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EN
In order to investigate the effect of the milling time on the corrosion resistance of the Mg65Zn30Ca4Pr1 alloy, powders of the alloy were prepared and milled for 13, 20, and 70 hours, respectively. The samples were sintered using spark plasma sintering (SPS) technology at 350◦C and pressure of 50 MPa. The samples were subjected to potentiodynamic immersion tests in Ringer’s solution at 37◦C. The obtained values of Ecorr were –1.36, –1.35, and –1.39 V, with polarization resistance Rp = 144, 189, and 101 Ω for samples milled for 13, 20 and 70 h, respectively. The samples morphology showed cracks and pits, thus signaling pitting corrosion.
EN
A TiC-Mo2C-WC-Ni alloy cermet was fabricated by high-energy ball milling (HEBM) and consolidation through spark plasma sintering. The TiC-based powders were synthesized with different milling times (6, 12, 24, and 48 h) and subsequently consolidated by rapid sintering at 1300°C and a load of 60 MPa. An increase in the HEBM time led to improved sinterability as there was a sufficient driving force between the particles during densification. Core-rim structures such as (Ti, W)C and (Ti, Mo)C (rim) were formed by Ostwald ripening while inhibiting the coarsening of the TiC (core) grains. The TiC grains became refined (2.57 to 0.47 µm), with evenly distributed rims. This led to improved fracture toughness (11.1 to 14.8 MPa·m1/2) owing to crack deflection, and the crack propagation resistance was enhanced by mitigating intergranular fractures around the TiC core.
EN
This study aimed to prepare Zr55Cu30Al10Ni5 bulk amorphous alloys by spark plasma sintering of raw amorphous alloy powders and investigate their microstructure and micromechanical behaviors. When the sintering temperature (Ts) was 675K, which was lower than the glass transition temperature (Tg) of the material, the sintered sample was almost fully amorphous but the density was lower. However, when Ts was 705K, which was higher than Tg, partial crystallization occurred, but the density was higher. The hardness of the bonding zone of the sintered sample at 675K was 5.291 GPa due to the lower density, which was lower than that at 705K, and the hardness at 705K was 8.836 GPa. The generation of thermodynamically stable intermetallic phases, the hardness, and the elastic modulus of the samples sintered above Tg were higher due to the higher density.
EN
In this work, hexagonal boron nitride powder was used for the lubrication of an interface of TiB2/Ti composite protected by an AlCrN coating and a ceramic Si3N4 ball. The wear behaviour of this tribo-pair in an oscillating motion was studied with an SRV tribotester at the temperature range from room temperature to 900 °C. The action of hexagonal boron nitride as a solid lubricant was analysed with the use of a 3D microscopy and energy-dispersive spectroscopy. The test results confirmed that under high-temperature conditions, the use of hexagonal boron nitride as a solid lubricant does not increase the wear resistance of the TiB2/Ti composite. The use of the AlCrN coating significantly reduces wear at the temperature up to 600 °C only, while the combined use of the AlCrN coating and hBN lubrication provides effective protection against wear even at the temperature up to 900 °C. Therefore, the synergy of the anti-wear action of the coating and the solid lubricant was proved.
PL
W niniejszej pracy wykorzystano heksagonalny azotek boru (hBN) jako smarującą międzywarstwę między podłożem kompozytowym z TiB2/Ti chronionym powłoką AlCrN a przeciwpróbką – kulką ceramiczną wykonaną z Si3N4. Testy tribologiczne wykonano z zastosowaniem stanowiska SRV. Zbadano zużycie ścierne w ruchu oscylacyjnym w zakresie od temperatury pokojowej do 900°C. Rola hBN jako stałego środka smarowego została zbadana z wykorzystaniem mikroskopii 3D oraz spektroskopii rentgenowskiej z dyspersją energii. Wyniki przeprowadzonych badań potwierdziły, że w warunkach wysokich temperatur zastosowanie heksagonalnego azotku boru pełniącego funkcję smaru stałego nie powoduje zwiększenie odporności na zużycie kompozytu TiB2/Ti. Zastosowanie powłoki AlCrN powoduje znaczącą redukcję zużycia jedynie do temperatury 600°C, podczas gdy łączne zastosowanie powłoki AlCrN i smarowania hBN stanowi skuteczną ochronę przed zużyciem nawet do 900°C. Wykazano zatem synergię przeciwzużyciowego działania powłoki i smaru stałego.
