Effects of powder processing on densification of titanium diboride based cermets

Abstract

The sinterability of TiB₂-Ni₃(Al,Ti) based cermets has been significantly improved by aggressive milling of the starting TiB₂-Ni-TiAl₃ powder mixtures. This technique improves not only liquid spreading by reducing TiAl₃ particle size but also eliminates alumina agglomerates and the associated porosity found after vacuum sintering. Liquid phase sintering of TiB₂-Ni-TiAl₃ powder mixtures involves the presence of Ni based secondary borides at low temperatures (1200°C), which react afterwards with TiAl₃ particles leading to the formation of the final TiB₂-Ni₃(Al,Ti) eutectic liquid. Apart from improving liquid spreading around TiB₂ grains, aggressive milling is also found to disperse alumina agglomerates, which reduces the porosity associated to these particles. By this refined procedure, the amount of binder phase required for full densification of TiB₂ cermets by sinter hipping has been reduced from a previous limit of 16 vol.-% to 10 vol.-%. The hardness of these TiB₂-10 vol.-%Ni₃(Al,Ti) cermets is in the range of ultrafine WC-Co hardmetals in spite of their much coarser microstructure.     

Metallurgical and mechanical characterisation of titanium based materials for endosseous applications obtained by selective laser melting

Abstract

The aim of the present work was to estimate the feasibility of selective laser melting (SLM) to produce Ti-hydroxyapatite bioactive composite materials for personalised endosseous implants. Mixtures of Ti6Al7Nb surface conditioned powder with hydroxyapatite up to 5 vol.-% were processed by SLM with the same scanning strategy and laser power in the range of 50–200 W. Specimens with porous structures were characterised from a structural and mechanical point of view. Irrespective to the initial hydroxyapatite content, density increased by increasing the laser power. The microstructure of manufactured parts mainly consisted of α′ martensite. In materials with 5 vol.-% hydroxyapatite, a phosphorous containing phase formed as a consequence of hydroxyapatite decomposition and interaction with the base Ti alloy. By increasing the laser power, the tensile strength increased mainly due to the density improvement of all the investigated materials.     

Stiffness variation of porous titanium developed using space holder method

Abstract

The excellent properties of Ti have resulted in its generalised use for bone implants. However, Ti is very stiff in comparison with human cortical bone, and this creates problems of bone weakening and loosening of the implant. This article discusses the mechanical properties (flexural and compressive strength, and stiffness) of porous Ti–6Al–4V specimens developed using the space holder method. These properties are examined relative to the production process parameters: compacting pressure and sintering time, as well as temperature, and the addition of spacer and its particle size. It is seen that when spacer is added, compressive strength decreases with the application of compacting pressure and that these are the most influential parameters. The developed pieces show a closed and unconnected porosity. Small additions of spacer (25 vol.-%) reduce stiffness to around half of that shown by the solid material, and the resulting pieces are strong enough to be used as bone substitute.     

Hipping after sintering of titanium diboride cermets

Abstract

A new fabrication route, an alternative to glass encapsulated hipping (GEHIP), has been developed to produce dense TiB₂ cermets. Key points of this technique, based on hipping after vacuum sintering (VS + HIP), are the use of Ni₃ (Al,Ti) as binder phase and the selection of the proper amount of additions. The main advantage of VS + HIP with respect to GEHIP is the simplification of the sintering procedure which avoids the glass encapsulation step that makes it more adaptable for industrial use. Successful application of VS + HIP requires a minimum binder content about 10 vol.-% below which a significant hardness reduction is observed owing to the presence of residual porosity as compared with GEHIP. The materials produced by this technique combine low density and high stiffness with high hardness and toughness values, thus giving a set of properties especially attractive for applications where inertial loads are responsible for failure.     

