B₄C ceramics were fabricated by spark plasma sintering (SPS) technique with 5 vol.% silicon as sintering additive. Optimization of SPS method production parameters for B₄C ceramics having geometries 50×50×5 mm, square cross section will be performed. The sintering process was carried out at different temperatures by applying 40 MPa of pressure under vacuum atmosphere. The effect of silicon additive, sintering temperature and different soaking times on density, vickers hardness, fracture toughness and microstructure were examined. The mechanical properties of the B₄C ceramics having silicon as additive were compared with the results of monolithic B₄C. The hardness and fracture toughness of the samples were evaluated by the vickers indentation technique. Microstructures of spark plasma sintered B₄C samples with different parameters in square cross section were characterized by using SEM technique.
In this study, the effect of milling speed on particle size and morphology of Cu25W composite powder produced by high-energy ball milling was investigated. For this aim, commercial elemental copper and tungsten powders were milled in a planetary-type ball mill for different milling durations. Ball-to-powder weight ratio was selected as 10:1. Three different milling speeds, namely 200, 300, and 400 rpm were used throughout the tests. In order to avoid agglomeration and to decrease the tendency of cold welding among powder particles, stearic acid in amount of 2 wt.% was used as a process control agent. The morphological and microstructural evolution of the milled powders was evaluated by scanning electron microscopy. In addition, the variation of particle size and powder morphology as a function of milling duration was determined. As a result of this effort, the milling duration was found to have strong effect on the structural evolution of the powder, and the optimum particle size as a function of milling speed was determined.
In this study, the effects of sintering time on hardness and wear behaviour were investigated of carbon nanotubes reinforced aluminium matrix composites. 1% multi wall carbon nanotubes (90% purity with 9.5 nm in diameter, 1.5 μm in length) and gas atomized 7075 Al alloy powders were mechanical milled for 120 min in a planetary ball mill. Mechanical milled aluminium composite powders were cold pressed under 520 MPa. Pre-shaped samples were sintered in atmosphere controlled furnace at 580°C for three different sintering times (1, 2, and 3 h). As a result of study, it was observed that the hardness values of composites were decreased with increasing sintering time and the weight loss was decreased. It was determined from worn surface SEM images that adhesive wear mechanisms were dominant.
W-1 wt% Ni (W1Ni) matrix composites reinforced with TiB_2 and La_2O_3 particles were fabricated via mechanical alloying and activated sintering methods. Powder blends with compositions of W1Ni-2 wt% TiB_2-x wt% La_2O_3 (x = 0.5, 1) were mechanically alloyed for 6 and 12 h. The results showed that increase in mechanical alloying duration to 12 h causes the decline of grain sizes of the W-Ni matrix to nanoscales. TiB_2/La_2O_3 particles have a significant effect on the density/microhardness values and wear amounts of the sintered samples.
Outstanding properties of sintered ceramics due to lower sintering temperatures and smaller grain sizes are of much attention to many researchers. In this study, YAG phase was formed successfully with mechanical activation of powder mixtures by high energy ball milling of powders at different speeds. The powders were compacted and sintered at three different temperatures to evaluate the sintering density, phase formation and grain formation. It was found that increasing activation time, which agitates the powder mixing more accurately, has led to an increase in the relative density, as compared to non-activated samples, sintered at same temperatures. Up to 95% ot the theoretical density were reached, indicating the partial liquid phase formation of Y-A related phases. YAG phase formation and crystallite size were evaluated using XRD and Debye-Scherrer formula. The studies of grain size and surface morphology were conducted using SEM. Since the mechanical activation of ceramic powders occurs by fragmentation and crack propagation, by brittle fracture of powders, the main mechanism of reduction of sintering temperature can be concluded to be the decreasing grain size, as well as the increasing strain on fine powder grains.
Reactive milling of NiO + Al powder mixture resulted in the formation of NiAl-Al_2O_3 nanocomposite powders, with a crystallite size of about 20 nm. The Hall-Williamson analysis revealed that NiAl showed an orientation dependent crystallite size after short processing time and orientation dependent internal strain after long milling time. Both anisotropies were removed by heating the powders in the differential scanning calorimetry. Calorimetric studies showed one exothermic effect attributed to the reduction reaction of NiO and endothermic one associated with melting of Al. Two methods were applied for powders compaction: resistance sintering and pulse electric discharge. In both cases the densities of about 90% of the theoretical value were achieved. A significant increase in average NiAl crystallites size in compacted samples was observed, up to several hundreds of nanometers.
