Fabrication of YBa2Cu3Ox superconductor using Y2BaCuO5, BaCuO2 and CuO

YBa₂Cu₃O _x superconductor was synthesized using Y₂BaCuO₅, BaCuO₂, and CuO powder mixture. Reaction temperatures were identified using differential thermal analysis (DTA) and thermogravimetry (TG) for syntheses of precursor powders and the powder mixtures. Appropriate reaction temperatures for Y₂BaCuO₅ and BaCuO₂ precursor powders were 950 and 930°C, respectively. Two endothermic reactions involving melt formations were identified on the DTA and TG curves of the powder mixture, and the liquid increased the reactivity of the YBa₂Cu₃O _x formation. Powder mixture samples were sintered at various temperatures ranging from 880 to 1000°C. Microstructural and X-ray powder diffraction studies showed YBa₂Cu₃O _x and impurities to be formed in the samples sintered at various temperatures. The samples sintered at 990 and 1000°C showed dense microstructures. The critical temperature was 84 K for the sample sintered at 880°C and rose to 92 K as the sintering temperature increased.     

Phase transformations of Ni-15 wt.% B powders during mechanical alloying and annealing

The formation of Ni-B binary intermetallic compounds was investigated by mechanical alloying (MA) of the Ni-15 wt.% B (≈ Ni-48 at.% B) powder mixture and subsequent heat treatment. It was found that an interstitial Ni(B) solid solution was formed at the early stage of milling, followed by the formation of Ni₃B intermetallic compound after 25 h of milling. On further milling, the Ni₃B transformed to Ni₂B and o-Ni₄B₃ (orthorhombic). Phase transformation during heating of Ni(B) solid solution phase up to 800 °C could be represented by Ni(B) → Ni₃B → Ni₂B. Other intermetallics can be formed by heat treatment of Ni(B) solid solution at temperatures above 800 °C.     

Effect of high energy ball milling on the displacement reaction in particulate reinforced Al–Si–Cu alloy matrix composite powders

The displacement reaction between Al and SiO₂ in an Al–3wt%Cu–3wt%Si–9wt%SiO₂ powder mixture has been studied when the mixture had been ball-milled, and compared with the reaction in the as-mixed powder. Diffusion couples consisting of Al/SiO₂ were formed during ball milling. The size of the composite powder particles and the diffusion couples was reduced by increasing the ball milling time. Differential thermal analysis and X-ray diffraction results showed that the displacement reaction between Al and SiO₂ did not occur in the as-mixed powder, but occurred in the as-milled powders in the temperature range of 640–680 °C. Furthermore, the onset temperature of the displacement reaction shifted to lower temperatures after increasing the ball milling time. On the basis of these results the milled powder was sintered at 640 °C in order to produce an Al–Cu–Si matrix composite reinforced with homogeneously distributed submicron-sized Al₂O₃ particles. This is much lower than the temperature required for the same reaction in other processes which are used to produce such composites, such as the melting infiltration process.     

Novel synthesis of TiN fine powders by nitridation with ammonium chloride

TiN fine powders were prepared by the reaction of TiH₂ with ammonium chloride at various temperatures under a flow of N₂/H₂ mixed gas. In a temperature range of 500-800°C, the powder samples obtained had a particle size of 3-20 nm, and a specific surface area of 30-60 m²/g. The particle size increased with the increase of the reaction temperature. The lattice parameters and the chemical analysis data showed that the TiN powder had the stoichiometric composition. The TiN powder prepared at temperatures of 600-800°C showed superconductivity with a transition temperature of 4.0-4.5 K.     

