Mechanical behaviors of Al2O3 nanoparticles reinforced polyetheretherketone

The precipitation kinetics of Si in an Al–1.7 wt.%Si alloy after different thermal treatments has been studied by means of transmission electron microscopy (TEM), dilatometry and differential scanning calorimetry (DSC). The results obtained are explained by a model based on simple nucleation and growth/dissolution laws and are compared with measured precipitate size distributions. The evolution of precipitates in water-quenched samples during linear heating depicts the exothermic formation of platelets and globular Si precipitates (200–300 °C). The endothermal dissolution of Si platelets starts at lower temperatures than that of the globular precipitates. Coarsening and finally dissolution of globular precipitates is observed with increasing temperature. Samples slowly cooled from the solution treatment temperature present mostly globular precipitates, which are nucleated during cooling. Here, an exothermal effect related to the growth of Si precipitates increasing their volume fraction is observed at relatively high temperatures (350–460 °C) during linear heating. The formed precipitates are stable up to 460 °C, where the modelled critical radius becomes bigger than most of the Si precipitates formed so far.     

Al-Cu合金析出相在等径角挤压中的演变

为了研究Al-Cu合金中两种不同析出相(θ′和θ相)在ECAP变形过程中的变化.采用透射电镜(TEM)和硬度测试方法研究了析出相形貌变化以及对合金性能的影响.结果表明:在本实验中,θ′和θ相其破碎、回溶速度明显不同,两者的破碎方式也不同.θ′相先是与基体失去取向关系,随后从其内部产生位错使其破碎,而θ相是被外部基体位错所切割、破碎.θ′相与位错的相互作用方式类似于绕过机制,θ相与位错的作用方式类似于切割机制.两种状态样品的硬度在变形过程中的变化趋势相同,但在第1道次后θ相状态样品的硬度增加值高于θ′相状态.     

Heat treatment and microstructure of an Fe---Ni---Co Invar alloy strengthened by intermetallic precipitation

Microstructural developments during the heat treatment of an Fe---Ni---Co---Al---Ti Invar alloy have been investigated using transmission electron microscopy. The primary strengthening mechanism is the formation of a fine distribution of spherical γ′-type intermetallic precipitates, while overaging is accompanied by the formation of η-type precipitates, with a plate morphology, that grow at the expense of γ′. The chemical composition of the precipitates has been determined by extracting them on a carbon foil followed by analysis using scanning transmission electron microscopy. The steps involved in the preparation of samples for electron microscopy are detailed. An estimate of the dissolution temperatures of γ′ and η has been made using a combination of hardness and grain size measurements. This information has been utilized to develop a heat treatment that produces very fine grain sizes while retaining an adequate level of strength.     

变形程度对强变形Al-4%Cu合金退火组织性能的影响

为了研究变形程度对强变形Al-4%Cu合金退火行为的影响,通过透射电镜观察和拉伸试验,研究了人工时效Al-4%Cu合金经过不同变形量的多向压缩变形(MAC),退火(120℃/60 min)后的显微组织和力学性能.研究表明:试样中的第二相在MAC过程中破碎溶回基体后,会在后续退火过程中再次析出,且析出相回溶的程度对退火组织性能的影响很大.含θ″相试样和含θ’相试样经MAC变形后,析出相完全回溶于基体,在退火过程中有新的第二相析出,试样强度升高;同时试样的的塑性也得到了提高,这与再析出粒子对超细晶粒长大的阻碍作用有关.析出相未完全回溶的含θ相试样,退火后强度低于退火前,析出相回溶和再析出交替进行.析出相基本回溶态强韧化效果最佳.     

Ni(3)Si(Al)/a-SiO(x) core-shell nanoparticles: characterization, shell formation, and stability

We have used an electrochemical selective phase dissolution method to extract nanoprecipitates of the Ni(3)Si-type intermetallic phase from two-phase Ni-Si and Ni-Si-Al alloys by dissolving the matrix phase. The extracted nanoparticles are characterized by transmission electron microscopy, energy-dispersive x-ray spectrometry, x-ray powder diffraction, and electron powder diffraction. It is found that the Ni(3)Si-type nanoparticles have a core-shell structure. The core maintains the size, the shape, and the crystal structure of the precipitates that existed in the bulk alloys, while the shell is an amorphous phase, containing only Si and O (SiO(x)). The shell forms around the precipitates during the extraction process. After annealing the nanoparticles in nitrogen at 700?°C, the tridymite phase recrystallizes within the shell, which remains partially amorphous. In contrast, on annealing in air at 1000?°C, no changes in the composition or the structure of the nanoparticles occur. It is suggested that the shell forms after dealloying of the matrix phase, where Si atoms, the main constituents of the shell, migrate to the surface of the precipitates.     