CuSn10 pre-alloyed bronze with iron and graphite powders were mixed, pressed and sintered for the bronze pad fabrication. The powder mix was pressed under pressure in the range of 100-600 MPa and sintered at temperatures between 780-850°C. The optimum compression was at 500 MPa and the optimal sintering temperatures was 730°C. 2 wt.% of graphite addition was sufficient to adjust the friction and wear properties of produced bronze pad samples. Optical microscope and SEM images showed that a homogenous powder mix was achieved. The produced bronze samples and the commercial ones were compared and beneficial properties of them were determined. The wear behaviours of both the produced friction materials and the commercial pads were examined. The coefficient of friction and wear rates were determined. The sintered bronze samples and the commercial bronze pads have exhibited similar wear behaviour, although the commercial one have contained ceramic particles.
This paper was focused on the effects of particle size and distribution on some properties of the SiC particle reinforced Cu composites. Copper powder produced by cementation method was reinforced with SiC particles having 1 and 30 μm particle size and sintered at 700°C. Scanning electron microscopy studies showed that SiC particles were dispersed in copper matrix homogeneously. The presence of Cu and SiC components in composites were verified by X-ray diffraction analysis technique. The relative densities of Cu-SiC composites determined by Archimedes' principle are ranged from 96.2% to 90.9% for SiC with 1 μm particle size, 97.0% to 95.0% for SiC with 30 μm particle size. Measured hardness of sintered compacts varied from 130 to 155 HVN for SiC having 1 μm particle size, 188 to 229 HVN for SiC having 30 μm particle size. Maximum electrical conductivity of test materials was obtained as 80.0% IACS (international annealed copper standard) for SiC with 1 μm particle size and 83.0% IACS for SiC with 30 μm particle size.
In the present work, the characterization and production of CoTi intermetallic materials produced by electric current activated sintering under 300 MPa uniaxial pressure in open air at 2000 A for 6 min was investigated. Cobalt powder with 10 μm size and titanium powder < 40 μm size having 99.9% and 99.5% purity, respectively, were used. The elemental powders were mixed in the stoichiometric ratio corresponding to the CoTi intermetallic, in a molar proportion of 1:1. Scanning electron microscopy and X-ray diffraction analysis were used to characterize produced samples. In microstructural examinations it was found that the sample has multi-phase microstructure. X-ray diffraction studies revealed that the phases are CoTi, CoTi_2, TiCo_2, and CoTiO_3. The relative density of test materials measured according to Archimedes' principle was 87.6%, and the microhardness of materials was about 646.74 HV_{0.1}.
The present study reports on Ni_3Al and Ti_3Al-based intermetallics coated on AISI 1010 steel substrate by one-step pressure assisted electric current activated sintering method. Ni, Ti, and Al elemental powders were mixed in the stoichiometric ratio corresponding to the Ni_3Al and Ti_3Al intermetallics at molar proportion of 3:1. The mixed coating powders were placed onto the steel substrate in a mold, and pressed with compressive stress of 100 MPa and then, electric current: 1100-1200 A, voltage 2.9-3.4 V was applied for 15 min during coating. As-synthesized coatings seem to have good adherence with many small porosities. The phases formed in the Ni_3Al coating layer were Ni_3Al as a major phase beside NiO and NiAl_2O_4 trace phases, which were confirmed by X-ray diffraction analysis. However, TiAl and Ti trace phases besides major Ti_3Al phase were detected in the Ti_3Al coating. The hardness of the Ni_3Al, Ti_3Al coatings and AISI 1010 substrate was approximately 321 ± 18, 445 ± 13 and 157 HV_{0.5}, respectively.
