3D printing by selective laser sintering (SLS) of high-dose drug delivery systems using pure brittle crystalline active pharmaceutical ingredients (API) is possible but impractical. Currently used pharmaceutical grade excipients, including polymers, are primarily designed for powder compression, ensuring good mechanical properties. Using these excipients for SLS usually leads to poor mechanical properties of printed tablets (printlets). Composite printlets consisting of sintered carbon-stained polyamide (PA12) and metronidazole (Met) were manufactured by SLS to overcome the issue. The printlets were characterized using DSC and IR spectroscopy together with an assessment of mechanical properties. Functional properties of the printlets, i.e., drug release in USP3 and USP4 apparatus together with flotation assessment, were evaluated. The printlets contained 80 to 90% of Met (therapeutic dose ca. 600 mg), had hardness above 40 N (comparable with compressed tablets) and were of good quality with internal porous structure, which assured flotation. The thermal stability of the composite material and the identity of its constituents were confirmed. Elastic PA12 mesh maintained the shape and structure of the printlets during drug dissolution and flotation. Laser speed and the addition of an osmotic agent in low content influenced drug release virtually not changing composition of the printlet; time to release 80% of Met varied from 0.5 to 5 h. Composite printlets consisting of elastic insoluble PA12 mesh filled with high content of crystalline Met were manufactured by 3D SLS printing. Dissolution modification by the addition of an osmotic agent was demonstrated. The study shows the need to define the requirements for excipients dedicated to 3D printing and to search for appropriate materials for this purpose.

The paper presents the unique approach to 3D printing by Selective Laser Sintering of high dose controlled release pharmaceutical dosage form, which contains almost exclusively drug substance - just crystalline paracetamol as a model drug substance and small amount of dye were used. Comprehensive printlet characterization, that included pore space analysis, drug release and subsequent dissolution modeling as well as exploratory analysis, revealed various degrees of freedom for tuning its functional properties i.e. dissolution performance. Two degrees of freedom were found substantial for the proposed approach: (1) the macro structure shaping in terms of active surface to volume ratio; (2) microstructure shaping in terms of pore space structure. The latter was found to have a great potential and can be modified by the manufacturing parameters, e.g. hatch spacing. The simplicity of the preparation and flexibility to control the dissolution performance of the pharmaceutical dosage are the advantages of the proposed approach.

The microstructure, mechanical properties, and friction-wear performance of (TiBx/TiSiyCz)x3 multilayer coatings deposited on the M2 steel by the pulsed laser deposition are investigated in detail in as-deposited state and after annealing at 500 °C for 5 min in air. Scanning and transmission electron microscopies are used to reveal microstructural changes caused by annealing. The influence of post-deposition annealing on hardness and Young modulus is studied in nanoindentation test. A scratch-test is applied to reveal changes in adhesion and the coefficient of friction (CoF) of coated samples with diamond before and after annealing. Friction-wear properties are also analyzed in dry sliding with Al2O3 and 100Cr6 steel in ball-on-disc tests. Our analysis shows that the post-deposition annealing leads to partial devitrification of the TiBx layers, where nanocrystalline TiB2 phase is identified, while the TiSiyCz layers retain amorphous. Annealing significantly increases mechanical properties of coated samples and adhesion of the (TiBx/TiSiyCz)x3 multilayer to steel substrates. Friction-wear properties of coated samples are also notably improved. The values of CoF for coated samples tested with diamond (in the scratch-test), alumina, and 100Cr6 steel (ball-on-disc tests) are in the range of 0.05–0.23, while for M2 steel the CoF values are 0.8, 0.45, and 0.8, respectively.

As part of the tests, a two-phase NiAl/Ni3Al alloy and a composite based on this alloy with 4 vol% addition of TiB2 were produced by the reactive FAST/SPS (Field Assisted Sintering Technology/Spark Plasma Sintering) sintering method. The sintering process was carried out at 1273 K for 30 s under an argon atmosphere. The effect of reactive SPS on the density, microstructure, and mechanical and tribological properties of a dual-phase Ni-Al intermetallic compound and Ni-Al-TiB2 composite was investigated. Products obtained were characterized by a high degree of sintering (over 99% of the theoretical density). The microstructure of sinters was characterized by a large diversity, mainly in regard to the structure of the dual-phase alloy (matrix). Compression tests showed satisfactory plastic properties of the manufactured materials, especially at high temperature (1073 K). For both materials at room temperature, the compressive strength was over 3 GPa. The stress–strain curves were observed to assume a different course for the matrix material and composite material, including differences in the maximum plastic flow stress depending on the test temperature. The brittle-to-ductile transition temperature was determined to be above 873 K. The research has revealed differences in the physical, mechanical and tribological properties of the produced sinters. However, the differences favourable for the composite were mostly the result of the addition of TiB2 ceramic particles uniformly distributed on grain boundaries.

