Thermal stability of cryomilled nanocrystalline aluminum containing diamantane nanoparticles

The thermal stability of nanoscale grains in cryomilled aluminum powders containing 1% diamantane was investigated. Diamantane is a diamondoid molecule consisting of 14 carbon atoms in a diamond cubic structure that is terminated by hydrogen atoms. The nanostructures of the resulting cryomilled powders were characterized using both transmission electron microscopy (TEM) and X-ray diffraction (XRD) techniques. The average grain size was found to be on the order of 22 nm, a value similar to that obtained for cryomilled Al without diamantane. To determine thermal stability, the powders were heated in an inert gas atmosphere at constant temperatures between 423 and 773 K (0.51T _m to 0.83T _m) for exposure times of up to 10 h. The average grain size for all powders containing diamantane was observed to remain in the nanocrystalline range (1–100 nm) for all exposures and was generally less than half of that for cryomilled pure Al heated under the same conditions. The thermal stability data were found to be consistent with a grain growth model based on drag forces exerted by dispersed particles against grain boundary migration. The present findings indicate that the presence of diamantane results in a substantial increase in the thermal stability of nanoscale grains in Al.     

Nanostructure in a Ti alloy processed using a cryomilling technique

A nanocrystalline Ti alloy with a uniform distribution of grains was synthesized using cryogenic mechanical milling. The effects of cryomilling parameters, such as milling time and ball to powder ratio (BPR), on the particle size, grain size, chemistry, and structure of cryomilled Ti powders were investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The experimental results show that nanocrystalline Ti powders with a grain size of about 20 nm can be prepared using the cryomilling technique. Compared to SPEX milling at room temperature, cryomilling led to lower contamination levels of oxygen, nitrogen, and iron in the cryomilled Ti powder. The average particle size initially increased from the original 55 μm to a maximum value of 125 μm after 2 h of milling, and then decreased to 44 μm after 8 h of milling. Both the average particle size and the grain size decreased as the BPR increased.     

Enhanced tensile ductility in a nanostructured Al–7·5%Mg alloy

Abstract

This paper reports work on the enhanced tensile ductility in a nanostructured Al–7·5%Mg alloy with a mean grain size of 90 nm processed via consolidation of cryomilled Al–Mg powders. An annealing treatment at a temperature of 773 K for 2·5 h modified the extruded microstructure slightly without causing significant grain growth, as revealed by TEM and XRD patterns. The annealing treatment significantly improved the ductility, with a remarkably small loss in strength. The observed high thermal stability of the cryomilled Al alloy was attributed to the existence of impurity elements introduced during cryomilling and the presence of a supersaturated solid solution. The reported phenomenon of enhanced tensile ductility was attributed to a mechanism involving dislocation activity in submicron grains during plastic deformation.     

水热介质pH值对纳米(Ce)ZrO2晶粒制备的影响

用水热法制得纳米 (Ce)ZrO2 粉体 ,其晶粒粒度为 3～ 7nm ,而且为单一分散。用XRD、TEM分析了水热媒介pH值对粒度、m相含量、晶粒形貌的影响关系。结果表明 :水热煤介 pH值增大 ,ZrO2 晶粒也增大 ;pH值减小至酸性时 ,ZrO2 晶粒中出现部分m相 ,且晶粒易团聚     

水热介质pH值对纳米(Ce)ZrO_2晶粒制备的影响

用水热法制得纳米 (Ce)ZrO2 粉体 ,其晶粒粒度为 3～ 7nm ,而且为单一分散。用XRD、TEM分析了水热媒介pH值对粒度、m相含量、晶粒形貌的影响关系。结果表明 :水热煤介 pH值增大 ,ZrO2 晶粒也增大 ;pH值减小至酸性时 ,ZrO2 晶粒中出现部分m相 ,且晶粒易团聚     

Microstructure of AA2024-SiC nanostructured metal matrix composites

Nanostructured metal matrix composites (NMMCs) in large-dimension billets were fabricated by hot isostatic pressing (HIPing) of cryomilled powders consisting of AA2024 alloy reinforced by 25 wt.% SiC particles. Microstructure of the bulk nanostructured composites and cryomilled powders was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). In addition, mechanical properties of the bulk nanocomposites were also addressed.     

