High density methane inclusions in Puguang Gasfield: Discovery and a T-P genetic study

Based on measurement of homogenization temperature of inclusions and Raman spectral analysis, high density methane inclusions were discovered in the Triassic reservoirs of Puguang Gasfield. The methane inclusions show a homogenization temperature Th = -117.5― -118.1℃, a corresponding density of 0.3455―0.3477 g/cm3, and a Raman scatter peak v1 shift varying between 2911―2910 cm-1, which signifies a very high density of methane inclusions. The salt water inclusions paragenetic with methane inclusions show a homogenization temperature Th=170―180℃. Based on the composition of methane inclusions as determined by Raman spectra, PVTsim software was used to simulate the trapping pressure for high density methane inclusions in geologic history, and the trapping pressure was found to be as high as 153―160 MPa. Even though Puguang Gasfield is currently a gas pool of normal pressure, and the fluid pressure for the gas pool ranges between 56―65 MPa. However, data from this study indicates that remarkable overpressure may be generated at the stage of mass production of gas cracked from oils in Cretaceous, as high density methane inclusions constitute key evidence for overpressure in gas pool in geologic history. Meanwhile, discovery of small amounts of H2S, CO2 or heavy hydrocarbon in part of the high density methane inclusions indicates that the geochemical environment for trapping of inclusions may be related to formation of H2S. Therefore, the observation results can help to explore the thermochemical sulfate reduction （TSR） conditions for oil cracking and H2S formation.     

夹杂物对Ti;Zr微合金钢中针状铁素体形成的影响

采用实验室真空感应炉,炼制了3炉35 kg钢锭.利用MMS-300型热模拟机对实验钢进行线能量为100 kJ/cm,峰值温度为1 400℃的大热输入焊接模拟实验.借助金相显微镜(OM)、扫描电子显微镜(SEM)、能谱分析仪(EDS)和电子探针显微镜(EPMA)对粗晶热影响区(CGHAZ)组织进行观察;研究了热循环后夹杂物的数量、大小、分布和组成对焊接热影响区(HAZ)中针状铁素体形成的影响.结果表明:在粗晶热影响区中针状铁素体的数量随小尺寸氧化物夹杂的数量和面积分数的增加而增加;针状铁素体在Ti,Zr为主的复合夹杂物上形核,这些夹杂物多以Ti,Zr氧化物为核心,表面析出MnS,尺寸在0.5~3...     

Specific structural features of LnZrOx (Ln: La, Sm) mixed oxides prepared by different methods

LnZrOx(Ln: La, Sm) mixed oxides of Ln: Zr = 1 were prepared by different methods(complex polymerized method, sorption of cations on starch from aqueous salt solution and conventional co-precipitation with additional redispersion of precipitate by ultra sound) and calcined at 700–1300 °C. Their specific structural features and changes were studied and discussed. Various characterization methods were used such as X-ray diffraction,Electron microscopy, Fourier-transform infrared and Raman spectroscopy, UV–Vis spectroscopy, X-Ray absorption fine structure and X-ray photoelectron spectroscopy.The formation of pyrochlore structure occurred at 1100–1300 °C from fluorite-like pseudocubic phase ZrO_2 regardless the method of preparation. This phase had a block-like structure consisting of ZrO_2 nanocrystals stabilized by Ln cations and residual anions such as hydroxyls and carbonates. The desorption of such anions with heating already started at 900 °C and lead to local changes of Zr cations coordination to octahedral and to the formation of pyrochlore nanodomains inclusions within fluorite-like phase. The increased cation mobility and further elimination of anions caused by further heating was accompanied by the formation of bulk pyrochlore phase at 1100–1300 °C. Even after calcination at 1300 °C the local microheterogeneity as well as defects were identified at domains boundaries or sintered microstructure. These specific features of the formed pyrochlores depend on the method of preparation.     

