High Pressure And High Temperature Research Articles

Transient temperature and pressure coupling model of cementing injection stage in ultra deep wells considering segmental rheological model, casing eccentricity and U-tube effect

The geological environments of ultra deep wells such as high temperature and high pressure (HTHP), narrow safety density window pose significant challenges to cementing operation. Considering segmental rheological model and density model, casing eccentricity, U-tube effect and viscous dissipation, this paper established a transient temperature and pressure coupling model during cementing injection stage of ultra deep wells. The segmental rheological model can describe the rheological properties of cementing fluids under HTHP much better. Considering casing eccentricity and viscous dissipation can accurately model the variation of temperature and pressure profiles. Taking U-tube effect into the model, the formation process of vacuum section at top of the casing can be simulated. The fully implicit finite-difference approach was used to solve the coupling model, and the calculation results were compared with field measurement data and simulation data to verify its accuracy. The calculation errors of the developed model are respectively 10% and 5% compared to field measurement data and Wellplan’s simulation data. Numerical simulations were conducted to reveal the cementing fluid distribution, transient temperature distribution and pressure distribution during the cementing injection stage. The simulation results show that the variety of cementing fluids with different density, rheological properties and thermophysical parameters complicates the change mechanism of temperature and pressure. The temperature and pressure distributions both present unsteady characteristics during cementing injection stage, which puts forward higher requirements of pressure control for narrow safety density window formation. The influence of temperature and pressure on rheology of cementing fluids can not be ignored, and segmental rheological model should be considered for accurate pressure prediction. Also the casing eccentricity can not be ignored for cementing pressure calculation in deviated or horizontal wells. Managed pressure cementing (MPC) has a greater advantage in dealing with narrow density window formation. The synergistic control of cementing fluid density and back pressure can keep the equivalent circulating density (ECD) within the safe density window. Through the application of the transient temperature and pressure coupling model, we can simulate the variations of key dynamic parameters during cementing injection stage and optimize the cementing parameters.

Experimental and modelling studies on static sag of solid weighting powders in Polysulfonate workover fluids at high temperature and high pressure

The solid weighting material in a high-density workover fluid is prone to static sag. Existing experimental methods cannot predict the parameters of the settling stability of workover fluids at high temperature and high pressure (HTHP). Therefore, in this study, static settlement experiments were carried out using a novel experimental setup. The experimental setup enables the measurement of the density profile of heavy workover fluids at HTHP. A multi-parameter correlation equation between the sag factor and particle diameter, particle density, base fluid density, workover fluid density and rheological parameters, aging time, temperature, and pressure was obtained using dimensional analysis and multivariate nonlinear regression methods. The results reveal that the settlement stability of the workover fluid decreases with the increase in temperature and pressure. Based on the multi-parameter correlation, the predicted and the measured values were compared and verified. The error between the predicted value and the measured value was within 5%. The average prediction error was 1.68%, and the maximum prediction error was 3.8%. These results reveal that the model proposed in this study can effectively predict the static sedimentation stability of the solid weighted Polysulfonate workover fluids. Furthermore, the proposed correlation can guide the properties adjustment of the workover fluids to achieve the required sag stability. This work provides a new approach to predict and control the sag stability of the solid weighted workover fluids.

Optimization of Co4Sb11.5Te0.5 thermoelectric performance through Al filling under high temperature and high pressure

