油气田含油废物热相处理技术研究

本文针对油气田含油废物热相处理时易结焦的问题,综合分析了含油废物、结焦物的主要成分,对结焦原因进行了分析,通过研究化学配方,优选了得到2wt%~3wt%膨松剂+1wt%~2wt%分散剂溶液,对含油废物进行改性处理,在热相处理后,可有效减缓结焦现象,确保热相处理装置长周期运行。

Microstructural evolution of AZ91 magnesium alloy during extrusion and heat treatment

Microstructural evolution of AZ91 magnesium alloy was investigated during homogenizing annealing treatment, hot extrusion and ageing treatment, respectively. The results exhibited that both the divorced eutectic β-Mg17Al12 and the precipitated β-Mg17Al12 phases appeared in the as-cast alloy. The β-Mg17Al12 phase dissolved into α-Mg matrix mostly and the structure kept fine after the optimized homogenization treatment at 380 °C for 15 h. Dynamic recrystallization and consequent grain refinement occurred during extrusion. The banded β-Mg17Al12 precipitates paralleled to the extrusion direction were observed after ageing treatment. The banded precipitation should be attributed to the solidification segregation which was elongated during the subsequent extrusion. Furthermore, the effects of temperature, holding time of homogenization and ageing treatment, and extrusion processing parameters on the microstructural evolution of AZ91 alloy were also discussed in details according to the experimental results.

Microstructure of cast γ-TiAl based alloy solidified from β phase region

The microstructures and phase transformation of Ti-43Al-4Nb alloy in as-cast and heat-treated states were investigated by using optical microscopy, scanning and transmission electron microscopy as well as differential scanning calorimetry. The results show that a fine microstructure of the as-cast alloy can be obtained by solidifying through the β phase. γ grains can nucleate directly from the β phase. The coexistence of β phase and γ phase along primary α grain boundaries contributes to the decrease in the grain size of the as-cast alloy. The phase transformation sequence during solidification of the Ti-43Al-4Nb alloy is suggested as L→L＋β→β→α＋β→α＋βr→α＋γ＋βr→lamellae（α2＋γ）＋γ＋βr. The microstructure of the alloy after heat treatment at 1 250 ℃ for 16 h exhibits a certain coarsening compared with that of the as-cast state. The remnant β phase can be removed by the heat treatment process due to the diffusion of Nb and the non-equilibrium state of β phase.

Influence of Ni_4Ti_3 precipitates on phase transformation of NiTi shape memory alloy

Ni Ti shape memory alloy samples were aged for 2 h at 573, 723 and 873 K, respectively. Two R-phase variants are observed in the Ni Ti samples aged at 573 and 723 K, where the orientation relationship between the two R-phase variants and the B2 matrix is determined. In the Ni Ti samples aged at 573 and 723 K, fine and homogeneous Ni4Ti3 precipitates are coherent with the B2 austenite matrix. The Ni4Ti3 particles precipitate in the grain interior and at the grain boundaries, where the heterogeneous Ni4Ti3 precipitates are coherent, semi-coherent and incoherent with the B2 matrix in the Ni Ti sample aged at 873 K. As for the Ni Ti sample aged at 873 K, one-stage phase transformation from B19＇ martensite to B2 austenite occurs on heating, but two-stage phase transformation of B2-R-B19＇ arises on cooling. The Ni Ti sample aged at 723 K shows two-stage phase transformation of B2-R-B19＇ on cooling as well, but exhibits two-stage phase transformation of B19＇-R-B2 on heating. The Ni Ti sample aged at 573 K exhibits three-stage transformation on cooling due to local stress inhomogeneity and local composition inhomogeneity around the Ni4Ti3 precipitates.

