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.     

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.     

Preparation and sintering behaviour of nanostructured alumina/titania composite powders modified with nano-dopants

Nanostructured alumina/titania composite powders were prepared by doping with small amounts of nanosized zirconia and ceria. The nanosized raw materials powders were reconstituted into nanostructured particles by ball milling, spray drying and heat treating. Then, the nanostructured reconstituted powders were cool-isostatic pressed and pressureless-sintered into bulk ceramics. The phase composition and microstructures of reconstituted powders and as-prepared ceramic composites were characterized by using X-ray diffractometer (XRD), scanning electron microscope (SEM) and energy-dispersive spectrometer (EDS). The sintering behaviour of the nanostructured ceramic composite powders and the effects of nano-dopants and sintering temperatures on the microstructures of the ceramic composites were investigated and discussed. It was found that nano-dopants could lower the sintering temperature and accelerate densification of ceramic composites.     

Synthesis of Cu-W nanocomposite by high-energy ball milling

The Cu-W bulk nanocomposites of different compositions were successfully synthesized by high-energy ball milling of elemental powders. The nanocrystalline nature of the Cu-W composite powder is confirmed by X-ray diffraction analysis, transmission electron microscopy, and atomic force microscopy. The Cu-W nanocomposite powder could be sintered at 300-400 degrees C below the sintering temperature of the un-milled Cu-W powders. The Cu-W nanocomposites showed superior densification and hardness than that of un-milled Cu-W composites. The nanocomposites also have three times higher hardness to resistivity ratio in comparison to Oxygen free high conductivity copper.     

Microstructure evolution and interface structure of Al-40 wt% Si composites produced by high-energy ball milling

High silicon content Al-Si composites with a composition of Al-40 wt% Si were fabricated via a highenergy ball milling method. The microstructure evolution of Al-40 wt% Si milled powders and sintered composites has been thoroughly studied by scanning electron microscopy, X-ray diffraction, energydispersive spectrometry and high-resolution transmission electron microscopy. The mechanism of ball milling Al-40 wt% Si powders has been disclosed in detail: fracture mechanism dominating in the early stages, followed by the agglomeration mechanism, finally reaching the balance between the fragments and the agglomerates. It has been found that the average particle sizes of mixed Al-Si powders can be refined to the nanoscale, and the crystallite sizes of Al and Si have been reduced to 10nm and 62nm upon milling for 2h–50h, respectively. The finally formed Al-Si interfaces after ball milling for 50h are wellcohesive. A dense and homogenous Al-40 wt% Si composite have been achieved by solid-state sintering at550?C. The results thus provide an effective support for producing bulk nanostructured Al-Si composites.     

Studies on copper-yttria nanocomposites: high-energy ball milling versus chemical reduction method

Oxide dispersion-strengthened copper-base composites are widely used for applications demanding high tensile strength, high hardness along with good electrical and thermal conductivity. Oxides of metals like aluminium, cerium, yttrium and zirconium are often used for this purpose as fine and uniformly distributed dispersoid particles in soft and ductile copper matrix. Such composites find applications as electrical contacts, resistance-welding tips, lead wires, continuous casting moulds, etc. In this investigation an attempt has been made to produce copper-yttria nanocomposites using two different morphologies of copper powder and two different processing routes namely, high-energy milling and in-situ chemical reduction. The synthesized powders were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) for their phase identification and morphological study. The nanocomposite powders in each case were subsequently processed to obtain bulk solids by classical powder metallurgy route of press-sinter-repress. The resultant bulk solid compacts were subjected to property evaluation. The study revealed that the properties of Cu-Y2O3 nanocomposites depend on the processing route used and in turn on the resultant powder morphology.     

Synthesis and properties of nanocrystalline CsI

The structure and properties of fine CsI powders prepared by spray pyrolysis and synthetic opal (SiO₂) based composites containing CsI in their pores have been studied by electron microscopy, X-ray diffraction, and luminescence spectrometry. The powders consisted of nanocrystalline particles which increased in size from 35 to 55 nm with increasing pyrolysis temperature. In the opal/CsI composites, the CsI nanocrystallites were about 45–50 nm in size and formed a single three-dimensional network between the SiO₂ spheres. In going from bulk crystals to their nanocrystalline analogs, the size effect on CsI luminescence leads to a reduction in luminescence yield, a redshift of the emission bands of the on-center and off-center self-trapped excitons (STEs), and an increase in the contribution of the off-center STEs to the net intrinsic emission yield. The emission decay kinetics of the off-center STEs is insensitive to the crystallite size.     