So far, the method of optimizing the thermoelectric properties of skutterudite CoSb3 is usually to achieve a breakthrough in high-properties thermoelectric merit by selecting excellent doping atoms and determining a reasonable percentage of atoms. In this study, we achieved the preparation of small atomic radius Al-filled Co4Sb11.5Te0.5 compounds by high-temperature and high-pressure (HTHP) synthesis methods. The thermoelectric properties of the samples AlxCo4Sb11.5Te0.5 were optimized from two dimensions: synthesis pressures (1.0 GPa, 1.5 GPa, 2.0 GPa) and Al filling concentration (x = 0.1, 0.2, 0.3, 0.5), ultimately achieving effective decoupling of electron-phonon transport properties. The experimental results show that Al doping can optimize the electrical transport properties of materials effectively, rapid synthesis method of HTHP can introduce abundant grain boundaries, diversification of grain sizes, a large number of dislocations and widely distributed nano second phase, etc. These microstructures in bulk materials form a multi-scale phonon scattering network in situ, which can effectively scatter phonons and reduce the lattice thermal conductivity effectively. After optimizing the synthesis pressure and Al filling concentration through orthogonal transformation, the sample Al0.3Co4Sb11.5Te0.5 prepared at a synthesis pressure of 1.5 GPa obtained a minimum lattice thermal conductivity value of 0.88 W m−1 K−1, a maximum power factor of 40.96 μ W cm−1 K−2 and a maximum zT value of 1.18 at 773.15 K.

A distinctive HPHT platform with different types of large-volume press subsystems at SECUF

Large-volume presses (LVPs) providing large volumes, liquid media, deformation capability, jump compression, and in situ measurements are in great demand for high-pressure research, particularly in the fields of geoscience, condensed matter physics, material science, chemistry, and biology. A high-pressure and high-temperature (HPHT) platform with different LVP subsystems, both solid-state and liquid environments, and nonequilibrium subsystems, has been constructed at the Synergetic Extreme Condition User Facility, Jilin University. This article describes the construction of the different subsystems and provides an overview of the capabilities and characteristics of the different HPHT subsystems. A large sample volume (1000 mm3) at 20 GPa is achieved through the use of a belt-type apparatus in the solid-state subsystem. HPHT conditions (1.8 GPa and 1000 K) are realized in the liquid subsystem through the use of a piston–cylinder-type LVP with optical diamond windows for in situ spectroscopic measurements. A maximum pressure jump to 10.2 GPa can be reached within 20 ms in the nonequilibrium subsystem with the use of an improved bladder-pressurization jump press. Some typical results obtained with different LVPs are briefly reviewed to illustrate the applications and advantages of these presses. In summary, the platform described here has the potential to contribute greatly to high-pressure research and to innovations in high-pressure technology.

Abnormal sintering behaviors of chromium carbide under high pressure and high temperature

Controlling grain behavior during high pressure and high temperature (HPHT) sintering is crucial for synthesizing high-performance bulk ceramic materials. Chromium carbide (Cr3C2), a representative transition metal carbide ceramic, finds extensive industrial applications owing to its exceptional combination of properties. In this study, the intricate grain behaviors in Cr3C2 under 15 GPa/25–1700 °C are revealed by HPHT methods. It is found that the mechanical and elastic properties of Cr3C2 exhibit a significant dependence on temperature-induced grain behavior. Particularly, the mechanical properties of Cr3C2 exhibit abnormal softening at 15 GPa/1200 °C and 15 GPa/1500 °C. Through characterization and analysis of the microstructure, it is confirmed that the significant change in mechanical properties stems from the abnormal sintering behaviors of distinctive competitive behavior of grain refinement and growth. The findings highlight the significant influence of the competitive behavior on microstructural evolution, which exhibits strong correlations with the mechanical properties.

Optimizing the Influence of Fly Ash as an Anti-Sagging Additive in Highly Deviated Geothermal Well Drilling Fluids Using Surface Response Method

Weighting materials such as barite and ilmenite are crucial for controlling fluid density during deep or ultra-deep drilling operations. However, sagging poses significant challenges, especially in highly deviated high-pressure and high-temperature (HP/HT) wells. This leads to inadequate well control, wellbore instability, and variations in hydrostatic pressure in extended-reach wells. Given the challenges of experimental research, reliable prediction models are imperative for evaluating the interaction between the ratio of anti-sagging additives, temperature, and wellbore inclination on sag factor (SF). This research presents statistical-based empirical models for predicting the SF at various wellbore inclinations (0°, 30°, 45°, 60°, 70°, 80°, and 90°) and assessing the influence of fly ash on the SF. The regression equations, developed using the Response Surface Methodology in Minitab 18 software, show high reliability, with R2 values approaching unity. Contour and surface response plots provide a clear understanding of the variable interactions. The analysis reveals that sagging is most severe at 60° to 65° inclination. At 400 °F and 60° inclination, adding 4 lb/bbl of fly ash reduces sagging in barite and ilmenite-densified fluid by 63.9% and 63.1%, respectively. Model validation shows high accuracy, with percentage errors below 3%. This study offers valuable insights for optimizing drilling fluid formulations in HP/HT well environments.