Metal injection moulding of low modulus Ti–Nb alloys for biomedical applications

Abstract

Titanium alloys containing β stabilising elements such as Nb, Zr and Ta are particularly promising as implant materials because of their excellent combination of low modulus, high strength, corrosion resistance and biocompatibility. A low elastic modulus is important for implants to avoid stress shielding and associated bone resorption. The difficulty of producing complex shapes of these alloys by conventional methods makes metal injection moulding (MIM) attractive. Ti–17Nb alloy parts with densities 94% of theoretical have been produced by MIM of a feedstock based on blended elemental powders. Scanning electron microscopy reveals a typical α?β Widmanstätten microstructure with a precipitated α phase layer along the grain boundaries. The parts exhibit an ultimate tensile strength of 768 MPa and a plastic elongation of over 5%. The modulus of elasticity, about 84 GPa, is more than 20% lower than that of cp Ti and Ti–6Al–4V.     

The bioactivity of titanium-cuttlefish bone-derived hydroxyapatite composites sintered at low temperature

ABSTRACT

The most limiting features of titanium as a bone substituent are lack of bioactivity and high Young’s modulus. We have prepared titanium-hydroxyapatite (Ti-HAp) composites using titanium hydride as sintering agent to provide titanium sintering at lower temperature and preserve the stability of apatite phase. After low temperature sintering, no hydroxyapatite decomposition was detected. Pure titanium samples sintered in the presence of hydride showed smooth surface indicating good densification at 800°C. Higher HAp content resulted in decreased density and higher porosity due to the formation of micro- and macro-pores caused by the integration of HAp particles into titanium matrix and titanium hydride decomposition. However, Vickers microhardness test showed increased hardness for Ti-HAp composite with 10% of HAp regarding pure Ti. The bioactivity of Ti-HAp composites evaluated in simulated body fluid significantly improved with HAp content. The presence of HAp has lowered the cytotoxic effect of Ti-based composites on Hek293 cells.     

Sintering behaviour and mechanical characterisation of Ti64/xTiN composites and bilayer components

Ceramic particle reinforcement can be used to improve the surface properties of Ti6Al4V (Ti64) alloy. Powder metallurgy route is a promising method to fabricate such reinforced Ti64 components. To assess the relevance of this technique, this work investigates the effect generated by the addition of TiN particles in Ti64 powder during free sintering. TiN reinforcement particles were randomly distributed in the Ti64 matrix with three different concentrations in two configurations: completely reinforced and unreinforced–reinforced bilayer. Dilatometry was used to obtain the shrinkage kinetics of samples at 1200, 1300 and 1400°C under inert atmosphere and to investigate the impact of reinforced particles on the sintering behaviour. The microstructure of sintered materials was shown to be lamellar in the unreinforced material and equiaxed in reinforced materials. Finally, the Vickers microhardness measurement showed the huge benefit of adding TiN particles to increase the mechanical strength of the Ti64 alloy.     

Iron Aluminium Alloys with Strengthening Carbides and Intermetallic Phases for High‐Temperature Applications

An overview of materials developments of iron aluminium alloys with strengthening precipitate phases is given. The discussion is focussed on recent studies on Fe‐Al‐based alloys with strengthening precipitates, such as κ‐phase Fe₃AlC_x, MC‐carbide and Laves phase. Alloys of the following alloy systems were investigated: Fe‐Al‐C, Fe‐Al‐Ta, Fe‐Al‐Ni, Fe‐Al‐Ti‐Nb, and Fe‐Al‐M‐C (M = Ti, V, Nb, Ta). The investigations were centred on microstructure, constitution, and mechanical properties of such Fe‐Al‐based alloys with Al contents ranging from 10 to 30 at. %. Mechanisms and problems are discussed and perspectives are outlined.     

Mo含量对(Ti,W,Ta)C-Ni系金属陶瓷组织与性能的影响

以(Ti,W,Ta)C固溶体粉末、金属Mo粉和Ni粉为原料,采用真空液相烧结法制备(Ti,W,Ta)C-x Mo-1%Ni金属陶瓷(x为质量分数,x=0~20%),研究Mo含量对(Ti,W,Ta)C-Ni系金属陶瓷的显微组织、物相组成、致密度和力学性能的影响。结果表明,随Mo含量增加,金属陶瓷的组织逐渐细化;Mo对(Ti,W,Ta)C-Ni系金属陶瓷的致密化具有较强的促进作用,使得金属陶瓷的烧结收缩率增加,孔隙减少;随Mo含量增加,(Ti,W,Ta)C-Ni系金属陶瓷的硬度提高,而抗弯强度先升高后降低。当Mo含量为15%时,(Ti,W,Ta)C-Ni系金属陶瓷的力学性能最优,硬度HRA和抗弯强度分别为90.2和1 661 MPa。     

