Effect of Particle Size on Deformation and Compaction Characteristics of Ascorbic acid and Potassium Chloride: Neat and Granulated Drug

Abstract

Deformation and compaction characteristics of two soluble drugs, ascorbic acid and potassium chloride, were investigated. Five different particle size fractions of ascorbic acid with mean particle size (d₅₀) ranging from 30–300μm and four different particle size fractions of potassium chloride with d₅₀ ranging from 20–400 μm were selected in the study. The compaction behavior of the drug substances as neat drugs or as granulated drugs were evaluated on both a Carver press and an instrumented single-punch tablet press. The results clearly show that mean particle size of the drug substances plays an important role in their compactibility. Intrinsic compactibility of both drug substances was slightly improved with increased particle size. Granulations of the drugs with polyvinyl pyrrolidone significantly improved their compactibility. However, this effect was more pronounced in the drug substance with finer particle size. The Heckel plots indicate that deformation characteristics of both granulated drugs were related to their original mean particle sizes. The granulations prepared from the coarser particle size (d₅₀ 250 μm to 400 μm) underwent two stages of deformation, so-called “brittle fracture” and “plastic deformation”. While the granulations prepared from the finer particle size predoninantly underwent “plastic deformation”. The results indicated that the plastic deformation of both granulated drugs was progressively enhanced whilst fragmentation of particles was correspondingly reduced as the particle size of the drugs was decreased. Scanning electron photomicrographs indicated that the granulation process changed the surface morphology of the drug particles imparting more “microirregularities” or “defects”, thereby providing greater “interparticulate bonding” as compared with the neat drugs. Optimum particle size range of ascorbic acid and potassium chloride for satisfactory compactibility was found to be 30–40 μm and 20–40 μm, respectively. The present study demonstrates the importance of selecting the appropriate particle size of drug for the development of tablet dosage forms.     

Effect of boron carbide particle size and volume fraction of TiB–TiC reinforcement on steady state creep behaviour of PM processed titanium matrix composites

Abstract

TiB–TiC reinforced titanium matrix composites (TMCs) were synthesised through pressureless sintering of titanium and boron carbide (B₄C) powder compacts. Effect of boron carbide (B₄C) particle size and volume fraction of TiB–TiC reinforcement on steady state compression creep behaviour of composites was investigated in the temperature range of 773–873 K. The creep rates of composites are found to be about two orders of magnitude lower than those of unreinforced titanium. The creep rates further lowered with decrease in size of B₄C particles (from 16 to 3 μm) used in preparation of composites as well as with increase in volume fraction of the TiB–TiC reinforcement from 10 to 30 vol.%. By using the concept of effective stress as well as incorporation of load transfer and substructural strengthening effect produced by the reinforcement into analysis, the entire creep data of Ti and the composites can be made to merge on to a single line within a scatter band of factor of 2–3 and can be represented by a unified power-law equation.     

Design aspects of processing of aluminium 6061 based metal matrix composites via powder metallurgy

Abstract

Acceptance of metal matrix composites for industrial applications depends upon improving properties using an economic production route, which includes the processing design. Two powder metallurgical routes have been used in the manufacture of Al 6061 metal matrix composites. The first involves blending, vacuum canning, and hot pressing from prealloyed powders and the second involves blending of elemental powders, liquid phase sintering, and subsequent hot rolling. These composites comprise 7·5 or 15 vol.-% of 7, 23, or 45 μm SiC particles. In this paper, the composite microstructure at each stage of the different processing routes has been examined and the aging behaviour investigated. Effects on the tensile properties of fabrication techniques, SiC particle size, and volume fraction are presented and discussed.

MST/3020     

Effect of dual size particle distribution on processing and properties of AZ91D/SiCp magnesium matrix composites prepared by rotation cylinder method

Abstract

Spiral fluidity and hardness and wear experiments were carried out to investigate the effect of dual size (5 and 50 μ m) SiC particle distributions on the fluidity, hardness, and wear resistance of Mg - 9.1Al - 0.7Zn (wt-%) alloy containing 10 vol.-% SiC particles, with the aim of tailoring properties to specific applications. Although a decrease in the fluidity of the composites is observed, as expected, in the presence of SiC particles, the fluidity of the composites with dual size particle distributions was in some instances better than that of composites containing the same volume fraction of single size particles. The hardness and wear resistance of the composites with dual size distributions were weakly dependent on the mixing ratio. In terms of complete molten processing and tailored mechanical properties, the optimum mixing ratio of 5 and 50 μm particles appears to be 1:2.     