Pressureless sintered ATZ and ZTA ceramic composites

Alumina-20 wt% zirconia (ATZ) and zirconia-20 wt% alumina (ZTA) composites were prepared by conventional sintering of commercial powders, with average particle sizes in the range 0.35–0.70 m. Sintering at 1650 °C for 4 h resulted in final densities up to 96%. Bending strength and hardness increased with the final density. The tetragonal volume fraction was strongly dependent on both the final density and tetragonal grain size. The relatively high fracture toughness of 9 MPa m^1/2 was associated with the highly dense microstructure consisting of tetragonal grains of the critical size.     

Effects of TiB2 on microstructure of nano-grained Cu–Cr–TiB2 composite powders prepared by mechanical alloying

Nano-grained CuCr25 and CuCr25–(2 wt%–10 wt%)TiB₂ composite powders were prepared by mechanical alloying method. The milled powders were characterized by SEM, FSEM, EDS, XRD, TEM and HTEM. The results indicate that average grain size of Cu, Cr and TiB₂ are less than 50 nm and each component disperses uniformly. The grain size of Cu and Cr decreased and the lattice distortion increased gradually as the TiB₂ content increased from 2 wt% to 10 wt%. The ultrafine TiB₂ particles play the role of “micro-milling balls” to compact, micro-etch, micro-frict and micro-cut with Cu and Cr so that the grain refinement and lattice strain are promoted.     

Grain growth behavior of nanocrystalline Inconel 718 and Ni powders and coatings

Nanocrystalline Inconel 718 and Ni powders were prepared using two approaches: methanol and cryogenic attritor milling. High velocity oxy-fuel (HVOF) spraying of milled Inconel 718 powders was then utilized to produce coatings with a nanocrystalline grain size. Isothermal heat treatments were carried out to study the thermal stability of the methanol milled and cryomilled powders, as well as the HVOF-derived coatings. All nanocrystalline Inconel 718 powders and coatings studied herein exhibited significant thermal stability against grain growth by maintaining a grain size around 100 nm following annealing at 1273 K for 60 min. In the case of the cryomilled nanocrystalline Ni powders, isothermal grain growth behavior was studied, from which the parameters required for the prediction of the microstructural evolution during a non-isothermal annealing were acquired. The theoretical simulation of grain growth behavior of nanocrystalline Ni during non-isothermal annealing conditions yields results that are in good agreement with the experimental results.     

Air-plasma spraying colloidal solutions of nanosized ceramic powders

Coatings prepared from nanosized powders were obtained by spraying ethanol-based colloidal solutions into a plasma plume. The powders investigated included 40 nm -Al₂O₃, 75 nm 8 wt% Y₂O₃-ZrO₂, and 750 nm 25 wt% CeO₂-ZrO₂. Spray distances from approximately 50 to 63 mm were required to achieve significant coating deposition. As observed in the TEM, the typical lamella morphology of air plasma sprayed oxide coatings was not observed in coatings fabricated from 40 nm -Al₂O₃, which was comprised of spherical powders that had partially sintered. However, lamellae were observed in the coatings prepared with both nanosized zirconia powders. The characteristic size of the lamella and the grains that comprised the zirconia coatings were nominally a few nanometers.     

High pressure sintering of diamond-SiC composite

Sintered polycrystalline compacts in the system diamond-10–50 wt% SiC having average grain size of less than 1 m were prepared at pressure of 6 GPa and temperature between 1400 and 1600 °C. Knoop indentation hardness of the compacts increased with diamond content and sintering temperature, and specimens with a Knoop indentation hardness greater 40 GPa were obtained. It was found that small amount of Al addition into the starting diamond-SiC powder was effective to improve relative density and Knoop indentation hardness of the compacts. The formation of graphite was also suppressed by the addition of Al. Microstructure observation by SEM and TEM suggested that Al segregated at the grain boundary and promoted the bonding between grains. Thin microtwins were observed in diamond grains, whereas fine wavy structures with slightly different orientations were observed in SiC grains, with or without Al addition.     

