stresses increased by 32%from the beginning of the crack growth until the wire broke.The increment in winding diameter decelerated the disclosure of the edge crack and reduced its length by 8.2%.The analysis of the influence of the winding pitch showed that decreasing the distance between the winding turns also led to a 33.6%reduction in the length of the straight crack and a 7.9%reduction in the maximum stres-ses on the strengthened pipeline cross-section.The analysis of the temperature effect on the pipeline material,within a range from-40℃ to+50℃,resulted in a crack length change of up to 5.8%.As the temperature dropped,the crack length decreased.Within such a temperature range,the maximum stresses were observed along the cen-tral area of the crack,which were equal to 413 MPa at+50℃ and 440 MPa at-40℃.The results also showed that the presence of the steel winding in the pipeline significantly reduced the length of crack propagation up to 8.4 times,depending on the temperature effect and design parameters of prestressing.This work integrated the existing methods for crack localization along steel gas pipelines.

High temperature and high pressure rheological properties of high-density water-based drilling fluids for deep wells

To maintain tight control over rheological properties of high-density water-based drilling fluids, it is essential to understand the factors influencing the theology of water-based drilling fluids. This paper examines temperature effects on the rheological properties of two types of high-density water-based drilling fluids （fresh water-based and brine-based） under high temperature and high pressure （HTHP） with a Fann 50SL rheometer. On the basis of the water-based drilling fluid systems formulated in laboratory, this paper mainly describes the influences of different types and concentration of clay, the content of a colloid stabilizer named GHJ-1 and fluid density on the rheological parameters such as viscosity and shear stress. In addition, the effects of aging temperature and aging time of the drilling fluid on these parameters were also examined. Clay content and proportions for different densities of brine-based fluids were recommended to effectively regulate the rheological properties. Four theological models, the Bingham, power law, Casson and H-B models, were employed to fit the rheological parameters. It turns out that the H-B model was the best one to describe the rheological properties of the high-density drilling fluid under HTHP conditions and power law model produced the worst fit. In addition, a new mathematical model that describes the apparent viscosity as a function of temperature and pressure was established and has been applied on site.

A new and reliable model for predicting methane viscosity at high pressures and high temperatures

In recent years, there has been an increase of interest in the flow of gases at relatively high pressures and high temperatures. Hydrodynamic calculation of the energy losses in the flow of gases in conduits, as well as through the porous media constituting natural petroleum reservoirs, requires knowledge of the viscosity of the fluid at the pressure and temperature involved. Although there are numerous publications concerning the viscosity of methane at atmospheric pressure, there appears to be little information available relating to the effect of pressure and temperature upon the viscosity. A survey of the literature reveals that the disagreements between published data on the viscosity of methane are common and that most investigations have been conducted over restricted temperature and pressure ranges. Experimental viscosity data for methane are presented for temperatures from 320 to 400 K and pressures from 3000 to 140000 kPa by using falling body viscometer. A summary is given to evaluate the available data for methane, and a comparison is presented for that data common to the experimental range reported in this paper. A new and reliable correlation for methane gas viscosity is presented. Predicted values are given for temperatures up to 400 K and pressures up to 140000 kPa with Average Absolute Percent Relative Error （EABS） of 0.794.

Pressure Prediction for High-Temperature and High-Pressure Formation and Its Application to Drilling in the Northern South China Sea

There are plentiful potential hydrocarbon resources in the Yinggehai and Qiongdongnan basins in the northern South China Sea. However, the special petrol-geological condition with high formation temperature and pressure greatly blocked hydrocarbon exploration. The conventional means of drills, including methods in the prediction and monitoring of underground strata pressure, can no longer meet the requirements in this area. The China National Offshore Oil Corporation has allocated one well with a designed depth of 3200 m and pressure coefficient of 2.3 in the Yinggehai Basin (called test well in the paper) in order to find gas reservoirs in middle-deep section in the Miocene Huangliu and Meishan formations at the depth below 3000 m. Therefore, combined with the '863' national high-tech project, the authors analyzed the distribution of overpressure in the Yinggehai and Qiongdongnan basins, and set up a series of key technologies and methods to predict and monitor formation pressure, and then apply the results to pressure prediction of the test well. Because of the exact pressure prediction before and during drilling, associated procedure design of casing and their allocation in test well has been ensured to be more rational. This well is successfully drilled to the depth of 3485 m (nearly 300 m deeper than the designed depth) under the formation pressure about 2.3 SG (EMW), which indicate that a new step in the technology of drilling in higher temperature and pressure has been reached in the China National Offshore Oil Corporation.