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 sour...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.展开更多
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 grai...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.展开更多
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 press...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.展开更多
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 le...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).展开更多
Nanodiamonds have outstanding mechanical properties,chemical inertness,and biocompatibility,which give them potential in various applications.Current methods for preparing nanodiamonds often lead to products with impu...Nanodiamonds have outstanding mechanical properties,chemical inertness,and biocompatibility,which give them potential in various applications.Current methods for preparing nanodiamonds often lead to products with impurities and uneven morphologies.We report a two-step high-pressure high-temperature(HPHT) method to synthesize nanodiamonds using naphthalene as the precursor without metal catalysts.The grain size of the diamonds decreases with increasing carbonization time(at constant pressure and temperature of 11.5 GPa and 700℃,respectively).This is discussed in terms of the different crystallinities of the carbon intermediates.The probability of secondary anvil cracking during the HPHT process is also reduced.These results indicate that the two-step method is efficient for synthesizing nanodiamonds,and that it is applicable to other organic precursors.展开更多
Accurate gas viscosity determination is an important issue in the oil and gas industries.Experimental approaches for gas viscosity measurement are timeconsuming,expensive and hardly possible at high pressures and high...Accurate gas viscosity determination is an important issue in the oil and gas industries.Experimental approaches for gas viscosity measurement are timeconsuming,expensive and hardly possible at high pressures and high temperatures(HPHT).In this study,a number of correlations were developed to estimate gas viscosity by the use of group method of data handling(GMDH)type neural network and gene expression programming(GEP)techniques using a large data set containing more than 3000 experimental data points for methane,nitrogen,and hydrocarbon gas mixtures.It is worth mentioning that unlike many of viscosity correlations,the proposed ones in this study could compute gas viscosity at pressures ranging between 34 and 172 MPa and temperatures between 310 and 1300 K.Also,a comparison was performed between the results of these established models and the results of ten wellknown models reported in the literature.Average absolute relative errors of GMDH models were obtained 4.23%,0.64%,and 0.61%for hydrocarbon gas mixtures,methane,and nitrogen,respectively.In addition,graphical analyses indicate that the GMDH can predict gas viscosity with higher accuracy than GEP at HPHT conditions.Also,using leverage technique,valid,suspected and outlier data points were determined.Finally,trends of gas viscosity models at different conditions were evaluated.展开更多
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 develope...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.展开更多
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...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.展开更多
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 sh...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.展开更多
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 co...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.展开更多
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 ...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.展开更多
Large diamond crystals were successfully synthesized by a FeNi C system using the temperature gradient method under high-pressure high-temperature conditions. The assembly of the growth cell was improved and the growt...Large diamond crystals were successfully synthesized by a FeNi C system using the temperature gradient method under high-pressure high-temperature conditions. The assembly of the growth cell was improved and the growth process of diamond was investigated. Effects of the symmetry of the carbon convection field around the growing diamond crystal were investigated systematically by adjusting the position of the seed crystal in the melted catalyst/solvent. The results indicate that the morphologies and metal inclusion distributions of the synthetic diamond crystals vary obviously in both symmetric and non-symmetric carbon convection fields with temperature. Moreover, the finite element method was applied to analyze the carbon convection mode of the melted catalyst/solvent around the diamond crystal. This work is helpful for understanding the growth mechanism of diamond.展开更多
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...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.展开更多
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 G...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).展开更多
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 spe...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.展开更多
The synergistic influences of boron,oxygen,and titanium on growing large single-crystal diamonds are studied using different concentrations of B_(2)O_(3) in a solvent-carbon system under 5.5 GPa-5.7 GPa and 1300℃-150...The synergistic influences of boron,oxygen,and titanium on growing large single-crystal diamonds are studied using different concentrations of B_(2)O_(3) in a solvent-carbon system under 5.5 GPa-5.7 GPa and 1300℃-1500℃.It is found that the boron atoms are difficult to enter into the crystal when boron and oxygen impurities are doped using B_(2)O_(3) without the addition of Ti atoms.However,high boron content is achieved in the doped diamonds that were synthesized with the addition of Ti.Additionally,boron-oxygen complexes are found on the surface of the crystal,and oxygen-related impurities appear in the crystal interior when Ti atoms are added into the FeNi-C system.The results show that the introduction of Ti atoms into the synthesis cavity can effectively control the number of boron atoms and the number of oxygen atoms in the crystal.This has important scientific significance not only for understanding the synergistic influence of boron,oxygen,and titanium atoms on the growth of diamond in the earth,but also for preparing the high-concentration boron or oxygen containing semiconductor diamond technologies.展开更多
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 addi...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.展开更多
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 ...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.展开更多
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 ...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.展开更多
基金Financial support comes from China National Natural Science Foundation(Grant No.51974352)as well as from China University of Petroleum(East China)(Grant Nos.2018000025 and 2019000011)。
文摘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.