EN
Doping is one of the possible ways to significantly increase the thermoelectric properties of many different materials. It has been confirmed that by introducing bismuth atoms into Mg sites in the Mg2Si compound, it is possible to increase career concentration and intensify the effect of phonon scattering, which results in remarkable enhancement in the figure of merit (ZT) value. Magnesium silicide has gained scientists’ attention due to its nontoxicity, low density, and inexpensiveness. This paper reports on our latest attempt to employ ultrafast self-propagating high-temperature synthesis (SHS) followed by the spark plasma sintering (SPS) as a synthesis process of doped Mg2Si. Materials with varied bismuth doping were fabricated and then thoroughly analyzed with the laser flash method (LFA), X-ray diffraction (XRD), scanning electron microscopy (SEM) with an integrated energy-dispersive spectrometer (EDS). For density measurement, the Archimedes method was used. The electrical conductivity was measured using a standard four-probe method. The Seebeck coefficient was calculated from measured Seebeck voltage in the sample subjected to a temperature gradient. The structural analyses showed the Mg2Si phase as dominant and Bi2Mg3 located at grain boundaries. Bismuth doping enhanced ZT for every dopant concentration. ZT = 0.44 and ZT=0.38 were obtained for 3wt% and 2wt% at 770 K, respectively.
EN
In this work, aluminum (Al)-based nanocomposites reinforced with graphite nanoplatelets (GnPs) have been fabricated by conventional sintering as well as spark plasma sintering (SPS) techniques, and their microstructure and mechanical properties have been studied. The powder metallurgy (PM) route has been adopted to fabricate the various Al–GnP nanocomposites. Characterization of the powder mixtures and the nanocomposites has been carried out through different characterization techniques, such as X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), and Raman spectroscopy. Compressive strength, Young's modulus, density, and Vickers microhardness of the various nanocomposites have also been determined. The HRTEM results show the formation of nonstoichiometric Al4C3 nanoparticles – during both conventional sintering and SPS – at the interface of the Al grains and GnP, which worsen the mechanical properties of the nanocomposites. SPSed nanocomposites show superior mechanical properties due to higher densification, finer grain size, and homogeneous nanofiller dispersion in the Al matrix, compared to the conventionally sintered Al–GnP nanocomposites.
PL
W artykule przedstawiono sposób wytworzenia kompozytów na osnowie miedzi umacnianych dodatkiem 5% wag. azotku tytanu. W tym celu zastosowano proces mechanicznej syntezy (MA) i iskrowego spiekania plazmowego (SPS). Zaobserwowano, że 10-cio godzinny proces mechanicznej syntezy doprowadził do utworzenia się struktury płatkowej mieszanki kompozytowej Cu-TiN. Cząstki azotku tytanu znajdują się wewnątrz plastycznej osnowy, jednakże ich rozmieszczenie nie jest w pełni równomierne. Artykuł przedstawia mikrostrukturę mieszanki kompozytowej uzyskanej zarówno podczas mechanicznej syntezy jak i po jej zakończeniu, a także mikrostrukturę uzyskanych spieków po procesie iskrowego spiekania plazmowego. Zamieszczono wyniki dotyczące gęstości, twardości i przewodności elektrycznej kompozytów.
EN
In the presented work, Cu matrix composites reinforced with 5% wt. of TiN were prepared by mechanical alloying (MA) and spark plasma sintering (SPS) method. During experiments it was observed that 10 hours of MA lead to a flake-like particle morphology. Titanium nitride particles are located inside copper matrix but their distribution is not completely homogeneous. This article shows microstructure of the powders during and after MA as well as SPS method. Density, hardness and electrical conductivity of the composites are also presented.
