Microstructural evolution of Cu–Nb oxide nanocomposite alloys during ball milling is investigated using a two-step ball-milling approach. In the first step, Cu and Nb powders are milled to create a two-phase alloy comprising a Cu-rich matrix containing a high density of 20- to 30-nm Nb precipitates. In the second step, this nanocomposite is co-milled with CuO, resulting in the reduction of CuO and the oxidation of the Nb nanoprecipitates. Transmission electron microscopy characterization shows that three distinct types of Nb oxide precipitates evolve at different levels of strain. First, nanocrystalline NbO particles (∼10 nm) are formed by dissolved Nb in Cu reacting with oxygen evolved from the CuO. Next, the Nb nanoprecipitates in Cu further reduce CuO to form Nb/Nb oxide and NbO/Nb oxide core–shell inclusions (20–30 nm). These inclusions coalesce during additional milling to form amorphous Nb oxide agglomerates (>700 nm after 50 h). The growth of Nb precipitates during step-one milling, the initial growth of NbO nanoparticles, and the formation of core–shell Nb oxide precipitates during step-two milling are attributed to the convective transport of atoms and clusters combined with shear-induced agglomeration.

An initial mixture of raw materials (batch) typically used for the manufacture of conventional soda-lime float glass was subjected to a mechanical activation process for 30 or 60 minutes in a planetary ball mill. An intensification of the chemical reactivity of the batch, which was directly related with the increase in the milling time, was observed. This accelerated the chemical reactions that took place during the batch melting process between sodium, calcium and magnesium carbonates and other components of the mixture, which happened at significantly lower temperatures with respect to the batch without mechanical activation. The heat of fusion of the batch, estimated using a methodology previously reported in the literature, indicated that the mechanical activation given to the initial mixture of raw materials decreased the energy consumed during the batch melting. This was also evidenced by a decrease in the temperature at which the release of CO2 ended, which was considerably larger than that previously reported in the literature based solely on the decrease in the particle size of a batch of similar composition achieved by dry sieving.

We present a fast method to prepare hybrid materials of polyaniline (PAni) with carbon nanotubes (CNTs, both undoped and nitrogen-doped) by ball milling without solvents or strong oxidants. PAni forms nanoparticles, attached to CNTs in a nanocomposite structure, with the nanotubes well dispersed among the polymer. This is achieved with only a few minutes of ball milling. Raman spectroscopy confirms that PAni was synthesized in its conductive state and suggests a good CNT–PAni interaction, particularly with nitrogen-doped CNTs. We found that water increased polymer yield, which we optimized, together with the nanocomposite conductivity, as function of amount of water and of oxidant (FeCl3). The nanocomposite conductivity is four orders of magnitude higher than that of PAni, for both types of nanotubes. Scanning electron microscopy and X-ray diffraction both show negligible damage to the CNT during this mechanosynthesis procedure, while dry milling and milling CNT in water without aniline does damage nanotubes, indicating that the reaction absorbs most of the mechanical energy.

Recent research has demonstrated that ternary aluminum-boron-iodine (Al-B-I2) materials prepared by mechanical milling are effective in generating biocidal combustion products. Such reactive materials are of interest for the munitions aimed to defeat stockpiles of biological weapons. In this research, ternary Mg∙B∙I2 composites were synthesized using two-stage milling. The first stage consisted of a binary B∙I2 powder prepared by mechanical milling, followed by addition of magnesium for iodine stabilization. Specific compositions for each ternary material were varied. Stability of the samples was assessed by their heating in argon at a constant rate using Thermo Gravimetric Analysis (TGA) and observing weight loss. Oxidation of the prepared powders was also studied by TGA. Ternary Mg∙B∙I2 composite powders prepared by two-stage milling were more stable than any of the previously prepared iodine-bearing materials with the same concentration of iodine (20 wt %). Particle size distributions were measured using low-angle laser light scattering. Powders were ignited using in an air-acetylene flame and in a constant volume explosion apparatus. Particle burn times and temperatures were measured optically. Substantially longer burn times and lower temperatures were observed for the prepared materials compared to the reference pure Mg powder.