Small-angle X-ray scattering study of precipitates in AlZnMgCu-1.0 wt.% Li alloy

The precipitate size, distribution and volume fraction in an AlZnMgCu-1.0 wt.% Li alloys during various aging conditions were investigated by small-angle X-ray scattering and transmission electron microscopy. According to the selected area diffraction patterns, the prime precipitates in this alloy are η′ phases, not δ′ phases. During the temperature ranging from 120 to 160 °C, the growing of precipitates in the 7055-1.0 wt.% alloys is not apparent. From 120 to 150 °C, the varieties of precipitate volume fraction depend on the competition between dissolution rate of GP zones and nucleation rate of η′. At 160 °C, the growing of η′ precipitates is undergoing a Lifshitz–Slyozov–Wagner coarsening process, and the prime thermodynamic reaction is the nucleation growth of η′ precipitates.     

Characterization of the evolution of the volume fraction of precipitates in aged AlMgSiCu alloys using DSC technique

Differential scanning calorimetry is used to quantify the evolution of the volume fraction of precipitates during age hardening in AlMgSiCu alloys. The calorimetry tests are run on alloy samples after aging for various times at 180 °C and the change in the collective heat effects from the major precipitation and dissolution processes in each run are used to determine the precipitation state of the samples. The method is implemented on alloys with various thermal histories prior to artificial aging, including commercial pre-aging histories. The estimated values for the relative volume fraction of precipitates are compared with the results from a newly developed analytical method using isothermal calorimetry and a related quantitative transmission electron microscopy work. Excellent agreement is obtained between the results from various methods.     

Effect of Microstructure on Thermal Expansion Coefficient of 7A09 Aluminum Alloy

The relationship between microstructure evolution and coeffcient of thermal expansion (CTE) of 7A09 alu- minum alloy was investigated in this paper. Differential scanning calorimetry (DSC) was combined with transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM) to investigate microstructure evolution taking place in 7A09 aluminum alloy during heating and cooling process. The corresponding CTE curves of the 7A09 alloy were recorded by thermal dilatometer. Results indicated that GPII zones and η phase were main precipitates in the highest strength tempered (T6) 7A09 alloy. The η phase was the main participate in 7A09 alloy during the cooling process. The nonlinear dependency existed between CTE and temperature in both changing temperature processes. During the heating process, obvious additional contraction of alloy volume was directly caused by phase transition, such as dissolution of η phase, transition from η to η phase and dissolution of η phase. The additional contraction could slow down the increase of CTE greatly and be expressed in the nonlinearity of CTE curve. Volume and energy changes of alloy system inffuenced the variation trend of CTE directly, which was caused by the precipitation of η phase during the cooling process. These effects were revealed by the corresponding nonlinear change of CTE.     

Ultrastructure study of hydroxyapatite precipitation on ceramic surfaces in dog model

Calcium phosphate (Ca–P) minerals were precipitated on porous alpha-tricalcium phosphate (α-TCP) after implantation in dog muscles for four weeks. Scanning electron microscopy (SEM) examinations indicated that the Ca–P precipitates exhibited flattened-hexagonal rod shapes. Electron diffraction revealed that the rod-like precipitates were hydroxyapatite (HA) elongated in the c-axis. High-resolution transmission electron microscopy (HRTEM) was used to analyze the ultrastructures of the precipitates. We found the evidence of octacalcium phosphate (OCP) structure embedding in a few rod-like HA precipitates. The orientation relationship of OCP/HA revealed in the precipitates was consistent with observations of the solid-state OCP/HA transformation in synthetic specimens, i.e., OCP (010)//HA (01¯0) and OCP (001)//HA (001¯).     

Dissolution and mineralization of sintered and thermally sprayed hydroxy-fluoroapatites

Hydroxyapatites are commonly used as bone cement, coatings on implants for dental and orthopaedic applications, but also as middle ear implants. These applications all require a different tissue healing response that can be attained by different manufacturing processes or by chemically modifying the composition. During implantation apatites undergo a process of dissolution and mineralization. The degree of dissolution is dependent upon the manufacturing process & is higher for thermally sprayed implant materials. This allows them to integrate to the natural bone. This study tests the dissolution and mineralization of fluoride containing hydroxyapatites through immersion in simulated body fluid. It shows that mineralization occurs more readily in hydroxyapatites than fluorapatites because of their higher dissolution rate. Mineralization was detected most readily by image analysis using scanning electron microscopy than by weight changes using a microbalance. Microscopy allowed small heterogeneous precipitates to be observed during the initial stages of mineralization.     