柠檬酸-凝胶燃烧法制备钇铝石榴石(Y_3Al_5O_(12))纳米粉体的研究

透明YAG多晶陶瓷具有优良的光学、力学与化学性能,逐渐成为新一代固体激光基质材料。分散均匀、团聚轻的纳米粉体有利于制备出高度透明的激光陶瓷。以Y2O3、Al(NO3)3·9H2O和柠檬酸为原料,采用柠檬酸凝胶燃烧法制备出黑色粉体,经1100℃烧结出尺寸小于50nm的YAG粉体。采用TG-DTA、XRD、FT-IR和TEM测试手段对YAG纳米粉体进行表征,采用谢莱公式计算出不同烧结温度下的晶粒尺寸。研究结果表明:YAG的析晶温度范围为850～900℃,烧结过程中出现赝YAG相物质,1050℃转变成纯YAG相,随着热处理温度的升高,晶粒呈线性增长,纳米粉体的TEM尺寸和采用谢莱公式计算的结果相一致。     

Processing of nanocrystalline FeAlX (X = Ni, Mn) intermetallics using a mechanical alloying and hot pressing techniques

Fe-40Al-40Ni-20 and Fe-40Al-40Mn-20 (all in at.%) intermetallics were mechanically alloyed for 40 h and followed by hot-pressing at 650°C under 450 MPa for 1 h. As resulted from the X-ray diffraction studies, the ordered B2 structure was formed in the Fe-40Al-40Ni-20 alloy while in the case of Fe-40Al-40Mn-20 alloy, the disordered Fe(Al) solid solution was observed. The chemically homogenous rounded particles of size of about 5 μm were identified using scanning analytical electron microscopy in alloys after 40 h of milling. TEM studies of milled powders revealed a nanostructure in both alloys with grain size of about 20 nm. The hot pressing process of milled powders allowed to obtain compacts with the density of about 87 and 89% of the theoretical one for Fe-40Al-40Mn-20 and Fe-40Al-40Ni-20 alloys, respectively. The micro-hardness measurements have shown that the alloy with the Ni addition possesses the hardness of about 1200 HV₂₀, whereas in the alloy with the Mn addition it is 1100 HV₂₀. The TEM investigations allowed to identify a nanocrystalline structure of compacts with a mean grain size below 50 nm, with B2 ordered structure in both alloys.     

Structural Characteristics of Rapidly Quenched Al-Si Alloys

The structure of rapldly quenched Al-Si alloys (1 and 4 wt-%Si) was systematically studied by optical and transmission electron microscopy (TEM ) as welI as X-ray djffractjon (XRD). ExperimentaIresults show that rapid solidification refines the grain size. extends the solid solubility of Si in Al and Introduces a high density ot defects which exist in the forms of vacancies, dislocations and dislocation loops. etc.. The decomposition process of the alloys was fol lowed by using differential scanning calorimeter (DSC) and the activation energy for precipitation of Si was obtained through Kissinger analysis. The precipitation behaviour of Supersaturated Si in both samples was further examined by TEM. It was found that Si mainly precipitated inside the grains in Al-1 wt-%Si alloy. while in Al-4 wt-%Si alloy. nearly all the Si precipitates distributed along the grain boundaries. This may be due to the structure difference between the alloys in as-quenched state     

In situ enhancement of toughness of SiC—TiB2 composites

A process based on liquid phase sintering and subsequent annealing for grain growth is presented to obtain the in situ enhancement of toughness of SiC–30 wt%, 50 wt%, and 70 wt% TiB2 composites. Its microstructures consist of uniformly distributed elongated -SiC grains, relatively equiaxed TiB2 grains, and yttrium aluminium garnet (YAG) as a grain boundary phase. The composites were fabricated from -SiC and TiB2 powders with the liquid forming additives of Al2O3 and Y2O3 by hot-pressing at 1850°C and subsequent annealing at 1950°C. The annealing led to the in situ growth of elongated -SiC grains, due to the phase transformation of SiC, and the coarsening of TiB2 grains. The fracture toughness of the SiC–50 wt% TiB2 composites after 6 h annealing was 7.3 MPa m1/2, approximately 60% higher than that of as-hot-pressed composites (4.5 MPa m1/2). Bridging and crack deflection by the elongated -SiC grains and coarse TiB2 grains appear to account for the increased toughness of the composites.     

Nano-structured intermetallic compound TiAl obtained by crystallization of mechanically alloyed amorphous TiAl, and its subsequent grain growth

The amorphization process during mechanical alloying (MA) was investigated for the Al-50at%Ti and Al-50at%Ti-10vol%TiB₂ powder mixtures. Pure metallic powders of Al and Ti were finely mixed and transformed to the amorphous phase after being milled for about 2880 ks. In the case of Al-50at%Ti-10vol%TiB₂ powder, the amorphous alloys with a fine dispersion of TiB₂ particles could be obtained for a shorter milling times than that required for the powders without TiB₂ ceramics. As a result of heat treatment for the mechanically alloyed amorphous powders, a nanocrystalline intermetallic compound of TiAl () could be produced. Subsequent grain growth of the phase during heat treatment was investigated by estimating the grain-growth exponent and the activation energy for grain growth. It was found from this estimation that the grain growth was further suppressed as the powders were mechanically alloyed for longer times. Furthermore, the addition of the TiB₂ particles that could be dispersed during MA finely and homogeneously in the amorphous matrix was found to be effective for suppression of the grain growth especially at elevated temperatures as well as for a long annealing.     