Lithium ion batteries are becoming more important because of their high energy density and design flexibility. The capacity of these batteries is usually cathode limited; so, it follows that increasing the capacity of the cathode is essential to raise the performance of such batteries. In this work, fractal dimension study is used to understand the behavior of a Li2TiO3 made by mechanical milling, as a way to improve their uses in energy storage. Digital image analysis allows the study of fractal dimension; X-ray, Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) analysis were used to analyze changes on the surface of samples from the current results the distinctive characteristics of the surfaces for each sample may be obtained, making it possible to predict a future behavior of the samples. MATLAB software FRACLAB 2.03 developed by INRIA was used as a tool.

Highly ion-conductive Li6PS5Cl Li-argyrodites were prepared through a high energy ball milling. Electrical and electrochemical properties were investigated. Ball-milled compounds exhibit a high conductivity of 1.33×10−4 S/cm with an activation energy of 0.3-0.4 eV and an electrochemical stability up to 7V vs. lithium. These results are obtained after only 10 hours of milling and with no additional heat treatment.

To validate the use of the Li6PS5Cl-based solid electrolyte, all-solid-state batteries using LiCoO2 and Li4Ti5O12 as active material have been realized. The optimization of the electrode composition led to a maximum of 46 and 27 mAh per gram of composite for LiCoO2 and Li4Ti5O12-based half-cells respectively. The assembled all-solid-state LiCoO2 / Li6PS5Cl / Li4Ti5O12 battery presents a sustainable reversible capacity of 27 mAh per gram of active material and a coulomb efficiency close to 99%.

Adding aluminum to propellants, pyrotechnics, and explosives is a common way to boost their energy density. A number of approaches have been investigated that shorten aluminum ignition delay, increase combustion rate, and decrease the tendency of aluminum droplets to agglomerate. Previous work showed that particles of mechanically alloyed Al-Mg powders burn faster than similarly sized particles of pure aluminum. However, preparation of mechanically alloyed powders with particle sizes matching those of fine aluminum used in energetic formulations was not achieved. This work is focused on preparation of mechanically alloyed, composite Al-Mg powders in which both internal structures and particle size distributions are adjusted. Binary powders with compositions in the range of 50 - 90 at. % Al were prepared and characterized. Milling protocol is optimized to prepare equiaxial, micron-scale particles suitable for laboratory evaluations of their oxidation, ignition, and combustion characteristics. Quantitative particle size analyses are done using low-angle laser light scattering. Electron microscopy and x-ray diffraction are used to examine particle morphology and phase makeup, respectively. Combustion of aerosolized powder clouds is studied using a constant volume explosion setup. For all materials, ignition and combustion characteristics are compared to each other and to those of pure Al. Compositions with improved performance (i.e., shorter ignition delay and faster pressurization rate) compared to pure Al are identified.

In this paper, efficacy of p-n junction p-CuO/n-ZnO composite is assessed as a potential photocatalyst by monitoring degradation of methylene blue (MB) in the presence of UV light. The p-n junction photocatalyst, p-CuO/n-ZnO, was prepared by ball milling of ZnO and CuO in water. The structural properties of p-CuO/n-ZnO composite were characterized by x-ray diffractometer and surface charge properties via zeta potential measurement. The degradation of MB in the presence of composite powder was monitored via UV-vis spectrometer. Various studies affecting the degradation rate of MB were conducted as a function of weight fraction of CuO in the composite and ball milling time. The highest degradation rate of MB was achieved in CuO (10 Wt.%)/ZnO for which high negative zeta potential was recorded. The MB degradation efficiency was found to decrease with the samples ball milled for time longer than 12 hours due to increased agglomeration of particles. The mechanisms that influence the photocatalytic activity of p-CuO/n-ZnO are discussed based on the p-n junction principle.