Effect of Ce,Co,B on formation of LaCo_(13)-structure phase in La(Fe,Si)_(13) alloys

The effect of Ce, Co, and B on the formation of 1：13 phase in La（Fe, Si）13 alloys was investigated by XRD, SEM and EDS. The results show that Co can improve the formation of 1：13 phase in as-cast LaFe11.6-xCoxSi1.4 alloys, but in as-cast and annealed LaFe11.6Si1.4-xCox alloys, it will hamper the formation of 1：13 phase and help the formation of a-Fe（Co, Si） solid solution. Ce2Fel7 phases will form when x reaches a certain value in as-cast and annealed La1-xCexFe11.5Si1.5 alloys. B can improve the formation of 1：13 phase accompanied with Fe2B phase in as-cast LaFe11.6-xBxSi1.4 alloys. B improves the formation of a-Fe solid solution in LaFe11.6Si1.4-xBx alloys, and there is almost only a-Fe in as-cast and annealed LaFe11.6Si0.9B0.5 alloy. In all, the introduction of Co, B, and Ce cannot eliminate the a-Fe phases in corresponding alloys prepared by the high-temperature and short-time annealing process.

Effects of isothermal process parameters on semisolid microstructure of Mg-8%Al-1%Si alloy

A Mg-8%Al-1%Si alloy with semisolid microstructure was fabricated by isothermal heat treatment process. The effects of isothermal process parameters such as holding temperature and holding time on the microstructure of Mg-8%Al-1%Si alloy were investigated. The results show that a non-dendritic microstructure could be obtained by isothermal heat treatment. With increasing holding temperature from 560 to 575 °C or holding time from 5 to 30 min, the liquid volume fraction increases, the average size of α-Mg grains grows larger and globular tendency becomes more obvious. In addition, the Mg2Si phase transforms from Chinese script shape to granule shape. The morphology modification mechanisium of Mg2Si phase in Mg-8%Al-1%Si alloy during the semisolid isothermal heat treatment was also studied.

Intermetallic phase evolution of 5059 aluminum alloy during homogenization

Intermetallic phase evolution of 5059 aluminum alloy during homogenization was investigated by means of optical microscopy （OM）, scanning electron microscopy （SEM）, transmission electron microscopy （TEM）, energy dispersive spectrometry （EDS）, differential scanning calorimetry （DSC） and X-ray diffraction analysis （XRD）. The results show that severe dendritic segregation exists in as-cast alloy. The dissolvable intermetallic phases in as-cast alloy consist of Zn-and Cu-rich non-equilibriumβ（Al3Mg2） phase, Fe-rich eutectic Al6Mn phase and equilibrium Mg2Si phase. During the homogenization, Zn- and Cu-rich non-equilibrium β （Al3Mg2） phase, Fe-rich eutectic Al6Mn phase and equilibrium Mg2Si gradually dissolve into matrix. Fine dispersed β（Al3Mg2） particles and rod-shaped Al6Mn particles form in the Al matrix after homogenization. The proper homogenization processing is at 450 °C for 24 h, which is consistent with the results of homogenizing kinetic analysis.

Study of NiSi/Si Interface by Cross-Section Transmission Electron Microscopy

Different silicidation processes are employed to form NiSi,and the NiSi/Si interface corresponding to each process is studied by cross-section transmission electron microscopy （XTEM）. With the sputter deposition of a nickel thin film,nickel silicidation is realized on undoped and doped （As and B） Si（001） substrates by rapid ther mal processing （RTP）. The formation of NiSi is demonstrated by X-ray diffraction and Raman scattering spectros- copy. The influence of the substrate doping and annealing process （one-step RTP and two-step RTP） on the NiSi! Si interface is investigated. The results show that for one-step RTP the silicidation on As-doped and undoped Si substrates causes a rougher NiSi/Si interface,while the two-step RTP results in a much smoother NiSi/Si interface. High resolution XTEM study shows that axiotaxy along the Si（111） direction forms in all samples, in which specific NiSi planes align with Si（111） planes in the substrate. Axiotaxy with spacing mismatch is also discussed.

Microstructure characterization on Mg-2Nd-4Zn-1Zr alloy duringheat treatment

The microstructures of Mg-2Nd-4Zn-1Zr alloy in the as-cast state and after heat treatment were investigated. Several kinds of secondary phases were found and characterized by transmission electron microscopy （TEM）, scanning electron microscopy （SEM） and X-ray diffraction （XRD）. In the as-cast alloy, the existing eutectic compounds are Mg-Nd-Zn ternary phases： T phases and W phases. After the heat treatment, with increasing the temperature or time, it was found that T phase almost dissolved into the α-Mg matrix, while a large amount of W phase remained in the matrix. On the other hand, with prolonging the time, the morphology of the phase changed from continuous network to the spherical shape along the grain boundary. The density of the W phase gradually decreased and finally it was coarsened and stabilized in the treatment process.

