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Single crystals of isomeric 1,2,3‐tribromobenzene (123TBB), 1,2,4‐tribromobenzene (124TBB) and 1,3,5‐tribromobenzene (135TBB) have been grown from different solvents and their structures determined by X‐ray diffraction at 100, 200 and 270 K. The melting‐point differences of ca 40 K between 135TBB, 123TBB and 124TBB have been correlated with the molecular symmetry and packing preferences in the crystal, as well as with the main types of intermolecular halogen interactions, i.e. Br...Br, Br...C (Br...π) and Br...H. The relationship between symmetry and melting point in Carnelley's rule has been extended to the accessibility of terminal atoms for the formation of intermolecular interactions, their occurrences and distribution, and the close packing. The electrostatic potential mapped on molecular surfaces demonstrates that in more symmetric molecules the more evenly distributed substituents are more accessible and form more optimum intermolecular interactions. [ABSTRACT FROM AUTHOR]

Trends in the melting points of analogous halogenated benzene isomers are rationalized in terms of molecular symmetry, crystal structure and interactions. [ABSTRACT FROM AUTHOR]

Distortions of the directional requirements in halogen…halogen contacts between hexachloroethane (HCE), C2Cl6, molecules lead to a loose crystal under ambient conditions. Single-crystal X-ray diffraction shows that the orthorhombic HCE phase of space group Pnma, with the molecules in the staggered conformation, extends at least from 85 to 305 K and from 0.1 MPa to 5.42 GPa. At ambient pressure, all intermolecular distances are longer than the sum of van der Waals radii, reached only at the pressure of ca. 1.2 GPa. [ABSTRACT FROM AUTHOR]

The structures of a series of the simplest aliphatic amines determined at high pressure by single crystal X-ray diffraction reveal systematic structure property relations involving intermolecular interactions and molecular symmetries. Five new polymorphs have been found: one of methylamine (phase II, space group Fdd2), two of dimethylamine (phase I, space group C2/c and phase II, P21/c), and two of trimethylamine (phase II, space group P21/n and phase III, P21/m). The methylamine and dimethylamine molecules are arranged according to the NH...N hydrogen bonds. The phase diagrams of methylamines have been outlined up to 6 GPa. [ABSTRACT FROM AUTHOR]

A new high-pressure crystal form of ethane has been revealed above 2.46 GPa/295 K. This phase IV is tetragonal, of space group P42/mnm, with the H atom disordered due to the molecular rotations about the C-C bond. The crystal structure has been determined by single-crystal X-ray diffraction up to 5.90 GPa. The structure of phase IV resembles the previously determined low-temperature plastic phase I (stable below 90.32 K), of cubic space group Im3m, metastable phase II observed between 89.78 and 89.68 K, as well as monoclinic phase III (space group P21/n) stable below 89.68 K. In phases III and IV, the molecules are arranged according to the weak electrostatic complementarity between neighbors. Liquid-ethane convection erodes the crystal plate, hence colorful interference pattern. At 2.46 GPa, ethane crystallizes in a new tetragonal phase IV with rotating molecules. Spectacular convection of liquid ethane above the single-crystal surface has been observed. [ABSTRACT FROM AUTHOR]

In pentachloroethane, C2HCl5, high pressure initially strongly compresses the C–H…Cl bonds in phase I; however, in phase II which is stable above 0.62 GPa the role of hydrogen bonds is diminished and molecular aggregation is dominated by halogen bonds Cl…Cl. Both phases have been determined by X-ray diffraction and the phase diagram of C2HCl5 has been outlined. The transition between phases I and II retains some relation between their structures and reduces the symmetry from class mmm (space group Pnma) to 2/m (space group P21/n11). The discontinuous transition, with the shear strain exceeding 21°, is so strong that its progress can be visually observed even for powdered samples. The single-crystal growth suggests a surface-roughening transition, as phase I grows in the form of dendrites combining into oval plates, while phase II forms prisms with sharp edges. [ABSTRACT FROM AUTHOR]

