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EN
Cu-Sn alloys have been known as bronze since ancient times and widely used as electrode materials, ornaments, tableware and musical instruments. Cu-22Sn alloy fabrication by hot forging process is a Korean traditional forged high-tin bronze. The tin content is 22 percent, which is more than twice that of bronze ware traditionally used in China and the West. Copper and tin have a carbon solubility of several ppm at room temperature, making Cu-Sn-C alloys difficult to manufacture by conventional casting methods. Research on the production of carbon-added copper alloys has used a manufacturing method that is different from the conventional casting method. In this study, Cu-22Sn-xC alloy was fabricated by mechanical alloying and spark plasma sintering. The carbon solubility was confirmed in Cu-Sn alloy through mechanical alloying. The lattice parameter increased from A0 to C2, and then decreased from C4. The microstructural characteristics of sintered alloys were determined using X-ray diffraction and microscopic analysis. As a result of comparing the hardness of Cu-22Sn alloys manufactured by conventional rolling, casting, and forging and Cu-22Sn-xC alloy by sintered powder metallugy, B0 sintered alloy was the highest at about 110.9 HRB.
EN
A 20 gram batch weight of NiTi alloy, with a nominal equiatomic composition, was produced by mechanical alloying with milling times of 100, 120, and 140 hours. The differential scanning calorimetry was used to analyze the progress of the crystallization process. The X-ray diffraction examined the crystal structure of the alloy at individual crystallization stages. The observation of the powders microstructure and the chemical composition measurement were carried out using a scanning electron microscope equipped with an energy-dispersive detector. After the milling process, the alloy revealed an amorphous-nanocrystalline state. The course of the crystallization process was multi-stage and proceeded at a lower temperature than the pure amorphous state. The applied production parameters and the stage heat treatment allowed to obtain the alloy showing the reversible martensitic transformation with an enthalpy of almost 5 J/g.
EN
This paper presents a comparative study of the preparation and characterisation of Fe38.5Co38.5 Nb7 P15Cu1 alloy produced by mechanical alloying (MA) and rapid quenching (RQ) method. In order to obtain the starting mixture (SS) in the present study, we opted for the replacement of elemental Nb and P powders with ferroalloy powders of niobium and phosphorus. Benzene was used as a control agent of the process (PCA) for wet MA. The samples obtained (powders and ribbons) were characterised by X-ray diffraction (XRD), differential scanning calorimetry (DSC), scanning electron microscopy (SEM), X-ray microanalysis (EDX), magnetic measurements M(H) and thermomagnetic measurements M(T). After 40 h of wet MA, the alloy was partially amorphous, and the ribbons obtained by RQ do not show an amorphous state. Also, the magnetic measurements show the influence of the method used on the magnetic properties.
EN
Nowadays, various small specimen test techniques have gained wide popularity and appreciation among researchers as they offer undoubtful benefits in terms of structural material characterisation. This paper focuses on small punch tests (SPTs) performed on small-sized disc specimens to assess the mechanical properties of 14Cr oxide dispersion strengthened (ODS) steel. A numerical model was established to support experimental data and gain deeper insight into complex strain states developing in a deformed specimen. Modern evaluation procedures were discussed for obtaining mechanical properties from the small punch force-deflection response and were compared with the literature. Applicability and universality of those relations at different test conditions were also studied. It appeared that different ball diameters used had negligible influence on yield point but strongly affected ultimate strength estimation. It was found that friction belongs to decisive factors determining strain distribution in samples, as dry conditions increase the peak strain and move its location farther from the punch pole.
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
Magnesium-based alloys are widely used in the construction, automotive, aviation and medical industries. There are many parameters that can be modified during their synthesis in order to obtain an alloy with the desired microstructure and advantageous properties. Modifications to the chemical composition and parameters of the synthesis process are of key importance. In this work, an Mg-based alloy with a rare-earth element addition was synthesized by means of mechanical alloying (MA). The aim of this work was to study the effect of milling times on the Mg-based alloy with a rare-earth addition on its structure and microhardness. A powder mixture of pure elements was milled in a SPEX 8000D high energy shaker ball mill under an argon atmosphere using a stainless steel container and balls. The sample was mechanically alloyed at the following milling times: 3, 5, 8 and 13 h, with 0.5 h interruptions. The microstructure and hardness of samples were investigated. The Mg-based powder alloy was examined by means of X-ray diffraction (XRD), scanning electron microscopy (SEM) and using a Vickers microhardness test. The results showed that microhardness of the sample milled for 13 h was higher than that of those with milling time of 3, 5 and 8 h.