Polymorphic transformation and powder characteristics of TiO2 during high energy milling

Many studies have indicated that the reactivity of reactants can be enhanced greatly by mechanical activation through high energy ball milling. To understand this enhanced reactivity, the polymorphic transformation and the evolution of the powder characteristics of TiO₂ and graphite mixtures during high energy ball milling was investigated using various analytical instruments. It was found that polymorphic transformation of anatase to srilankite and rutile took place during milling. Furthermore, amorphization of crystalline phases and crystallization of the amorphous phase occurred at the same time during milling. High energy milling also led to ultrafine crystallites, large specific surface areas, and substantial amounts of defects in the powder particles. Effects of the graphite addition and the milling temperature on the polymorphic transformation and the evolution of the powder characteristics were also investigated. It was proposed that the polymorphic transformation of TiO₂ during milling could be explained in terms of the temperature-pressure phase diagram if the temperature rise and high pressure at the collision site were taken into consideration.     

Mechanochemical Synthesis of Magnesium Aluminate Spinel in Oxide-Hydroxide Systems

This work presents results of the mechanochemical pretreatments of binary mixtures of hydroxides and oxides of Mg and Al powders (activated in the energy-intensive planetary ball mill for 10 h). The effect of mechanical activation on the conversion to MA spinel and on the solid-state synthesis in the temperature range 600–1200°C has been investigated. Structural changes, as a consequence of milling, were followed by X-ray diffraction analysis and the degree of conversion to spinel was determined by chemical analysis, by leaching of the products of synthesis. The aim of the intensive milling of powdery mixture has been to achieve so-called "soft" mechanical synthesis or, at least, of a partial chemical reaction, and thus, to initiate the high-temperature solid-state synthesis of MA spinel at a lower temperature than 1400°C. Pure MA spinel was prepared by synthesis of these mechanochemically activated powders at a low temperature as 1000°C. The obtained results indicate that high-energy ball milling can effectively decrease the synthesis temperature.     

Synthesis of TiC by controlled ball milling of titanium and carbon

Titanium and carbon powder mixtures with compositions of Ti_100−x C _x (x = 50, 40, 30) were milled under a helium atmosphere using a magneto ball mill. Controlled ball milling was performed in a higher energy impact mode and a lower energy shearing mode. For Ti₅₀C₅₀ and Ti₆₀C₄₀ powder mixtures milled in impact mode, TiC was formed via a mechanically-induced self-propagating reaction (MSR). When milling Ti₇₀C₃₀ in impact mode, the reaction to form TiC proceeded gradually as milling progressed; indicating that, for milling conditions that lead to the formation of TiC via MSR, a minimum carbon content is required to sustain the self-propagating reaction to form TiC. Milling in shearing mode resulted in the gradual formation of TiC during milling. This study found that increasing the carbon content of the starting powder mixture slowed the milling process. Replacing the activated carbon starting powder with high purity graphite was found to have little effect on the ignition time; indicating that the slowing of the milling process is not due to graphite acting as a lubricant during milling. Rather, this slowing of the milling process is most likely due to an increased carbon content resulting in an increase in the volume of the powder mixture. This would have a similar effect during milling to decreasing the ball:powder weight ratio (BPR), which is known to slow the milling process.     

Carbothermal synthesis of TiB<Subscript>2</Subscript> powders of micron size

The characteristic details of the carbothermal synthesis of TiB₂ powders from the stoichiometric mixture TiO₂–H₃BO₃–C at temperatures lower 1700 K are investigated using thermal analysis (ТG—thermogravimetry and DSC—differential scanning calorimetry), as well as X-ray diffraction and scanning electron microscopy. In the temperature interval 300 K → 1673 K → 1273 K and at a heating rate of 10 K/min, the reaction in the powder mixture begins at approximately 1300 K and ends at 1470 K during cooling. After 3 h of isothermal synthesis at 1473 K, the TiB₂ yield is more than 90%. The resulting products are hexagonal plate-like crystals 5–10 μm across with thickness of 3 to 4 μm. Kinetic analysis showed that in the temperature range of 1330 to 1673 K the TiB₂ synthesis reaction is of the first-order, and the calculated activation energy of the process is 315 ± 24 kJ/mol.     