Pyrazine molecules aggregate by remarkably similar CH···N hydrogen bonds into four polymorphs. Of eight CH···N bonds to each molecule, six H-bonds are very similar for all pyrazine structures. A diagram of four crystalline phases has been outlined and their low-temperature and high-pressure structures determined. Phase I is metastable and occurs only within the ambient-pressure region of phase II. [ABSTRACT FROM AUTHOR]

The compression and thermal expansion of crystalline 1,2,4-trichlorobenzene, C6H3Cl3, 124TCB, investigated under isobaric and isothermal conditions, are in reverse relation, as for most of crystals, however, the isochoric strain along direction c is clearly different from those along a and b. Single crystals of 124TCB have been in situ grown under isochoric and isobaric conditions, at 270 K/0.1 MPa and 295 K/0.16 GPa, and also at 100 K/0.1 MPa and 295 K/0.64 GPa, when the unit-cell volume is similar. All crystallizations yielded the same phase, of monoclinic space group P21/n, with two symmetry-independent molecules (Z′ = 2). The structure is governed by Cl…Cl and Cl…H interactions and the molecules are all nearly parallel to the [001] direction. Systematic differences of these specific contacts afford rationalizing the isochoric strain of the crystal. The phase diagram of 124TCB has been outlined. [ABSTRACT FROM AUTHOR]

Pressure affects the competition between C-HX hydrogen bonds and X⋯X halogenhalogen interactions. In bromomethane, CH3Br, pressure changes the molecular arrangement of the two solid-state phases of this compound: low-pressure phase α is dominated by halogenhalogen interactions, whereas above 1.5 GPa the β phase is governed by C-H⋯halogen bonds. The CH3Br phase α is isostructural with solid CH3I of orthorhombic space group Pnma, while CH3Br phase β is polar, isostructural with CH3Cl and CH3CN crystals, of orthorhombic space group Cmc21. The crystal structures of CH3Cl (b.p. = 249.1 K) and CH3Br (b.p. = 276.7 K) have been determined by high pressure single-crystal X-ray diffraction up to 4.38 GPa and 2.85 GPa, respectively. In CH3Br, pressure of 1.5 GPa enforces the close packing and opposite electrostatic-potential matching between molecular surfaces in contact. The interweaved C-H⋯X bonded diamondoid networks of β-CH3X are similar to those of acetonitrile, H2O ice VII and solidified X2 halogens. The phase diagrams of CH3Br and CH3Cl have been constructed. [ABSTRACT FROM AUTHOR]

The effect of zirconium diboride (ZrB2) and titanium diboride (TiB2) on the microstructure as well as the physical, mechanical, and tribological properties of composites based on 316 L steel is presented. Each reinforcing phase was added to the base alloy in the amount of 5 wt% and 10 wt%. The composites were fabricated by the SPS process (Spark Plasma Sintering). The results show that the weight fraction of the reinforcing phase affects the physical, mechanical, and tribological properties of the sintered composites. The sintered materials were characterized by a very high level of density. The addition of TiB2 has proved to be effective in increasing the hardness and compressive strength of the composites. The hardness of the composites with the addition of 10% TiB2 increased by 100% compared to the hardness of sintered 316L steel. It was found that introducing ZrB2 to the steel matrix significantly improved the wear resistance of the composites. The results showed that compared to 316L steel with the wear rate of 519 × 10−6 mm3/Nm, the wear rate of the composites containing 10% ZrB2 decreased more than twice, i.e., to 243 × 10−6 mm3/Nm. [ABSTRACT FROM AUTHOR]

At ambient conditions two liquids, bromoethane, C2H5Br (MBE, m.p. 154.6 K) and iodoethane, C2H5I (MIE, m.p. 162.1 K), have been crystallized under both isobaric and isochoric conditions using in situ low‐temperature and high‐pressure techniques. The single‐crystal X‐ray diffraction studies, supported by the isothermal compressibility and isobaric differential scanning calorimetry measurements, allowed the monitoring and analysis at low temperature and high pressure of the effects of externally induced changes in MBE and MIE. The monoclinic MBE and MIE crystals are found to be isostructural. They are stable, in the investigated regimes, i.e. down to 100 K/0.1 MPa and up to ∼295 K/3.7 GPa, without undergoing any symmetry or phase change. Both the contraction and compression is mainly noted for the intermolecular separation distances. The Hirshfeld surface analysis of intermolecular contacts clearly shows the nature of occurrence and hierarchy of interactions pointing out the role played by Br/I...Br/I contacts, in particular at ambient temperature and high‐pressure conditions. The preferences for the formation of intermolecular contacts in MIE are more pronounced and do not require such extreme conditions as in the case of MBE. It is notable that the Br/I...Br/I and Br/I...H contacts could be basically classified as type‐I interactions. [ABSTRACT FROM AUTHOR]