7
Content available Mechanical alloying of Mg-Zn-Ca-Er alloy
EN
Magnesium-based materials constitute promising alternatives for medical applications, due to their characteristics, such as good mechanical and biological properties. This opens many possibilities for biodegradable materials to be used as less-invasive options for treatment. Degradation is prompted by their chemical composition and microstructure. Both those aspects can be finely adjusted by means of proper manufacturing processes, such as mechanical alloying (MA). Furthermore, MA allows for alloying elements that would normally be really hard to mix due to their very different properties. Magnesium usually needs various alloying elements, which can further increase its characteristics. Alloying magnesium with rare earth elements is considered to greatly improve the aforementioned properties. Due to that fact, erbium was used as one of the alloying elements, alongside zinc and calcium, to obtain an Mg₆₄Zn₃₀Ca₄Er₁ alloy via mechanical alloying. The alloy was milled in the SPEX 8000 Dual Mixer/Mill high energy mill under an argon atmosphere for 8, 13, and 20 hours. It was assessed using X-ray diffraction, energy dispersive spectroscopy and granulometric analysis as well as by studying its hardness. The hardness values reached 232, 250, and 302 HV, respectively, which is closely related to their particle size. Average particle sizes were 15, 16, and 17 μm, respectively.
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
In the paper, hydrogenation and corrosion properties of three kinds of nanocrystalline La1.5Mg0.5Ni7 type alloys obtained by mechanical alloying (MA) method are discussed in view of their application as anodic materials for Ni/MH batteries. Partial substitutions of cobalt for nickel and gadolinium for lanthanum and then magnetron sputtering of the intermetallic powders with amorphous nickel distinctly change functional parameters of the hydrogen storage material. It is shown that 5.5 at.% cobalt addition markedly improves the alloy activation but worsens its corrosion resistance in concentrated KOH solution. On the other hand, partial substitution of lanthanum by Gd (2.2 at.%) ensures large exchange currents for H2O/H2 system. Presence of Ni coatings on alloy particles is generally advantageous from the material H-storage properties, although they slow down a little hydrogen transport during electrode discharge.
PL
W artykule przedyskutowano właściwości wodorochłonne i korozyjne trzech rodzajów nanokrystalicznych stopów typu La1.5Mg0.5Ni7 – pod kątem ich aplikacji jako materiałów anodowych dla ogniw typu Ni/MH. Materiały wytwarzano metodą mechanicznej syntezy (metoda MA) i modyfikowano poprzez częściowe podstawianie niklu kobaltem bądź lantanu gadolinem a następnie poprzez magnetronowe napylanie uzyskanych proszków amorficznym niklem. Modyfikacje te wyraźnie zmieniają właściwości funkcjonalne badanych stopów wodorochłonnych. Pokazano, że dodatek 5,5 % at. kobaltu wyraźnie skraca aktywację stopu ale pogarsza jego odporność korozyjną w stężonym roztworze KOH. Z kolei częściowe podstawienie lantanu gadolinem (2,2 % at.) zapewnia materiałowi wysokie gęstości prądu wymiany układu H2O/H2. Obecność powłok Ni na cząstkach proszku jest generalnie korzystna z punktu widzenia właściwości sorpcyjnych materiałów, jednakże powłoki te nieco hamują transport wodoru podczas rozładowywania elektrod.
EN
Purpose: This paper explains mechanical synthesis which uses powders or material chunks in order to obtain phases and alloys. It is based on an example of magnesium powders with various additives, such as zinc, calcium and yttrium. Design/methodology/approach: The following experimental techniques were used: X-ray diffraction (XRD) method, scanning electron microscopy (SEM), determining particle size distributions with laser measuring, Vickers microhardness. Findings: The particle-size of a powder and microhardness value depend on the milling time. Research limitations/implications: Magnesium gained its largest application area by creating alloys in combination with other elements. Magnesium alloys used in various industry contain various elements e.g. rare-earth elements (REE). Magnesium alloys are generally made by casting processes. Consequently, the search for new methods of obtaining materials such as mechanical alloying (MA) offers new opportunities. The MA allows for the production of materials with completely new physico-chemical properties. Originality/value: Thanks to powder engineering it is possible to manufacture materials with specific chemical composition. These materials are characterized by very high purity, specified porosity, fine-grain structure, complicated designs. These are impossible to obtain with traditional methods. Moreover it is possible to refine the process even further minimalizing the need for finishing or machining, making the material losses very small or negligible. Furthermore material manufactured in such a way can be thermally or chemically processed without any problems.
