Numerical simulation and experimental verification of a novel double-layered split die for high-pressure apparatus used for synthesizing superhard materials

Based on the principles of massive support and lateral support, a novel double-layered split die(DLSD) for high-pressure apparatus was designed to achieve a higher pressure-bearing capacity and larger sample cavity. The stress distributions of the DLSDs with different numbers of divided blocks were investigated by the finite element method and compared with the stress distributions of the conventional belt-type die(BTD). The results show that the cylinders and first-layer supporting rings of the DLSDs have dramatically smaller stresses than those of the BTD. In addition, increasing the number of divided blocks from 4 to 10 gradually increases the stress of the cylinder but has minimal influence on the stress of the supporting rings. The pressure-bearing capacities of the DLSDs with different numbers of divided blocks, especially with fewer blocks, are all remarkably higher than the pressure-bearing capacity of the BTD. The contrast experiments were also carried out to verify the simulated results. It is concluded that the pressure-bearing capacities of the DLSDs with 4 and 8 divided blocks are 1.58 and 1.45 times greater than that of the BTD. This work is rewarding for the commercial synthesis of high-quality, large-sized superhard materials using a double-layered split high-pressure die.

Function of large-volume high-pressure apparatus at SECUF

Pressure allows the precise tuning of a fundamental parameter, the interatomic distance, which controls the electronic structure and virtually all interatomic interactions that determine material properties. Hence, pressure tuning is an effective tool in the search for new materials with enhanced properties. To realize pressure tuning on matter, large-volume press （LVP） apparatuses have been widely used not only to synthesize novel materials but also to implement the in situ measurement of physical properties. Herein, we introduce the LVP apparatuses, including belt-type, cubic anvil, and 6-8 type multi-anvil, that will be constructed at the Synergetic Extreme Condition User Facility （SECUF） at Jilin University. Typically, cell volumes of 1000 mm3 can be obtained at 20 GPa in a belt-type apparatus that is significantly larger than that obtained in a 6-8 type multi-anvil apparatus at the same pressure. Furthermore, the in situ measurement of physical prop- erties, including thermological, electrical, and mechanical behaviors, is coupled to these LVP apparatuses. Some typical results of both synthetic experiments and in situ measurements obtained from the LVP apparatuses are also reviewed.

Influence of introducing Zr,Ti,Nb and Ce elements on externally solidified crystals and mechanical properties of high-pressure die-casting Al–Si alloy

High pressure die casting(HPDC)AlSi10Mn Mg alloy castings are widely used in the automobile industry.Mg can optimize the mechanical properties of castings through heat treatment,while the release of thermal stress arouses the deformation of large integrated die-castings.Herein,the development of non-heat treatment Al alloys is becoming the hot topic.In addition,HPDC contains externally solidified crystals(ESCs),which are detrimental to the mechanical properties of castings.To achieve high strength and toughness of non-heat treatment die-casting Al-Si alloy,we used AlSi9Mn alloy as matrix with the introduction of Zr,Ti,Nb,and Ce.Their influences on ESCs and mechanical properties were systematically investigated through three-dimensional reconstruction and thermodynamic simulation.Our results reveal that the addition of Ti increased ESCs'size and porosity,while the introduction of Nb refined ESCs and decreased porosity.Meanwhile,large-sized Al_3(Zr,Ti)phases formed and degraded the mechanical properties.Subsequent introduction of Ce resulted in the poisoning effect and reduced mechanical properties.

A novel rapid cooling assembly design in a high-pressure cubic press apparatus

In traditional high-pressure–temperature assembly design, priority has been given to temperature insulation and retention at high pressures.This limits the efficiency of cooling of samples at the end of experiments, with a negative impact on many studies in high-pressure Earth andplanetary science. Inefficient cooling of experiments containing molten phases at high temperature leads to the formation of quench textures,which makes it impossible to quantify key compositional parameters of the original molten phase, such as their volatile contents. Here,we present a new low-cost experimental assembly for rapid cooling in a six-anvil cubic press. This assembly not only retains high heatingefficiency and thermal insulation, but also enables a very high cooling rate (∼600 ℃/s from 1900 ℃ to the glass transition temperature).Without using expensive materials or external modification of the press, the cooling rate in an assembly (∼600 ℃/s) with cube lengths of38.5 mm is about ten times faster than that in the traditional assembly (∼60 ℃/s). Experiments yielding inhomogeneous quenched melttextures when the traditional assembly is used are shown to yield homogeneous silicate glass without quench textures when the rapid coolingassembly is used.