The results of corrosion studies of composite materials obtained by two state-of-the –art methods of powder metallurgy are presented in the article. The main goal of the studies was determination of high-temperature corrosion resistance of steel-matrix composites reinforced with 8 vol.% TiB2. Thermogravimetric analyses were conducted at 1100ºC in air in 24 h cycle. Microstructure of the composited after thermogravimetric studies was observed at scanning electron microscope.

Results of compressionand corrosion-resistance tests of NiAl alloys with 1.0 and 2.0 wt.% of titanium are described. The compression tests conducted at a wide range of temperatures, and the strain rate showed that an increase in titanium content causes increased brittleness at room temperature, while at higher temperatures, an increase of hardness and strength is observed. The analysis of electrochemical corrosion resistance showed that alloys containing Ti are characterized by considerable resistance to sulfuric acid VI, because the emerging titanium oxide prevents the active solubilization of the alloy. Besides, microstructure observations performed at various levels of deformation, which allowed us to identify the mechanisms responsible for fracture of the studied alloys.

Results of compression and corrosion resistance tests of NiAl alloys with 1.0 and 2.0 wt.% of titanium are described. The compression tests conducted in a wide range of temperature and strain rate showed that increase of titanium content causes increase of brittleness at room temperature, while at higher temperatures an increase of hardness and strength is observed. The analysis of electrochemical corrosion resistance showed that the alloys containing Ti are characterized by considerable resistance to sulfuric acid VI, because the emerging titanium oxide prevents active solubilizing of the alloy. Besides, microstructure observations performed at various levels of deformation which allowed to identify mechanisms responsible for fracture of the studied alloys.

The results of corrosion studies of composite materials obtained by two methods of powder metallurgy are presented in the article. The main goal of the studies was to determine the high-temperature corrosion resistance of steel-matrix composites reinforced with 8 vol.% TiB2. Thermogravimetric analyses were conducted at 1100°C in air during a 24 h cycle. The microstructure of the composite after thermogravimetric studies was observed with a scanning electron microscope.

The paper presents the results of tribological tests conducted on an A339/SiC/10p composite reinforced with SiC particles. The test method used in the research was the ball-on-disc method combined with variable abrasion test parameters. Different materials were used for the counter-specimen (steel, Al2O3, SiC), variable load (5 and 10N) and sliding speed (0.1 and 0.5 m/s). It was found that the use of a counter-specimen made from a material of higher hardness significantly reduced the friction coefficient and the specific wear rate of the tested A339/SiC/10p composite. On the other hand, in all the friction pairs, an increase in the load while maintaining the same test conditions caused a decrease in the friction coefficient value and an increase in the specific wear rate. Additionally, in the Al2O3 counter-specimens, an abnormal decrease in the friction coefficient was observed with an increasing load, but it had no impact on the results of the specific wear rate.

The paper presents the results of tribological tests conducted on an A339/SiC/10p composite reinforced with SiC particles. The test method used in the research was the ball-on-disc method combined with variable abrasion test parameters. Different materials were used for the counter-specimen (steel, Al2O3, SiC), variable load (5 and 10N) and sliding speed (0.1 and 0.5 m/s). It was found that the use of a counter-specimen made from a material of higher hardness significantly reduced the friction coefficient and the specific wear rate of the tested A339/SiC/10p composite. On the other hand, in all the friction pairs, an increase in the load while maintaining the same test conditions caused a decrease in the friction coefficient value and an increase in the specific wear rate. Additionally, in the Al2O3 counter-specimens, an abnormal decrease in the friction coefficient was observed with an increasing load, but it had no impact on the results of the specific wear rate.

The AISI316L stainless steel composites reinforced with 2,4,6,and 8 vol%titanium diboride（TiB 2 ） particles were sintered by the high pressure-high temperature method.Ball-on-disk method was carried out to study wear behavior of the composites.Tests were carried out at room temperature.The TiB 2 particles improved the hardness and tribological properties of the composites.The friction coefficient of the composites decreased with the increasing content of TiB 2 .The reduction of the wear rate with the increasing of the content of TiB 2 particles in the steel matrix was also observed.It is demonstrated that the friction coefficient of composites with the same content of TiB 2 particles depend on the sintering conditions.

The aim of the work was to investigate the influence of silver as a modifying constituent on structure formation in Ni-P based glass forming matrix. Nickel-phosphorus-based Ni80P20, Ni78Ag2P20 and Ni76Ag4P20 alloys were prepared from 99.95 wt % Ni, 99.95 wt % Ag, and Ni-P master alloy. The alloys were melt-spun in helium. The microstructure of the melt-spun ribbons was investigated by XRD, a light microscope and a transmission electron microscope. Then the tensile tests were performed. The alloys with silver show lower tensile strength with respect to the fully amorphous Ni80P20 ribbon. The ductility of the amorphous matrix melt-spun Ni78Ag2P20 and Ni76Ag4P20 alloys was improved by addition of silver forming fcc-Ag precipitates in comparison with Ni80P20amorphous alloy. SEM observations of the fracture surfaces show different character of the fractured samples. The pattern and the number of the crack lines changes, depending on the silver content. For the fully amorphous Ni80P20 alloy simple brittle cracks are observed, however the alloys with silver content show more developed surfaces near the fractured regions and form crack lines arranged 60° with loading direction.