Effect of annealing temperature on CrN microspheres synthesized by CAP technology

CrN microspheres were synthesized by using a cathodic arc plasma source system. The obtained samples were annealed in air at temperatures of 300-800 ℃ for 60 min. The influence of annealing temperature on the microstructure and surface morphology of the CrN microspheres was investigated. The CrN microspheres were characterized by means of scanning electron microscopy, transmission electron microscopy and X-ray diffraction analysis. The results show that the CrN nanoparticles arranged into leaf-like structures before annealing. With the rising of the annealing temperature, the size of CrN crystal nanoparticals became larger. When the annealing temperature exceeded the oxidation point(500 ℃), the CrN was oxidized and the leaf-like structure was broken. With further increase of the annealing temperature(700 ℃), the arrangement of CrN nanoparticles was changed from leaf-like structure to be discrete.     

Effects of carbon diffusing field in alloy solvent on the growth of tower-shape diamond single crystal

High-quality type-Ib tower-shape diamond single crystals were synthesized in cubic anvil high pressure apparatus (SPD-6×1200) at 5.4 GPa and 1250-1450°C. The (100) face of seed crystal was used as the growth face, and FeNiMnCo alloy was used as the solvent/catalyst. Two kinds of carbon diffusing fields (type-B and type-G) were simulated by finite element method (FEM). Using the two kinds of carbon diffusing fields, many diamond single crystals were synthesized. The effects of carbon diffusing fields on the ...     

Mg-Zr处理对FH40级船板钢铸态夹杂物特征的影响

采用定量金相及SEM-EDS手段对Mg,Zr及Mg-Zr处理FH40级船板铸钢中夹杂物粒径分布、平均粒径、总数量、总面积及成分、形貌等特征进行系统研究.结果表明,Mg,Zr及Mg-Zr处理后铸锭夹杂物平均粒径下降,夹杂物总数量增加.Mg的质量分数为0024%时,夹杂物中MgO平均质量分数为1257%,变质不充分;Mg的质量分数增加至0072%后,夹杂物中MgO平均质量分数为3558%,实现了氧化铝向MgO·Al2O3的充分变质,且夹杂物粒径明显减小.003%Zr处理后,铸锭夹杂物以Al2O3+MnS,Al-Zr-O+MnS为主;低Mg+高Zr,高Mg+低Zr,高Mg+高Zr处理炉次试验钢铸锭中均发现了含Zr夹杂物,其中高Mg+高Zr炉次形成了ZrO2夹杂,该类夹杂物被MgO·Al2O3包裹,团聚现象明显.     

Precipitation behavior of BN type inclusions in 42CrMo steel

Automobile crankshaft steel 42CrMo, which requires excellent machinability and mechanical properties, cannot be manufactured by traditional methods. To achieve these qualities, the formation behavior of boron nitride (BN) inclusions in 42CrMo steel was studied in this article. First, the precipitation temperature and the amount of BN type inclusions with different contents of boron and nitrogen in molten steel were calculated thermodynamically by FactSage software. Then the morphology and the size of BN type inclusions as well as the influence of cooling methods on them were investigated by scanning electron microscopy. Furthermore, the effects of cooling rate and the contents of B and N in molten steel on the morphology, size, and distribution of BN type inclusions were studied quantitatively and detailedly by directional solidification experiments. It is found that different BN inclusions in molten steel can form by controlling the cooling rate and the contents of B and N, which is important for obtaining the excellent machinability of 42CrMo steel.     