Single-phase samples of YCrxFe1−xO3 were synthesized by a mechanochemical method. X-ray diffraction data show linear reduction in the lattice parameters of YCrxFe1−xO3 perovskites with the Cr content, indicating that Cr ions substitute for Fe ions to form a solid solution. Magnetic measurements show hysteresis loops at 5K. The substitution of Cr for Fe enhances the magnetization for up to x=0.33 Cr doping level. For higher doping levels, 0.33<x<1, the system behaves as a frustrated system. At x=1, YCrO3 behaves as a week ferromagnet with TN ~140 K. The chloride salt based machenochemical method offers simple synthesis route for the synthesis of pure multiferroic compounds.

Atom probe tomography is used to investigate the clustering of Y-Ti-O in a 14%Cr-2%W-0.3%Ti & 0.3% Y2O3 ODS steel. The clusters in the consolidated material are compared to clusters observed in the powder prior to consolidation. A higher density of smaller clusters is observed in the powder, and the clusters are found to contain more O and less Y.

A solid state mechanochemical reaction (MCR) method for synthesizing AlN powder with aluminum and melamine powders as the reactants was proposed and put into practice. It was found that the solid state MCR between aluminum and melamine is an instantaneous and exothermic reaction. For a certain charge ratio, a critical ball milling time is needed for the MCR to occur. The higher the charge ratio, the faster the MCR. Cryogenic environments help to accelerate the MCR between Al and melamine. In addition to the direct one-step MCR synthesis approach mentioned above, AlN powder can also be synthesized by pre-ball-milling Al and melamine powders followed by heat treatment. Using this two-step approach, the heat treatment temperature is only about 638 °C, which is much lower than that used in other ways for synthesizing AlN powder. The lower heat treatment temperature can be attributed to the combined effect of both the adoption of melamine and the high reactivity of powders caused by ball milling. Comparatively, the present solid state MCR method for synthesizing AlN powder may be more cost-effective and hence more promising to be used to industrially produce both AlN powder and in situ AlNP reinforced aluminum matrix composites.

Zr0.5Hf0.5Ni0.8Pd0.2Sn0.99Sb0.01 composites with various concentrations of WO3 inclusions were synthesized by mechanical alloying using high energy shaker mill. High density hot pressed pellets of the synthesized materials were characterized using powder X-ray diffraction and transmission electron microscopy and their thermoelectric properties were investigated in the temperature range from 300 to 750 K. The electrical conductivity of the composites at 300 K decreases from 2500 S/cm for 0 wt.% WO3 alloy to 2200 S/cm for the composite with 2 wt.% WO3 inclusion. The electrical conductivity of composites containing 5 wt.% and 10 wt.% WO3 inclusions showed sharp increases with increasing WO3 content. The electrical conductivity of the composites monotonically decreases with rising temperature. All samples showed n-type semiconducting behavior and the thermopower values decrease with increasing WO3 content. The lattice thermal conductivity of the composites increases with increasing WO3 content. However, these values are about 30% lower than that of Zr0.5Hf0.5Ni0.8Pd0.2Sn0.99Sb0.01 alloy prepared by high temperature solid-state techniques. The synthesized composites showed lower figure of merit than the half-Heusler matrix due to large reduction in the thermopower values with increasing WO3 content.

Yb14MnSb11 is a very promising thermoelectric material for high temperature applications. This compound is a member of a large family of Zintl phases with a “14-1-11” A14MPn11 stoichiometry (Pn = P, As, Sb, Bi; A = Ca, Ba, La, Sr, Yb, Eu; M = Mn, Al, Cd, Ga, In, Nb, Zn). Yb14MnSb11 exhibits low lattice thermal conductivity values and a p-type semimetallic behavior with values of the non-dimensional figure of merit zT peaking at 1.4 above 1200 K. There is significant interest in investigating how substitutions on any of the atomic sites impact the charge carrier concentration and mobility, band gap and lattice thermal conductivity. Recent reports have studied substitutions on the Yb and Mn sites with the goal of reducing hole carrier concentration and improving carrier mobility values.