Preparation of superconducting YBa2Cu3O7−x powders by a solution technique

Bulk superconducting YBa₂Cu₃O_7–x powder has been synthesized by a solution technique using a mixture of Ba-ethylenediaminetetra-acetic acid (EDTA) and [Y, Cu]-citric acid complexes. A light-blue, molecular-level, homogeneously mixed precursor was prepared, and transferred to powder form through vacuum drying. The vacuum-dried powder was decomposed at 800 °C for 4 h under flowing oxygen, then heat treated at high temperature from 850 to 950 °C for 6–12 h. The results ofT _c measurements and X-ray analysis show that the orthorhombic, superconducting phase can be formed at temperatures above 850 °C following low-temperature annealing. A sharp transition (T2 K) and high density can be achieved after 930 °C heat treatment. The 930 °C heat treated sample shows aJ _c value of 510 A cm^–2. It is concluded that this solution technique provides better stoichiometric control and lower reaction temperature than the conventional solid-state sintering process.     

Role of intensive milling in mechano-thermal processing of TiAl/Al2O3 nano-composite

In this research a nano-composite structure containing of an intermetallic matrix with dispersed Al₂O₃ particles was obtained via mechanical activation of TiO₂ and Al powder mixture and subsequent sintering. The mixture has been milled for different lengths of time and then as a subsequent process it has been sintered. Phase evolutions in the course of milling and subsequent sintering of the milled powder mixture were investigated. Samples were characterized by XRD, SEM, DTA and TEM techniques.The results reveal that the reaction begins during milling by formation of Al₂O₃ and L1₂ Al₃Ti and further milling causes partial amorphization of powder mixture. DTA results reveal that milling of the powder mixture causes solid state reaction between Al and TiO₂ rather than liquid–solid reaction. Also, it was observed that the exothermicity of aluminothermic reduction is reduced by increasing the milling time and the exothermic peak shifts to lower temperatures after partial amorphization of powder mixture during milling. Phase evolutions of the milled powders after being sintered reveal that by increasing the milling time and formation of L1₂ Al₃Ti in the milled powder, intermediate phase formed at 500 °C changes from D0₂₂ Al₃Ti to Al₂₄Ti₈ phase.     

Mechanosynthesis mechanism of TiC powders

Abstract

During ball milling of a powder mixture of elemental titanium and graphite, TiC is synthesised by a combustion reaction. The factors controlling the reaction kinetics have been investigated using X-ray photoelectron spectroscopy and differential thermal analysis. In the incubation period before a combustion reaction, the carbon atoms diffuse along the grain boundaries of Ti, resulting in the mixing of the reactants on a nanometre scale. A transitional bonded state (Ti … C) is formed, reducing the ignition temperature for a combustion reaction. In addition, a minimum adiabatic temperature of 1800 K is necessary for the occurrence of combustion during the mechanosynthesis process.     

Effects of stearic acid on synthesis of nanocomposite WC–MgO powders by mechanical alloying

The effects of stearic acid as a process control agent (PCA) on the synthesis of WC–MgO by mechanical alloying have been investigated. 0–2.0 wt% of stearic acid is added into the mixture of WO₃, Mg, and graphite powders in high-energy planetary ball milling experiments, and the as-milled powders are characterized by XRD and TEM. Results show that the mechanochemical reaction among WO₃, Mg, and graphite to form WC–MgO can be changed from a mechanically induced self-propagating reaction (MSR) to a gradual reaction by the addition of stearic acid in the range from 1.2 to 1.8 wt%, when other milling parameters are maintained at the same level. It has also been found that with the addition of stearic acid, the crystallite and particle size of WC–MgO powders can be refined, the homogeneity of particle size can be improved and the powder yield can be increased.     