72A钢非金属夹杂物行为

采用多种方法对酒钢72A钢中非金属夹杂物进行了调查，对夹杂物的类型，来源，数量及尺寸进行了讨论，实验证明，铸坯中夹杂物有60%外来杂夹物，40%为脱氧产物，引起线材拔脆断的主要原因是外来大颗粒脆性夹杂，而控制好脱氧产物和外来杂夹物的组成，形貌，大小及分布，是解决线材拉拔脆断的关键。     

Sintering behaviour of feldspar and influence of electric charge effects

The characterization of feldspar for electric porcelain and the behaviour of these materials after heating at 1230℃ were studied. X-ray diffraction (XRD) and scanning electronic microscopy (SEM) were used to identify the present phases and the densification level. Feldspar sand was treated by flotation. The floated feldspar is constituted by microcline, quartz, and minor amounts of albite. The microstructure of sintered feldspar at 1230℃ is essentially vitreous with open microporosities. The dielectrical properties of composites were characterized by using the induced courant method (ICM), which indicates that the charge trapping capacity depends on the mineralogical and chemical composition of feldspar.     

High-temperature mechanical properties of near-eutectoid steel

The high-temperature mechanical properties of near-eutectoid steel were studied with a Gleeble-1500 simulation machine. Zero strength temperature (ZST), zero ductility temperature (ZDT), hot ductility curves, and strength curves were measured. Two brittle zones and one plastic zone were found in the temperature range from the melting point to 600℃. Embrittlement in zone I is caused by the existence of liquid film along dendritic interfaces. Ductility loss in zone III mainly results from precipitates and inclusions as well as S segregation along grain boundaries. Pearlite transformation also accounts for ductility deterioration in the temperature range of 700–600℃. Moreover, the straightening temperature of the test steel should be higher than 925℃ for avoiding the initiation and propagation of surface cracks in billets.     

电渣重熔过程冷却强度对含镁H13钢中碳化物的影响

研究电渣重熔过程冷却强度对含镁H13钢凝固组织和碳化物偏析的影响.采用光学显微镜、扫描电镜、透射电镜、X射线衍射仪等分析凝固组织及碳化物的特征.研究发现,钢锭的凝固组织均为马氏体组织、残余奥氏体及一次碳化物.H13钢电渣锭中主要析出的一次碳化物为V8C7、MC、M23 C6及M6C.随着冷却强度增加,电渣锭边部碳化物的尺寸减小且分布更加均匀,但是碳化物的类型不发生变化.电渣重熔过程中冷却强度增加促进钢中镁对夹杂物的变性能力,经过镁变性后生成的MgO· Al2O3为TiN的析出提供形核质点,MgO· Al2 O3和TiN的复合夹杂物能够促进一次碳化物异质形核,从而细化一次碳化物.     

稀土处理钢中夹杂物对晶内针状铁素体形成的影响

分析了稀土处理钢中夹杂物的特征（夹杂物种类、尺寸分布和体积分数）对微观组织中针状铁素体形成的影响.结果表明,钢中夹杂物种类和体积分数对针状铁素体组织的形成非常重要.稀土氧化物（包含稀土氧硫化物）与铁素体具有低至1.9%的错配度降低针状铁素体在夹杂物表面的形核能垒,从而促使它在稀土氧化物上形核.反之,稀土硫化物与铁素体具有高达42.5%的错配度不能诱导生成针状铁素体组织.此外,微观组织中针状铁素体的体积分数随着夹杂物体积分数的增加而增大,当钢中夹杂物体积分数是9.5×10-4时其体积分数达到53%.     

Preparation of high-strength Al-Mg-Si-Cu-Fe alloy via heat treatment and rolling

An Al-Mg-Si-Cu-Fe alloy was solid-solution treated at 560°C for 3 h and then cooled by water quenching or furnace cooling. The alloy samples which underwent cooling by these two methods were rolled at different temperatures. The microstructure and mechanical properties of the rolled alloys were investigated by optical microscopy, scanning electron microscopy, transmission electron microscopy, X-ray diffraction analysis, and tensile testing. For the water-quenched alloys, the peak tensile strength and elongation occurred at a rolling temperature of 180°C. For the furnace-cooled alloys, the tensile strength decreased initially, until the rolling temperature of 420°C, and then increased; the elongation increased consistently with increasing rolling temperature. The effects of grain boundary hardening and dislocation hardening on the mechanical properties of these rolled alloys decreased with increases in rolling temperature. The mechanical properties of the 180°C rolling water-quenched alloy were also improved by the presence of β″ phase. Above 420°C, the effect of solid-solution hardening on the mechanical properties of the rolled alloys increased with increases in rolling temperature.     