Effect of SiC Nanoparticles Content and Mg Addition on the Characteristics of Al/SiC Composite Powders Produced via In Situ Powder Metallurgy Method

In the present study, the effect of the nanosized SiC particles loading and Mg addition on the characteristics of Al/SiC composite powders produced via a relatively new method called “in situ powder metallurgy” (IPM) was investigated. Specified amounts of SiC particles (within a size range of 250 to 600 µm) together with SiC nanoparticles (average size of 60 nm) were preheated and added to aluminum melt. This mixture was stirred via an impeller at a certain temperature for a predetermined time. The liquid droplets created by this process were then subsequently cooled in air and screened through 250 µm sieve to separate micron-sized SiC particles from solidified aluminium powder particles containing nanosized SiC particles. Results of SEM and TEM studies together with microhardness measurements revealed that the commercially pure (CP) Al could not embed as-received SiC particles. However, the nanosized particles were distributed uniformly in the Al-1 wt% Mg powders. The process yield and microhardness of the Al-1Mg composite powders increased with increasing the contributed amount of nanosized SiC particles.     

Mechanical response of nanocrystalline steel obtained by mechanical attrition

The mechanical properties of bulk specimens of nanocrystalline 0.55% C steel with a grain size of 30 nm and a relative density higher than 97% have been determined. Samples were obtained by cold compaction and warm sintering at 425 °C of nanocrystalline powders obtained by mechanical attrition in a planetary ball mill. In both processes an Ar protective atmosphere was used in order to avoid oxygen contamination. X-ray diffraction (XRD) and Transmission electron microscopy (TEM) analysis indicated that a volume-averaged grain size of 30 nm is maintained after the warm consolidation processes. TEM studies also showed equiaxed ferrite with no dislocations inside the grains. However, the grain size distribution was no homogeneous as large grains of 100 nm were observed. An average hardness of 8.5 GPa was obtained, in good agreement with other bulk specimens of nanocrystalline Fe or eutectoid carbon steel prepared by other authors. Compression tests of bulk specimens at a strain rate of 10⁻⁴ s⁻¹ showed a compression strength near 2,500 MPa with an absolute lack of ductility. Nanoindentation measurements at room temperature provided a strain rate sensitivity parameter of 0.012, indicating that the deformation mechanism is somehow governed by diffusion mechanisms.     

Effect of grain size on strain rate sensitivity of cryomilled Al–Mg alloy

Al–Mg alloy powder was cryomilled to achieve a nanocrystalline (NC) structure having an average grain size of 50 nm with high thermal stability, and then consolidated by quasi-isostatic forging. The consolidation resulted in a bulk material with ultrafine grains of about 250 nm, and the material exhibited enhanced strength compared to conventionally processed Al–Mg alloy. The hardness of as-cryomilled powder, the forged ultrafine-grained (UFG) material, and the conventional coarse-grained (CG) alloy were measured by nanoindentation using various loading rates, and the results were compared with strain rate sensitivity (SRS) from uniaxial compression tests. Negative SRS was observed in the cryomilled NC powder and the forged UFG material, while the conventional alloy was relatively insensitive to strain rate. The dependence on loading rate was stronger in the NC powders than in the UFG material.     

Mixed phase F-doped SnO2 film and related properties deposited by ultrasonic spraying

Fluorine-doped tin oxide thin films with amorphous/crystal mixed phases were deposited on silicon and quartz sheets by an ultrasonic spraying method and investigated with XPS, XRD, AFM and TEM techniques. The XRD spectra and the results of TEM analysis show that nanoscale amorphous clusters were formed within the grain boundary region. At room temperature, electron transportation is predominantly limited by amorphous defect scattering of the crystal grain boundary region. The minimum electrical resistivity 4.0×10⁴cm was obtained through decreasing the amorphous phase fraction and the preferred orientation arrangement of the crystal grains. A 0.8-eV shift exists between the tin 3d binding energy in thin films having the preferred crystallite orientation with (1 1 0) plane parallel to the substrate and that with the (2 0 0) plane parallel to the substrate.