Molecular arrangements have been determined at the lowest limits of pressure ranges of benzene phase I, at 0.15 GPa, and phase II at 0.91 and 0.97 GPa, all at 295 K. All intermolecular contacts both in phase I and phase II to about 1.0 GPa exceed the sums of van der Waals radii; however, the transition between phases I and II does not affect the pattern of CH···π(arene) hydrogen bonds. In phase I the molecules are CH···π bonded approximately perpendicular into sheets, and there are substantial voids between the molecules within the sheets. The mechanism of transition to phase II involves a collapse of the voids, simultaneous with a shift of the CH···π bonded sheets. The thickness of sheets increases, which partly compensates the volume reduction due to the voids collapse; hence, the transition exhibits a large hysteresis of two GPa and a sluggish character at 295 K. No other phases of benzene have been observed between 0.15 and 5.0 GPa. High pressure transition between benzene phases I and II, involving a collapse of intermolecular voids, exhibits a huge pressure hysteresis of 2 GPa at 295 K and an intriguingly tiny volume change. It has been explained by determining the crystal structures of benzene I and II at their lowest stability limits. [ABSTRACT FROM AUTHOR]

Titanium diboride (TiB2) is a hard, refractory material, attractive for a number of applications, including wear-resistant machine parts and tools, but it is difficult to densify. The spark plasma sintering (SPS) method allows producing TiB2-based composites of high density with different sintering aids, among them titanium silicides. In this paper, Ti5Si3 is used as a sintering aid for the sintering of TiB2/10 wt % Ti5Si3 and TiB2/20 wt % Ti5Si3 composites at 1600 °C and 1700 °C for 10 min. The phase composition of the initial powders and produced composites was analyzed by the X-ray diffraction method using CuKα radiation. The microstructure was examined using scanning electron microscopy, accompanied by energy-dispersive spectroscopy (EDS). The hardness was determined using a diamond indenter of Vickers geometry loaded at 9.81 N. Friction–wear properties were tested in the dry sliding test in a ball-on-disc configuration, using WC as a counterpart material. The major phases present in the TiB2/Ti5Si3 composites were TiB2 and Ti5Si3. Traces of TiC were also identified. The hardness of the TiB2/Ti5Si3 composites was in the range of 1860–2056 HV1 and decreased with Ti5Si3 content, as well as the specific wear rate Wv. The coefficient of friction for the composites was in the range of 0.5–0.54, almost the same as for TiB2 sinters. The main mechanism of wear was abrasive. [ABSTRACT FROM AUTHOR]

Several procedures have been employed for validating structural models refined on poor quality single-crystal diffraction data. Analysis of intra- and intermolecular distances in the structures of 2,2-aziridinedicarboxamide polymorphs proved to be a robust means, and a means independent of the chosen unit cell and symmetry, of detecting several incorrect atom-type assignments in the reported structure of the triclinic polymorph of 2,2-aziridinedicarboxamide [Brückner (1982). Acta Cryst. B 38, 2405–2408]. The corrected model, refined in the space group , rules out the existence of any conformational polymorphism in this compound. Small differences in the powder-diffraction patterns calculated for the original and corrected structures of the triclinic polymorph illustrate the sensitivity of the above method for polymorph validation. [ABSTRACT FROM AUTHOR]