EN
In this work, we have designed a new high entropy alloy containing lightweight elements, e.g., Al, Fe, Mn, Ti, Cu, Si by high energy ball milling and spark plasma sintering. The composition of Si was kept at 0.75 at% in this study. The results showed that the produced AlCuFeMnTiSi0.75 high entropy alloy was BCC structured. The evolution of BCC1 and BCC2 phases was observed with increasing the milling time up to 60 h. The spark plasma sintering treatment of milled compacts from 650-950°C showed the phase separation of BCC into BCC1 and BCC2. The density and strength of these developed high entropy alloys (95-98%, and 1000 HV) improved with milling time and were maximum at 850°C sintering temperature. The current work demonstrated desirable possibilities of Al-Si based high entropy alloys for substitution of traditional cast components at intermediate temperature applications.
EN
An optimum route to fabricate the Ni-based superalloy with homogeneous dispersion of Y2O3 particles is investigated. Ni-based ODS powder was prepared by high-energy ball milling of gas-atomized alloy powders and Y2O3 particles treated with a high-pressure homogenizer. Decrease in particle size and improvement of dispersion stability were observed by high-pressure homogenization of as-received Y2O3 particles, presumably by the powerful cavitation forces and by collisions of the particles. Microstructural analysis for the ball-milled powder mixtures reveal that Ni-based ODS powders prepared from high-pressure homogenization of Y2O3 particles exhibited more fine and uniform distribution of Ni and Y elements compared to the as-received powder. These results suggested that high-pressure homogenization process is useful for producing Ni-based superalloy with homogeneously dispersed oxide particles.
EN
WC-Co cemented carbides were consolidated using spark plasma sintering in the temperature 1400°C with transition metal carbides addition. The densification depended on exponentially as a function of sintering exponent. Moreover, the secondary (M, W)Cx phases were formed at the grain boundaries of WC basal facet. Corresponded, to increase the basal facets lead to the plastic deformation and oriented grain growth. A higher hardness was correlated with their grain size and lattice strain. We suggest that this is due to the formation energy of (M, W)Cx attributed to inhibit the grain growth and separates the WC/Co interface.
EN
In this study, a novel composite was fabricated by adding the Hafnium diboride (HfB2) to conventional WC-Co cemented carbides to enhance the high-temperature properties while retaining the intrinsic high hardness. Using spark plasma sintering, high density (up to 99.4%) WC-6Co-(1, 2.5, 4, and 5.5 wt. %) HfB2 composites were consolidated at 1300°C (100°C/min) under 60 MPa pressure. The microstructural evolution, oxidation layer, and phase constitution of WC-Co-HfB2 were investigated in the distribution of WC grain and solid solution phases by X-ray diffraction and FE-SEM. The WC-Co-HfB2 composite exhibited improved mechanical properties (approximately 2,180.7 kg/mm2) than those of conventional WC-Co cemented carbides. The high strength of the fabricated composites was caused by the fine-grade HfB2 precipitate and the solid solution, which enabled the tailoring of mechanical properties.
12
Content available remote Modyfikowane materiały WC-Co wytwarzane metodą Spark Plasma Sintering
PL
W pracy przedstawiono wyniki badań ceramicznych materiałów o osnowie węglika wolframu, wytwarzanych metodą spiekania prądem impulsowym – Spark Plasma Sintering. Przedmiotem badań była ceramika o osnowie WC-Co przeznaczona na narzędzia skrawające lub matryce. Celem badań było opracowanie składów materiałów oraz zastosowanie metody SPS w małoseryjnym procesie produkcyjnym elementów maszyn. Badano właściwości spieków otrzymywanych zarówno z komercyjnych mieszanek WC-Co, jak również z nowoopracowanych mieszanek kompozytowych na bazie komercyjnych, modyfikowanych dodatkami faz metalicznych (stop kowar Fe/Ni/Co, Co), ceramicznych (wiskery SiC, włókna Al2O3, TiB2, B4C, Ti3SiC2), supertwardych (cBN) i grafenu. Dla każdego materiału zoptymalizowano parametry spiekania pozwalające na otrzymanie wymaganych właściwości fizycznych i mechanicznych (w tym gęstości pozornej, modułu Younga, twardości, odporności na pękanie i odporności na zużycie ścierne). Najlepszymi właściwościami odznaczał się materiał węglikowy G35N z dodatkiem 4% mas. włókien Al2O3. Taki dodatek włókien Al2O3 spowodował zwiększenie twardości węglika G35N z 1190 HV30 do 1510 HV30 przy zachowaniu jego odporności na pękanie na poziomie 16-17 MPa•m1/2. Natomiast zastosowanie fazy metalicznej Fe-Ni-Co jako modyfikatora węglika H10 spowodowało zwiększenie odporności na pękanie KIC z 9,7 MPa•m1/2 do 16,4 MPa•m1/2.