High energy ball milling has been shown to be a convenient method of synthesis to prepare Yb14MnSb11 and it has been used here to explore the solid solution systems derived from this compound by substituting Sb with Bi. High energy ball milling is a non-equilibrium process and not all of the 14-1-11 compounds are easily formed with this method. Characterization of the synthesized compositions was done by X-ray diffraction, electron microprobe, and high temperature measurements of the electrical and thermal transport properties up to 1275 K. The experimental results on undoped and doped solid solution samples are compared to that of pure Yb14MnSb11 samples prepared by the same high energy ball milling technique.

Light element complex hydrides (e.g. NaBH4) together with metal hydrides (e.g. MgH2) are considered two primary classes of solid state hydrogen storage materials. In spite of drawbacks such as unfavourable thermodynamics and poor kinetics, enhancements may occur in reactive hydride composites by nanostructuring of reactant phases and formation of more stable product phases (e.g. MgB2) which lower overall reaction enthalpy and allow reversibility. One potential system is based on mixing NaBH4 and MgH2 and subsequent ball milling, which in a 2:1 molar ratio can store considerable amounts of hydrogen by weight (up to 7.8 wt%). A study of the 2NaBX4 + MgX2 → MgB2 + 2NaX + 4X2 (X=D,H) reaction is assessed by means of in-situ neutron diffraction with different combinations of hydrogen and deuterium on the X position. The desorption is established to begin at temperatures as low as 250 °C, starting with decomposition of nanostructured MgX2 due to joint effects of nanostructured MgX2 and its reducing effect at NaBX4. Analyses of background profile, due to the high incoherent neutron scattering of hydrogen, as a function of temperature demonstrate direct correlation of H/D desorption reactions with relative phases amount.

Mg-Li-Al alloy was prepared by ingot casting and then underwent subsequent reactive ball milling. A Mg-Li-Al-H complex hydride was obtained under a 0.4 MPa hydrogen atmosphere at room temperature, and as high as 10.7 wt% hydrogen storage capacity was achieved, with the peak desorption temperature of the initial step at approximately 65 °C. The evolution of the reaction during milling, as well as the effect of Li/Al ratio in the raw materials on the desorption properties of the hydrides formed, were studied by x-ray diffraction and simultaneous thermogravimetry and differential scanning calorimetry techniques. The results showed that mechanical milling increases the solubility of Li in Mg, leading to the transformation of bcc β(Li) solid solution to hcp α(Mg) solid solution, the latter continues to incorporate Li and Al, which stimulates the formation of Mg-Li-Al-H hydride. A lower Li/Al ratio resulted in faster hydrogen desorption rate and a greater amount of hydrogen released at a low temperature range, but sacrificing total hydrogen storage capacity.

We show a drastically improved gas–solid reaction between NH3 and LiH by mechanical treatment for LiH, generating a hydrogen gas even at room temperature. The results of x-ray photoelectron spectroscopy showed that the mechanical pretreatment was effective in reducing a hydroxide phase from the surface of LiH. It was also possible to successfully recycle back LiNH2, which is the byproduct of this hydrogen desorption reaction, to LiH under 0.5-MPa H2 flow at 573 K. Thus, the LiH–NH3 system provides a recyclable H2 storage system to generate H2 at room temperature with 8.1 mass% and 4.5 kg/100 L hydrogen capacity.

A set of Bragg peaks consistent with a hexagonal Bravais lattice was observed in the x-ray powder diffraction pattern of cubic pyrochlore rubidium tungstoniobate (RbNbWO6) subjected to high-energy ball milling. The calculated lattice parameters for this hexagonal phase are similar to those of compounds with tungsten bronze structure. In fact, the powder pattern of the hexagonal phase could be refined with a structural model based on the tungsten bronze structure. The hexagonal phase produced by high-energy ball milling of RbNbWO6 transforms back to the pyrochlore structure upon heating to 773 K in air. A similar phase was obtained by ball milling the mixture RbNbWO6 + WO3, but, in this case, the stoichiometric hexagonal tungsten bronze compound thus obtained remained stable up to 1273 K.

