Fracture toughness of some high density PM steels

Tensile strengths, impact energies, and fracture toughness data are presented for pure Fe-0.5 C, Astaloy A with 0.2 and 0.6%C, and for Distaloy AB-0.6%C at relative densities of about 0.9, achieved by conventional pressing and sintering, and at close to 1.0, achieved by powder forging. At low relative density, properties are controlled by sizes of sinter necks; it is postulated that toughness scales as (x/a)4, x/a being the ratio of neck diameter to particle diameter. At high relative density, microvoid coalescence and good toughness is observed for low strength microstructures whereas cleavage and poor toughness is a concomitant of high strength.

Structural properties of a family of hydrogen-bonded co-crystals formed between gemfibrozil and hydroxy derivatives of t-butylamine, determined directly from powder X-ray diffraction data

We report the formation and structural properties of co-crystals containing gemfibrozil and hydroxy derivatives of t-butylamine H2NC(CH3)3-n(CH2OH)n, with n=0, 1, 2 and 3. In each case, a 1:1 co-crystal is formed, with transfer of a proton from the carboxylic acid group of gemfibrozil to the amino group of the t-butylamine derivative. All of the co-crystal materials prepared are polycrystalline powders, and do not contain single crystals of suitable size and/or quality for single crystal X-ray diffraction studies. Structure determination of these materials has been carried out directly from powder X-ray diffraction data, using the direct-space Genetic Algorithm technique for structure solution followed by Rietveld refinement. The structural chemistry of this series of co-crystal materials reveals well-defined structural trends within the first three members of the family (n=0, 1, 2), but significantly contrasting structural properties for the member with n=3. © 2007 Elsevier Inc. All rights reserved.

The development of a modified dissolution method suitable for investigating powder mixtures

A novel dissolution method was developed, suitable for powder mixtures, based on the USP basket apparatus. The baskets were modified such that the powder mixtures were retained within the baskets and not dispersed, a potential difficulty that may arise when using conventional USP basket and paddle apparatus. The advantages of this method were that the components of the mixtures were maintained in close proximity, maximizing any drug:excipient interaction and leading to more linear dissolution profiles. Two weakly acidic model drugs, ibuprofen and acetaminophen, and a selection of pharmaceutical excipients, including potential dissolution-enhancing alkalizing agents, were chosen for investigation. Dissolution profiles were obtained for simple physical mixtures. The f1 fit factor values, calculated using pure drug as the reference material, demonstrated a trend in line with expectations, with several dissolution enhancers apparent for both drugs. Also, the dissolution rates were linear over substantial parts of the profiles. For both drugs, a rank order comparison between the f1 fit factor and calculated dissolution rate, obtained from the linear section of the dissolution profile, demonstrated a correlation using a significance level of P=0.05. The method was proven to be suitable for discriminating between the effects of excipients on the dissolution of the model drugs. The method design produced dissolution profiles where the dissolution rate was linear for a substantial time, allowing determination of the dissolution rate without mathematical transformation of the data. This method may be suitable as a preliminary excipient-screening tool in the drug formulation development process.

Die load and stresses in press forging

Several axi-symmetric EN3B steel components differing in shape and size were forged on a 100 ton joint knuckle press. A load cell fitted under the lower die inserts recorded the total deformation forces. Job parameters were measured off the billets and the forged parts. Slug temperatures were varied and two lubricants - aqueous colloidal graphite and oil - were used. An industrial study was also conducted to check the results of the laboratory experiments. Loads were measured (with calibrated extensometers attached to the press frames) when adequately heated mild steel slugs were being forged in finishing dies. Geometric parameters relating to the jobs and the dies were obtained from works drawings. All the variables considered in the laboratory study could not, however, be investigated without disrupting production. In spite of this obvious limitation, the study confirmed that parting area is the most significant geometric factor influencing the forging load. Multiple regression analyses of the laboratory and industrial results showed that die loads increase significantly with the weights and parting areas of press forged components, and with the width to thickness ratios of the flashes formed, but diminish with increasing slug temperatures and higher billet diameter to height ratios. The analyses also showed that more complicated parts require greater loads to forge them. Die stresses, due to applied axial loads, were investigated by the photoelastic method. The three dimensional frozen stress technique was employed. Model dies were machined from cast araldite cylinders, and the slug material was simulated with plasticene. Test samples were cut from the centres of the dies after the stress freezing. Examination of the samples, and subsequent calculations, showed that the highest stresses were developed in die outer corners. This observation partly explains why corner cracking occurs frequently in industrial forging dies. Investigation of die contact during the forging operation revealed the development of very high stresses.

