Low-temperature compaction of Ti-6Al-4V powder using equal channel angular extrusion with back pressure

Equal channel angular extrusion (ECAE), with simultaneous application of back pressure, has been applied to the consolidation of 10 mm diameter billets of pre-alloyed, hydride-dehydride Ti-6Al-4V powder at temperatures ≤400 °C. The upper limit to processing temperature was chosen to minimise the potential for contamination with gaseous constituents potentially harmful to properties of consolidated product. It has been demonstrated that the application of ECAE with imposed hydrostatic pressure permits consolidation to in excess of 96% relative density at temperatures in the range 100-400 °C, and in excess of 98% at 400 °C with applied back pressure ≥175 MPa. ECAE compaction at 20 °C (back pressure = 262 MPa) produced billet with 95.6% relative density, but minimal green strength. At an extrusion temperature of 400 °C, the relative density increased to 98.3%, for similar processing conditions, and the green strength increased to a maximum 750 MPa. The relative density of compacts produced at 400 °C increased from 96.8 to 98.6% with increase in applied back pressure from 20 to 480 MPa, while Vickers hardness increased from 360 to 412 HV. The key to the effective low-temperature compaction achieved is the severe shear deformation experienced during ECAE, combined with the superimposed hydrostatic pressure.

Microstructure, magnetic and mechanical properties of Ni-Zn ferrites prepared by Powder Injection Moulding

Nowadays, the electronic industry demands small and complex parts as a consequence of the miniaturization of electronic devices. Powder injection moulding (PIM) is an emerging technique for the manufacturing of magnetic ceramics. In this paper, we analyze the sintering process, between 900 °C and 1300 °C, of Ni–Zn ferrites prepared by PIM. In particular, the densification behaviour, microstructure and mechanical properties of samples with toroidal and bar geometry were analyzed at different temperatures. Additionally, the magnetic behaviour (complex permeability and magnetic losses factor) of these compacts was compared with that of samples prepared by conventional powder compaction. Finally, the mechanical behaviour (elastic modulus, flexure strength and fracture toughness) was analyzed as a function of the powder loading of feedstock. The final microstructure of prepared samples was correlated with the macroscopic behaviour. A good agreement was established between the densities and population of defects found in the materials depending on the sintering conditions. In general, the final mechanical and magnetic properties of PIM samples were enhanced relative those obtained by uniaxial compaction.

Comparison of different extrusion methods for compaction of powders

Densification of metallic powders by means of extrusion is regarded as a very attractive processing technique that allows obtaining a high level of relative density of the compact. However, the uniformity of the relative density depends on that of strain distribution and on the processing parameters. Several variants of extrusion can be used for compaction of metal particulates, including the conventional extrusion (CE) and equal channel angular pressing (ECAP), often referred to as equal-channel angular extrusion. Each of these processes has certain advantages and drawbacks with respect to compaction. A comparative study of these two extrusion processes influencing the relative density of compacts has been conducted by numerical simulation using commercial finite element software DEFORM2D. The results have been validated by experiments with titanium and magnesium powders and chips.

The effect of hydrogenation on the ECAP compaction of Ti–6Al–4V powder and the mechanical properties of compacts

The effect of hydrogen content on the compaction of Ti–6Al–4V powder at low temperatures, namely 500 °C, using equal channel angular pressing (ECAP) with back pressure has been investigated. The properties of the compacts before and after a heat treatment and de-hydrogenation cycle have been determined. Compaction of powder by ECAP (500 °C and 260 MPa) has shown maximum levels of relative density of 99.3% and 99.4% when charged with 0.05–0.1 wt.% and 0.61–0.85 wt.% of hydrogen, respectively. After the de-hydrogenation heat treatment the diffusion bonding between individual powder particles was completed and the microstructure was altered, depending on the level of hydrogen content. Two local maxima of 99.2% and 98.1% were observed in the measured density of consolidated compacts for hydrogen contents between 0.05 wt.% and 0.1 wt.% and between 0.61 wt.% and 0.85 wt.%, respectively. However, the mechanical properties of the compacts within these two ranges of hydrogen content were significantly different due to a difference in the observed microstructure. An exceptionally high ductility of 29%, in combination with a relatively high strength of ~560 MPa, was measured in a shear punch test on specimens which had a prior hydrogen level of 0.05 wt.% before the heat treatment. It was shown that material consolidated from powder hydrogenated to low levels of hydrogen before compaction has the potential to offer substantial improvements in mechanical properties after a suitable heat treatment.

Shear deformation with imposed hydrostatic pressure for enhanced compaction of powder

In this paper equal channel angular extrusion with back pressure was used to compact Ti-6Al-4V powder at 400 °C, achieving relative densities of 98.3-98.6% and green strengths up to 750 MPa. The novelty of the approach arises from the notion that severe shear deformation is an important factor for consolidation. Improved compaction is related to enhanced self-diffusion through the creation of additional diffusion paths (defects) and the imposed hydrostatic pressure. The role of deformation mechanisms in improving compaction is discussed. © 2008 Acta Materialia Inc.