The Influence of Cyclic Loading on the Mechanical Properties of Well Cement

The cyclic loading generated by injection and production operations in underground gas storage facilities can lead to fatigue damage to cement sheaths and compromise the integrity of wellbores. To investigate the influence of cyclic loading on the fatigue damage of well cement, uniaxial and triaxial loading tests were conducted at different temperatures, with maximum cyclic loading intensity ranging from 60% to 90% of the ultimate strength. Test results indicate that the compressive strength and elastic modulus of well cement subjected to monotonic loading under high-temperature and high-pressure (HTHP) testing conditions were 14–21% lower than those obtained under ambient testing conditions. The stress–strain curve exhibits stress–strain hysteresis loops during cyclic loading tests, and the plastic deformation capacity is enhanced at HTHP conditions. Notably, a higher intensity of cyclic loading results in more significant plastic strain in oil-well cement, leading to the conversion of more input energy into dissipative energy. Furthermore, the secant modulus of well cement decreased with cycle number, which is especially significant under ambient test conditions with high loading intensity. Within 20 cycles of cyclic loading tests, only the sample tested at a loading intensity of 90% ultimate strength under an ambient environment failed. For samples that remained intact after 20 cycles of cyclic loading, the compressive strength and stress–strain behavior were similar to those obtained before cyclic loading. Only a slight decrease in the elastic modulus is observed in samples cycled with high loading intensity. Overall, oil-well cement has a longer fatigue life when subjected to HTHP testing conditions compared to that tested under ambient conditions. The fatigue life of well cement increases significantly with a decrease in loading intensity and can be predicted based on the plastic strain evolution rate.

Performance evaluation of the nano-biodegradable drilling fluid using the greenly synthesized zinc nanorods and gundelia seed waste

Addressing the increasing demand for green additives in drilling fluids is essential for the sustainable development of the oil and gas industry. Fluid loss into porous and permeable formations during drilling presents significant challenges. This study introduced an innovative, environmentally sustainable drilling fluid known as nano-biodegradable drilling fluid (NBDF). The NBDF formulation incorporates greenly synthesized zinc nanorods (ZNRs) and gundelia seed shell powder, with ZNRs derived from Cydonia oblonga plant extracts using an eco-friendly method. The research developed multiple drilling fluid variants for experimentation: a reference drilling fluid (BM); biodegradable drilling fluid (BDF) with particle sizes of 75, 150, 300, and 600 µm at concentrations ranging from 0.5 to 1 wt% (GSMs); a drilling nanofluid (DNF) with ZNRs at a 0.1 wt% concentration (ZNR); and NBDF combining both nano and gundelia waste (GS-ZNR). Experimental tests were conducted under various temperature and pressure conditions, including low temperature and low pressure (LTLP) and high temperature and high pressure (HTHP). Rheological and filtration measurements were performed to assess the impact of the nano-biodegradable additives on flow behavior and fluid loss. Results indicated that incorporating 1 wt% of gundelia seed shell powder with a particle size of 75 µm led to a 19.61% reduction in fluid loss compared to BM at 75 °C and 200 psi. The performance of the same GSM improved by 31% under identical conditions when 1 wt% of zinc ZNRs was added. Notably, the GS-ZNR formulation demonstrated the most effective performance in reducing fluid loss into the formation, decreasing mud cake thickness, and enhancing the flow behavior of the non-Newtonian reference drilling fluid. This study highlights the relevance of particle size in the effectiveness of biodegradable additives and underscores the potential of NBDF to address environmental concerns in the oil and gas drilling industry.