The use of lubricants in iron powder metallurgy

This investigation has been concerned with the behaviour of solid internal lubricant during mixing, compaction, ejection, dewaxing and sintering of iron powder compacts. Zinc stearate (0.01%-4.0%) was added to irregular iron powder by admixing or precipitation from solution. Pressure/density relationships, determined by continuous compaction, and loose packed densities were used to show that small additions of zinc stearate reduced interparticle friction during loose packing and at low compaction pressures. Large additions decreased particle/die-wall friction during compaction and ejection but also caused compaction inhibition. Transverse rupture strengths were determined on compacts containing various stearate based lubricants and it was found that green strength was reduced by the interposition of a thin lubricant layer within inter~particle contacts. Only materials much finer than the iron powder respectively) were able to form such layers. Investigations were undertaken to determine the effect of the decomposition of these lubricants on the development of mechanical properties in dewaxed or sintered compacts. Physical and chemical influences on tensile strength were observed. Decomposition of lubricants was associated with reductions of strength caused by the physical effects of pressure increases and removal of lubricant from interparticle contacts. There were also chemical effects associated with the influence of gaseous decomposition products and solid residues on sintering mechanisms. Thermogravimetry was used to study the decomposition behaviour of various lubricants as free compounds and within compacts. The influence of process variables such as atmosphere type, flow-rate and compact density were investigated. In a reducing atmosphere the decomposition of these lubricants was characterised by two stages. The first involved the rapid decomposition of the hydrocarbon radical. The second, higher temperature, reactions depended on lubricant type and involved solid residues. The removal of lubricant could also markedly affect dimensional change.

Study of the deposition, properties and applications of electroless deposits containing particles

The deposition efficiencies of a number of electroless nickel and cobalt plating solutions were studied and in the case of nickel compared with a commercial plating solution Nifoss 80. At the optimum plating conditions (92ºC and pH 4.5) Nifoss 80 produced nickel layers most efficiently, the alkaline cobalt solution operated most efficiently at 90ºC and pH 9. The methods of producing compostte layers containing 2-3 µm carbide particles and chromium powder is described. Nickel and cobalt layers containing approximately 27% carbide particles, or 40% (Ni) and 30% (Co) chromium particles by volume were obtained. This value is independent of the particle concentration in the plating solution within the range (20~200 g/l). Hardness of the nickel. as deposited was 515 Hv, this was increased to a maximum of 1155 Hv by heat treatment at 200ºC for 5 hours in vacuum. Incorporation. of .chromium carbide particles resulted in a maximum hardness of 1225 Hv after heating at 500ºC for 5 hours in vacuum and chromium particles resulted in a maximum hardness of 16S0 Hv after heat treatment at 400ºC for 2 hours in vacuum. Similarly the hardness of cobalt as deposited was 600 Hv, this was increased to a maximum of 1300 Hv after heat treatment at 400ºC for 1 hour. Incorporation of chromium carbide particles resulted jn a maximum hardness of 1405 Hv after heating at 400ºC for 5 hours in vacuum and chromium particles resulted in a maximum hardness of 1440 Hv after. heat treating for 2 hours at 400ºC in vacuum. The structure of the deposits was studied by optical and scanning electron microscopy. The wear rate and coefficient of friction was determined by a pin and disc method. Wear rate and coefficient of friction decreased with increase in hardness. The wear resistance of the materials was also determined using a simulated forging test. Dies made of standard die steel were coated and the wear rates of the layers as deposited and after heat treatment were compared with those of uncoated tools. The wear resistance generally increased with hardness, it was 50-75% more than the uncoated die steel. Acetic acid salt spray test and outdoor exposure for six months was used to study the corrosion behaviour of the deposits and potentiodynamic curves plotted to find their corrosion potential. Nickel deposit exhibited less staining than carbide composite deposits and nickel-chromium deposits had the most noble corrosion potential.

Powder painting of aluminium

The mechanisms involved in the production of chromate-phosphate conversion coatings on aluminium have been investigated. A sequence of coating nucleation and growth has been outlined and the principle roles of the constituent ingredients of the chromate-phosphate solution have been shown. The effect of dissolved aluminium has been studied and its role in producing sound conversion coatings has been shown. Metallic contamination has been found to have a dramatic influence on chromate-phosphate coatings when particular levels have been exceeded. Coating formation was seen to be affected in proportion to the level of contaminaton; no evidence of sudden failure was noted. The influence of substrate and the effect of an acidic cleaner prior to conversion coating have been studied and explained. It was found that the cleaner ages rapidly and that this must .be allowed for when attempting to reproduce industrial conditions in the laboratory. A study was carried out on the flowing characteristics of polyester powders of various size distributions as they melt using the hot-stage microscopy techniques developed at Aston. It was found that the condition of the substrate (ie extent of pretreatment), had a significant effect on particle flow. This was explained by considering the topography of the substrate surface. A number of 'low-bake' polyester powders were developed and tested for mechanical, physical and chemical resistance. The best formulation had overall properties which were as good as the standard polyester in many respects. However chemical resistance was found to be slightly lower. The charging characteristics of powder paints during application by means of electrostatic spraying was studied by measuring the charge per unit mass and relating this to the surface area. A high degree of correlation was found between charge carried and surface area, and the charge retained was related to the powder's formulation.