The structure of 1,2,3-trichloropropane, ClCH2CHClCH2Cl, in-situ crystallized in a diamond–anvil cell, has been determined by single-crystal X-ray diffraction at 0.28 and 0.35 GPa. A melting point at 295 K and 0.22 GPa has been determined. The molecular conformation of aliphatic chain and terminal Cl atoms is approximately C2 symmetric. Of the intermolecular contacts, the tightest are the Cl⋯Cl and then the Cl⋯H contacts, whereas the H⋯H distances are considerably longer than the sum of the van der Waals radii and leave narrow voids in the structure. The elevated pressure reduces the H⋯H separations but hardly affects the Cl⋯Cl distances. The crystal growth rates, compression and types of intermolecular interactions in the structures can be correlated with the directions of the Cl⋯Cl contacts, which can be considered the main motif responsible for the molecular arrangement in the structure. [ABSTRACT FROM AUTHOR]

Dibromomethane, CH2Br2, and diiodomethane, CH2I2, have been in situ pressure-crystallized in a diamond–anvil cell and their structures determined by single-crystal X-ray diffraction at 0.61 and 0.16 GPa, respectively. The pressure-frozen CH2Br2 crystal is isostructural with its C2/ c phase obtained by cooling. CH2I2 is known to form several phases at low temperature, one of which is isostructural with CH2Br2. However, pressure freezing leads to the polar Fmm2 phase. The formation of the polar CH2I2 structure at 0.16 GPa has been rationalized by the electrostatic and anisotropic van der Waals interactions of the I atoms. No ferroelectric behaviour of the Fmm2 polar phase II of CH2I2 has been determined. The diffraction, calorimetric and dielectric constant studies reveal considerable temperature hysteresis of transformations between the CH2I2 phases, as well as metastable regions strongly dependent on the sample shape and history. [ABSTRACT FROM AUTHOR]

Ti(C,N)-reinforced alumina-zirconia composites with different ratios of C to N in titanium carbonitride solid solutions, such as Ti(C0.3,N0.7) (C:N = 30:70) and Ti(C0.5,N0.5) (C:N = 50:50), were tested to improve their mechanical properties. Spark plasma sintering (SPS) with temperatures ranging from 1600 °C to 1675 °C and pressureless sintering (PS) with a higher temperature of 1720 °C were used to compare results. The following mechanical and physical properties were determined: Vickers hardness, Young's modulus, apparent density, wear resistance, and fracture toughness. A composite with the addition of Ti(C0.5,N0.5)n nanopowder exhibited the highest Vickers hardness of over 19.0 GPa, and its fracture toughness was at 5.0 Mpa·m1/2. A composite with the Ti(C0.3,N0.7) phase was found to have lower values of Vickers hardness (by about 10%), friction coefficient, and specific wear rate of disc (Wsd) compared to the composite with the addition of Ti(C0.5,N0.5). The Vickers hardness values slightly decreased (from 5% to 10%) with increasing sintering temperature. The mechanical properties of the samples sintered using PS were lower than those of the samples that were spark plasma sintered. This research on alumina–zirconia composites with different ratios of C to N in titanium carbonitride solid solution Ti(C,N), sintered using an unconventional SPS method, reveals the effect of C/N ratios on improving mechanical properties of tested composites. X-ray analysis of the phase composition and an observation of the microstructure was carried out. [ABSTRACT FROM AUTHOR]

Ti(C 0.5 ,N 0.5)-reinforced alumina matrix composites with an addition of 2 wt% ZrO 2 were tested to determine residual stresses of Al 2 O 3 and Ti(C 0.5 ,N 0.5) phases. The advanced sintering technique (spark plasma sintering ―SPS) at various temperatures of 1600°C and 1700°C was used. Vickers hardness HV1, Young's modulus E, apparent density ρ and indentation fracture toughness K IC(HV) were evaluated. An indirectly residual stress measurement by the XRD method using the sin2 ψ technique was applied. Compressive residual stresses in both phases: α-Al 2 O 3 and Ti(C 0.5 ,N 0.5) were observed. Residual stresses of α-Al 2 O 3(226) are in the range between −204 ± 20 MPa and −120 ± 20 MPa (for 1600 °C and 1700 °C respectively) are lower compared to Ti(C 0.5 ,N 0.5) (420), for which the stresses are in the range of between −292 ± 20 MPa and −256 ± 20 MPa (for 1600 °C and 1700 °C respectively). The results exhibit the influence of the sintering temperature on the residual stresses of the tested phases. The residual stresses revealed at 1700°C are lower by about 40% for α-Al 2 O 3(226) and much less for Ti(C 0.5 ,N 0.5) (420) , by only about 15%. Microstructure studies using scanning electron microscopy, X-ray and electron diffraction phase analysis were used. [ABSTRACT FROM AUTHOR]