Structure and properties of FeCoNiCrCu_(0.5)Al_x high-entropy alloy

Effects of Al content and heat treatment on the structure,hardness and electrochemical properties of FeCoNiCrCu0.5Alx high-entropy alloys were investigated.The phase structure of as-cast alloys evolves from FCC phase to BCC phase with the increase of Al content.The stable phase of FeCoNiCrCu0.5Alx high-entropy alloys will transform from FCC phase to FCC＋BCC duplex phases when x value increases from 0.5 to 1.5.The hardness of BCC phase is higher than that of FCC phase,and the corrosion resistance of BCC phase is better than FCC phase in chlorine ion and acid medium.High hardness and good corrosion resistance can be obtained in as-cast FeCoNiCrCu0.5Al1.0 alloy.

Coupled models of heat transfer and phase transformation for the run-out table in hot rolling

Mathematical models are been proposed to simulate the thermal and metallurgical behaviors of the strip occtLrring on the run-out table （ROT） in a hot strip mill. A variational method is utilized for the discretization of the governing transient conduction-convection equation, with heat transfer coefficients adaptively determined by the actual mill data. To consider the thermal effect of phase transformation during cooling, a constitutive equation for describing austenite decomposition kinetics of steel in air and water cooling zones is coupled with the heat transfer model. As the basic required inputs in the numerical simulations, thermal material properties are experimentally measured for three carbon steels and the least squares method is used to statistically derive regression models for the properties, including specific heat and thermal conductivity. The numerical simulation and experimental results show that the setup accuracy of the temperature prediction system of ROT is effectively improved.

Microstructure and mechanical properties of strontium-modified ADC12 alloy processed by heat treatment

The effects of heat treatment and strontium （SO addition on the microstructure and mechanical properties of ADC12 alloys were investigated, and two-stage solution treatment was introduced. The results indicated that the addition of Sr obviously refined the microstructure of ADC12 alloys. When 0.05 wt% Sr was added into the alloy, the eutectic Si phase was fully modified into fine fibrous structure; a-A1 and fl-A15FeSi phases were best refined; and the eutectic AlzCu phase was modified into block-like AlzCu phase that continuously distributed at the grain boundary. The ultimate tensile strength （UTS） （270.63 MPa） and elongation （3.19%） were increased by 51.2% and 73.4% respectively compared with unmodified alloys. After the two-stage solution treatment （500 ~C, 6 h＋520 ~C, 4 h）, for 0.05 wt% Sr modified ADC12 alloys, the Si phases transformed into fine particle structure and AlzCu phases were fully dissolved. The peak hardness value of the alloys processed by the two-stage solution treatment was increased by 8.3% and 6.8% respectively compared to solution treatment at 500 ~C and 520 ~C. After the aging treatment （175 ~C, 7 h）, the hardness and UTS were increased by 38.73% and 13.96% respectively when compared with the unmodified alloy.

Effects of heat treatment conditions and Y-doping on structure and phase transition temperature of VO2 powders

The VO2 powders were prepared by hydrothermal synthesis.The effects of heat treatment conditions and Y-doping on the structure and phase transition temperature of VO2 were studied.The XRD,SEM and TEM results show that the heat treatment temperature has a significant effect on the crystal transformation of VO2 precursor.Increasing temperature is conducive to the transformation of precursor VO2(B)to ultrafine VO2(M).The Y-doping affects the structure of VO2.Y^3+can occupy the lattice position of V4+to form YVO4 solid solution,which can increase the cell parameters of VO2.Due to the lattice deformation caused by Y-doping,the aggregation of particles is prevented,and the grain is refined obviously.DSC curves show that Y-doping can reduce the phase transition temperature of VO2(M).After adding 9 at.%Y,the phase transition temperature can be reduced from 68.3 to 61.3℃.