Sliding wear behaviour of Al-Si-Cu composites reinforced with SiC particles

Abstract

The sliding wear behaviours of an unreinforced monolithic Al-Si-Cu alloy and SiC particles reinforced composites containing 5, 13, 38 and 50 vol.-% with diameters of 5.5, 11.5 and 57μm were investigated. The results showed that the wear resistance of the composites is much higher than the monolithic alloy, and the larger and the more SiC particles, the higher the enhancement of the wear resistance. Metallographic examinations revealed that the subsurface of worn composites was composed of both fragmented particles and deformed matrix alloy. The depth of the particle fracture zone in the subsurface varied in the range of 20-35 μm at a sliding distance of 1.8 km, while the plastic deformation zone of the worn subsurface on monolithic alloy was more than 100 μm. Scanning electron microanalyses of the worn surface, subsurface microstructure and debris suggested that the depth of the particle fracture zone became smaller as the diameter of SiC particles increased. Increasing the hardness and decreasing the applied wear stress changed the debris morphology from flake to very small lumps.     

Critical reinforcement size for cavity nucleation during superplastic deformation of metal matrix composites

Abstract

A high strain rate superplastic composite Al–Cu–Mg/Si₃N_4p has been investigated to estimate the critical particle size for cavity nucleation. Specimens superplastically deformed to a strain of 0.2 at 773 K contained no liquid phase whereas those deformed at 783 K contained liquid phase. The critical particle size, i.e. the smallest size to nucleate a cavity, obtained experimentally was 0.5 µm dia. for deformation at 773 K and 0.4 µm for deformation at 783 K. The critical particle size for deformation at 773 K can be estimated accurately using Stowell's equation for critical strain rate. However, for deformation at 783 K when liquid phase was present, the predicted critical strain rate was much lower than the experimental strain rate for critical particle size for cavity nucleation. It is suggested that the actual critical strain rate was increased by an increase in diffusivity at the interfaces and grain boundaries due to the presence of liquid phase.     

Effect of alumina particle size and thermal condition of casting on microstructure and mechanical properties of stir cast Al–Al2O3 composites

Abstract

Metal matrix composites are considered as a distinct category of the advanced materials, which have low weight, high strength, high modulus of elasticity, low thermal expansion coefficient and high wear resistance. Among them, Al–Al₂O₃ composites have achieved significant attention due to their desired properties. In the present research, Al–Al₂O₃ composites with 5 vol.-% alumina were produced by stir casting at a temperature of 800°C. Two different particle sizes of alumina were used as 53–63 and 90–105 μm. The microstructure of the samples was evaluated by SEM. In addition, the mechanical properties of the samples were measured, and hence, the optimum temperature and particle size of alumina to be added to the Al matrix were determined. The results demonstrated the positive effect of alumina on improving the properties of Al–Al₂O₃ composites.     

Wear behaviour of ZnAl27/TiCp metal matrix composites under sliding conditions

Abstract

The effect of TiC content on the wear resistance of a Zn–Al alloy was investigated under 300–900 N loads. Sliding tests were carried out to study the wear behaviour of TiC_p reinforced ZnAl27 metal matrix composites (MMCs) against AISI type 1050 steel in a block on ring apparatus. The ZnAl27/TiC_p MMCs, which were prepared by the addition of 5, 10, and 15 vol.-% TiC_p, were produced by powder metallurgy, and the size of particulates was varied at 80, 20, and 5 νm. The powders were uniaxially cold compacted by increasing the pressure up to 250 MPa. Wear tests were carried out in an incremental manner, i.e. 300 m per increment and 1800 m in total. The results of these tests were used to investigate the relationship between weight loss, microstructure, surface hardness, friction coefficient, particle size, and particulate percentage. It was observed that TiC_p particulate reinforcement is beneficial in increasing the wear resistance of ZnAl27 alloy, and TiC particulates in MMCs tend to reduce the extent of plastic deformation in the subsurface region of the matrix, thereby delaying the nucleation and propagation of subsurface microcracks.     