This paper analyses the key findings of a study devoted to PET-modified bitumen. The research program was run according to the D-optimal experimental plan based on a factorial design. Five factors, i.e., the type of polymer (source), the type of bitumen (qualitative factors), PET amount, mixing rate, and mixing temperature (quantitative factors), controlled the bitumen–polymer mixing process. The experiment included a series of determinations of bitumen's rheological characteristics obtained by MSCR (Jnr, R) and G*/sin(δ) at 50 °C, 60 °C, and 70 °C. The low-temperature properties of the composite (critical temperature) were evaluated using a BBR test. The findings showed that bitumen modification with PET primarily reduced the creep susceptibility of the bituminous–polymer mixture. The low-temperature characteristics of the modified bitumen played a secondary but essential role. The amount of polymer and the mixing rate interacted with the temperature, significantly reducing the stiffness of the composite, while the type and amount of bitumen had a substantial effect on the results obtained in the BBR test. It is worth noting that when combining bitumen and plastomer, special attention should be paid to ensuring a high level of homogeneity of the mixture by controlling the parameters of the mixing process accordingly. The tests and analyses provided crucial models (GLM), which allowed for the prediction of the plastomer-modified bitumen's low- and high-temperature properties. The resulting relationships between factors and the identification of their impact on the bitumen properties enable a better understanding of the process of bitumen modification with PET. The conclusions presented here serve as a basis for future optimisation of the modified bitumen composition. The performed studies indicate that the use of >3% plastomer in bitumen 70/100 allows for a reduction in its susceptibility (MSCR) to below 0.5 kPa−1, making it suitable for bituminous mixtures for high-traffic roads. No significant increase in critical temperature (BBR) was observed. [ABSTRACT FROM AUTHOR]

High‐nitrogen‐content compounds 6‐azido‐1,2,4‐triazolo[4,3‐b]pyridazine (C5H3N7) and its 3‐methyl derivative (C6H5N7) have been in situ crystallized in a diamond‐anvil cell and their structures determined by single‐crystal X‐ray diffraction. Under ambient and high‐pressure conditions the crystallizations yield the same phases: the C5H3N7 anhydrate and C6H5N7 hydrated clathrate. In both the structures there are clearly distinguished regions of short CH...N and N...N intermolecular contacts, the latter involving exclusively the azide groups. High pressure initially increases the contents of water in the channel pores of the clathrate. [ABSTRACT FROM AUTHOR]

The article focuses on the study of isostructural polymorphs of ethynylbenzene which force to freeze the phenylacetylene (PA) favors cooperative. It is inferred that ethynylbenzene is the prototypic aromatic hydrocarbon where cohesive forces are dominated by CH-interactions. According to the study, the density of PAx at 0.4GPa of 1.131 g cm is slightly higher than the PAa, and the analogous compounds was lower.

• A novel composite ablator based on silicone resin and B 4 C ceramics is shown. • Methylpolysiloxane ablation rates significantly reduced by formed B 2 O 3 on surface. • Methylpolysiloxane pyrolyses to SiOC and SiO 2. • The presence of B 4 C promotes β-SiC crystallisation during pyrolysis and ablation. Before siloxane resin matrix composites could be successfully used as ablative materials, their mechanism of high-temperature degradation must be investigated in depth. In this study, degradation mechanism, ablation resistance and degradation kinetics of both methylpolysiloxane and the methylpolysiloxane - B 4 C (10 wt%) composite were investigated.. The presence of B 4 C resulted in a higher final sample mass in thermogravimetric tests in synthetic air up to 1500C (85% vs 81%), while during ablation tests it reduced linear and mass ablation rates by 45% and 54%, respectively. The XRD and SEM/EDS studies provided an estimate of the phase contributions formed as a result of exposure to corrosive conditions. The effect of the presence of powders on the amount of SiO 2 glassy phase, β-SiC crystalline phase and free carbon precipitates formed is apparent. [ABSTRACT FROM AUTHOR]