Formation mechanism of titanium silicide by mechanical alloying

The syntheses of five titanium silicides (Ti₃Si, TiSi₂, Ti₅Si₄, Ti₅Si₃, and TiSi) by mechanical alloying (MA) have been investigated. Rapid, self-propagating high temperature synthesis (SHS) reactions were involved in producing the last three materials during room temperature high-energy ball-milling of elemental powders. Such reactions appeared to occur through ignition by mechanical impact in the fine powder mixture formed after a critical milling period. From in-situ thermal analyses, each critical milling period for the formation of Ti₅Si₄, Ti₅Si₃, and TiSi was observed to be 22, 35.5 and 53.5 minutes, respectively. However, the formation of Ti₃Si and TiSi₂ did not occur even after 360 minutes of milling of as-received Ti and Si powder mixture, due to the lack of homogeneity of the powder mixture. Other ball-milling procedures were employed for the syntheses of Ti₃Si and TiSi₂ using different sizes of Si powder and milling medium materials. Ti₃Si was synthesized by milling a Ti and 60 minutes premilled Si powder mixture for 240 minutes. -TiSi₂ and TiSi₂ were produced by high energy partially stabilized zirconia (PSZ) ball-milling for 360 minutes in a steel vial followed by jar-milling of a Ti and 60 min premilled Si powder mixture for 48 hr. The formation of Ti₃Si and TiSi₂ occurs through a slow solid state diffusion reaction, and the product(s) and reactants coexist for a certain period of time. The formation of titanium silicides by MA and the reaction rate appeared to depend on the homogeneity of the powder mixture, milling medium materials, and heat of formation of the product involved.     

Synthesis and Characterization of CuNi Magnetic Nanoparticles by Mechano-Thermal Route

In the present investigation, Cu_0.5Ni_0.5 nanoparticles were synthesized using high energy ball milling of a mixture of Cu₂O, NiO, and graphite powders. The mixture of powders was milled up to 50 h. The 30 h milled sample was heat treated at various temperatures for 1 h in a vacuum tube furnace. The effects of milling time and heat treatment temperature on the powder particle characteristics were studied employing X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), differential thermal analysis (DTA), and vibrating sample magnetometer (VSM) techniques. XRD results indicated incomplete formation of Cu_0.5Ni_0.5 after 30 h of milling. Further heat treatment at 500 ^°C led to the formation of a single phase Cu_0.5Ni_0.5 powder. FESEM and TEM images of the heat treated sample showed spherical Cu_0.5Ni_0.5 nanoparticles with a mean particle size of 15 nm. Magnetic properties data measured by VSM of the above sample are correlated well with the XRD results. Coercivity and saturation magnetization have been approximately achieved at 25 Oe and 18 emu/g, respectively.     

Chemical reaction assisted transient liquid phase bonding of alumina in combination with cold isostatic pressing

Abstract

A new method of transient liquid phase (TLP) bonding of alumina specimens has been developed using a mixture of aluminium powder and silica powder as insert materials. A chemical reaction of aluminium with silica occurs in the inter layer to produce alumina and silicon. Some of the specimens were subjected to cold isostatic pressing (cipping) before bonding to improve the bonding strength. Specimens with an interlayer of powder mixture were joined for Al/SiO₂ ratios of 1 : 0.84 and 1 : 0.42, but did not join for an interlayer with a theoretical ratio of 1 : 1.67. When specimens were subjected to cipping before bonding, bonds were far stronger than bonds without cipping in a temperature range from room temperature to elevated temperatures above the melting point of aluminium. In the mechanical test (bending test), fracture occurs at the boundary between the alumina matrix and the interlayer at room temperature, and in the interlayer at temperatures above the melting point of aluminium.     

Synthesis reactions of Cr2AlC from Cr-Al4C3-C by pulse discharge sintering

The reaction process of ternary compound Cr₂AlC synthesis was studied. Powder mixture of Cr, Al₄C₃ and graphite at the composition of Cr:Al:C = 2:1.1:1 was processed by pulse discharge sintering in vacuum in the temperature range of 850 to 1350 °C. The synthesized materials were analyzed by X-ray diffraction (XRD) and scanning electron microscopy (SEM) equipped with an energy dispersive spectrum (EDS) system. It was found that the amount of Cr₂AlC phase increased significantly in the temperature range of 950 to 1150 °C at the consumption of Cr and Al₄C₃ as well as an intermediate phase Cr₂Al. Predominantly single-phase Cr₂AlC with small amount of Cr₇C₃ was obtained as the sintering temperature is above 1250 °C. It is presumed that Cr₂AlC phase is formed near Al₄C₃ particle by the diffusion of Cr and the reaction of the diffused Cr with Al₄C₃.     