基金the National Natural Science Foundation of China(Grant No.12074273)。
文摘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.
基金funded by the CNOOC Scientific Research Project“Study of cementing key properties and its matching technology of LD-10 gas field”(Grant No.CCL2019ZJFN1227).
文摘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.
文摘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).
基金Project supported by the National Key R&D Program of China(Grant No.2018YFB0406500)the National Natural Science Foundation of China(Grant Nos.U1804155,U1604263,and 11804307)the China Postdoctoral Science Foundation(Grant Nos.2018M630830 and 2019T120631).
文摘Nanodiamonds have outstanding mechanical properties,chemical inertness,and biocompatibility,which give them potential in various applications.Current methods for preparing nanodiamonds often lead to products with impurities and uneven morphologies.We report a two-step high-pressure high-temperature(HPHT) method to synthesize nanodiamonds using naphthalene as the precursor without metal catalysts.The grain size of the diamonds decreases with increasing carbonization time(at constant pressure and temperature of 11.5 GPa and 700℃,respectively).This is discussed in terms of the different crystallinities of the carbon intermediates.The probability of secondary anvil cracking during the HPHT process is also reduced.These results indicate that the two-step method is efficient for synthesizing nanodiamonds,and that it is applicable to other organic precursors.
文摘Accurate gas viscosity determination is an important issue in the oil and gas industries.Experimental approaches for gas viscosity measurement are timeconsuming,expensive and hardly possible at high pressures and high temperatures(HPHT).In this study,a number of correlations were developed to estimate gas viscosity by the use of group method of data handling(GMDH)type neural network and gene expression programming(GEP)techniques using a large data set containing more than 3000 experimental data points for methane,nitrogen,and hydrocarbon gas mixtures.It is worth mentioning that unlike many of viscosity correlations,the proposed ones in this study could compute gas viscosity at pressures ranging between 34 and 172 MPa and temperatures between 310 and 1300 K.Also,a comparison was performed between the results of these established models and the results of ten wellknown models reported in the literature.Average absolute relative errors of GMDH models were obtained 4.23%,0.64%,and 0.61%for hydrocarbon gas mixtures,methane,and nitrogen,respectively.In addition,graphical analyses indicate that the GMDH can predict gas viscosity with higher accuracy than GEP at HPHT conditions.Also,using leverage technique,valid,suspected and outlier data points were determined.Finally,trends of gas viscosity models at different conditions were evaluated.
基金Supported by National Key R&D Program of China(Grant No.2022YFB3401901)Key Program of National Natural Science Foundation of China(Grant No.U2067221)+2 种基金Sichuan Provincial Science and Technology Planning Project(Grant Nos.2022JDJQ0019 and 2022ZYD0029)Funds for China Postdoctoral Science Foundation(Grant No.2022M713008)Sichuan Provincial Innovative Talent Funding Project for Postdoctoral Fellows(Grant No.BX202225).
文摘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.
基金Project supported by the National Natural Science Foundation of China(Grant No.51172089)the Education Department of Henan Province,China(Grant No.12A430010)the Fundamental Research Funds for the Universities of Henan Province,China(Grant No.NSFRF140110)
文摘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.