Mechanical alloying and subsequent heat treatment of Ag-Zn powders

Microstructural evolution during mechanical alloying of Ag and Zn, and subsequent heat treatments were investigated. The mechanical alloying was carried out in a SPEX 8000D miller. The microstructural characterization was obtained by X-ray diffraction （XRD）, transmission electron microscopy （TEM） and scanning electron microscopy （SEM）. The thermal behavior was studied using differential scanning calorimetry （DSC）. Based on the results obtained, it can be concluded that at the early stages of milling was possible to detect the ε, β, β′, α solid solutions and remaining Zn. Later, the ε, β, β′ and Zn phases disappeared while the Zn concentration of the α solid solution was strongly increased. After 7.2 ks of milling, the mechanical alloying process reached a steady state. During this period, both the composition and crystallite size of the α solid solution remained practically unchanged. On the other hand, subsequent heat treatments of milled powders showed that the α solid solution could also be obtained by the combination of mechanical alloying and heat treatment. Finally, the evolution of the microstructure during milling and annealing was combined to propose an optimal processing route in order to obtain a α solid solution.

Study on Grain Refining and Metamorphism of ZL111 Aluminium Alloys

Vacuum sintering and ball milling methods were employed in the preparation process of Ti-C grain refine- ment and the ability of refiners with varying ratios of Ti and C to refine ZL111 crystal grains was tested. The refinement effect of the Ti-C ratios on tensile strength, elongation percentage, Brinell hardness, pro-eutectoid αAl and the size of the Si phase of ZL111, after modification by rare-earth and strontium nitrate, were studied by means of metallographic examination, SEM and mechanical property tests. The results show that there is an obvious increase in the tensile strength and elongation percentage of refined ZL111 with these new Ti and C refiner compounding powders, while Brinell hardness remained more or less constant. The pro-eutectoid αAl is considerably reduced in size and the Si phase shows a finer and rounder structure. The refiner exhibits a good grain refining performance when the Ti-C ratio is 25:1, for Al crystals can favorably easily form nuclei and grow up along the TiC surface thanks to the TiAl3 generated by sur- plus Ti and Al. The mechanical properties have clearly been improved by the addition of strontium nitrate to ZL111. The effective factors in the modification of mechanical properties of ZL111 are in order of importance: strontium nitrate, Ti-C ratio and rare earth.

Changes in organic structure and mineral phases transformation of coal during heat treatment on laboratory scale

Structural changes due to coalification and oxidation influence the coal quality, geochemically and petrologically. Understanding of the coal structures helps to predict the behaviour of coal at various processes. The objective of this paper is to study the changes in organic structure and mineral phase transformation during combustion. Different density fractions were generated and then heated at different temperatures from 200 to 1000 ℃. Petrography, Fourier transform infrared spectroscopy （FTIR） and X-ray diffraction （XRD） were carried out on all the density fractions aimed to accomplish this objective. Here, through petrography, it was observed that the vitrinite and liptinite macerals disappear at higher temperature while porous inertinite is seen. The inertinite structure is exposed which is assumed by the presence of -OH and C-O-C stretches with the aromatic nucleus （CH） and three to four adjacent H from FTIR spectra. Moreover, it can be concluded that aliphatic groups get collapsed at high temperature. In case of inorganic matter, through XRD and FTIR, it is also revealed that with increasing temperature, clay minerals converted into elemental oxides. Hence, this study is suggesting that the structures of coal are altered by the degree of contact metamorphism.

Phase change materials as quenching media for heat treatment of 42CrMo4 steels

In the present work,paraffin phase change material is used as quenchant for the heat treatment of 42CrMo4 alloy and compared with water,air,and CuO doped paraffin.The samples were prepared based on ASTM E 8M-98 standard for tensile test and then heated up to 830°C,kept for 4 h in an electric resistance furnace and then quenched in the mentioned media.Elastic modulus,yield strength,ultimate tensile strength,elongation,and modulus of toughness were determined according to the obtained stress?strain curves.Moreover,the hardness and microstructural evolution were investigated after the heat treatment at different media.The samples quenched in paraffin and CuO-doped paraffin are higher in ultimate tensile strength(1439 and 1306 MPa,respectively)than those quenched in water(1190 MPa)and air(1010 MPa).The highest hardness,with a value of HV 552,belonged to the sample quenched in CuO-doped paraffin.The microstructural studies revealed that the non-tempered steel had a ferrite/pearlite microstructure,while by quenching in water,paraffin and CuO-doped paraffin,ferrite/martensite microstructures were achieved.It is also observed that using the air as quenchant resulted in a three-phase bainite/martensite/ferrite microstructure.