Dynamic recrystallisation of as cast austenite in 18–8 stainless steel

Abstract

Dynamic recrystallisation behaviour of an as cast 0Cr18Ni9Ti stainless steel during hot deformation was investigated by hot compression test at a temperature range of 950–1200°C and strain rate of 5 × 10^-3–1 × 10^-1 s^-1. Change of austenite grain size owing to dynamic recrystallisation was also studied by microstructural observation. The experimental results showed that the hot deformation conditions, such as temperature, strain, and strain rate determine the dynamic recrystallisation behaviour for the as cast stainless steel, and the dynamically recrystallised grain size is determined by the deformation conditions and is independent of the strain.     

On CTE of SPS consolidated SiCp/Al composites with various particle size distributions

Abstract

The coefficient of thermal expansion (CTE) of spark plasma sintering consolidated SiC_p/Al composites with various size distributions was investigated with the combination of experimental measurements and modelling analyses. The CTE of the composites decreased with increasing particle volume fraction, and large particles played a major role in the decline of CTE. The measured CTE lay between the predictions of Kerner model and Schapery lower bound, but the possible formation of percolating particle network and the influence of matrix plasticisation led to the slight deviation of the experimental values from model predictions. A CTE peak appeared for all the composites with increasing temperature to about 250–300°C due to the action of matrix plasticisation filling the microvoids in the composites. The composites with mixed particles of substantially different sizes were prone to concentrate thermal stresses on large particles, which induced an early appearance of matrix plastic deformation that can result in a comparably low CTE peak temperature.     

Cast metal matrix composites

Abstract

Metal matrix composites have been available in certain forms for at least two decades, e.g. boron fibre reinforced aluminium and various dispersed phase alloys and cermets. Recently, a range of alumina and silicon carbide fibres, whiskers, and particles with diameters <20 μm have become available. The possibilities of incorporating these materials into metals to improve stiffness, wear resistance, and elevated temperature strength without incurring weight penalties have attracted the attention of design engineers in the aerospace and automobile industries. The aim of the present paper is to outline the manufacturing processes for such composites, in particular those based upon liquid metal technology, e.g. squeeze casting and spray forming. Some of the mechanical and physical properties which have been determined for these materials are described. An analysis of how matrix alloy selection may influence tensile and fracture behaviour of short fibre and particle reinforced composites is attempted.

MST/770     

基于同步辐射X射线的SiC颗粒/Al复合材料变形损伤

通过原位X射线成像系统研究了两种SiC粒径配比（45 μm和（45+100）μm）对70vol% SiC颗粒（SiC_P）/Al复合材料变形损伤行为的影响。在准静态压缩加载下,利用X射线数字图像相关方法（XDIC）计算了SiC_p/Al复合材料在不同变形阶段的应变场分布。宏观应力-应变曲线表明,因颗粒尺寸引起的SiC_p/Al复合材料的强度差异较小,但粒径配比为45 μm的SiC_P/Al的延展性明显优于（100+45）μm的SiC_P/Al。细观应变场分析表明,粒径配比为（100+45）μm的SiC_P/Al比45 μm的SiC_P/Al更早出现变形损伤带,且前者在变形后期其应变场不均匀性更高。这是由于（100+45）μm SiC_P/Al中更早在大颗粒附近出现应变集中点,而且这些集中点会迅速长大和汇聚进而形成宏观裂纹,导致材料更早失效和破坏。因此,减小颗粒尺寸和促进颗粒均匀分布有利于提高颗粒增强金属基复合材料的延展性。断口回收分析表明:两种颗粒尺寸的SiC_P/Al复合材料的断裂模式都属于脆性断裂,且断口中都发现有颗粒破坏和界面脱粘现象存在。      

Effect of process parameters on microstructural variables of a commercial TC6 titanium alloy disc

