Search

Elemental powders of Co, Ni and Al in the proper amounts to obtain Co(35)Ni(40)Al(25) and Co(40)Ni(35)Al(25) nominal compositions were ball milled in a high-energy mill for 80 h. After 40 h of milling, the formation of a Co (Ni, Al) solid solution with f.c.c. structure was verified by a change of the original lattice parameter and crystallite size. Analytical transmission electron microscopy observations and X-ray diffraction measurements of the final Co (Ni, Al) solid solution showed that the crystallite size scattered from 4 to 8 nm and lattice parameter a = 0.36086 nm. The chemical EDS point analysis of the milled powder particles allowed the calculation of the e/a ratio and revealed a high degree of chemical homogeneity of the powders. Hot pressing in vacuum of the milled powders resulted in obtaining compacts with a density of about 70% of the theoretical one. An additional heat treatment increased the density and induced the martensitic transformation in a parent phase. Selected area diffraction patterns and dark field images obtained from the heat-treated sample revealed small grains around 300 nm in diameter consisting mainly of the ordered gamma phase (gamma'), often appearing as twins, and a small amount of the L1(0) ordered martensite.

Ball milling of easy glass forming Ti(25)Zr(17)Ni(29)Cu(29) alloys lead to the formation of an amorphous structure accompanied by a substantial increase of powder microhardness. The powders show clear glass transition effect and a few stage crystallization starting above 500 degrees C. High-resolution transmission electron microscope technique allowed identifying nanocrystalline inclusions as Cu(12)NiTi(7) within the amorphous powder. The amorphous powders mixed with nanocrystalline iron or silver powders were hot pressed to form composites. A narrow 200 nm broad intermediate single-phase layer at the amorphous-phase/iron interface containing all elements present in the composite was identified using transmission electron microscope and high-angle annular dark field detector techniques. scanning transmission electron microscopy energy dispersive spectroscopy line profile showed gradual change of composition within the intermediate zone. Amorphous phase contains small nanocrystals of size close to 10 nm identified using High-resolution transmission electron microscope as Cu(12)NiTi(7.) Compression tests have shown better plasticity of composites than in the case of pure hot-pressed amorphous powder; furthermore, high elastic limit of composites and the ultimate compression stress of about 1800 MPa for composites containing 20% Fe and near 700 MPa for those with 20% Ag.

Amorphous powder of composition corresponding to Ni60Ti20Zr20 (in at%) was obtained by ball milling in a high-energy mills starting from pure elements. Formation of the amorphous structure was observed already after 20 h of milling, although complete amorphization occurred after 40 h. The microhardness of powders increased from about 30 HV for pure elements to above 400 HV (1290 MPa) after 40 h of milling. Transmission electron microscopy (TEM) allowed to identify nanocrystalline inclusions of intermetallic phases of size 2-10 nm. Uniaxial hot pressing was performed in vacuum at temperature below the crystallization T(x) it is 510 degrees C and pressure of 600 MPa, Mixed amorphous powders and nanocrystalline silver powders were used to form a composite, in which microhardness was near 970 MPa HV and 400 HV for the amorphous phase and nanocrystalline silver, respectively. The compression strength of the composite containing 20 wt% of nanocrystalline Ag powder was equal to 600 MPa and plastic strain was 2%. Microstructure studies showed low porosity of composites of less than 1%, uniform distribution of the silver phase and a transition zone between both components, about 150 nm thick, where diffusion of nickel, niobium and zirconium into silver was observed. High-resolution TEM allowed identifying the structure of nanocrystalline inclusions in the amorphous matrix after hot pressing as either Ni(3)Zr or Ni(17)Nb(3). The identification was performed basing on measurements of angles and interatomic distances using inverse Fourier transformed images with enhanced contrast using Digital Micrograph computer program.

Summary Atomized 6061 aluminium alloy powders with and without the addition of 2 wt% Zr were milled for 80 h in a planetary ball mill and hot pressed in vacuum. The milled powders showed microhardness of about 170 HV, which increased after hot pressing up to 260 HV and up to 280 HV for powders without and with the Zr additions, respectively. Compression tests showed the high yield stress of 300 MPa obtained for the hot-pressed sample produced from the initial powders compared with ultimate compression strength of above 800 MPa for that of the milled sample and slightly higher for that with Zr additions. The effect of hot pressing on the structure of powders was investigated using a conventional analytical and high-resolution electron microscopy and high angle annular dark-field scanning transmission electron microscopy combined with energy dispersive X-ray microanalysis. The samples of initial powders hot pressed in vacuum showed a cell structure with particles of the Mg2Si and AlFeSi phases in intercell areas. In the milled and hot-pressed sample, the homogeneous structure of small grains of size below 200 nm was observed. The AlFeSi and Mg2Si particles with size 20–100 nm were uniformly distributed as well as the Zr rich particles in the Zr containing alloy. The Zr-rich particles containing up to 80 at% Zr were identified as a metastable fcc cubic phase with lattice parameter a= 0.48 nm.