In this study we have investigated fabrication of in situ metallic- intermetallic Ti-TiAl₃ composites from powder mixture containing 40 wt % Ti-Al, 50 wt % Ti-Al and 60 wt % Ti-Al by electric current activated sintering method. Powder mixtures without additive were compressed uniaxially under 130 MPa of pressure and sintered 2000 A current for 20 minutes in a steel mould. Microstructures of sintered samples were investigated by optic and scanning electron microscopes, phases in samples were analyzed by XRD and their hardness was measured by Vickers hardness tester. Optic and scanning electron microscopes investigations showed that microstructures of samples were consisting of two components: Main component was titanium aluminide and other was metallic titanium. Besides this there was a trace amount of aluminium oxide in the sintered body. XRD analyses also demonstrated that main phase is TiAl₃. It was determined that as weight percentage of titanium in the mixture was decreasing, also the amount of metallic titanium has decreased in the sintered body. Additionally, average hardness values of samples were about 500 HV
In this study, TiNi intermetallic compounds were produced by electric current activated sintering in open air under an uniaxial pressure of 200 MPa at a maximum of 1200 A for 10 min using Ni powder (99.8% purity, 4-7 μm), Ti powder (99.5% purity, less than 44 μm). The elemental powders were mixed in the stoichiometric ratio corresponding to the TiNi intermetallic at molar proportion of 1:1. Scanning electron microscopy and X-ray diffraction analysis were used to characterize produced samples. X-ray diffraction studies revealed that the dominant phases are TiNi, NiTi_2, Ni_3Ti, TiO, and Ni_2Ti_3. Scanning electron microscopy examinations showed a dense microstructure with very low amount of porosity. The relative density of test materials measured according to Archimedes' principle was 96.8%, and the microhardness of materials was about 773.6 ± 123 HV_{0.05}.
This paper is intended to highlight the effect of copper addition on the pitting corrosion resistance of aluminium-base powder metallurgy parts. Results obtained on these mechanically alloyed (MA) specimens are compared with parts of MA-Al without added copper, as well as with commercial aluminium alloys. Immersion tests from 2 to 96 hours in 3.5% NaCl solutions, and potentiostatic techniques, were used to study the pitting corrosion. It was concluded that copper addition, in a similar way that in commercial aluminium alloys, produces a negative effect on the pitting corrosion resistance, because of the formation of Al₂Cu. These precipitates produce galvanic cells that favour the specimen pit. Therefore, increasing the copper content of MA-Al, although improving their ductility, worsens the pitting corrosion resistance of these alloys.
Agglomeration is the main problem that prevents large-scale implementation of nanodiamonds in the production of composites. Mechanical alloying was applied for crushing the agglomerates and to obtain uniform distribution of the primary nanodiamond particles in aluminium matrix composites. The commonly used X-ray diffraction method fails to detect non-agglomerated diamond nanoparticles 5 to 6 nm in size, if they are incorporated in a metal matrix. Synchrotron radiation was used for the identification of non-agglomerated nanodiamonds. Scanning electron microscopy and synchrotron investigation showed that mechanical alloying does not lead to transformation of the diamond structure into other allotropic forms of carbon and the nanodiamond reinforcing particles are uniformly distributed in the aluminium matrix.
In this study, the effect of mechanical alloying parameters, namely the effect of process control agent, ball-to-powder weight ratio and milling duration, on the synthesis of Cu25W composite powder was investigated. Planetary-type ball milling equipment was used to conduct mechanical alloying experiments. Stearic acid was used as the process control agent in order to establish a balance between cold welding and fracturing. The optimum amount of stearic acid was determined as a function of particle size and milling time at constant speed. By using this optimum amount of process control agent, three different ball-to-powder weight ratio values were also employed, and the effect of ball-to-powder weight ratio on particle size and morphology of Cu25W composite powders was investigated. The microstructural evolution of the milled powders was characterized using scanning electron microscopy and laser diffraction analysis. The test results have shown that the morphology and particle size distribution of the milled powders change significantly depending upon the milling parameters. In addition, higher ball-to-powder weight ratio values tend to lower the milling duration for the same amount of particle size reduction. However, particle size reduction suffers beyond the maximal value of ball-to-powder weight ratio, especially in the later stages of mechanical alloying.
Hydroxyapatite (HA: Ca_{10}(PO₄)₆(OH)₂) can be synthesized using several methods or manufactured from natural materials such as coral or bone after removal of the organic matter by heating (denoted as NHA). The "in vitro" and "in vivo" studies showed that the natural apatite was well tolerated and has better osteoconductive properties than synthetic HA. In addition, the exploitation of natural source represents an economical way of synthesizing NHA by means of sintering, rather than by sol-gel techniques. For these reasons, the NHA was manufactured from cortical bovine bones in all our studies. Moreover, there has been much effort to improve the mechanical properties of HA by introducing foreign oxides or finding out other alternative processes such as grain growth control. Indeed, encouraging lower AGS instead of exaggerated grain growth may be jugged useful for many applications. Since the works carried out on the correlation between AGS and physico-chemical properties of NHA were very limited, the present study was mainly focused on its grain growth. A carful combination between the main parameters controlling NHA production such as milling techniques, compacting pressure, sintering temperature and holding time may lead to an interesting NHA based bio-ceramics. In this way, a simple and energetically vibratory multidirectional milling system using bimodal distribution of highly resistant ceramics has been used for obtaining sub-micron sized NHA powders. For example, the AGS was ranged between 0.75 and 1.40 μm (using intercept method) when NHA samples were sintered at 1250°C for 15 and 480 min, respectively.