EN
The effect of replacing iron with transition metals (M = Mn, Cr, Co) on the microstructure of mechanically alloyed Al65 Cu20 Fe15 quasicrystalline powder was examined by X-ray diffraction and transmission electron microscopy methods. Powders of various compositions were milled in a high-energy planetary ball mill up to 30 hours at a rotation speed 350 rpm using WC milling media. The amount of the fourth additions was constant in all powders and Fe atoms were replaced with Mn, Cr or Co in a 1:1 ratio, while the content of the Al and Cu was selected in two ways: they remained the same as in the initial ternary Al65 Cu20 Fe15 alloy or changed to obtain e/a ratio = 1.75 (optimal for icosahedral quasicrystalline phase). Quasicrystalline phase formed in the quaternary Al65 Cu20 Fe7.5 M7.5 powders, whereas in the second group of compositions only crystalline phases were identified.
EN
The paper presents the results of research on the Al-V2O5 composite manufactured by means of the mechanical alloying and powder metallurgy method. Observation of the microstructure and X-ray chemical composition (XRD) analysis of the composite after extrusion were carried out. One of the most desirable features of metallic composites – apart from mechanical properties – is their resistance to increased impact temperature. It was observed that the formation of intermetallic phases due to the chemical reaction between strengthening particles and the composite matrix depends primarily on the annealing conditions of the material. The hardness of the annealed samples, depending on the annealing temperature, were discussed with respect to the material microstructure transformation. Despite the high-temperature, annealing at 473–773K, the material hardness did not change significantly, and remained approx.125 HV. However, at higher annealing temperatures, i.e. 823K, the chemical reaction between the components leads to the formation of the Al10V particles and increases hardness.
PL
W pracy przedstawiono wyniki badań kompozytu Al-V2O5, który wytworzono metodą mechanicznej syntezy. Przeprowadzono obserwację mikrostruktury oraz rentgenowską analizę składu chemicznego (XRD) kompozytu po procesie wyciskania. Jedną z najbardziej pożądanych cech kompozytów metalicznych – oprócz własności mechanicznych – jest ich odporność na oddziaływanie podwyższonej temperatury. Powstawanie faz międzymetalicznych na skutek reakcji chemicznej pomiędzy cząstkami umacniającymi a osnową kompozytu zależy przede wszystkim od warunków wyżarzania materiału kompozytowego. W pracy przedstawiono zależność twardości od temperatury wyżarzania (473–823 K). Twardość materiału nie zmienia się znacząco w dość wysokiej temperaturze wyżarzania jak w przypadku aluminium (473–773 K), a jej wartość osiąga średni poziom 125HV2. Stwierdzono, że reakcja chemiczna między składnikami podczas wyżarzania w temperaturze 823 K prowadzi do powstania fazy międzymetalicznej Al10V, co powoduje wzrost twardości kompozytu.
EN
The effects of different types of process control agents (PCA) on the microstructure evolution of Ni-based oxide dispersion-strengthened superalloy have been investigated. Alloy synthesis was performed on elemental powders having a nominal composition of Ni-15Cr-4.5Al-4W-2.5Ti-2Mo-2Ta-0.15Zr-1.1Y2O3 in wt % using high energy ball milling for 5 h. The prepared powders are consolidated by spark plasma sintering at 1000°C. Results indicated that the powder ball-milled with ethanol as PCA showed large particle size, low carbon content and homogeneous distribution of elemental powders compared with the powder by stearic acid. The sintered alloy prepared by ethanol as PCA exhibited a homogeneous microstructure with fine precipitates at the grain boundaries. The microstructural characteristics have been discussed on the basis of function of the PCA.