Recent advances of high-pressure generation in a multianvil apparatus using sintered diamond anvils

The tried and tested multianvil apparatus has been widely used for high-pressure and hightemperature experimental studies in Earth science. As a result, many important results have been obtained for a better understanding of the components, structure and evolution of the Earth. Due to the strength limi- tation of materials, the attainable multianvil pressure is generally limited to about 30 GPa （corresponding to about 900 km of the depth in the Earth） when tungsten carbide cubes are adopted as second-stage anvils. Compared with tungsten carbide, the sintered diamond is a much harder material. The sintered diamond cubes were introduced as second-stage anvils in a 6--8 type multianvil apparatus in the 1980s, which largely enhanced the capacity of pressure generation in a large volume press. With the development of material synthesis and processing techniques, a large sintered diamond cube （14 ram） is now available. Recently, maximum attainable pressures reaching higher than 90 GPa （corresponding to about 2700 km of the depth in the Earth） have been generated at room temperature by adopting 14-mm sintered diamond anvils. Using this technique, a few researches have been carried out by the quenched method or combined with synchrotron radiation in situ observation. In this paper we review the properties of sintered diamond and the evolu- tion of pressure generation using sintered diamond anvils. As-yet unsolved problems and perspectives for uses in Earth Science are also discussed.

Nano-scale Reinforcements and Properties of Al-Si-Cu Alloy Processed by High-Pressure Torsion

To improve the comprehensive mechanical properties of Al-Si-Cu alloy,it was treated by a high-pressure torsion process,and the effect of the deformation degree on the microstructure and properties of the Al-Si-Cu alloy was studied.The results show that the reinforcements(β-Si andθ-CuAl_(2)phases)of the Al-Si-Cu alloy are dispersed in theα-Al matrix phase with finer phase size after the treatment.The processed samples exhibit grain sizes in the submicron or even nanometer range,which effectively improves the mechanical properties of the material.The hardness and strength of the deformed alloy are both significantly raised to 268 HV and 390.04 MPa by 10 turns HPT process,and the fracture morphology shows that the material gradually transits from brittle to plastic before and after deformation.The elements interdiffusion at the interface between the phases has also been effectively enhanced.In addition,it is found that the severe plastic deformation at room temperature induces a ternary eutectic reaction,resulting in the formation of ternary Al+Si+CuAl_(2)eutectic.

Experimental and Finite Element Analysis of Corroded High-Pressure Pipeline Repaired by Laminated Composite

Repairs of corroded high-pressure pipelines are essential for fluids transportation under high pressure.One of the methods used in their repairs is the use of layered composites.The composite used must have the necessary strength.Therefore,the experiments and analytical solutions presented in this paper are performed according to the relevant standards and codes,including ASME PCC-2,ASME B31.8S,ASME B31.4,ISO 24817 and ASME B31.G.In addition,the experimental tests are replicated numerically using the finite element method.Setting the strain gauges at different distances from the defect location,can reduce the nonlinear effects,deformation,and fluctuations due to the high pressure.The direct relationship between the depth of an axial defect and the stress concentration is observed at the inner side edges of the defect.Composite reparation reduces the non-linearities related to the sharp variation of the geometry and a more reliable numerical simulation could be performed.

Cubic anvil cell apparatus for high-pressure and low-temperature physical property measurements

We will build a cubic anvil cell （CAC） apparatus for high-pressure and low-temperature physical property measurements in the synergic extreme condition user facility （SECUF）. In this article, we first introduce the operating principle, the development history, and the current status of the CAC apparatus, and subsequently describe the design plan and technical targets for the CAC in SECUF. We will demonstrate the unique advantages of CAC, i.e., excellent pressure homogeneity and large hydrostatic pressure capacity, by summarizing our recent research progresses using CAC. Finally, we conclude by providing some perspectives on the applications of CAC in the related research fields.

CO_(2)high-pressure miscible flooding and storage technology and its application in Shengli Oilfield,China

There are various issues for CO_(2)flooding and storage in Shengli Oilfield,which are characterized by low light hydrocarbon content of oil and high miscible pressure,strong reservoir heterogeneity and low sweep efficiency,gas channeling and difficult whole-process control.Through laboratory experiments,technical research and field practice,the theory and technology of CO_(2)high pressure miscible flooding and storage are established.By increasing the formation pressure to 1.2 times the minimum miscible pressure,the miscibility of the medium-heavy components can be improved,the production percentage of oil in small pores can be increased,the displacing front developed evenly,and the swept volume expanded.Rapid high-pressure miscibility is realized through advanced pressure flooding and energy replenishment,and technologies of cascade water-alternating-gas(WAG),injection and production coupling and multistage chemical plugging are used for dynamic control of flow resistance,so as to obtain the optimum of oil recovery and CO_(2)storage factor.The research results have been applied to the Gao89-Fan142 in carbon capture,utilization and storage(CCUS)demonstration site,where the daily oil production of the block has increased from 254.6 t to 358.2 t,and the recovery degree is expected to increase by 11.6 percentage points in 15 years,providing theoretical and technical support for the large-scale development of CCUS.