EN
The paper presents the results of research on ceramic materials with a tungsten carbide matrix produced by the method of sintering with pulse current – Spark Plasma Sintering. The subject of the research was ceramics with a WC matrix designed for cutting tools or dies. The aim of the research was to develop material compositions and to use SPS method in the production process of a small batch of machine parts. The properties of the sinters obtained from commercial WC-Co and from newly-designed composite materials based on commercial mixtures modified with the addition of metallic (Fe/Ni/Co, Co), ceramic (SiC whiskers, Al2O3 fibres, TiB2, B4C, Ti3SiC2), and super-hard (cBN) phases, and graphene were investigated. For each material, the sintering parameters were optimized to obtain the required physical and mechanical properties (including apparent density, Young’s modulus, hardness, fracture toughness and abrasion resistance). The best properties were obtained for the G35N carbide material with the addition of Al2O3 fibres (4 wt%). Such an addition of Al2O3 fibres increased the hardness of G35N carbide from 1190 HV30 to 1510 HV30 while maintaining its fracture toughness at 16-17 MPa•m1/2. In the case of H10 carbide material, the use of the metallic phase Fe-Ni-Co as a modifier resulted in the increase in fracture toughness KIC from 9.7 MPa•m1/2 to 16.4 MPa•m1/2.
EN
This paper presents the technology of powder sintering by the spark plasma sintering method, also known as the field assisted sintering technique. The mechanisms, compared to other sintering techniques, advantages of this system, applied modifications and the history of the development of this technique are presented. Spark Plasma Sintering (SPS) uses uniaxial pressing and pulses of electric current. The direct flow of current through the sintered material allows high heating rates to be reached. This has a positive effect on material compaction and prevents the grain growth of sintered compact. The SPS mechanism is based on high-energy spark discharges. A low-voltage current pulse increases the kinetics of diffusion processes. The SPS temperature is up to 500 ◦C lower than the sintering temperature using conventional methods. The phenomena that occur during sintering with the Field Assisted Sintering Technology (FAST)/SPS method give great results for consolidating all types of materials, including those which are nonconductive. This method is used, among others, in relation to metals, alloys and ceramics, including advanced and ultra-high-temperature ceramics. Due to the good results and universality of this method, in recent years it has been developed and often used in research institutions, but also in industry.
EN
One of the ways to decrease thermal conductivity is nano structurization. Cobalt triantimonide (CoSb3) samples with added indium or tellurium were prepared by the direct fusion technique from high purity elements. Ingots were pulverized and re-compacted to form electrodes. Then, the pulsed plasma in liquid (PPL) method was applied. All materials were consolidated using rapid spark plasma sintering (SPS). For the analysis, methods such as X-ray diffraction (XRD), scanning electron microscopy (SEM) and scanning transmission electron microscopy (STEM) with a laser flash apparatus (LFA) were used. For density measurement, the Archimedes’ method was used. Electrical conductivity was measured using a standard four-wire method. The Seebeck coefficient was calculated to form measured Seebeck voltage in the sample placed in a temperature gradient. The preparation method allowed for obtaining CoSb3 nanomaterial with significantly lower thermal conductivity (10 Wm–1K–1 for pure CoSb3 and 3 Wm–1K–1 for the nanostructured sample in room temperature (RT)). The size of crystallites (from SEM observations) in the powders prepared was about 20 nm, joined into larger agglomerates. The Seebeck coefficient, α, was about –200μVK–1 in the case of both dopants, In and Te, in microsized material and about −400 μK−1 for the nanomaterial at RT. For pure CoSb3 , α was about 150 μVK−1 and it stood at −50 μVK−1 for nanomaterial at RT. In bulk nanomaterial samples, due to a decrease in electrical conductivity and inversion of the Seebeck coefficient, there was no increase in ZT values and the ZT for the nanosized material was below 0.02 in the measured temperature range, while for microsized In-doped sample it reached maximum ZT = 0.7 in (600K).