In this paper, the impurity influences of BNNTs on photoluminescence (PL) analysis have been investigated systematically. Similar PL spectra were obtained from bulk disk of the cold-pressed BNNTs and dispersed individual BNNTs deposited on CaF2 substrate. Metal impurities such as Fe and Au do not affect PL emissions of the BNNTs strongly possibly because Au doping creates sever structural damages but do not change the electronic structure.

CuInGaSe2 (CIGS) is a prominent thin-film photovoltaic material. However, commonly used physical vapour deposition and sputtering techniques used to fabricate CIGS thin-film photovoltaic (PV) devices are complex and expensive. Therefore non-vacuum deposition techniques such as paste coating, spray pyrolysis and electro deposition are gaining more attention in recent years. Our intention is to choose a low cost non-vacuum technique like mechano-chemical synthesis of CIGS powder, followed by screen printing. Mechano chemical synthesis is a process that induces physical and/or chemical change in the compounds by mechanical energy, such as pulverization, friction or compression. This method has some advantages for the mass production of CIGS solar cells, high productivity and short processing cycle time. In the present work CIGS powders suitable for screen-printing ink has been prepared by ball milling. High purity elemental copper granules (>99.9% pure), selenium and indium powders (>99.9% pure) and fine chips of gallium (>99.9% pure) were used as the starting materials. Ball milling was carried out for an optimized composition of CuIn0.75Ga0.25Se2 using a SPEX-8000 mixer/mill at 1200 rpm for 1.5 hours. X-ray diffraction analysis of the milled powder shows the presence of (112), (220)/ (204), (312)/ (116), (400) and (332) peaks corresponding to CIGS chalcopyrite structure with a preferential orientation along (112) peak. The average grain size calculated by Scherrer’s formula is about 12.24 nm. Crystallographic structure of the prepared CIGS powder was analyzed by Rietveld analysis using X-ray powder diffraction data. Geometry optimization of the structure was performed and the basic structural properties have been evaluated by density functional approximation and compared with experimental results. Density of states has been simulated for the same structure inorder to have a better understanding of the distribution of atomic orbitals. FESEM analysis shows the agglomeration of nano particles. Particle size varied from 11 to 30nm. Final composition of the milled powder studied by Energy dispersive X-ray analysis gives 24.39 at% Cu, 21.42 at% In, 7.22 at% Ga and 46.97 at% Se. HRTEM analysis reveals the presence of nano crystalline particles. The interplanar distance (d-spacing) corresponding to (112), (220)/ (204), (512)/ (417) and (620)/ (604) diffraction peaks has been estimated and compared with standard values and the corresponding diffraction pattern has been simulated with simulaTEM software. CIGS ink is prepared by proper mixing of the powder with a suitable organic binder (ethyl cellulose). Screen printing is carried out on glass substrates, followed by annealing at 5 different temperatures of 300,350,400,450 and 500 degrees, in order to form a porous CIGS film. XRD analysis was carried out to study the structure of screen printed CIGS.

Large-scale, high-density, and patterned carbon nanotubes (CNTs) on both pure Si and quartz (SiO2) substrates have been produced using different approaches. The CNTs were synthesized by pyrolysis of the ball-milled iron phthalocyanine (FePc) in a tube furnace under a Ar-5% H2 gas flow. Because patterned CNTs are difficult to grow directly on smooth and perfect single-crystalline Si wafer surface, mechanical scratches were created to help the selective deposition and growth of CNTs on the scratched areas. This simple process does not require pre-deposition of any metal catalysts. For SiO2 substrates, which can be readily covered by a CNT film, patterned CNTs are produced using a TEM grid as mask to cover the areas where CNTs are not needed. The growth temperature and vapor density have strong influence on the patterned CNT formation. The scratch areas with a special structure and a higher surface energy help the selective nucleation of CNTs.