Abstract

The interaction between the deformation behaviour and the microstructure evolution is the main characteristic in the forging process of titanium alloy and this interaction is researched using finite element (FE) simulation. Coupled simulation of deformation behaviour with microstructure evolution has been carried out by means of a new constitutive equation presented by Li et al. (Mater. Sci. Technol., 2004, 20, 1256–1260). The effect of deformation temperature, hammer velocity,height reduction and shear factor on the microstructure variables, including grain size and volume fraction, has been studied in the forging process of the TC6 titanium alloy disc with deformation temperatures of 880–940°C, hammer velocities of 1·2–12 000 mm min^?1 and shear factor (m) of the friction of 0·1–0·4. The simulated results show that deformation temperature, hammer velocity and height reduction have a significant effect on themicrostructure evolution and this effect is more significant on the microstructure evolution in hot forging than that in isothermal forging. The simulated results are in good agreement with the experimental results.     

Hall–Petch behaviour of 316L austenitic stainless steel at room temperature

Abstract

The room temperature plastic deformation behaviour of two different batches (with differences in chemical composition) of 316L austenitic stainless steel has been studied. By thermomechanical treatments, a wide range of grain sizes varying from 2·7 to 64·0 νm was obtained in this study. The different microstructural parameters, such as grain size, distribution of grain size and shape, dihedral angle distribution, and grain aspect ratio were measured for annealed and deformed specimens of the two batches. The Hall–Petch behaviour of batch 1 showed two distinctly different linear regions, one in the fine grain size range (d≤6νm) and the other in the coarse grain size range (d6νm). The Hall–Petch parameter K _H (?) was significantly higher in the fine grain regime than coarse grain regime at all strains. Hardness measurements were also performed across the grain at different strain levels. The applicability of the Hall–Petch relationship was assessed in batch 1 and batch 2. It was observed that the Hall–Petch relationship was applicable in the coarse grain regime and Kocks composite relationship in the fine grain regime of batch 1. In batch 2 of 316L austenitic stainless steel, a single linear Hall–Petch relationship could describe the deformation behaviour over the entire range of grain size (from 2.9 to 46 νm) studied. The variation of the Hall–Petch and Kocks composite parameters with strain was discussed in terms of changes in the microstructural parameters.     

Investigation of impact behaviour of aluminium based SiC particle reinforced metal–matrix composites

In this paper, the impact behaviour of aluminium and silicon carbide (SiC) particle reinforced aluminium matrix composites under different temperature conditions was determined. Charpy impact tests were performed on as extruded and heat treated specimen at temperatures varying from −176 to 300 °C. Composite specimens based on aluminium alloys of 2124, 5083 and 6063 and reinforced by SiC particles were manufactured. Two different SiC sizes of 157 μm and 511 μm and two different extrusion ratios of 13.63:1 and 19.63:1 were used. The results of instrumented impact tests were compared with the microstructural and fractographic observations. The failure mechanisms and deformation behaviour of unreinforced alloys and composites were assessed. The impact behaviour of composites was affected by clustering of particles, particle cracking and weak matrix-reinforcement bonding. Agglomeration of particles reduced the impact strength of Al 2124 and 6063 based composites. Alumınum 6063 alloys and composites showed a better impact strength. The impact strength of 6063 composites increased with particle size and extrusion ratio. The effects of the test temperature on the impact behaviour of all materials were not very significant.     

Effect of integrated extrusion–equal channel angular pressing temperature on microstructural characteristics of low carbon steel

Abstract

In the present research, a combined forward extrusion–equal channel angular pressing was developed and executed for the deformation of a plain carbon steel. In this method, two different deformation steps, including forward extrusion and equal channel angular pressing, take place successively in a single die. The deformation process was performed at different deformation start temperatures (800, 930 and 1100°C). Three-dimensional finite element simulation was used to predict the strain and temperature variations within the samples during deformation. With microstructural observations and the results of finite element simulation, the main grain refinement mechanisms were studied at different deformation temperatures. The results show that the forward extrusion–equal channel angular pressing is effective in refining the ferrite grains from an initial size of 32 μm to a final size of ～0·9 μm. The main mechanisms of grain refinement were considered to be strain assisted transformation, dynamic strain induced transformation and continuous dynamic recrystallisation, depending on the deformation temperature.     