EN
Due to air pollution, global warming and energy shortage demands new clean energy conversion technologies. The conversion of industrial waste heat into useful electricity using thermoelectric (TE) technology is a promising method in recent decades. Still, its applications are limited by the low efficiency of TE materials in the operating range between 400-600 K. In this work, we have fabricated Cu0.005 Bi0.5Sb1.495Te3 powder using a single step gas atomization process followed by spark plasma sintering at different temperatures (623, 673, 723, and 773 K), and their thermoelectric properties were investigated. The variation of sintering temperature showed a significant impact on the grain size. The Seebeck coefficient values at room temperature increased significantly from 127 μVK to 151 μV/K with increasing sintering temperature from 623 K to 723 K due to decreased carrier concentration. The maximum ZT values for the four samples were similar in the range between 1.15 to 1.18 at 450 K, which suggest these materials could be used for power generation in the mid-temperature range (400-600 K).
EN
The effect of TiC content on the microstructure and mechanical properties of a nanocrystalline Fe-Mn alloy was investigated by XRD analysis, TEM observation, and mechanical tests. A sintered Fe-Mn alloy sample with nano-sized crystallites was obtained using spark plasma sintering. Crystallite size, which is used as a hardening mechanism, was measured by X-ray diffraction peak analysis. It was observed that the addition of TiC influenced the average size of crystallites, resulting in a change in austenite stability. Thus, the volume fraction of austenite at room temperature afterthe sintering process was also modified by the TiC addition. The martensite transformation during cooling was suppressed by adding TiC, which lowered the martensite start temperature. The plastic behavior and the strain-induced martensite kinetics formed during plastic deformation are discussed with compressive stress-strain curves and numerical analysis for the transformation kinetics.
EN
This research describes effects of Si addition on microstructure and mechanical properties of the Al-Cr based alloys prepared manufactured using gas atomization and SPS (Spark Plasma Sintering) processes. The Al-Cr-Si bulks with high Cr and Si content were produced successfully using SPS sintering process without crack and obtained fully dense specimens close to nearly 100% T. D. (Theoretical Density). Microstructure of the as-atomized Al-Cr-Si alloys with high contents of Cr and Si was composed multi-phases with hard and thermally stable such as Al13Cr4Si4, AlCrSi, Al8Cr5 and Cr3Si intermetallic compounds. The average hardness values were 703 Hv for S5, 698 Hv for S10 and 824 Hv for S20 alloy. Enhancement of hardness value was resulted from the formation of the multi-intermetallic compound with hard and thermally stable and fine microstructure by the addition of high Cr and Si using rapid solidification and SPS process.
EN
In this study, Fe-40wt% TiB2 nanocomposite powders were fabricated by two different methods: (1) conventional powder metallurgical process by simple high-energy ball-milling of Fe and TiB2 elemental powders (ex-situ method) and (2) high-energy ball-milling of the powder mixture of (FeB+TiH2 ) followed by reaction synthesis at high temperature (in-situ method). The ex-situ powder was prepared by planetary ball-milling at 700 rpm for 2 h under an Ar-gas atmosphere. The in-situ powder was prepared under the same milling condition and heat-treated at 900°C for 2 h under flowing argon gas in a tube furnace to form TiB2 particulates through a reaction between FeB and Ti. Both Fe-TiB2 composite powder compacts were sintered by a spark-plasma sintering (SPS) process. Sintering was performed at 1150°C for the ex-situ powder compact and at 1080°C for the in-situ powder for 10 minutes under 50 MPa of sintering pressure and 0.1 Pa vacuum for both processes. The heating rate was 50°/min to reach the sintering temperature. Results from analysis of shrinkage and microstructural observation showed that the in-situ composite powder compacts had a homogeneous and fine microstructure compared to the ex-situ preparation, even though the sintered densities were almost the same (99.6 and 99.8% relative density, respectively).