Structural refinement of 00Cr13Ni5Mo2 supermartensitic stainless steel during single-stage intercritical tempering

The 00Cr13Ni5Mo2 supermartensitic stainless steel was first tempered at 570–730℃ for 2 h to observe the microstructure and hardness changes. The tempering temperature was set to 600, 650, and 700℃, which is below, equal to, and above the austenite transformation start temperature, respectively, for each holding period to investigate the effects of tempering time on the structure and properties of the steel. The microstructure of the specimens was examined by optical microscopy and transmission electronic microscopy, and the phase composition was detected by X-ray diffraction. As expected, lath refinement was observed in the steel tempered at 700℃, and the refinement degree significantly depended on the tempering time. Contrary to normal steel softening by tempering, the hardness performance of the steel was significantly enhanced primarily because of the refinement of martensite laths after single-stage intercritical tempering. It is believed that the reverse transformation of martensite (α′) to austenite (γ) is responsible for the refinement.     

大功率风电机组用轴承钢中非金属夹杂物特征及来源分析

采用非水溶液电解法萃取大功率风电机组用轴承钢轧材中的非金属夹杂物,结合SEM和EDS分析,对夹杂物的形貌、尺寸、成分及类型进行表征,并分析其可能来源。结果表明,该风电轴承钢轧材中非金属夹杂物主要包括Al-Ca-Si-Mg系氧化物和Al-Ca-Si-Mg系硫化物两大类;在钢中T[O]含量仅为0.0007%时,仍存在以SiO2为主的Al-Ca-Si-Mg系大型夹杂物。     

Mechanisms of two-stage martensitic transformation in Ti-Ni-Hf alloy powder

The Ti-Ni-Hf shape memory alloy powders were prepared by plasma rotating electrode process. And the powders were featured with the perfect sphericity and smooth surface. Moreover, the grain size was refined in the Ti-Ni-Hf alloy powders due to the rapid cooling rate during plasma rotating electrode process. It was found that the Ti-Ni-Hf alloy powders had the typical self-accommodation configuration including spear-like, mosaic-like and lath-like martensite. Various twins, such as (001) compound twin, (011) type I twin as well as {111} type I twin, were observed in Ti-Ni-Hf alloy powders. Differing from the bulk Ti-Ni-Hf alloy, two-stage transformation corresponding to B2⇌B19’ martensitic transformation was detected in the as-received Ti-Ni-Hf alloy powders. In addition, the martensitic transformation behaviors were closely related to the annealing temperatures. The Ti-Ni-Hf alloy powders with low annealing temperature of 500 ​°C still exhibited two-stage martensitic transformation, while two-stage martensitic transformation changed into single martensitic transformation in the Ti-Ni-Hf alloy powders with the higher annealing temperature of 900 ​°C. And finally the possible mechanisms for the evolution of martensitic transformation behaviors were discussed.     

Nano to micro size transition of hydroxyapatite in porcine bone during heat treatment with low heating rates

This work focuses on the changes of raw hydroxyapatite obtained from porcine bones during heat treatment with heating rates of 2.5 and 5.0 °C/min between 600 °C and 1100 °C. High-Resolution transmission electron microscopy (HR-TEM) images showed that raw hydroxyapatite was formed by high-ordered nanometric platelet crystals with a length of around 18 nm and width around 7 nm. High-Resolution scanning electron microscopy (HR-SEM) images evidenced the coalescence phenomena during heating giving. It was found that the growth of the crystals and the transition from nano to a micro-size occurred at around 700 °C. And the changes in the full width at half maximum (FWHM) for the characteristic (002) plane of the X-ray diffraction patterns and the FWHM of the characteristic Raman band at 960 cm-1 for ν1 PO43- exhibited the transition from nano to a micro size, that was confirmed by HR-SEM images and the thermogravimetric (TG) analysis. The porosity of the BIO-HAp changes from intra nanometric to intercrystalline.     