A novel optical high-pressure apparatus for studying the combustion of solid propellant under periodic strain

The combustion of solid propellants can provide tremendous thrust to drive solid rocket motors.Solid propellant grains are subjected to mechanical loads during practical combustion applications.The causes of mechanical loads include,but are not limited to,impulsive loads during ignition and periodic loads(>5 Hz)due to mechanical oscillation[1,2].

Effects of Instantaneous High-pressure on Denaturalization of β-Lactoglobulin

[ Objective] The study aimed to explore the denaturalization law of β-Iactoglobulin （β-LG） under instantaneous high-pressure（IHP） con- dition. [Methed] Using fresh milk as testing material, effects of pressure, feed temperature and treatment time on the denaturalization of β-LG were studied via SDS-PAGE electrophoresis and sulfhydryl content detection after IHP treatment. [ Result] IHP could induce the agglomeration and depo- lymerization Of β-LG. The agglomeration of the β-LG increased with the elevated pressure from 20 to 60 MPa, but 80 MPa pressure led to depolyme- rization. The effect of feed temperature （25 -45 ℃） was similar to that of the pressure, while the influence of treatment time （2 -8 min） was not obvious. [ Conclusion] The study provided a theoretical basis for the elimination of allergens in β-LG and the application of IHP technology in milk treatment.

Tectonic Evolution of an Early Precambrian High-Pressure Granulite Belt in the North China Craton

A large-scale high-pressure granulite belt (HPGB), more than 700 km long, is recognized within the metamorphic basement of the North China craton. In the regional tectonic framework, the Hengshan-Chengde HPGB is located in the central collision belt between the western block and eastern block, and represents the deep crustal structural level. The typical high-pressure granulite (HPG) outcrops are distributed in the Hengshan and Chengde areas. HPGs commonly occur as mafic xenoliths within ductile shear zones, and underwent multipile deformations. To the south, the Hengshan-Chengde HPGB is juxtaposed with the Wutai greenstone belt by several strike-slip shear zones. Preliminary isotopic age dating indicates that HPGs from North China were mainly generated at the end of the Neoarchaean, assocaited with tectonic assembly of the western and eastern blocks.

Effect of high-pressure homogenization on stability of emulsions containing zein and pectin

The aim of this study was to investigate the effect of high-pressure homogenization on the droplet size and physical stability of different formulations of pectin–zein stabilized rice bran oil emulsions. The obtained emulsions, both before and after passing through highpressure homogenizer, were subjected to stability test under environmental stress conditions,that is, temperature cycling at 4 °C/40 °C for 6 cycles and centrifugal test at 3000 rpm for 10 min. Applying high-pressure homogenization after mechanical homogenization caused only a small additional decrease in emulsion droplet size. The droplet size of emulsions was influenced by the type of pectin used;emulsions using high methoxy pectin(HMP) were smaller than that using low methoxy pectin(LMP). This is due to a greater emulsifying property of HMP than LMP. The emulsions stabilized by HMP–zein showed good physical stability with lower percent creaming index than those using LMP, both before and after passing through high-pressure homogenizer. The stability of emulsions after passing through high-pressure homogenizer was slightly higher when using higher zein concentration, resulting from stronger pectin–zein complexes that could rearrange and adsorb onto the emulsion droplets.

A study of hydrate plug formation in a subsea natural gas pipeline using a novel high-pressure flow loop

The natural gas pipeline from Platform QKI8-1 in the southwest of Bohai Bay to the onshore processing facility is a subsea wet gas pipeline exposed to high pressure and low temperature for a long distance. Blockages in the pipeline occur occasionally. To maintain the natural gas flow in the pipeline, we proposed a method for analyzing blockages and ascribed them to the hydrate formation and agglomeration. A new high-pressure flow loop was developed to investigate hydrate plug formation and hydrate particle size, using a mixture of diesel oil, water, and natural gas as experimental fluids. The influences of pressure and initial flow rate were also studied. Experimental results indicated that when the flow rate was below 850 kg/h, gas hydrates would form and then plug the pipeline, even at a low water content （10%） of a water/oil emulsion. Furthermore, some practical suggestions were made for daily management of the subsea pipeline.