Crystalline – Amorphous AA4048 – Al60Nb40 composites processed by mechanical alloying and powder compaction

Commercial crystalline AA4048 powders and mechanically alloyed amorphous Al₆₀Nb₄₀ (at.%) powders were used for fabrication of crystalline-amorphous composites containing 10, 20 and 30?vol% of amorphous phase. High pressure high temperature technique was used for powders compaction. The applied pressure was 7.7?GPa and temperature was in the range 600–1000?°C. The powders and bulk samples were characterized by structural investigations (X-ray diffraction, scanning electron microscopy, energy dispersive spectroscopy, X-ray fluorescence spectroscopy), hardness and microhardness tests and measurements of density. The obtained sinters revealed relative density above 98.7%. The amorphous component was observed as agglomerates or as single particles surrounding the grains of crystalline AA4048 phase. The crystallization of amorphous phase was not observed. Simultaneously, up to 2.5?wt% of Fe was detected as impurity from milling media. Significant increase of hardness was observed, from 226 to 288HB, resulting from the presence of amorphous component which prevent from cracks propagation during deformation.     

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.     

Enhanced ionic conductivity of AgI nanowires/AAO composites fabricated by a simple approach

AgI nanowires/anodic aluminum oxide (AgI NWs/AAO) composites have been fabricated by a simple approach, which involves the thermal melting of AgI powders on the surface of the AAO membrane, followed by the infiltration of the molten AgI inside the nanochannels. As-prepared AgI nanowires have corrugated outer surfaces and are polycrystalline according to scanning electron microscopy (SEM) and transmission electron microscopy (TEM) observations. X-ray diffraction (XRD) shows that a considerable amount of 7H polytype AgI exists in the composites, which is supposed to arise from the interfacial interactions between the embedded AgI and the alumina. AC conductivity measurements for the AgI nanowires/AAO composites exhibit a notable conductivity enhancement by three orders of magnitude at room temperature compared with that of pristine bulk AgI. Furthermore, a large conductivity hysteresis and abnormal conductivity transitions were observed in the temperature-dependent conductivity measurements, from which an ionic conductivity as high as 8.0 × 10(2)?Ω(-1)?cm(-1) was obtained at around 70?°C upon cooling. The differential scanning calorimetry (DSC) result demonstrates a similar phase transition behavior as that found in the AC conductivity measurements. The enhanced ionic conductivity, as well as the abnormal phase transitions, can be explained in terms of the existence of the highly conducting 7H polytype AgI and the formation of well-defined conduction paths in the composites.     

Processing of Ceramic Based Nanocomposite Using α-Al2O3 Powder and FeCl2 Solution as Starting Materials

Alumina-iron nanocomposite powders were prepared by a two-step process. In the first step, α-Al2O3-FeCl2 powder mixture was formed by mixing α-Al2O3 powders with FeCl2 solution followed by drying. In the second step, the FeCl2 in the dry power mixture was selectively reduced to iron particles. A reduction temperature of 750℃ for 15 min in dry H2 was chosen based on the thermodynamic calculations. The concentration of iron in FeCl2 solution was calculated to be 20 vol. pct in the final composite. Two techniques were used to produce composite bulk materials. The Al2O3 nanocomposite powders were divided to two batches. The first batch of the produced mixture was hot pressed at 1400℃ and 27 MPa for 30 min in a graphite die. To study the effect of oxygen on the Al2O3/Fe interface bonding and mechanical properties of the composite, the second batch was heat treated in air at 700℃ for 20 min to partially oxidize the iron particles before hot pressing. Characterization of the composites was undertaken by conventional density measurements, X-ray diffractometry （XRD）, scanning electron microscopy （SEM）, transmission electron microscopy （TEM） and electron probe micro analysis （EPMA）. The suggested processing route （mixing, reduction and hot pressing） produces ceramic-metal nanocomposite much tougher than the pure Al2O3. The fracture strength of the produced Al2O3/Fe nanocomposite is nearly twice that of the pure Al2O3. The presence of spinel phase, FeAl204, as thick layer around the Fe particles in the Al2O3 matrix has a detrimental effect on interfacial bonding between Fe and AI203 and the fracture properties of the composite.     