Enhancement of Rheological Properties of Nano-Fe2O3-Modified Drilling Fluids

Summary In this study, we explore the potential of using nanoparticles (NPs) to enhance the properties of water-based drilling fluids (WBDFs). Specifically, we investigate the effects of nano-Fe2O3 on the rheological behavior of drilling fluid muds under high-temperature and high-pressure (HTHP) conditions to determine the optimal concentration of Fe2O3 NPs to maintain consistent rheology and improve drilling fluid systems. Results show that as temperature increases, the rheological properties of water-based muds (WBMs) decrease, leading to compromised structural integrity. To address this issue, nano-Fe2O3 is introduced into the system. We prepared and evaluated six WBM formulations with varying weight percentages of Fe2O3 NPs, and found that an optimal NP concentration of 2.5 g wt% resulted in a 13.8% reduction in American Petroleum Institute (API) filtrate volume and a 40% reduction in filter-cake thickness. Under conditions of 300°F temperature and 10,000 psi pressure, consistent reductions were observed in the rheological properties of plastic viscosity (PV), yield point (YP), and gel strength with the addition of Fe2O3 NPs. The YP-PV span was measured at 2.7, and the yield strength was determined to be 11 lb/100 ft2. Regarding fluid loss, Drilling Mudcake A containing 0.5 wt% NPs experienced a loss of 6 mL of fluid after 30 minutes, whereas Mudcake E containing 3 wt% NPs exhibited a fluid loss of 5.1 mL in the API filter press test. According to the Bingham plastic model, Muds E and F, containing 2.5 wt% and 3 wt% NPs, respectively, displayed the maximum shear stress vs. shear rate. This highlights the efficacy of nano-Fe2O3 in adjusting the properties of drilling fluids, presenting opportunities for enhanced performance and efficiency in drilling operations.

Evaluation of the effect of oxygen addition on charge carrier transport properties in single-crystal diamond growth

The effects of oxygen addition during single-crystal diamond growth by microwave plasma CVD method on crystal surface morphology and charge carrier transport properties were evaluated. Diamond single-crystals were homoepitaxially grown on (001) surface of high-pressure and high-temperature (HPHT) synthesized type IIa single-crystal diamond substrates with a fixed methane concentration of 1 % and oxygen concentrations of 0–0.8 %. Inverted pyramid-shaped pits were generated as the oxygen concentration increased. The free exciton recombination emission intensity in the cathodoluminescence spectrum reached a maximum at oxygen concentration of 0.5 %. The samples with oxygen concentrations of 0.5 % and 0.8 % showed excellent charge collection efficiency and energy resolution. On the other hand, the mobility-lifetime (μτ) product was only (7.1 ± 1.7) × 10−5 cm2/V, which is approximately 1/4 of that of the sample with 0.2 % methane and no oxygen addition.

Effects of high-temperature and high-pressure immersion corrosion durations on the fretting tribo-corrosion behaviors of Inconel 690 alloy

An Inconel 690 alloy tube acting as a steam generator tube has been widely applied in the second and third generations of nuclear power plants using pressurized water reactors. However, its entire service process is always accompanied by high-temperature and high-pressure (HTHP) liquid medium corrosion and various fretting mechanical damage behaviors. This study first immerses the Inconel 690 alloy tube in HTHP corrosive medium for different lengths of time (0, 4, 8, and 12 h); then, a fretting tribo-corrosion test rig is used to investigate the effect of different fretting mechanical parameters on the surface damage mechanism and electrochemical dynamic response of each test sample. Results show that the corrosion rate of the Inconel 690 alloy tube has significantly increased after being treated by HTHP immersion corrosion, which is mainly due to the pre-existing corrosion products.