A six-component Fe50Ni10Cu20P10Si5B5 immiscible alloy was arc-melt in argon and it was melt-spun from various temperatures. The morphology and chemical composition of the cross-section of the ingot and melt-spun ribbons were analysed with a scanning electron microscope SEM/EDS. The melt-spun ribbon was investigated by a transmission electron microscope (TEM). The melting range of the alloy was investigated by means of differential thermal analysis (DTA) and for reference, the temperature change during free cooling of the alloy was controlled by pyrometer in the melt spinning device. The slow cooling rate resulted in the fractal surface structures formed by the Fe-rich regions and Cu-rich regions typical for the alloying system with a miscibility gap. The structures of the melt-spun ribbons were dependent on ejection temperatures before the melt spinning. The lower ejection temperatures resulted in the formation of the structures separated into Fe-rich and Cu-rich regions. This was due to rapid cooling within the miscibility gap. Ejection at higher temperatures led to the formation of a uniform amorphous/crystalline composite.

Purpose: Purpose of this paper is to determine the effect of Equal Channel Angular Pressing (ECAP) processing on the microstructure and hardness of α+β brasses. The effect of deformation temperature and number of passes was investigated particularly on the shape and size of grains of both phases. Design/methodology/approach: The specially constructed channel with 90° pressing angle, allowing heating of the tool with the sample was used for ECAP processing. The grain size was investigated using optical and transmission electron microscopy. The hardness and measurements microhardness were used to determine the effect of ECAP on the hardness of both phases. Findings: Significant grain refinement down to 300 nm from the initial 20 mm was observed after ECAP processing at 300°C. At 400°C grain refinement occurred down to 1-3 mm. Frequent microtwins were observed within α phase. The microhardness of the β phase was higher than that of α phase, 235 HV and 173 HV respectively. Research limitations/implications: The limitation is a size of the sample which makes difficult future applications. Another one is elevated temperature (minimum 300°C) otherwise the samples forms crack. This limits also the grain refinement which is above the range of nanomaterials. Practical implications: Significant grain refinement allows to increase the hardness and strength of the sample preserving a good plasticity. The limitation is the size of the channel what limits the application. The material could be used in such cases when high strength of brasses is needed with sufficient plasticity and good conductivity. Originality/value: In this paper detailed TEM studies were performed for α+β brasses showing high density of microtwins and higher density of dislocations within α phase, than in the β phase. Higher hardness of the β phase results from the ordering, which hinder deformation of this phase.

Purpose: of this paper was to investigate the effect of grain refinement in AZ31 magnesium alloy processed by ECAP and to study microstructure evolution and hardness response of AZ31 alloy associated with ECAP processing. Design/methodology/approach: The microstructure of AZ31 magnesium alloy after two passes of equal channel angular pressing at 150°C, 180°C and 250°C was studied by means of metallographic and transmission electron microscopy. The hardness changes after ECAP processing were determined by Vickers hardness. Findings: The grain refinement in AZ31 magnesium alloy was successfully carried out using ECAP processing at 150, 180 and 250°C. The grain size decreases nearly 10 times after 2 passes of ECAP at 150 and 180°C, but microstructure is characterized by bimodal grains structure. The rather homogenous grains were achieved after ECAP processing at 250°C. Processes of dynamic recrystallization during ECAP were observed. The hardness increase related to grain refinement proceeded by ECAP is in accordance with Hall-Petch relationship. Research limitations/implications: The ECAP processing were carried out only after 2 passes, therefore in order to describe in detail the microstructural changes connected with grain refinement, the analysis of more passes of ECAP processing should be done. Practical implications: The development of highly ductile magnesium alloys allows to apply these materials as structural materials. The grain refinement of materials leads to the significant improvement of the mechanical properties and plasticity. The present results extend the knowledge about grain refinement in AZ31 alloy proceeded by ECAP. Originality/value: The microstructural studies of AZ31 alloy after grain refining by ECAP processing performed by transmission electron microscopy were presented.

Improved mechanical properties of materials with ultra-fine grained structure (nanostructure) are very frequently reported and severe plastic deformation is commonly proposed as a method to obtain such materials. High pressure torsion, although it cannot supply big dimension samples, generally leads to the highest degree of grain refinement The paper shows the influence of the phenomenon of intensive shear deformation during high pressure torsion (HPT) processing on the changes in structure, grain size, mechanical properties and solid solubility. The study is performed on copper brasses exemplified by CuZn30, CuZn37 and CuZn29Mn11, severely deformed up to high deformation degree (epsilon = 18.1 under 2 GPa pressure). The alpha + beta brasses are particularly interesting as the deformation of two-phase alpha + beta brasses shows the ability to superplastic deformation; additionally the better grain refinement and relation of alpha/beta phase contents influence superplastic deformation.