Processing of Ceramic Based Nanocomposite Using α-Al2O3 Powder and FeCl2 Solution as Starting Materials

Alumina-iron nanocomposite powders were prepared by a two-step process. In the first step, α-Al2O3-FeCl2 powder mixture was formed by mixing α-Al2O3 powders with FeCl2 solution followed by drying. In the second step, the FeCl2 in the dry power mixture was selectively reduced to iron particles. A reduction temperature of 750℃ for 15 min in dry H2 was chosen based on the thermodynamic calculations. The concentration of iron in FeCl2 solution was calculated to be 20 vol. pct in the final composite. Two techniques were used to produce composite bulk materials. The Al2O3 nanocomposite powders were divided to two batches. The first batch of the produced mixture was hot pressed at 1400℃ and 27 MPa for 30 min in a graphite die. To study the effect of oxygen on the Al2O3/Fe interface bonding and mechanical properties of the composite,the second batch was heat treated in air at 700℃ for 20 min to partially oxidize the iron particles before hot pressing. Characterization of the composites was undertaken by conventional density measurements, X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron probe micro analysis (EPMA). The suggested processing route (mixing, reduction and hot pressing)produces ceramic-metal nanocomposite much tougher than the pure Al2O3. The fracture strength of the produced Al2O3/Fe nanocomposite is nearly twice that of the pure Al2O3. The presence of spinel phase,FeAl2O4, as thick layer around the Fe particles in the Al2O3 matrix has a detrimental effect on interfacial bonding between Fe and Al2O3 and the fracture properties of the composite.     

NiAl-B composites with nanocrystalline intermetallic matrix produced by mechanical alloying and consolidation

Powder mixtures with equiatomic Ni–Al stoichiometry and with the addition of 5, 10, 20 and 30 vol% of boron were mechanically alloyed in a high-energy SPEX mill. Differential scanning calorimetry (DSC) was used for examination of the thermal behaviour of the milled powders. The mechanically alloyed powders and powders after DSC examinations were investigated by X-ray diffraction (XRD). For all the powder mixtures, a nanocrystalline NiAl intermetallic phase was formed during milling. With the increase of boron concentration in the mixtures, more intense refinement of the NiAl grain size during mechanical alloying was observed. Scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS) examinations showed that the produced powders have composite structure, with boron particles uniformly distributed in the nanocrystalline NiAl intermetallic matrix. The density of the composite powders decreases with the increase of boron content, following the rule of mixture.The produced powders were subjected to consolidation by hot-pressing at 800 °C under the pressure of 7.7 GPa for 180 s. The produced bulk materials were investigated by XRD, SEM and EDS as well as characterised by hardness, density and open porosity measurements. It was found that during applied consolidation process the nanocrystalline structure of the NiAl matrix was maintained. The average hardness of the bulk composite samples is in the range of 10.58–12.6 GPa, depending on boron content, increases with the increase of boron content, and is higher than that of the NiAl intermetallic reference sample (9.53 GPa). The density of the bulk composite samples is the same as that of the corresponding powders after milling, decreases with the increase of boron content and is lower than that of the NiAl reference sample. To the best of our knowledge, the NiAl-B composites with nanocrystalline intermetallic matrix have been produced for the first time.     

The influence of oxygen and nitrogen contamination on the densification behavior of cryomilled copper powders during spark plasma sintering

It has been found difficult to fully densify some mechanically milled pure metal powders by spark plasma sintering (SPS). In this study, the densification behavior of cryomilled, nanostructured (NS) Cu powders during SPS was related to changes to the chemistry of the powders. The results showed that the presence of very small amounts of O and N in the powders, which were introduced during cryomilling and handling, significantly influenced the densification response. Moreover, reduction/removal of O/N via thermal annealing of the powders before SPS led to complete densification of the powders during subsequent SPS. The mechanisms responsible for this behavior were ascertained: O and N existed in the cryomilled powders in the form of thermally unstable compounds, and the subsequent thermal decomposition of these compounds during SPS generated the gaseous species, leading to porosity formation and incomplete densification; annealing of the powders before SPS removed the gases which resulted from thermal decomposition, thereby facilitating complete consolidation during subsequent SPS.     

多重结构Ti-B4C/Al2024复合材料的组织和力学性能

为了研究多重结构对铝基复合材料力学性能的影响,将气雾化态Al2024合金粉末与球磨不同时间的Ti-10%(质量分数,下同)B_4C复合粉末混合,采用热压烧结和热挤压的方法制备多重结构Ti-B_4C/Al2024复合材料。通过X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)和拉伸试验机对不同材料的显微组织与力学性能进行观察和测试,并对多重结构复合材料的强韧化行为进行讨论。结果表明:Ti-B_4C/Al2024复合材料多重结构包括基体Al2024、核壳结构Ti/Al₁₈Ti_2Mg_3组织和B_4C颗粒。向Al2024中加入5%预先球磨6h后的Ti-B_4C粉末时,其屈服强度从107MPa提高到122MPa,并且表现出与热挤压Al2024合金几乎相同的伸长率。当球磨时间延长至12h时,试样5TB-12h的伸长率可达到16.4%。然而,复合材料的伸长率随着Ti-B_4C添加量的增加而降低。     

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.     