Protolith ages and timing of peak and retrograde metamorphism of the high-pressure granulites in the Shandong Peninsula,eastern North China Craton

High-pressure （HP） granulites widely occur as enclaves within tonalite-trondhjemite- granodiorite （TTG） gneisses of the Early Precambrian metamorphic basement in the Shandong Peninsula, southeast part of the North China Craton （NCC）. Based on cathodoluminescence （CL）, laser Raman spec- troscopy and in-situ U-Pb dating, we characterize the zircons from the HP granulites and group them into three main types： inherited （magmatic） zircon, HP metamorphic zircon and retrograde zircon. The inher- ited zircons with clear or weakly defined magmatic zoning contain inclusions of apatites, and 207pb/206pb ages of 2915--2890 Ma and 2763--2510 Ma, correlating with two magmatic events in the Archaean base- ment. The homogeneous HP metamorphic zircons contain index minerals of high-pressure metamor- phism including garnet, clinopyroxene, plagioclase, quartz, rutile and apatite, and yield 207pb/2066pb ages between 1900 and 1850 Ma, marking the timing of peak HP granulite facies metamorphism. The retrograde zircons contain inclusions of orthopyroxene, plagioclase, quartz, apatite and amphibole, and yield the youngest 207pb/206pb ages of 1840-1820 Ma among the three groups, which we correlate to the medium to low-pressure granulite facies retrograde metamorphism. The data presented in this study suggest subduction of Meso- and Neoarchean magmatic protoliths to lower crust depths where they were subjected to HP granulite facies metamorphism during Palaeoproterozoic （1900-1850 Ma）. Subse- quently, the HP granulites were exhumated to upper crust levels, and were ovel-printed by medium to low-pressure granulite and amphibolite facies retrograde event at ca. 1840--820 Ma.

Gas Film Disturbance Characteristics Analysis of High-Speed and High-Pressure Dry Gas Seal

The dry gas seal（DGS） has been widely used in high parameters centrifugal compressor, but the intense vibrations of shafting, especially in high-speed condition, usually result in DGS＇s failure. So the DGS＇s ability of resisting outside interference has become a determining factor of the further development of centrifugal compressor. However, the systematic researches of which about gas film disturbance characteristics of high parameters DGS are very little. In order to study gas film disturbance characteristics of high-speed and high-pressure spiral groove dry gas seal（S-DGS） with a flexibly mounted stator, rotor axial runout and misalignment are taken into consideration, and the finite difference method and analytical method are used to analyze the influence of gas film thickness disturbance on sealing performance parameters, what＇s more, the effects of many key factors on gas film thickness disturbance are systematically investigated. The results show that, when sealed pressure is 10.1MPa and seal face average linear velocity is 107.3 m/s, gas film thickness disturbance has a significant effect on leakage rate, but has relatively litter effect on open force; Excessively large excitation amplitude or excessively high excitation frequency can lead to severe gas film thickness disturbance; And it is beneficial to assure a smaller gas film thickness disturbance when the stator material density is between 3.1 g/cm3 to 8.4 g/cm3; Ensuring sealing performance while minimizing support axial stiffness and support axial damping can help to improve dynamic tracking property of dry gas seal. The proposed research provides the instruction to optimize dynamic tracking property of the DGS.

Mechanisms and capacity of high-pressure soaking after hydraulic fracturing in tight/shale oil reservoirs

Huff-n-puff by water has been conducted to enhance oil recovery after hydraulic fracturing in tight/shale oil reservoirs.However,the mechanisms and capacity are still unclear,which significantly limits the application of this technique.In order to figure out the mechanisms,the whole process of pressurizing,high-pressure soaking,and depressurizing was firstly discussed,and a mechanistic model was established.Subsequently,the simulation model was verified and employed to investigate the significances of high-pressure soaking,the contributions of different mechanisms,and the sensitivity analysis in different scenarios.The results show that high-pressure soaking plays an essential role in oil production by both imbibition and elasticity after hydraulic fracturing.The contribution of imbibition increases as the increase in bottom hole pressure(BHP),interfacial tension,and specific surface area,but slightly decreases as the oil viscosity increases.In addition,it first decreases and then slightly increases with the increase in matrix permeability.The optimal soaking time is linear with the increases of both oil viscosity and BHP and logarithmically declines with the increase in matrix permeability and specific surface area.Moreover,it shows a rising tendency as the interficial tension(IFT)increases.Overall,a general model was achieved to calculate the optimal soaking time.