Effect of shot peening on surface characteristics and high-temperature corrosion behaviour of super 13Cr martensitic stainless steel

Super 13Cr, as an economy stainless steel (SS) for oil country tubular goods, needs stable corrosion resistance in high-pressure and high-temperature (HPHT) downhole medium. Severe plastic deformation (SPD) are the surface modification technology to improve mechanical properties, fatigue behavior and corrosion resistance of metals, and shot peening (SP) has been the most widely used SPD process. However, there are quite limited studies about the microsutructure evolution, residual stress, and high-temperature corrosion behavior of SP-treated martensitic SS. In this study, super 13Cr martensitic SS was treated by SP with various air pressures and nozzle speeds. The surface characteristics and high-temperature corrosion behaviour in 3.17 mol/L K2HPO4 solution were investigated through finite element model analysis, characterization of residual stress and microstructure, as well as electrochemical and stress corrosion cracking (SCC) tests at 160 °C and 10 MPa. The results showed that SP-treated super 13Cr could generate high-level compressive residual stress and SPD microstucture, including nano-sized equiaxed grains, gradient lamellar structure and fragmented carbides. Increasing air pressure contributed to achieve uniform nanocrystalline, but tended to generate high dislocation density and surface defects. The improving effect of SP treatment at low air pressure of 0.15 MPa on passivation ability was limited, and high air pressure adversely impacted corrosion resistance. SP-treated specimens showed high SCC susceptibility, due to the introduction of more surface defects, high angle grain boundaries, and dislocations.

Microwave solvothermal synthesis and HTHP sintering of CoSb3/rGO composites: In-situ synthesis and enhanced thermoelectric properties

The utilization of CoSb3-based thermoelectric materials is currently confined to aviation applications, primarily attributed to their elevated thermal conductivity (κ) values. The incorporation of a nanostructuring approach, coupled with the introduction of a secondary phase, has demonstrated efficacy in diminishing the thermal conductivity (κ) values of CoSb3 materials. Here, the CoSb3/reduced graphene oxide (CoSb3/rGO) composites are obtained by sintering the as-synthesized powders, which ultra-fast synthesized in situ via microwave solvothermal method, under the High-temperature and High-Pressure (HTHP) conditions. The influence of reduced graphene oxide (rGO) on the structural and thermoelectric characteristics of CoSb3 composites has been systematically explored. In this study, CoSb3 nanoparticles with an average size of ∼33 nm exhibit uniform distribution, being effectively anchored onto the 2D sheets of rGO. In this work, the lattice thermal conductivity of CoSb3/rGO composites decreased with the addition of rGO. Based on the Debye-Callaway model, we attribute this to the effective scattering of phonons by the interface formed between the CoSb3 nanocrystals and the lamellar rGO. As a result, the CoSb3/rGO composite, containing 2 wt% graphene, exhibits a significantly enhanced maximum thermoelectric figure of merit (ZT) value, reaching ∼0.325 at 700 K. This represents an impressive improvement of approximately 300 % compared to the ZT value of the graphene-free CoSb3 bulk counterpart, which is ∼0.106. This study demonstrates the microwave solvothermal synthesis and HTHP sintering are in favor for an efficient, economical, and controllable synthesis of CoSb3/rGO composites, which provides a novel strategy for securing better thermoelectric performance.

Enhanced thermoelectric performance of MoSe2 under high pressure and high temperature by suppressing bipolar effect

The electrical transport property of layered MoSe2 has a strong response to high pressure by enhancing the inter-layer interaction. However, the narrowed bandgap under high pressure will cause the bipolar effect (i.e., the thermally excited minority carriers contribute to a Seebeck coefficient with the opposite sign to the majority carriers) at high temperatures to degrade the thermoelectric (TE) performance. Hence, suppressing the bipolar effect is important to optimize the TE performance of MoSe2 under high pressure and high temperature (HPHT). In this study, the degradation of TE performance caused by the bipolar effect under HPHT in MoSe2 is investigated. It is found that in MoSe2, the electrical conductivity was improved significantly by pressure; however, the bipolar effect led to a significantly degraded Seebeck coefficient at high temperatures. By injecting massive carriers beforehand, the bipolar effect was suppressed to make a dominant type of p-type charge carries, achieving an increased Seebeck coefficient with increasing temperature, resulting in an improved power factor from 29.3 μW m−1 K−2 in MoSe2 to 285.7 μW m−1 K−2 in Mo0.98Nb0.02Se2 at 5.5 GPa, 1110 K. Combined with the reduced thermal conductivity by point defect scattering on phonons, a maximum ZT value of 0.11 at 5.5 GPa, 1110 K. This work highlights the significance of suppressing the bipolar effect under HPHT for optimizing TE performance in such layered semiconductors.