EN
We investigated the austenite stability and mechanical properties in FeMnNiC alloy fabricated by spark plasma sintering. The addition of Mn, Ni, and C, which are known austenite stabilizing elements, increases its stability to a stable phase existing above 910°C in pure iron; as a result, austenitic microstructure can be observed at room temperature, depending on the amounts of Mn, Ni, and C added. Depending on austenite stability and the volume fraction of austenite at a given temperature, strain-induced martensite transformation during plastic deformation may occur. Both stability and the volume fraction of austenite can be controlled by several factors, including chemical composition, grain size, dislocation density, and so on. The present study investigated the effect of carbon addition on austenite stability in FeMnNi alloys containing different Mn and Ni contents. Microstructural features and mechanical properties were analyzed with regard to austenite stability.
PL
W artykule przedstawiono metody metalurgii proszków wykorzystywane do wykonywania wyrobów z proszków metalicznych i ceramicznych w Sieci Badawczej Łukasiewicz – Instytucie Obróbki Plastycznej. Do wytwarzania zaawansowanych materiałów metalicznych, ceramicznych oraz kompozytowych zastosowano nowoczesną metodę spiekania iskrowo-plazmowego z wykorzystaniem urządzenia SPS HP D 25-3. Urządzenie to pozwala na realizację procesów spiekania w temperaturze do 2200°C z jednoczesnym prasowaniem z siłą do 250 kN w próżni, atmosferze azotu, argonu lub wodoru. Z kolei do wykonywania wyrobów z proszków na bazie żelaza stosowana jest konwencjonalna metoda prasowania jednoosiowego na zimno i następującego po nim spiekania swobodnego w atmosferze azotowo-wodorowej zdysocjowanego amoniaku z wykorzystaniem gniazda badawczo-doświadczalnego GSMP-75 wyposażonego w piec wgłębny retortowy PSF-12/75. Maksymalna temperatura spiekania wynosi 1200°C. Ponadto omówiono przykładowe prace naukowo-badawcze zrealizowane w ramach zarówno projektów międzynarodowych finansowanych z 7 PR UE oraz Horyzontu 2020, jak i projektów krajowych realizowanych we współpracy z przemysłem. Zaprezentowano wybrane wyniki badań dotyczące kompozytowych sektorów tnących stosowanych w piłach do cięcia kamieni, kompozytowych elektrod nasadkowych stosowanych w zrobotyzowanych stanowiskach zgrzewania punktowego oraz płytek skrawających wykonanych z węglików spiekanych stosowanych w obróbce mechanicznej metali. Poza tym wskazano gałęzie przemysłu, na potrzeby których ŁUKASIEWICZ – INOP wykonuje prace naukowo-badawcze oraz realizuje wdrożenia. Zaprezentowano także ofertę współpracy dla przemysłu.
EN
The article presents the powder metallurgy methods used to make products from metallic and ceramic powders in the Łukasiewicz Research Network – Metal Forming Institute. To produce advanced metallic, ceramic and composite materials, the method of spark plasma sintering employing an SPS HP D 25-3 was used. This device allows sintering processes to be performed at temperatures up to 2200°C with simultaneous compaction with a force of up to 250 kN in vacuum, and in a nitrogen, argon or hydrogen atmosphere. On the other hand, to make products from iron-based powders, the conventional method of cold uniaxial pressing and subsequent free sintering in a nitrogen-hydrogen atmosphere of dissociated ammonia employing a GSMP-75 research and testing socket equipped with a PSF-12/75 retort furnace is used. The maximum sintering temperature is 1200°C. In addition, examples of scientific and research work carried out as part of international projects financed from EU FP7 and Horizon 2020, as well as national projects executed in cooperation with industry are discussed. Selected research results concerning composite cutting sectors used in saws for cutting stones, composite cap electrodes used in robotic spot welding stations and cutting inserts made of cemented carbides used in metal machining were presented. In addition, the branches of industry were identified for which the Łukasiewicz Research Network – Metal Forming Institute performs scientific and research works and executes implementations. A cooperation offer for industry was also presented.
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