Improving the fracture toughness of MgO–Al2O3–SiO2 glass/molybdenum composites by the microdispersion of flaky molybdenum particles

The flake-forming behaviour of powders of molybdenum, niobium, nickel, BS 316 S 12, Ni–17Cr–6Al–0.6Y, iron, titanium and Ti–6Al–4V, using a wet ball mill, was investigated. MgO–Al₂O₃–SiO₂ (MAS) glass composites reinforced with these flaked particles were fabricated, and improvements in flexural strength evaluated. The MAS glass composites reinforced with flaky metallic particles such as molybdenum, niobium, iron, nickel and Ni–17Cr–6Al–0.6Y, showed an improvement. The effect of molybdenum particle size on the flake-forming behaviour of molybdenum, flexural strength and fracture toughness of MAS glass/molybdenum composites, were investigated. The flake-forming behaviour shows a high degree of dependence on molybdenum particle size and, upto a size of 32 μm, becomes conspicuous with increasing particle size. At 32 μm, the aspect ratio reaches a value of 17 and, above 32 μm, flake forming saturates. Fracture toughness is closely related to flake-forming behaviour and the more marked the flake forming, the greater is the increase in fracture toughness. A composite of MAS glass with flaky molybdenum particles has a greater improvement effect on fracture toughness than composites with SiC whiskers, SiC platelets or ZrO₂ particles. This is closely linked to plastic deformation of the flaky metallic particles at the crack tip at the time of fracture. This revised version was published online in November 2006 with corrections to the Cover Date.     

Static recrystallisation and recrystallisation during hot deformation of Al–1Mg–1Mn alloy

Abstract

Plane strain compression tests at 5 s^?1 and at temperatures of 270–480°C have been carried out on an Al–1Mg–1Mn alloy containing a bimodal distribution of intermetallic particles and after a prior heat treatment to coarsen all particles to greater than 1 μm in size. During the heat treatment, recrystallisation of the initially hot worked material only proceeded with coarsening of the fine particles. During subsequent hot deformation, thin foil electron microscopy revealed that identical subgrain structures were developed in the two materials by dynamic recovery at temperatures below 450°C. At higher temperatures, the initially recrystallised material showed localised particle stimulated dynamic recrystallisation. The subsequent static recrystallisation rate was more than 10³ times faster in the material free from small particles.

MST/751     

Preparation of zirconium diboride nanopowders in a sodium tetraborate ionic melt

Reactions between zirconium powder 10–15 μm in particle size and microcrystalline boron 10–20 μm in particle size in an Na₂B₄O₇ ionic melt have been studied at temperatures from 600 to 850°C and reaction times from 5 to 10 h. The results demonstrate that ZrB₂ forms starting at 750°C. According to scanning electron microscopy data, the ZrB₂ powder consists of particles 90–95 nm in average size. The crystallite size evaluated from X-ray diffraction data is 85 nm.     

Fabrication and mechanical properties of PLA/HA composites: A study of in vitro degradation

The adverse effects of stress shielding from the use of high-modulus metallic alloy bio-implant materials has led to increased research into developing polymer–ceramic composite materials that match the elastic modulus of human bone. Of particular interest are poly-l-lactic acid–hydroxyapatite (PLA/HA)-based composites which are fully resorbable in vivo. However, their bioresorbability has a deleterious effect on the mechanical properties of the implant. The purpose of this study is to investigate, from a micromechanistic perspective, the in vitro degradation behavior of such composites manufactured using a simple hot-pressing route for two different hydroxyapatite particles: a fine-grained (average particle size ∼5 μm) commercial powder or coarser whiskers (∼ 25–30 μm long, ∼ 5 μm in diameter). We observed that composites with ceramic contents ranging between 70 and 85 wt.% have mechanical properties that match reasonably those of human cortical bone. However, the properties deteriorate with immersion in Hanks' Balanced Salt Solution due to the degradation of the polymer phase. The degradation is more pronounced in samples with larger ceramic content due to the dissolution of the smaller amount of polymer between the ceramic particles.