Boron carbide (B₄C) ceramics were produced by spark plasma sintering technique with 5, 10, 15, and 20 vol.% aluminum (Al) in order to improve sintering behaviours of B₄C ceramics. B₄C ceramics were produced, having square cross-section and 50 × 50 × 5 mm³ dimensions. The sintering process was carried out at different temperatures by applying 40 MPa of pressure with 100°C/min under vacuum. The effects of various amounts of Al additive and sintering temperature on density, vickers hardness, fracture toughness and microstructure were examined. The hardness and fracture toughness of the samples were evaluated by the Vickers indentation technique. Microstructures of the samples were characterized by scanning electron microscopy technique. Fast neutron attenuation properties of the ceramics having highest density were also investigated.
This paper reports results of a study aimed at understanding the precipitation processes occurring during the annealing of two Al-Sc-Zr-based alloys with and without Mn prepared by powder metallurgy with subsequent hot extrusion at 350°C. Samples were isochronally annealed up to ≈ 570°C. Precipitation behaviour was studied by electrical resistometry and differential scanning calorimetry. Mechanical properties were monitored by microhardness HV1 measurements. Transmission electron microscopy examinations and X-ray diffraction of specimens quenched from temperatures of significant resistivity changes helped to identify the microstructural processes responsible for these changes. Fine (sub)grain structure develops and fine coherent Al_3Sc and/or Al_3(Sc,Zr) particles precipitate during extrusion in both alloys. The distinct changes in resistivity (at temperatures above ≈ 330°C) of the Al-Mn-Sc-Zr alloy are mainly caused by precipitation of Mn-containing particles. The easier diffusion of Mn atoms along the (sub)grain boundaries is responsible for the precipitation of the Al_6Mn and/or Al_6(Mn,Fe) particles at relatively lower temperatures compared to the temperature range of precipitation of these particles in the classical mould-cast Al-Mn-Sc-Zr alloys The apparent activation energy for precipitation of the Al_3Sc and Al_6Mn particles in the Al-Mn-Sc-Zr alloy was determined as (106 ± 10) kJ mol^{-1} and (152 ± 33) kJ mol^{-1}, respectively.
Mechanical alloying was used to synthesize LaNi_5-type hydrogen storage materials. X-ray diffraction analysis showed that, after 30 h milling, the starting mixture of the elements was decomposed into an amorphous phase. Following the annealing in high purity argon at 700°C for 0.5 h, X-ray diffraction confirmed the formation of the CaCu_5-type structures. The nanocrystalline materials were used as negative electrodes for a Ni-MH_x battery. A partial substitution o Ni by Al or Mn in LaNi_{5-x}M_x alloy leads to an increase in discharge capacity. On the other hand, the alloying elements such as Al, Mn and Co greatly improved the cycle life of LaNi_5 material. For example, in the nanocrystalline LaNi_{3.75}Mn_{0.75}Al_{0.25}Co_{0.25} powder, discharge capacities of up to 258 mA h g^{-1} (at 40 mA g^{-1} discharge current) were measured. The band structure ab initio calculations showed that 3g sites are preferred by Al, Co, and Mn atoms in the unit cell.
SiC ceramics were fabricated by spark plasma sintering technique with the use of Al_2O_3 additive. The sintering process was carried out at three different temperatures in the range of 1700-1800C applying two different pressures 40 and 80 MPa under vacuum atmosphere. The effect of additive, different temperatures and pressures on densification behaviour, density, Vickers hardness, fracture toughness, and microstructure were examined. The hardness and fracture toughness of the samples were evaluated by the Vickers indentation technique. Microstructure of spark plasma sintered SiC samples were characterized by using scanning electron microscopy technique. The highest value of fracture toughness 5.9 ± 0.2 MPa m^{1/2} was achieved with the addition of 5 vol.% Al_2O_3.
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