A gas chromatography system for measuring carbonaceous gases released at high-pressure and high-temperature conditions.

Carbonates or carbon-bearing materials may release gases under high pressure and high temperature (HP-HT) conditions. Characterizing the species and quantifying the volumes of these carbonaceous gases are critical for understanding carbon chemistry. However, the volatile nature of carbonaceous gas poses technical challenges in their collection, speciation, and quantification during HP-HT experiments. To address these challenges, we have developed a system that integrates sample collection, gas transportation, chemical conversion, and measurement of carbonaceous gases trapped within the large volume press capsules. The system comprises a capsule-crushing device for thorough sample pulverization, a mechanizer coupled with a flame ionization detector, a gas-sealing and transport interface, and gas chromatography for detection. To evaluate the system's capabilities, we quantified the gas volumes released from encapsulated kerogen quenched from 1.9GPa to 873, 973, and 1073K. The collected gas chromatography signals were compared to those obtained from standard mixed-gases. The volumes of CO2, CH4, and C2H6 in the samples were successfully derived from the signal peak area through calibration. The relative standard deviation value of two runs at 3GPa and 1073K is 1.956%, suggesting good reproducibility. Our system thus provides a robust solution for investigating carbon chemistry under HP-HT conditions.

Improvement of the microstructure of hydration products in cement paste by epoxy resin under high temperature and high pressure

This study develops a resin cement paste (RCP) with excellent elastic deformation and strength at high temperature and high pressure (HTHP) and determines the reinforcement-toughening mechanism of the resin in the cement paste using XRD, TG, Si29 MAS NMR, SEM, and nitrogen adsorption methods. The results showed that in the RCP, the resin mixture (RM) reduced the porosity of the RCP. The RM did not change the crystalline structure of hydration products in the paste, but some calcium ions diffused from the cement matrix into the RM. The calcium/silica ratio of the cement matrix decreased and layered hydration products were formed around the RM. Thus, in the RCP the content of hydration products containing layered gel pores (pore diameter of 3.8 nm) increased; compared with pure cement paste, the average chain length of the hydration products in the RCP increased from 3.09 to 3.46 when cured at 90 °C and 21 MPa for 28 d. Moreover, there was excellent cementation of the RM and cement matrix at HTHP. Compared with pure cement paste, the compressive strength and tensile strength of RCP containing 15 % RM increased by 14.61 % and 11 %, respectively, and the Young’s modulus decreased from 5.01 GPa to 4.56 GPa.

Structural and superconducting properties in hard Mo2BC

The utilization of high-hardness superconducting materials enhances and broadens the applications of superconductors. In this study, a high-hardness Mo2BC superconductor is synthesized using the high-pressure and high-temperature (HPHT) method. Our results demonstrate that it exhibits zero-resistance and Meissner effect below a superconducting critical temperature (Tc) of 7.0 K. The upper critical magnetic field of 4.3 T and the lower critical magnetic field of 226 Oe were obtained by data fitting, respectively. Type-II superconducting properties were confirmed by critical states analysis and Ginzburg-Landau (GL) parameters. Specific thermal properties revealed a Debye temperature as 565.1 K, while an electron-phonon coupling (EPC) parameter λ of 0.588 indicated properly coupled BCS conventional superconductivity. Mo2BC exhibits a Vickers hardness of up to 18.2 GPa, significantly surpassing that of traditional superconducting ceramics. It can be attributed to the robust covalent boron-zigzag-chains coupled with appropriate covalent [Mo6C] octahedrons within a non-centrosymmetric structure. The coexistence of both superconductivity and high hardness enables the versatility of Mo2BC, thereby laying the way for the development of high-hardness superconductors.