The aim of this study was to carry out the consolidation of zirconium diboride-reinforced composites using the SPS technique. The effect of the adopted method of powder mixture preparation (mixing in Turbula or milling in a planetary mill) and of the reinforcing phase content and sintering temperature on the microstructure, physical properties, strength and tribological properties of sintered composites was investigated. Experimental data showed that the maximum relative density of 94–98% was obtained for the composites sintered at 1100 °C. Milling in a planetary mill was found to contribute to the homogeneous dispersion and reduced clustering of ZrB2 particles in the steel matrix, improving in this way the properties of sintered steel + ZrB2 composites. Morphological and microstructural changes caused by the milling process in a planetary mill increase the value of Young's modulus and improve the hardness, strength and wear resistance of steel + ZrB2 composites. Higher content of ZrB2 in the steel matrix is also responsible for the improvement in Young's modulus, hardness and abrasive wear resistance. [ABSTRACT FROM AUTHOR]

Abstract The wear resistance and tribological characteristics of spark plasma sintered ZrB 2 + B 4 C, ZrB 2 + SiC and ZrB 2 + ZrC composites were investigated under dry sliding conditions at applied loads of 5 N and 50 N in air. The microstructure, deformation and damage characteristics were studied using scanning electron microscopy, confocal electron microscopy, a focused ion beam and atomic force microscopy. The friction coefficient values were very similar for all composites with values ranging from 0.63 to 0.72 and with the lowest value recorded for the ZrB 2 + SiC composite at a 5 N applied load. The ZrB 2 + ZrC composite was the most wear resistant, with wear rates at a 5 N load of 6.15 × 10−6 mm3/(N·m) and at a 50 N of 7.3 × 10−6 mm3/(N·m). None, or a very limited number of grain pull-outs and/or lateral fractures of grains were found during the wear tests. At the 5 N load, abrasive grooves connected with deformations and Hertzian crack formations were the main wear mechanisms in all systems, with limited crack formations in the ZrB 2 + ZrC composite. Tribofilm formations connected with debris origin, oxidation and tribochemical reactions were dominant in all composites, with similar chemical compositions but different sizes and thicknesses at the 50 N load. Highlights • To enhance the oxidation resistance, COF, WR and KIC different additives (SiC, B 4 C and ZrC) have been introduced to ZrB 2. • Detailed understanding of the tribological characteristics of Zirconium Diboride composites. • Description and understanding of tribochemical reactions. [ABSTRACT FROM AUTHOR]

The deformation of the cold recycled mixture with foamed bitumen in a recycled base with an innovative three-component road binder and foamed bitumen is analysed. Numerical simulation results for the pavement constructed, based on laboratory test results, were verified against the data from the monitoring system installed on the road trial section. In addition, environmental effects, such as air temperature and humidity levels in the pavement structure layers, were considered. Thermal analyses were conducted to identify the thermal properties of the pavement materials under steady heat transfer rate. Determining temperature distribution in the road cross-section in combination with relaxation functions determined for individual pavement layers contributed to the high effectiveness of the numerical simulation of deformation and displacement in the recycled base and the entire pavement. The experimental method of identifying thermal properties allows a fast and satisfactory prediction of temperature distribution in the pavement cross-section. [ABSTRACT FROM AUTHOR]