EN
Ag and Cu powders were mechanically alloyed using high-energy planetary milling to evaluate the sinter-bonding characteristics of a die-attach paste containing particles of these two representative conductive metals mixed at atomic scale. This resulted in the formation of completely alloyed Ag-40Cu particles of 9.5 μm average size after 3 h. The alloyed particles exhibited antioxidation properties during heating to 225°C in air; the combination of high pressure and long bonding time at 225°C enhanced the shear strength of the chip bonded using the particles. Consequently, the chips sinter-bonded at 225°C and 10 MPa for 10 min exhibited a sufficient strength of 15.3 MPa. However, an increase in bonding temperature to 250°C was detrimental to the strength, due to excessive oxidation of the alloyed particles. The mechanically alloyed phase in the particle began to decompose into nanoscale Ag and Cu phases above a bonding temperature of 225°C during heating.
PL
W artykule przedstawione zostały własności technologiczne proszków kompozytowych Cu/TiN, które mają istotny wpływ na zdolność proszku do zagęszczenia, a w konsekwencji na dalsze procesy prasowania i spiekania. Gęstość nasypowa, gęstość nasypowa z usadem, jak i sypkość proszku, zależy przede wszystkim od kształtu cząstek, ich rozmiaru, jak również chropowatości powierzchni. Badaniom własności technologicznych poddane zostały mieszanki proszków kompozytowych na osnowie miedzi z 5, 10 i 15% wag. dodatkiem azotku tytanu. Proszki kompozytowe Cu/TiN wytworzone zostały na drodze mechanicznej syntezy, gdzie czas mielenia wyniósł 10 h.
EN
This article presents the technological proporties of Cu/TiN composite powders which have significant impact on the powder’s ability to compaction and consequently on further pressing and sintering process. Bulk density, tap density and powders flowability depends primarily on the shape of the particles, their size and surface roughness. In the article, the investigations of technological proporties were subjected to mixtures of composite powders on a copper reinforced with 5, 10, 15% wt. TiN. Addition of titanium nitride. Cu/TiN composite powders were produced by mechanical alloying, where the milling time was 10 hours.
EN
The development of a new deposition method allowing to obtain thick composite coatings is of both scientifically and practical importance. The one presented in this paper is based on a negative side effect taking place during the mechanical synthesis of alloys, i.e. sticking of milled material to the surfaces of both the vial and balls. The experiment covered the comilling of NiAl (~45 µm) with 15 wt.% CrB2 (~40 µm) powders together with nickel platelets used as the substrates and steel balls. The above processing performed at 200 rpm resulted in a steady increase in the thickness of the rubbed-in buildup on the platelet surfaces allowing coatings of 4, 11, 22 and 33 µm to be produced after 4, 8, 16 and 32 hours. The OM, XRD and TEM investigations showed that such coatings are characterized by a gradient microstructure with heavily dislocated but coarser grains near the substrate and a more porous inner part formed with rounded well fused agglomerates of greatly refined crystallites. The CrB2 were only slightly larger than the NiAl ones and were distributed quite uniformly. Most of the coating was found well fused with the substrate, but occasional voids and porosity at the substrate/coating interface were also noted. It is worth noting that applying the proposed method allowed the authors to produce a thick, gradient and mostly nano-crystalline NiAl and CrB2 composite coating.
PL
Rozwój nowych metod osadzania powłok kompozytowych jest istotny z naukowego i praktycznego punktu widzenia. Metoda proponowana obecnie bazuje na negatywnym zjawisku zachodzącym w czasie mechanicznej syntezy stopów, tj. oklejaniem mielonym materiałem kul i naczynia w którym prowadzony jest proces. Obecny eksperyment obejmował współmielenie stalowymi kulami proszków NiAl (~45 μm) z 15 wt.% CrB2 (~40 μm) z płytkami Ni zastosowanymi jako podłoża. Proces ten, prowadzony przy 200 obr./min, skutkował ciągłym powiększaniem grubości powłok do 4, 11, 22 i 33 μm odpowiednio po 4, 8, 16 i 32 godz. Badania z wykorzystaniem mikroskopii optycznej, transmisyjnej oraz dyfraktometrii rentgenowskiej wykazały, że powłoki te charakteryzuje budowa gradientowa z warstwą silnie zdefektowanych, ale stosunkowo dużych krystalitów przy podłożu stopniowo zastępowanych nanokrystalicznym porowatym materiałem w formie silnie spojonych aglomeratów. Krystality CrB2 wykazywały niewiele mniejsze rozdrobnienie od NiAl oraz w przybliżeniu równomierny rozkład w intermetalicznej osnowie. Powłoki w większej części wykazywały dobre spojenie z podłożem, ale obecność pustek oraz porowatości penetrującej od granic z podłożem była dokumentowana. Należy podkreślić, że zastosowanie proponowanej metody umożliwia wytworzenie grubych, gradientowych i w przeważającej części nanokrystalicznych kompozytowych powłok.