基金Project supported by the National Natural Science Foundation of China (Grant No. 51172089)the Program for New Century Excellent Talents in University of China
文摘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.
基金This research project was granted by the Knowledge-Innovation Program sponsored by the Chinese Academy of Sciences(KZCX3-SW-124).
文摘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.
基金Supported by the National Natural Science Foundation of China under Grant No 51172089the Natural Science Foundation of Guizhou Province Education Department under Grant No KY[2013]183the Natural Science Foundation of Guizhou Province Science and Technology Agency under Grant Nos LH[2015]7232 and LH[2015]7228
文摘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.
基金Project supported by the National Natural Science Foundation of China (Grant Nos. 50572032, 50731006, and 50801030)the Young Scientists Fund of the National Natural Science Foundation of China (Grant Nos. 51001042 and 51002045)
文摘Large diamond crystals were successfully synthesized by a FeNi C system using the temperature gradient method under high-pressure high-temperature conditions. The assembly of the growth cell was improved and the growth process of diamond was investigated. Effects of the symmetry of the carbon convection field around the growing diamond crystal were investigated systematically by adjusting the position of the seed crystal in the melted catalyst/solvent. The results indicate that the morphologies and metal inclusion distributions of the synthetic diamond crystals vary obviously in both symmetric and non-symmetric carbon convection fields with temperature. Moreover, the finite element method was applied to analyze the carbon convection mode of the melted catalyst/solvent around the diamond crystal. This work is helpful for understanding the growth mechanism of diamond.
基金supported by the National Natural Science Foundation of China (Grant Nos. 51772120, 11704340, 11604246, and 11865005)the Scientific and Technological Project in Henan Province+2 种基金China (Grant No. 202102210198)the Natural Science Foundation of Guangxi (China)(Grant No. 2018GXNSFAA281024)Doctor Start-up Foundation of Guangxi University of Science and Technology (Grant No. 20Z38)。
文摘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.
文摘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).
基金Funded by the National Natural Science Foundation of China (Nos.50572067,10772126)
文摘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.
基金supported by the National Natural Science Foundation of China(Grant Nos.11804305,12004341,11704340,and 12004342)the Key Research Project of Higher Education Institution of Henan Province,China(Grant No.19A140006)+2 种基金the Scientific and Technological Project in Henan Province,China(Grant No.202102210198)the Natural Science Foundation of Chongqing,China(Grant No.cstc2019jcyjmsxmX0391)the Science and Technology Research Program of Chongqing Municipal Education Commission,China(Grant No.KJQN201901405)。
文摘The synergistic influences of boron,oxygen,and titanium on growing large single-crystal diamonds are studied using different concentrations of B_(2)O_(3) in a solvent-carbon system under 5.5 GPa-5.7 GPa and 1300℃-1500℃.It is found that the boron atoms are difficult to enter into the crystal when boron and oxygen impurities are doped using B_(2)O_(3) without the addition of Ti atoms.However,high boron content is achieved in the doped diamonds that were synthesized with the addition of Ti.Additionally,boron-oxygen complexes are found on the surface of the crystal,and oxygen-related impurities appear in the crystal interior when Ti atoms are added into the FeNi-C system.The results show that the introduction of Ti atoms into the synthesis cavity can effectively control the number of boron atoms and the number of oxygen atoms in the crystal.This has important scientific significance not only for understanding the synergistic influence of boron,oxygen,and titanium atoms on the growth of diamond in the earth,but also for preparing the high-concentration boron or oxygen containing semiconductor diamond technologies.
基金supported by the Doctoral Fund of Henan Polytechnic University,China(Grant Nos.B2013-013 and B2013-044)the Research Projects of Science and Technology of the Education Department of Henan Province,China(Grant Nos.14B430026 and 12A430010)
文摘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.
基金Project supported by the National Natural Science Foundation of China (Grant No. 50572032)
文摘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.
基金Project supported by the National Natural Science Foundation of China (Grant Nos. 50572032 and 50731006)
文摘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.