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1.
Acta Biomater ; 98: 67-80, 2019 10 15.
Article in English | MEDLINE | ID: mdl-31254685

ABSTRACT

Microstructural refinement of magnesium (Mg) alloys is beneficial for mechanical and corrosion properties, both of which are critical for their successful application as temporary implant materials. One method of achieving a refined microstructure is through rapid solidification via gas-atomization-powder production. In this study we investigated spark plasma sintering (SPS) as a potential processing method for maintaining this refined microstructure while achieving a range of porosities up to full densification. We characterized the microstructural evolution as a function of sintering temperature from 250 to 450 °C for the alloy WE43 using multi-scale correlative microscopy techniques, including light microscopy and scanning and transmission electron microscopy-based methods. The spatial distribution of the two major alloying elements, neodymium (Nd) and yttrium (Y), was determined and the intermetallic phases they form identified using energy dispersive X-ray spectroscopy in conjunction with electron diffraction. The gas-atomized powder microstructure consists of Mg-rich dendrites and a percolating interdendritic Mg-Nd-Y ternary phase with structure Mg14Nd2Y, surrounded by a high Nd and Y content in solid solution. This microstructure is maintained up to a sintering temperature of 350 °C, while with higher sintering temperatures segregation of Nd and Y dominates. The percolating ternary phase breaks up into faceted globular precipitates with structure Mg5Nd, which is isomorphous to Mg14Nd2Y. Y comes out of solution and migrates to previous powder-particle surfaces, possibly forming Y2O3. Sample densities ranged from 64 to 100% for sintering temperatures of 250 to 450 °C, respectively, and the grain size remained constant at about 10 µm. SPS is demonstrated to be an attractive alternative method for processing Mg alloys to a wide range of porosities and fine microstructures. The microstructural refinement achieved by SPS holds the potential for slow and homogeneous corrosion. STATEMENT OF SIGNIFICANCE: This study presents the impact spark plasma sintering (SPS) has on the microstructure of WE43, a magnesium alloy used for biodegradable implants. SPS is of great interest in this context as it is scalable, rapid, and has the potential for tuning density while maintaining a refined microstructure. The microstructure and density are explored from the gas-atomized powder to the densified material using electron microscopy and chemical mapping from the macro- to the nano-level. The insights gained reveal an original evolution of rare-earth element distribution with an isomorphous chemistry change, while the microstructure develops from the non-equilibrium state (powder) towards an equilibrium structure upon sintering. This study, including measurements of mechanical performance, sets the premises of SPS for the fabrication of Mg-based implants with tunable characteristics.


Subject(s)
Alloys/chemistry , Biocompatible Materials/chemistry , Magnesium/chemistry , Materials Testing/methods , Plasma Gases/chemistry , Electrons , Hardness , X-Ray Diffraction
2.
J Mech Behav Biomed Mater ; 53: 239-249, 2016 Jan.
Article in English | MEDLINE | ID: mdl-26344856

ABSTRACT

Laser remelting of commercially pure titanium (CP-Ti) surface was done in a nitrogen rich inert atmosphere to form in situ TiN/Ti composite coating. Laser surface remelting was performed at two different laser powers of 425 W and 475 W. At each power, samples were fabricated with one or two laser scans. The resultant material was a nitride rich in situ coating that was created on the surface. The cross sections revealed a graded microstructure. There was presence of nitride rich dendrites dispersed in α-Ti matrix at the uppermost region. The structure gradually changed with lesser dendrites and more heat affected α-Ti phase maintaining a smooth interface. With increasing laser power, the dendrites appeared to be larger in size. Samples with two laser scans showed discontinuous dendrites and more α-Ti phase as compared to the samples with one laser scan. The resultant composite of TiN along with Ti2N in α-Ti showed substantially higher hardness and wear resistance than the untreated CP-Ti substrate. Coefficient of friction was also found to reduce due to surface nitridation. Leaching of Ti(4+) ions during wear test in DI water medium was found to reduce due to laser surface nitriding.


Subject(s)
Coated Materials, Biocompatible/chemistry , Lasers , Titanium/chemistry , Materials Testing , Mechanical Phenomena , Surface Properties , Water
3.
J Mech Behav Biomed Mater ; 32: 335-344, 2014 Apr.
Article in English | MEDLINE | ID: mdl-24388220

ABSTRACT

Laser surface melting (LSM) of Ti6Al4V alloy was carried out with an aim to improve properties such as microstructure and wear for implant applications. The alloy substrate was melted at 250W and 400W at a scan velocity of 5mm/s, with input energy of 42J/mm(2) and 68J/mm(2), respectively. The results showed that equiaxed α+ß microstructure of the substrate changes to mixture of acicular α in ß matrix after LSM due to high cooling rates in the range of 2.25×10(-3)K/s and 1.41×10(-3)K/s during LSM. Increasing the energy input increased the thickness of remelted region from 779 to 802µm and 1173 to 1199µm. Similarly, as a result of slow cooling rates under present experimental conditions, the grain size of the alloy increased from 4.8µm to 154-199µm. However, the hardness of the Ti6Al4V alloy increased due to LSM melting and resulted in lowest in vitro wear rate of 3.38×10(-4)mm(3)/Nm compared to untreated substrate with a wear rate of 6.82×10(-4)mm(3)/Nm.


Subject(s)
Lasers , Materials Testing , Mechanical Phenomena , Titanium/chemistry , Alloys , Hardness , Surface Properties
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