Effect of heat treatments on microstructure and mechanical properties of sand cast Al−2Li−2Cu−0.5Mg−0.2Sc−0.2Zr alloy

This study focused on modifying heat treatment schemes to enhance the mechanical properties of sand cast Al−2Li−2Cu−0.5Mg−0.2Sc−0.2Zr alloy.Different three-stage solution treatment schemes((460℃,32 h)+(520℃,24 h)+(530/540/550℃,4/12/24/32 h))and aging temperatures(125,175,225℃)were designed for comparison.The microstructure evolutions were analyzed by optical microscopy(OM),scanning electron microscopy(SEM)and transmission electron microscopy(TEM).The results showed that the three-stage solution treatment of(460℃,32 h)+(520℃,24 h)+(530℃,12 h)could dissolve most of the secondary phases.The TEM results illustrated that fineδ'(Al_(3)Li)particles were homogeneously distributed in the matrix after aging at 175℃for 8 h,accompanied by a small amount of lath-shaped S′(Al_(2)CuMg)and plate-like T_(1)(Al_(2)CuLi)phases.The best comprehensive properties of yield strength of 376 MPa,ultimate tensile strength of 458 MPa and elongation of 4.1%were obtained by the optimal heat treatment scheme((460℃,32 h)+(520℃,24 h)+(530℃,12 h)+(175℃,8 h)).

Evolution in microstructure and mechanical properties during back-annealing of AlMnFeSi alloy

An Al-Mn-Fe-Si model alloy was subjected to two homogenization treatments, to achieve materials with different levels of Mn in solid solution and dispersoid densities, followed by cold rolling and back-annealing. Characterization of homogenization and deformation structures with respect to the effect of different microchemistries and strains on the structures was performed. Time-temperature-transformation （TTT） diagram with respect to precipitation and recrystallisation as a basis for analysis of the degree of concurrent precipitation was established. The TTT-diagram shows a strong effect of Mn concentration in solid solution and dispersoid density on the softening behavior. Recrystallization which finishes without the effect of concurrent precipitation results in an even, fine and equiaxed grain structure. Precipitation prior to or during recrystallization （concurrent） does retard the softening kinetics and leads to a coarse grain structure. However, the effect also depends on the duration of recrystallization and amount of precipitation. Recrystallization proceeding over a long time combined with a large amount of concurrent precipitation has a strong effect, otherwise the effect will be limited. Pre-existing fine and dense dispersoids （mean size 0.1 μm） before back-annealing do also lead to a coarse grain structure after recrystallization no matter whether additional concurrent precipitation occurs.

Effects of annealing at 800 and 1000℃ on phase precipitates and hardness of Al_(7)Cr_(20)Fe_(x)Ni_(73)−x alloys

The effects of Fe content on the microstructure,phase constituents and microhardness of the as-cast,800℃or 1000℃-annealed Al_(7)Cr_(20)Fe_(x)Ni_(73)−x(x=13−66)alloys were investigated.Not all these alloys are composed of the single FCC phase.The BCC and B2 phases are found.It is confirmed that the BCC phase in the Al7Cr20Fe66Ni7 alloy is transformed from the FCC phase at about 900℃ during cooling.While in the 800℃-annealed Al7Cr20Fe60Ni13 alloy,the FCC phase is stable and the hardness decreases.After annealing at 1000℃,for the precipitation of the B2 particles,the Al content in the FCC phase decreases,which results in decreasing of the alloy hardness.Moreover,after annealing at 800℃,a small amount of Al-rich B2 particles precipitate at the phase boundary and some nanocrystal BCC phase precipitates in the FCC matrix,which increases the hardness of the Al_(7)Cr_(20)Fe_(x)Ni_(73)−x(x=41−49)alloys.These results will help to the composition design and processing design of the Al−Cr−Fe−Ni based high-entropy alloys.