Pure CO2 fluids in the Sarekoubu gold deposit at southern margin of Altai Mountains in Xinjiang, West China

Sarekoubu gold deposit occurs in metamorphosed acid volcanic rocks and volcaniclastic rocks of Devonian Kangbutiebao Formation along the southern margin of Altai Mountains in Xinjiang, West China. Pyritization, silicification and carbonatization are developed in wallrocks, and main gold mineralization stages are pyrite-quartz stage (Ⅱ)and polymetallic sulfide stage (Ⅲ). Primary fluid inclusions are often seen in main gold mineralization stages, which are almost pure CO2 liquid inclusions (Lco2) under room temperature with high densities of 0.85--1.07 g/cm^3. CO2-rich inclusions (Lco2-LH2O) and H2O-rich inclusions (LH2O-LCo2)are subordinate. Fluid inclusions in stage Ⅰ (polymetallic sulfide stage) are more complex than in stage Ⅱ, containing CO2-CH4 system with -78.1-61.9℃ of solid CO2 melting temperatures and -33.7-17.7℃ of partial homogenization temperatures. The trapping pressures of high densities are estimated to be 150-350 MPa. Laser Raman microprobe was used to confirm the composition of pure CO2 liquid inclusions. δ^13C values of CO2 inclusions range from -10.73‰ to -21.15‰, which are similar to some of fluids in the mantle-derived minerals that contain surface organic carbon by subduction recycling. These characteristics differ from many hydrothermal gold deposits. CO2 fluids have a regional source related to post-collisional orogeny.     

升温速率对砂浆渗透性及微观结构的影响

为了研究升温速率对砂浆渗透性以及微观结构的影响,现以3种升温速率（5℃/min、10℃/min、15℃/min）加热砂浆至500℃。通过新的实验技术允许在围压下用气体同时测量砂浆的渗透率和孔隙率,并采用核磁共振（NMR）和扫描电镜（SEM）技术,观察损伤后试样的T2谱图分布、孔径分布和裂缝演变情况。结果表明：在500℃下,随着升温速率的增大,砂浆气体渗透率与孔隙率逐渐增大。在加卸载围压的过程中,与孔隙率相比砂浆的气体渗透率对围压更敏感。不同升温速率作用后的砂浆T2谱图均出现2个波峰,主波峰的分布占据了3个数量级。随着升温速率增大,砂浆的孔径分布向右移动,孔径增大。高温作用后,砂浆致密结构变得多孔疏松,升温速率越快,其内部裂缝宽度越大。     

Effects of CeO2 on the XPS valence band spectra of coal under the combustion initialization stage at 400°C

In order to get the catalytic mechanism of CeO₂ on graphite and coal at 400°C, the morphologies of coal, graphite, and CeO₂ before and after combustion were analyzed through X-ray photoelectron spectroscopy (XPS). It is found that the particle size of coal is mostly between 11.727 and 64.79 μm, while the particle size of CeO₂ is between 1.937 and 11.79 μm. The agglomeration of coal and CeO₂ can be seen by scanning electron microscopy (SEM) after reaction. XPS results show that with the addition of CeO₂, the intensity of binding energy gets stronger, but there is no energy peak transition. Comparing the character of coal with and without the addition of CeO₂, it can be seen that the C-C bond fractures first at 400°C, while the C-H energy-band takes electrons at the same time to be far away from the Fermi level, and the O 2s, O 2p, and C sp hybrid orbitals are all excited. Adding CeO₂ can enhance the activity of the whole coal. In addition, through XPS analysis, combined with the oxygen transfer theory and the electron transfer theory, the catalytic mechanism of CeO₂ for pulverized coal combustion could be obtained.