Mechanical and microstructure of reinforced hydroxyapatite/calcium silicate nano-composites materials

In this study, the nano sized hydroxyapatite (HA) and calcium silicate (CS) powders prepared by both chemical precipitation and sol–gel methods respectively. Biphasic nano-composites materials containing different ratios of HA and CS were fabricated and assessed using X-ray diffraction (XRD), Fourier transmission infrared reflectance (FT-IR), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) techniques. The effect of variation of ratios between HA and CS on mechanical properties, microstructure and in vitro study was studied. The results proved that the mechanical properties were enhanced with increasing the CS ratio in the composite. In vitro study proved the formation and nucleation of apatite onto composites surfaces which contain low content of CS after one week of immersion. Finally, it is concluded that the HACS composites containing high HA content at the expense of CS content will be promising for bone substitute’s applications, especially in load bearing sites.     

Fabrication and characterization of interconnected porous biodegradable poly(ε-caprolactone) load bearing scaffolds

In this study, poly(ε-caprolactone) (PCL)/poly(ethylene oxide) (PEO) (50:50 wt%) immiscible blend was used as a model system to investigate the feasibility of a novel solventless fabrication approach that combines cryomilling, compression molding and porogen leaching techniques to prepare interconnected porous scaffolds for tissue engineering. PCL was cryomilled with PEO to form blend powders. Compression molding was used to consolidate and anneal the cryomilled powders. Selective dissolution of the PEO with water resulted in interconnected porous scaffolds. Sodium chloride salt (NaCl) was subsequently added to cryomilled powder to increase the porosity of scaffolds. The prepared scaffolds had homogeneous pore structures, a porosity of ~50% which was increased by mixing salt with the blend (~70% for 60% wt% NaCl), and a compressive modulus and strength (ε = 10%) of 60 and 2.8 MPa, respectively. The results of the study confirm that this novel approach offers a viable alternative to fabricate scaffolds.     

Large-scale and shape-controlled synthesis and characterization of nanorod-like nickel powders under microwave radiation

The nanorod-like nickel powders were fabricated via hydrothermal liquid phase reduction route under microwave irradiation with hydrazine hydrate as a reducing agent as well as polyvinyl alcohol as a dispersant and/or structure directing agent. The morphology and structure of as-prepared products could be easily tuned by adjusting process parameters such as pH value and microwave irradiation time. The resulting materials were characterized by X-ray diffraction (XRD), scanning electron microscope, transmission electron microscopy and selected-area electron diffraction (SAED). The results demonstrated that pure nickel powders with face-centered cubic (fcc) structure were prepared at relatively mild condition and no characteristic peaks of nickel oxide in the XRD pattern were found. The phenomenon of lattice expansion for Ni powders was explained in details according to the XRD theory. As-prepared Ni sample was of obvious shape anisotropy with length diameter ratio of 5. Magnetic measurements shown that the magnetic properties of nanorod-like (fcc) Ni powders were quite different from those of hexagonal closed-packed (hcp) Ni nanoparticles. Furthermore, it had more strong ferromagnetic properties than that of Ni powders both bulk and nanoparticles.     

Synthesis and Characterizations of Nanocrystalline WC-Co Composite Powders by a Unique Ball Milling Process

In order to explore the high efficiency of fabricating nanocrystalline WC-Co composite powders, this paper presented a unique high energy ball milling process with variable rotation rate and repeatious circulation, by which nanocrystalline WC-10Co-0.8VC-0.2Cr3C2 (wt pct) composite powders with mean grain size of 25 nm were prepared in 32 min, and the quantity of the powders for a batch was as much as 800 grams. The as-prepared powders were analyzed and characterized by chemical analysis, X-ray diffraction (XRD), transmission electron microscopy (TEM) and differential thermal analysis (DTA). The results show that high energy ball milling with variable rotation rates and repeatious circulation could be used to produce nanocrystalline WC-Co powder composites with high efficiency. The compositions of the powders meet its specifications with low impurity content. The mean grain size decreases, lattice distortion and system energy increase with increasing the milling time. The morphology of nanocrystalline WC