Mechanical and microstructural properties of titanium/hydroxyapatite functionally graded material fabricated by spark plasma sintering

ABSTRACT

In this article, different functionally graded material specimens were made from titanium powder and hydroxyapatite (HA) submicron particles. The spark plasma sintering method was applied to fabricate the specimens. Two kinds of starting powder mixture were used: mixed powder and ball-milled powder. Percentage of HA was changed from 0 vol.-% to 40 vol.-% in the different number of layers (2, 3 and 5-layer). The effects of the number of the layers and ball-mill process were investigated on microstructure, microhardness, compressive strength and fracture surface. The results show that the grain size has been enhanced by increasing the amount of HA in the layers. In addition, the Vickers microhardness has been first increased by enhancing the percentage of HA, while it has been decreased in the layers with a higher amount of it. Furthermore, the highest compressive strength could be achieved in the five-layer samples. Moreover, specimens with ball-milled powder have higher microhardness and less compressive strength.     

Structural Analysis,Electrochemical Behavior,and Biocompatibility of Novel Quaternary Titanium Alloy with near β Structure

This article analyses the microstructure, electrochemical behavior, and biocompatibility of a novel Ti-20Nb-10Zr-5Ta alloy with low Young’s modulus (59 GPa) much closer to that of bone, between 10 and 30 GPa, than Ti and other Ti alloys used as implant biomaterial. XRD and SEM measurements revealed a near β crystalline microstructure containing β phase matrix and secondary α phase, with a typical grain size of around 200 μm. The corrosion behavior in neutral Ringer solution evidenced: self-passivation behavior characterizing a very resistant passive film; an easy passivation as a result of favorable influence of the alloying elements Nb, Zr, and Ta that participate with their passive oxides to the formation of the alloy passive film; low corrosion and ion release rates corresponding with very low toxicity. In MEM solution, the novel alloy demonstrated very high corrosion resistance and no susceptibility to localized corrosion. Biocompatibility was evaluated on in vitro human osteoblast-like and human immortalized pulmonary fibroblast cell (Wi-38) lines and the new Ti-20Nb-10Zr-5Ta alloy exhibited no cytotoxicity. The new Ti-20Nb-10Zr5Ta alloy is a promising material for implants due to combined properties of low elastic modulus, very low corrosion rate, and good biocompatibility.     

Effect of C/Ti ratio on the compressive properties and wear properties of the 50 vol.-% submicron-sized TiCx/2014Al composites fabricated by combustion synthesis and hot press consolidation

In this study, in situ 50?vol.-% TiC_x/2014Al composites with different C/Ti molar ratios (0.6, 0.7, 0.8, 0.9 and 1) were successfully produced by the method of combustion synthesis and hot press consolidation. The microstructure and the mechanical properties of the composites were investigated. Microstructure characterisation of the TiC_x/2014Al composites showed relatively uniform distribution of the TiC_x particles with the particle size in the range of 200–900?nm. With the increase of the C/Ti molar ratio, the yield strength (σ_0.2) and the ultimate compression strength (σ_UCS) increased first then decreased, and the fracture strain (ε_f) increased. The σ_0.2, σ_UCS and the abrasive wear resistance of the 50?vol.-% TiC_x/2014Al composites reached the highest value when the value of the C/Ti molar ratio comes to 0.8. The σ_0.2, σ_UCS and ε_f of the 50?vol.-% TiC_x/2014Al composites with the C/Ti molar ratio of 0.8 are 1094?MPa, 1454 and 6.13%, respectively.     

Microstructural investigation of as cast and PREP atomised Ti–6Al–4V alloy

Abstract

A microstructure characterisation of Ti–6Al–4V is conducted for cast, extruded and micrometre sized particles. The plasma rotating electrode process is used to produce spherical Ti–6Al–4V powders from an alloy electrode. The process parameters and their impact on the material properties are described. The effects of electrode rotation speed on the particle size distribution, particle shape and crystal structure are investigated in detail. Optical microscopy and scanning electron microscopy are used for microstructural characterisation. The analysis shows that cast and extruded Ti–6Al–4V alloys have equiaxial α and α+β phase structures, while plasma rotating electrode processed powder from the same alloy compositions has an acicular or martensitic (α) structure. The microstructure scale depends on the particle size. Microhardness measurements are used to assess mechanical property dependence on the microstructure of this alloy. The rapidly cooled alloy particles have much higher hardness than cast or extruded bulk alloy.     