Mechanical milling of fullerene with carbide forming elements

Mechanical alloying of Ti, V, Cr, Mo and W with fullerene (C₆₀(C₇₀)) and graphite reveals that fullerene is more reactive than graphite. The formation heat of carbide is the driving force for reaction in the mechanical alloying process. Higher heat of formation results in the direct formation of carbide in Ti-C systems, and the formation of carbide in V-C systems during the subsequent heating of milled powder. In the systemsc with lower carbide heat of formation, a mixture of metal with carbon is obtained by ball milling. No carbide was obtained even after heating the milled powders up to 973 K. Small amount of fullerene remained when milled with Mo and W for 10 hours.     

Al-V-graphite interface reactions: an XAFS study of the reactions in a composite interface system

The high temperature reaction properties of a metal matrix composite interface have been observed in this research by X-ray reflectivity and X-ray absorption fine structure (XAFS) coupled to Auger electron spectroscopy (AES). This study was taken from the vantage point of the vanadium diffusion barrier interfacial layer in a model aluminum-graphite metal-matrix laminate composite. The interfacial couple of aluminum and vanadium was analysed to ascertain the reaction species at temperatures between 200 and 350 °C. X-ray reflectivity and glancing angle XAFS showed that the initial Al-V reaction occurred at 325 °C where the aluminum-rich intermetallic Al₃V formed. Small angle XAFS was used to analyse the higher temperature interfacial changes in the temperature range of 300–500 °C. Further interactions occurred at 500 °C, where interdiffusion of Al, C and O occurred leading to phase formation of the vanadium, dependent on the graphite basal plane orientation. AES, used to determine the initial compositions and those resulting from the high temperature heat treatments, complemented the XAFS results.     

Difference in carbo-thermal reduction reaction kinetics of NiO in microwave E- and H-fields

A powder mixture of NiO and graphite was heated in a single mode-microwave (MW) applicator at 2.45 GHz for carbo-thermal reduction of NiO. The specimen was placed in the wave guide at maximum positions of either electric (E) field or magnetic (H) field and kept at a constant temperature.A tendency was observed that the reduction rate at 600 °C was larger in the H-field than in the E-field. Considering the fact that NiO can be heated only in the E-field, while graphite can be heated in both fields, graphite particles in the powder mixture might be selectively heated in the H-field. Hence, it is postulated that a microscopic temperature gradient is formed more in the H-field, which caused the gas convection, then the mass transfer and the gas-solid reaction is enhanced, so the enhanced reduction kinetics resulted, eventually.     

A study on NiAl produced by pressure-assisted combustion synthesis

The production of intermetallic compound was carried out in an electrical resistance furnace in open air under 150 MPa uniaxial pressure at 1050 °C for 1 hour using aluminum powder with 15 μm size and Carbonyl-nickel powder with 4-7 μm size having 99% and 99.8% purity, respectively. The formation temperature of intermetallic compound was determined by Differential Scanning Calorimeter analysis, and exothermic reaction of powder mixture was determined to occur at 655 °C. Optical microscope, scanning electron microscopy and X-ray diffraction analysis were used to characterize produced samples. These samples consist of single phase NiAl with very low porosity. Based on the Archimedes' principle, the relative density of the samples was 99.6%. The microhardness of the samples was approximately 367 ± 17 HV_1.0. It was observed that NiAl intermetallic exhibited good oxidation resistance at high temperatures in open atmosphere. The distribution of alloying elements within intermetallic compound was determined by energy-dispersive X-ray spectroscopy.