Zr-2.5Cu and Zr-10Cu powder mixtures were consolidated in the extrusion process and using the spark plasma sintering technique. In these studies, material tests were carried out in the fields of phase composition, microstructure, hardness and tensile strength for Zr-Cu materials at room temperature (RT) and 400 °C. Fractography analysis of materials at room temperature and 400 °C was carried out. The research took into account the anisotropy of the materials obtained in the extrusion process. For the nonequilibrium SPS process, ZrCu2 and Cu10Zr7 intermetallic compounds formed in the material at sintering temperature. Extruded materials were composed mainly of α-Zr and ZrCu2. The presence of intermetallic compounds affected the reduction in the strength properties of the tested materials. The highest strength value of 205 MPa was obtained for the extruded Zr-2.5Cu, for which the samples were cut in the direction of extrusion. For materials with 10 wt.% copper, more participation of the intermetallic phase was formed, which lowered the mechanical properties of the obtained materials. In addition to brittle intermetallic phases, the materials were characterized by residual porosity, which also reduced the strength properties. [ABSTRACT FROM AUTHOR]

Materials were obtained from commercial zirconium powders. 1 mass%, 2.5 mass% and 16 mass% of niobium powders were used as the reinforcing phase. The SPS method and the extrusion method classified as the SPD method were used. Relative density materials of up to 98% were obtained. The microstructure of the sintered Zr-xNb materials differs from that of the extruded materials. Due to the flammability of zirconium powders, no mechanical alloying was used; only mixing of zirconium and niobium powders in water and isopropyl alcohol. Niobium was grouped in clusters with an average niobium particle size of about 10 μm up to 20 μm. According to the Zr-Nb phase equilibrium system, the stable phase at RT was the hexagonal α-phase. The tests were carried out for materials without the additional annealing process. The effect of niobium as a β-Zr phase stabilizer is confirmed by XRD. Materials differed in their phase composition, and for both methods the β-Zr phase was present in obtained materials. A very favorable effect of niobium on the increase in corrosion resistance was observed, compared to the material obtained from the powder without the addition of niobium. [ABSTRACT FROM AUTHOR]

The research concerns the optimisation of sintering zirconium by spark plasma sintering (SPS) and modification of microstructures by introducing the manganese component. The problems of preparing mixtures for sintering were investigated. An additive of 2.5 wt% and 5 wt% manganese micropowders and 1 wt% and 2.5 wt% manganese nanopowders were utilized. An increase in the oxygen content in sintered mixtures made of zirconium and manganese along with an increase in their milling time in water was found. 100 rpm was determined as a safe mixing speed. The introduction of manganese nanopowders into zirconium did not significantly improved the homogeneity of the material. Manganese in larger quantities accumulates at the grain boundaries. The material is very difficult to machining, which is indicated by difficulties in sample preparation. • The conditions of high-speed mixing and sintering by the SPS method did not cause the entire manganese content to react to form ZrMn 2. • Due to the explosiveness of the mixture, 200 rpm was adopted as the optimal speed of homogenization of mixtures. • Mechanical milled Zr–Mn mixtures tend to oxidize. [ABSTRACT FROM AUTHOR]

The sintering behaviours, phase compositions, microstructures, and mechanical properties of Al 2 O 3 -based matrix composites reinforced with up to 20 vol% of cubic boron nitride (cBN, super-hard phase) were investigated. The materials were prepared via the method of spark plasma sintering (SPS). Additionally, pure cBN powder was treated under identical SPS conditions for the purpose of comparison. The temperatures at which hexagonal boron nitride (hBN, graphite-like phase) was detected in pure cBN and in cBN dispersed in the Al 2 O 3 + 10 TiN matrix were 1600 °C and 1300 °C, respectively. The presence of additives in the Al 2 O 3 matrix had a pronounced influence on the formation of hBN, with TiN > ZrO 2 > pure Al 2 O 3. All the composites exhibited quite good improvements in fracture toughness, of about 1.5 MPa·m1/2 on average over that of Al 2 O 3. Crack deflection on cBN grains was identified as the main toughening mechanism of the ceramics investigated. Unlabelled Image • Composites containing cubic boron nitride (cBN) have been sintered at low pressure. • Spark plasma sintering (SPS) method allows to obtain full dense composite at 1300 °C. • Al 2 O 3 -based composites with cBN have better fracture toughness than pure Al 2 O 3. • During SPS pure cBN is more stable then cBN dispersed in ceramic matrix. • TiN promotes of graphite-like, hexagonal boron nitride formation most extensively. [ABSTRACT FROM AUTHOR]