合金元素对机械合金化和放电等离子烧结Ti-Nb基合金显微组织的影响

β-Ti型结构的钛基材料在生物材料领域具有广泛的应用前景。本文采用机械合金化法和放电等离子烧结制备β-Ti型Ti-Nb基合金,研究不同Nb,Fe含量对合金显微组织及力学性能的影响。利用扫描电镜(SEM)、X射线衍射仪(XRD)和透射电镜(TEM)等手段分析合金的显微组织变化情况。结果表明:机械合金化过程中,粉末的平均粒度减小,当球磨时间超过60 h时粉末易发生团聚。当球磨转速为300 r/min,球料比为12:1,Ti和Nb的质量分数分别为64%和24%时,球磨100 h后制备的粉体材料中具有一定体积的非晶相。该粉末在1 000℃下通过放电等离子烧结(SPS)制备具有均匀细小的球状晶粒组织的Ti-Nb合金,其强度、伸长率和弹性模量分别为2 180MPa,6.7%和55 GPa。通过控制Nb,Fe的含量,可以促进β-Ti相形成,获得高强度和低杨氏模量的Ti-Nb合金。     

Mechanical Properties of β–Ti-35Nb-2.5Sn Alloy Synthesized by Mechanical Alloying and Pulsed Current Activated Sintering

A developed Ti-35?pct Nb-2.5?pct Sn (wt pct) alloy was synthesized by mechanical alloying using high-energy ball-milled powders, and the powder consolidation was done by pulsed current activated sintering (PCAS). The starting powder materials were mixed for 24 hours and then milled by high-energy ball milling (HEBM) for 1, 4, and 12 hours. The bulk solid samples were fabricated by PCAS at 1073?K to 1373?K (800 °C to 1100 °C) for a short time, followed by rapid cooling to 773?K (500 °C). The relative density of the sintered samples was about 93?pct. The Ti was completely transformed from ?? to ??-Ti phase after milling for 12 hours in powder state, and the specimen sintered at 1546?K (1273 °C) was almost transformed to ??-Ti phase. The homogeneity of the sintered specimen increased with increasing milling time and sintering temperature, as did its hardness, reaching 400?HV after 12 hours of milling. The Young??s modulus was almost constant for all sintered Ti-35?pct Nb-2.5?pct Sn specimens at different milling times. The Young??s modulus was low (63.55 to 65.3 GPa) compared to that of the standard alloy of Ti-6Al-4V (100 GPa). The wear resistance of the sintered specimen increased with increasing milling time. The 12-hour milled powder exhibited the best wear resistance.     

Influence of Cr removal on the microstructure and mechanical behaviour of a high-entropy Al0.8Ti0.2CoNiFeCr alloy fabricated by powder metallurgy

We report a systematic study on the influence of Cr removal on the microstructure and mechanical behaviour of an ultra-fine grained (UFG) high-entropy alloy (HEA), Al_0.8Ti_0.2CoNiFeCr, fabricated via spark plasma sintering (SPS) of mechanically alloyed (MA’ed) powders from constituent elemental powders. The MA’ed Al_0.8Ti_0.2CoNiFeCr powders consist principally of a BCC phase (～85 vol.-%) with a small amount of FCC phase (～15 vol.-%), whereas the MA’ed Al_0.8Ti_0.2CoNiFe powders present similar phases to those in the MA’ed Al_0.8Ti_0.2CoNiFeCr powders. Interestingly, the SPS processed UFG Al_0.8Ti_0.2CoNiFeCr alloy contains mostly an FCC phase (～78 vol.-%) and some BCC phase (～22 vol.-%); in contrast, the SPS processed UFG Al_0.8Ti_0.2CoNiFe alloy consists of a slightly enriched BCC phase (～53 vol.-%) and an FCC phase (～47 vol.-%). In addition, the SPS processed Al_0.8Ti_0.2CoNiFe alloy exhibits slightly higher yield strength, compressive strength and hardness but lower plasticity than those of the SPS processed Al_0.8Ti_0.2CoNiFeCr alloy.