Characterization and evaluation of melibiose as novel excipient in tablet compaction

Lactose is probably the most used tablet excipient in the field of pharmacy. Although lactose is thoroughly characterized and available in many different forms there is a need to find a replacer for lactose as a filler/binder in tablet formulations because it has some downsides. Melibiose is a relatively unknown disaccharide that has not been thoroughly characterized and not previously used as an excipient in tablets. Structurally melibiose is close to lactose as it is also formed from the same two monosaccharides, glucose and galactose. Aim of this research is to characterize and to study physicochemical properties of melibiose. Also the potential of melibiose to be used as pharmaceutical tablet excipient, even as a substitute for lactose is evaluated. Current knowledge about fundamentals of tableting and methods for determinating of deformation behavior and tabletability are reviewed. In this research Raman spectroscopy, X-ray powder diffraction (XRPD), near-infrared spectroscopy (NIR) and Fourier-transform infrared spectroscopy (FT-IR) were used to study differences between two melibiose batches purchased from two suppliers. In NIR and FT-IR measurements no difference between materials could be observed. XPRD and Raman however found differences between the two melibiose batches. Also the effects of moisture content and heating to material properties were studied and moisture content of materials seems to cause some differences. Thermal analytical methods, differential scanning calorimetry (DSC) and thermogravimetry (TG) were used to study thermal behaviour of melibiose and difference between materials was found. Other melibiose batch contains residual water which evaporates at higher temperatures causing the differences in thermal behaviour. Scanning electron microscopy images were used to evaluate particle size, particle shape and morphology. Bulk, tapped and true densities and flow properties of melibiose was measured. Particle size of the melibiose batches are quite different resulting causing differences in the flowability. Instrumented tableting machine and compression simulator were used to evaluate tableting properties of melbiose compared to α-lactose monohydrate. Heckel analysis and strain-rate sensitivity index were used to determine deformation mechanism of melibiose monohydrate in relation to α–lactose monohydrate during compaction. Melibiose seems to have similar deformation behaviour than α-lactose monohydrate. Melibiose is most likely fragmenting material. Melibiose has better compactibility than α – lactose monohydrate as it produces tablets with higher tensile strength with similar compression pressures. More compression studies are however needed to confirm these results because limitations of this study.

The impact of powder flowing properties on dosator filling system operation

Purpose: To study the impact of powder flow properties on dosator filling systems, with particular focus on improvements in dose weight accuracy and repeatability. Method: This study evaluates a range of critical powder flow properties such as: flow function, cohesion, wall friction, adhesion to wall surfaces, density/compressibility data, stress ratio “K” and gas permeability. The characterisations of the powders considered in this study were undertaken using an annular shear cell using a sample size of 0.5 litres. This tester also incorporated the facility to measure bed expansion during shear in addition to contraction under consolidation forces. A modified Jenike type linear wall friction tester was used to develop the failure loci for the powder sample in conjunction with multiple wall samples (representing a variety of material types and surface finishes). Measurements of the ratio of applied normal stress versus lateral stress were determined using a piece of test equipment specifically designed for the purpose. Results: The correct characterisation of powders and the incorporation of this data into the design of process equipment are recognised as critical for reliable and accurate operation. An example of one aspect of this work is the stress ratio “K”. This characteristic is not well understood or correctly interpreted in many cases – despite its importance. Fig 1 [Omitted] (illustrates a sample of test data. The slope of the line gives the stress ratio in a uniaxial compaction system – indicating the behaviour of the material under compaction during dosing processes. Conclusions: A correct assessment of the bulk powder properties for a given formulation can allow prediction of: cavity filling behaviour (and hence dosage), efficiency of release from dosator, and strength and stability of extruded dose en route to capsule filling Influences over the effectiveness of dosator systems have been shown to be impacted upon by: bed pre-compaction history, gas permeability in the bed (with respect to local density effects), and friction effects for materials of construction for dosators

Use of residual hydrogen to produce CP-Ti powder compacts for low temperature rolling

The present work investigates the optimal level of residual hydrogen in partially de-hydrogenated powder to produce CP-Ti plate compacts using ECAP with back pressure which are subsequently rolled at low temperature. A comparative study of the compaction of two TiH₂ powders and a CP-Ti powder, with particle sizes 150 um, 50um and 45 um respectively, has been carried out. The hydride powders have also been compacted in a partially de-hydrogenated state. The optimal level of residual hydrogen with respect to the density of the resulting compact and the associated mechanical properties has been defined. ECAP at 300°C produced compacts from these partially de-hydrogenated powders of 99.5% theoretical density, while CP-Ti was compacted to almost full theoretical density under the same ECAP conditions. Therefore, the compaction of powder by ECAP does not benefit from temporary hydrogen alloying.

These compacts then were rolled at temperatures ranging from room temperature to 500°C with an 80% reduction in a single pass. Heat treatment after the rolling can modify the microstructure to improve the resulting mechanical properties and in this regard the temporary alloying with hydrogen has been observed to offer some significant benefits. It is shown the ECAP followed by low temperature rolling is a promising route to the batch production of fully dense CP-Ti wrought product from powder feedstock that avoids the need to subject the material to temperatures greater than 500°C. This low temperature route is expected to be efficient from an energy point of view and it also avoids the danger of interstitial contamination that accompanies most high temperature powder processing.