EN
Mg60 Zn35 Ca5 amorphous powder alloys were synthesized by mechanical alloying (MA) technique. The results of the influence of high-energy ball-milling time on amorphization of the Mg60 Zn35 Ca5 elemental blend (intended for biomedical application) were presented in the study. The amorphization process was investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM). Initial elemental powders were mechanically alloyed in a Spex 8000 high-energy ball mill at different milling times (from 3 to 24 h). Observation of the powder morphology after various stages of milling leads to the conclusion that with the increase of the milling time the size of the powder particles as well as the degree of aggregation change. The partially amorphous powders were obtained in the Mg60 Zn35 Ca5 alloy after milling for 13-18h. The results indicate that this technique is a powerful process for preparing Mg60 Zn35 Ca5 alloys with amorphous and nanocrystalline structure.
EN
Discovery of superconductivity of MgB2 with a critical temperature of -234 °C has offered the promise of important large-scale applications. Except for the other featured synthesis methods, mechanical activation, performed by high-energy ball mills to synthesis of bulk form of MgB2 or as a first step of wire and thin film production has considered as an effective alternative production route in recent years. The aim of the present study was to determine the effect of process variables such as the ball-to-powder weight ratio (BPR), size of ball, milling time, annealing temperature and contribution of process control agent (toluene) on the product size, morphology and conversion level of precursor powders to MgB2 after subsequent heat treatment. Although, the test results revealed relatively lower weight percent of MgB2 phase formation compared with the literature, the reduced milling time, BPR and sinterability of pre-alloyed powder to MgB2 at lowered temperature (630 °C) enhanced the applicability of mechanical alloying with SPEX mill.
EN
Copper matrix composites containing ceramic particles such as carbides, borides, or nitrides have attracted much attention over the last few years. The increased interest in such materials has mainly been created by their high electrical and thermal conductivity, good mechanical and tribological properties, and microstructural stability. Among other nitrides, the titanium nitride seems to be considered as an attractive reinforcement due to its high hardness, excellent electrical conductivity, and stability at high temperatures. Moreover, its good corrosion resistance proves the uniqueness of the TiN particles above any other nitrides. In this work, Cu-10 wt.% TiN composite powders were produced by mechanical alloying and sintered by the spark plasma sintering (SPS) technique under different temperatures. The morphology and powder particle size after mechanical synthesis were inspected by a scanning electron microscopy (SEM) for all of the powder samples; chemical composition analyses (EDS) were also performed. The hydrostatic method was used to measure the density of the composite samples to analyze the influence of milling time on the process of consolidation in the composite powders.
PL
Kompozyty na osnowie miedzi zbrojone cząstkami ceramicznymi, m.in. węglikami, borkami i azotkami, w ostatnich latach wzbudziły spore zainteresowanie z uwagi na wysoką przewodność cieplną i elektryczną oraz dobre właściwości mechaniczne i tribologiczne przy równoczesnym zachowaniu stabilnej mikrostruktury. Zastosowanie azotku tytanu jako zbrojenia kompozytu jest korzystne ze względu na: wysoką twardość, doskonałą przewodność elektryczną, odporność na korozję oraz stabilność w wysokich temperaturach. W pracy przedstawiono mieszankę kompozytową Cu-10% wag. TiN, wytworzoną w procesie mechanicznej syntezy, którą następnie poddano spiekaniu za pomocą iskrowego spiekania plazmowego (SPS). Zbadano mikrostrukturę, wielkość cząstek, a także przeprowadzono analizę składu chemicznego (EDS, Energy Dispersive Spectroscopy) za pomocą skaningowego mikroskopu elektronowego (SEM). Metodą hydrostatyczną wykonano pomiar gęstości wytworzonych spieków w celu analizy wpływu czasu mielenia na proces konsolidacji proszku kompozytowego.
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