Study of tensile deformation behaviour of M250 grade maraging steel using acoustic emission

Tensile testing of solution annealed and thermally aged (755 K for various durations in the range of 0.25–100 h) specimens of M250 grade maraging steel has been carried out along with acoustic emission (AE) monitoring. Results have shown that strength increases and ductility decreases upon ageing up to 10 h and this has been attributed primarily to the precipitation of Ni₃Ti. Continued increase in strength up to 40 h of ageing has been attributed primarily to the precipitation of Fe₂Mo in addition to Ni₃Ti. Increase in ductility for 10–40 h of ageing has been attributed to dissolution of needle like Ni₃Ti precipitates and formation of fine spherical Fe₂Mo. Ageing beyond 40 h decreases strength and increases ductility due to the reversion of martensite to austenite and coarsening of the precipitates. The AE generated during tensile deformation depends on the ageing time. Increased occurrence of shearing of the precipitates by dislocations and increased brittleness of the matrix up to 10 h ageing increases the AE. The decrease in the AE beyond 10 h of ageing is due to the occurrence of deformation by Orowan looping, dissolution of Ni₃Ti precipitates and austenite reversion. The scanning electron microscopy (SEM) of the fracture surfaces has shown ductile fracture characterized by dimples and changes in the size and shape of the dimples with ageing time.     

Effect of aging treatment on fracture toughness in ZM61 magnesium alloy

The effect of aging treatment on fracture toughness in Mg–6Zn–1Mn (wt-%) was investigated by optical microscopy, scanning electron microscopy, transmission electron microscopy, scanning transmission electron microscopy, uniaxial tensile and fracture toughness tests, respectively. The results showed that the fracture toughness of Mg–6Zn–1Mn alloy can be enhanced by aging treatment. The fracture toughness and strength showed a reverse trend in single aged and double aged alloy. Synergetic effect of fine grains and precipitates improved the fracture toughness more sharply than aging treatment. The precipitate free zones and grain boundary precipitates made the largest contribution to the reduction of toughness. Under as extruded and aged conditions, the main origins of cracks were elastic incompatibility and plastic deformation.     

Microstructure optimization of austenitic Alloy 800H (Fe-21Cr-32Ni)

The microstructural evolution, specifically of grain boundaries, precipitates, and dislocations in thermomechanically processed (TMP) Alloy 800H samples was characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), electron backscattered diffraction (EBSD), transmission electron microscopy (TEM), and atomic force microscopy (AFM). The TMP not only significantly increased the fraction of low-Σ coincidence site lattice boundaries, but also introduced nanoscale precipitates in the matrix and altered the distribution of dislocations. Statistical analysis indicates that the morphology and distribution of grain boundary precipitates were dependent on grain boundary types. The microstructure optimization played a synergistic effect on the significantly increased strength with comparable ductility and enhanced intergranular corrosion resistance and creep-fatigue life compared to the as-received samples.     

Nano-precipitation in hot-pressed silicon carbide

Heat treatments at 1300°C, 1400°C, 1500°C, and 1600°C in Ar were found to produce nanoscale precipitates in hot-pressed silicon carbide containing aluminum, boron, and carbon sintering additives (ABC-SiC). The precipitates were studied by transmission electron microscopy (TEM) and nano-probe energy-dispersive X-ray spectroscopy (nEDS). The precipitates were plate-like in shape, with a thickness, length and separation of only a few nanometers, and their size coarsened with increasing annealing temperature, accompanied by reduced number density. The distribution of the precipitates was uniform inside the SiC grains, but depleted zones were observed in the vicinity of the SiC grain boundaries. A coherent orientation relationship between the precipitates and the SiC matrix was found. Combined high-resolution electron microscopy, computer simulation, and nEDS identified an Al₄C₃-based structure and composition for the nano-precipitates. Most Al ions in SiC lattice exsolved as precipitates during the annealing at 1400 to 1500°C. Formation mechanism and possible influences of the nanoscale precipitates on mechanical properties are discussed.     

Copper Oxide Precipitates in NBS Standard Reference Material 482

Copper oxide has been detected in the copper containing alloys of NBS Standard Reference Material (SRM) 482. This occurrence is significant because it represents heterogeneity within a standard reference material that was certified to be homogeneous on a micrometer scale. Oxide occurs as elliptically to spherically shaped precipitates whose size differs with alloy composition. The largest precipitates occur in the Au20-Cu80 alloy and range in size from submicrometer up to 2 μm in diameter. Precipitates are observed using light microscopy, electron microscopy, and secondary ion mass spectrometry (SIMS). SIMS has demonstrated that the precipitates are present within all the SRM 482 wires that contain copper. Only the pure gold wire is precipitate free. Initial results from the analysis of the Au20-Cu80 alloy indicate that the percentage of precipitates is less than 1 % by area. Electron probe microanalysis (EPMA) of large (2 μm) precipitates in this same alloy indicates that precipitates are detectable by EPMA and that their composition differs significantly from the certified alloy composition. The small size and low percentage of these oxide precipitates minimizes the impact that they have upon the intended use of this standard for electron probe microanalysis. Heterogeneity caused by these oxide precipitates may however preclude the use of this standard for automated EPMA analyses and other microanalysis techniques.     