In situ experimental study on TBM excavation with high-pressure water-jet-assisted rock breaking

China’s first high-pressure hydraulically coupled rock-breaking tunnel boring machine(TBM) was designed to overcome the rock breaking problems of TBM in super-hard rock geology, where high-pressure water jet system is configured, including high-flow pump sets, high-pressure rotary joint and high-pressure water jet injection device. In order to investigate the rock breaking performance of high-pressure water-jet-assisted TBM, in situ excavation tests were carried out at the Wan’anxi Water Diversion Project in Longyan, Fujian Province, China, under different water jet pressure and rotational speed. The rock-breaking performance of TBM was analyzed including penetration, cutterhead load, advance rate and field penetration index. The test results show that the adoption of high-pressure water-jet-assisted rock breaking technology can improve the boreability of rock mass, where the TBM penetration increases by 64% under the water jet pressure of 270 MPa. In addition, with the increase of the water jet pressure, the TBM penetration increases and the field penetration index decreases. The auxiliary rock-breaking effect of high-pressure water jet decreases with the increase of cutterhead rotational speed. In the case of the in situ tunneling test parameters of this study, the advance rate is the maximum when the pressure of the high-pressure water jet is 270 MPa and the cutterhead rotational speed is 6 r/min. The technical superiority of high-pressure water-jet-assisted rock breaking technology is highlighted and it provides guidance for the excavation parameter selection of high-pressure hydraulically coupled rock-breaking TBM.

Application of high-pressure water jet technology and the theory of rock burst control in roadway

This paper puts forward using high-pressure water jet technology to control rock burst in roadway, and analyzes the theory of controlling rock burst in roadway by the weak structure zone model. The weak structure zone is formed by using high-pressure water jet to cut the coal wall in a continuous and rotational way. In order to study the influence law of weak structure zone in surrounding rock, this paper numerically analyzed the influence law of weak structure zone, and the disturbance law of coal wall and floor under dynamic and static combined load. The results show that when the distance between high-pressure water jet drillings is 3 m and the diameter of drilling is 300 mm, continuous stress superposition zone can be formed. The weak structure zone can transfer and reduce the concentrated static load in surrounding rock, and then form distressed zone. The longer the high-pressure water jet drilling is, the larger the distressed zone is. The stress change and displacement change of non-distressed zone in coal wall and floor are significantly greater than that of distressed zone under dynamic and static combined load. And it shows that the distressed zone can effectively control rock burst in roadway under dynamic and static combined load. High-pressure water jet technology was applied in the haulage gate of 250203 working face in Yanbei Coal Mine, and had gained good effect. The study conclusions provide theoretical foundation and a new guidance for controlling rock burst in roadway.

Effects of ultrasound on the desulfurization performance of hot coal gas over Zn-Mn-Cu supported on semi-coke sorbent prepared by high-pressure impregnation method

Zn-Mn-Cu/SC（U） sorbent was hydrothermally synthesized by ultrasound-assisted high-pressure impregnation method with semi-coke（SC）as support and the mixed solution of zinc nitrate,manganese nitrate and copper nitrate as active component precursors.The desulfurization performances of hot coal gas on the prepared sorbent at a mid-temperature of 500°C were tested in fixed-bed reactor.Morphology and pore structure of the prepared sorbent were also characterized by TEM,N2adsorption/desorption isotherms and XRD.For comparison,the sorbent of Zn-Mn-Cu/SC prepared by conventional high-pressure impregnation was also evaluated and characterized in order to study the effects of ultrasound treatment.Zn-Mn-Cu/SC（U） sorbent prepared by high-pressure impregnation under ultrasound-assisted condition showed a better desulfurization performance than Zn-Mn-Cu/SC.It could remove H2 S from 1000×10-6m3/m3 to 0.1×10-6m3/m3 at 500°C and maintained for 12.5 h with the sulfur capacity of 7.74%,in which both the breakthrough time and sulfur capacity were about 32% and 51% higher than those of Zn-Mn-Cu/SC sorbent.The introduction of ultrasound during high-pressure impregnation process greatly improved the morphology and pore structure of the sorbent.The ultrasonic treatment made particle size of active components smaller and made them more evenly disperse on semi-coke support,which provided more opportunities to contact with H2S in coal-based gases.However,there were no any difference in compositions and existing forms of active components on the Zn-Mn-Cu/SC and Zn-Mn-Cu/SC（U） sorbents.