Two powder alloys from the beta phase region of compositions Co(28.5)Ni(36.5)Al(35) and Co(35)Ni(30)Al(35) were ball milled for 80 h in a high energy ball mill. The formation of amorphous structure was observed after 40 h of milling and further milling did not change their structure. The analytical and high-resolution transmission electron microscopy (TEM, HREM) examination of powder structure showed that nanoparticles of L1(0) phase of size of about 5 nm were present within the amorphous matrix. The vacuum hot pressing of the milled powders under pressure of 400 MPa at 700 degrees C for 12 min resulted in the formation of compacts with density of about 70% of the theoretical one. The additional heat treatment at 1300 degrees C for 6 h followed by water quenching, led to significant improvement of density and induced the martensitic transformation manifested by a broad heat effect. The characteristic temperatures of the transformation were determined using DSC measurements, which revealed only small differences within the examined alloys compositions. TEM structure studies of heat-treated alloys allowed to identify the structure of an ordered beta (B2) phase and L1(0) martrensite.

ZrNiTiCu and ZrNiTiCuAl alloys were amorphized using either a melt-spinning or ball-milling process in a high-energy planetary mill. The elemental powders were initially blended to the desired composition (in at.%) of Zr, 65; Cu, 27.5; Al, 7.5 and of Ti, 25; Zr, 17; Cu, 29; Ni, 29, respectively. The composition of alloys was chosen to be the same as for the bulk amorphous ZrCuAl and easy glass-forming ZrNiTiCu alloys. An almost fully amorphous structure was obtained after 80 h of milling in the case of both compositions. Transmission electron microscopy studies of ball-milled powders revealed the presence of nano-crystallites [2-5 nm for ZrCuAl and smaller (1-3 nm) for the ZrTiNiCu alloy]. High-resolution transmission electron microscopy of melt-spun ZrNiTiCuAl ribbons provided evidence of the amorphous structure.

The effect of mechanical alloying on the microstructure of atomized 6061 aluminium alloy powder and 6061 powder with a zirconium addition was studied in the work. The atomized 6061 aluminium alloy powder and 6061 powder with addition of 2 wt.% Zr were milled in a planetary ball mill and investigated using X-ray diffraction measurements, conventional and high-resolution electron microscopy (TEM/HRTEM) and high-angle annular dark field scanning transmission electron microscopy combined with energy dispersive X-ray microanalysis. An increase of stresses was observed in milled powders after the refinement of crystallites beyond 100 nm. In the powder with zirconium addition, some part of the Zr atoms diffused in aluminium forming a solid solution containing up to 0.5 wt.% Zr. The remaining was found to form Zr-rich particles containing up to 88 wt.% Zr and were identified as face centred cubic (fcc) phase with lattice constant a= 0.48 nm. That fcc phase partially transformed into the L1(2) ordered phase. Eighty-hour milling brought an increase of microhardness (measured with Vickers method) from about 50 HV (168 MPa) for the initial 6061 powder to about 170 HV (552 MPa). The addition of zirconium had no influence on the microhardness.

Two Ti alloys with compositions Ti-10Ta and Ti-10Nb (at.%) were milled in a high-energy mill for a maximum of 80 h in an argon atmosphere. A nanocrystalline structure of alpha-Ti(X) (X = Ta or Nb) solid solution was formed in both investigated alloys after milling, as shown by X-ray diffraction. Transmission electron microscopy observations of powders milled for 80 h revealed chemical inhomogeneity of particles in nanometre-scale regions and an average crystallite size of about 10 nm. The pulse plasma sintering method was applied for hot consolidation of milled powders. The mean density of pulse plasma sintering compacts of Ti-Nb alloy was about 99.5% of the theoretical value, whereas the density of the Ti-10Ta sample was lower, close to 92% of the theoretical value. Transmission electron microscopy observation of compacted samples showed that the sintering process caused the formation of a two-phase alpha + beta structure in both investigated alloys, with a mean grain size of 220 nm. The chemical inhomogeneity and high degree of deformation in nanometre-scale regions of milled powders led to a martensitic transformation, resulting in formation of a 9R martensite structure.