Texture Evolution in Heavily Cold-Rolled FeCo-2V Alloy during Annealing

The recrystallization texture evolution in heavily cold-rolled (93%) FeCo-2V alloy with annealing temperature and time was investigated by X-ray diffraction and electron backscatter diffraction. It was found that the orientation density of α-fiber texture component fluctuates with increasing annealing temperature and time. The transmission electron microscopy images show that abundant precipitates appear inside the recrystallized grains and around the grain boundaries. The amount and size of the precipitate...     

Dissolution studies of hydroxyapatite and glass-reinforced hydroxyapatite ceramics

In the continuous agitation assays, glass-reinforced hydroxyapatite (GR-HA) was shown to form a calcium phosphate (CaP) layer, but hydroxyapatite (HA) only formed dispersed precipitates. The formation of this layer was first detected on the GR-HA with a 7.5% glass addition (7.5 GR-HA) after only 3 days of immersion in simulated body fluid (SBF). The time required for layer formation decreased as the amount of glass added to the HA increased. The dissolution rate of the materials followed a similar pattern, i.e. the dissolution rate for GR-HA was higher than for HA, and increased with the addition of glass. The immersion of 7.5 GR-HA in water showed almost linear dissolution kinetics over the immersion periods (3, 7, 15, 30 and 60 days). The concentration of calcium ions in solution and the scanning electron microscopy (SEM) analysis of the 7.5 GR-HA specimens immersed in water and in SBF revealed a clear competition between the material dissolution and the precipitation of a CaP phase. Fourier transformed infrared spectroscopy with alternated total reflectance (FTIR-ATR) analysis indicated that the CaP phase that formed during longer immersion times (30 and 60 days) could be a carbonate-substituted CaP precipitate.As expected from previous work, the GR-HA behavior in terms of its in vitro bioactivity is higher than HA because a homogeneous CaP layer is formed and the precipitation occurs faster. From the dissolution test and in accordance with the chemical composition of the samples, GR-HA was more soluble than HA.     

The effect of high temperature exposure on dendritic segregation in a conventionally cast Ni based superalloy

Dendritic segregation in conventionally cast, commercially heat treated and exposed MarM002 turbine blades has been investigated using scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). During casting Cr, Co and W segregate to the dendrites and Hf, Ti and Ta segregate to the eutectics. As a result of the dissolution of precipitates in the dendrites and coarsening of precipitates in the eutectics this segregation aggravates during exposure at 1000°C. At this high exposure temperature homogenisation of dendritic segregation does not occur because it involves long diffusion distances and a low driving force compared with dissolution and coarsening of precipitates.     

Q460FRW耐火钢的组织稳定性

采用Thermo-Calc热力学软件计算Q460FRW耐火钢的平衡态析出相。利用金相显微镜、扫描电子显微镜、透射电子显微镜观察和分析Q460FRW耐火钢600℃保温处理前后的基体与析出相演变。结果表明:600℃下的平衡态析出相由M7C3,M23C6(M=Fe,Cr,Mo,Mn)和MX(M=Nb,Ti;X=C,N)构成。热机械控制工艺下,组织主要由粒状贝氏体和针状铁素体构成。600℃保温处理后,粒状贝氏体中的M/A组元逐渐分解,针状铁素体逐渐转变为块状铁素体。随600℃下保温时间的延长,富Cr/Mn的M7C3相尺寸持续增加,富Nb/Ti的MX相尺寸在小幅度增加后保持稳定,未发现M23C6型析出相。在保温过程中,Mo主要以固溶态存在,其对耐火性能的作用主要为固溶强化。     

Alkali-aggregate reaction—identifying reactive silicates in complex aggregates by ESEM observation of dissolution features

A petrographic examination can only be used to qualify a concrete aggregate in regard to its potential for AAR when the reactivity of the corresponding lithologies and minerals are known. In this study, two complex Swiss aggregates with polished surfaces were immersed in an alkaline solution in order to identify reactive minerals. Afterwards, dissolution and precipitation phenomena were investigated by environmental scanning electron microscopy.In general, quartz is the most reactive mineral in both aggregates. Feldspar, biotite and chlorite exhibit dissolution phenomena, and liberate alkalis and calcium. Various morphological types of gels are formed as precipitates on the polished surface: thin calcium silicate hydrate structures exhibiting card house morphology; small agglomerates (2–20 μm) with a smooth surface; and large agglomerates (20–500 μm) characteristic of common ASR reaction products. These gels mainly consist of Si and Ca with variable amounts of Na, Mg, Fe and Al.