Effect of extreme environments on aging of fluoroelastomers

Fluoroelastomer compositions are used in extreme environments, such as high pressure and high temperature (HPHT), in a wide range of applications in the oil and gas industry. As hydrocarbon production is expanded to deeper formations, and operating temperature and pressure become higher, the material performance of these elastomers becomes more important. Hence, fluoroelastomers face new challenges and require further understanding when these undergo aging. In this study, a practical fluoroelastomer (FKM) composition was aged in deionized water and an alkaline hydraulic fluid up to 31 MPa, 225 °C and 168 hrs. High pressure, high temperature and aging time have deleterious effects on the physical and mechanical properties of FKMs in both the fluids. Spectroscopically, under these conditions, two hydrocarbon-related bands at 2917 and 2850 cm−1 and three fluorocarbon bands at 886, 1158 and 1396 cm−1 in the Fourier Transform Infrared spectra decreased in intensity after aging. The temperature, at which the rate of degradation was maximum, measured through thermogravimetry also decreased under HPHT conditions. It was further observed that the filler particles bound to the rubber leached out during the aging experiment to cause a color change of the fluid. The tensile sheet was delaminated with cracks on the surface under extreme conditions due to rapid changes in the properties of the surface compared to the bulk. Based on the characterization of the aged rubber vulcanizate and the particles leached out into the aging fluid, a mechanism of HPHT aging of FKM vulcanizate is proposed, which would be helpful in designing fluorocarbon compositions in extreme environments.

Utilizing phased array ultrasound technique to examine seal surface contact status in premium connections

Premium connections are commonly employed in wells subjected to high temperature and high pressure (HTHP) conditions. The key parameter in evaluating the sealing capability of premium connections is the contact condition between the sealing surface. This paper presents a method based on phased array ultrasound testing (PAUT) technique to examine the metal-to-metal contact states of the seal surface in premium conditions, and presents experimental work on contact status of the seal surface in premium tubing connections using PAUT, testing impacts of torque, seal surface defects and thread compounds dosage. The experimental findings demonstrate an inverse relationship between the observed ultrasonic reflection amplitude and the applied torque on the premium. Additionally, there is a robust exponential correlation manifested between the ultrasonic reflection amplitude and the torque exerted on the premium. The ultrasonic reflection amplitude at the defect of the seal surface increases. Under equivalent make-up torque conditions, the ultrasonic reflection amplitude on the sealing surface of premium connections escalates as the dosage of thread compounds diminishes, and the importance of precise control of the amount of thread compound used was confirmed. These data demonstrate that PAUT provides a reliable detection technique for performance assessment on premium connections, both in quality control and field inspection.

High-pressure high-temperature synthesis and characterization of B10C

The boron-rich boron carbide materials have been traditionally synthesized by adding boron powder to B4C material and subjecting it to hot pressing sintering for materials composition containing 8.8–20 at. % carbon in boron (composition range of B10.4C to B4C). Our study explores a synthesis route for B10C starting from high-purity boron and carbon and direct conversion under high pressure and high temperature (HPHT) conditions of 2000 °C and 6–8 GPa. Synthesis was verified via x-ray diffraction analysis, showing the conversion of the high-purity boron and carbon powder mixture into a hexagonal B10C structure (R-3m space group) with lattice parameters of a = b = 5.6115 Å and c = 12.197 Å. The concentration of boron was measured through x-ray photoelectron spectroscopy, confirming the B10C ratio. The measured nanoindentation mean hardness of B10C was 40 GPa. Raman spectroscopy of the HPHT synthesized sample shows characteristic vibrational breathing modes of boron icosahedron and an additional intense band at a vibrational frequency of 380 cm−1. This Raman band, which appears notably weaker in earlier studies and B4C samples, is assigned to the linear chain of B–B–B and attributed to the maximal incorporation of boron within the hexagonal structure.