Special theme block on high entropy alloys, guest edited by Paula Alvaredo Olmos, Universidad Carlos III de Madrid, Spain, and Sheng Guo, Chalmers University, Gothenburg, Sweden.     

PM processing and characterisation of Ti–7Fe low cost titanium alloys

Abstract

This work studies a set of low cost beta alloys with the composition Ti–7Fe, processed by conventional powder metallurgy (PM). The materials were prepared by conventional blending of elemental Ti hydride–dehydride powder with three different Fe powder additions: water atomised Fe, Fe carbonyl and master alloy Fe–25Ti. The optimal sintering behaviour and the best mechanical properties were attained with the use of Fe carbonyl powder, which reached a sintered density of up to 93% of the theoretical density, with UTS values of 800 MPa in the ‘as sintered’ condition. Coarse water atomised powder particles promoted reactive sintering, and coarse porosity was found due to the coalescence of Kirkendall porosity and by the pores generated during the exothermic reaction between Ti and Fe. The addition of Fe–25Ti produced brittle materials, as its low purity (91·5%) was found to be unsuitable for formulating Ti alloys.     

Effect of various sintering methods on microstructures and mechanical properties of titanium and its alloy (Ti–Al–V–X): A review

Titanium having high demand in aircraft industries because of its mechanical properties like high strength to weight ratio, high temperature performance and it’s resistant to corrosion. Therefore, Titanium and its alloys are used in airplane and engine applications. One of the major usages of alloy in the aircraft industries are Titanium alloy. By using Powder Metallurgy, the powder materials are compacted and sintered in the furnace to achieve high densities for the further process of the samples. In this paper reviews the various research investigations of Titanium and its alloy (Ti–% Al–% V–% X alloy), to optimize the microstructure and mechanical properties by various sintering methods like Conventional, Spark plasma and Microwave sintering techniques. From this the major advantages in the Spark plasma sintering tend to reduce the sintering time with high temperatures, achieving higher densities and improved microstructures tends to improve the mechanical properties of the material.     

Distinguishing the influence of aluminium and vanadium additions on microstructural evolution and densification behaviour during the sintering of ti6Al,ti4V and ti6al4v

In this work, the influence of pure Al (Ti6Al) and V (Ti4?V) powder additions on the sintering behaviour of a coarse CP-Ti powder compact was investigated. Pure Al melts and spreads to form intermetallic layers at the CP-Ti surface, causing swelling and prevention of sintering and shrinkage below 1050°C. Ti4?V compacts do not swell and begin to sinter at 990°C. The sinter rate for both Ti4?V and Ti6Al are similar at 1200°C and higher than the CP-Ti compact alone. Aluminium melting distributes this element better than the dispersed V particles, leading to more rapid homogenisation. When both pure Al and V are present (Ti6Al4?V), the sintering rate at 1200°C is similar to that of Ti6Al and Ti4?V. However, swelling is increased and homogenisation is slower, resulting in a reduced sintering aid effect compared to Ti6Al and Ti4?V.     

Investigation of the strengthening mechanism and corrosion behaviours of Vanadis 4 extra tool steel adding ZrC−TiC powders through vacuum sintering,and sub-zero and heat treatments

ABSTRACT

In the present research, different ratios of zirconium carbide (ZrC) and titanium carbide (TiC) powders were added to Vanadis 4 Extra (V4 Extra) steel powders. The composite powders (V4 Extra?ZrC?TiC) utilised vacuum sintering at 1275, 1300, 1325 and 1350°C for 1?h, respectively. The experimental results showed that good mechanical properties were obtained by the addition of 1.8 mass% ZrC and 1.2 mass% TiC (Z1.8T1.2) sintered at 1350°C for 1?h. Meanwhile, the apparent porosity was decreased to 0.02 vol.-%, and the transverse rupture strength (TRS) and hardness reached 1872?±?24?MPa and 82.5 HRA, respectively. When optimally sintered V4 Extra composites (Z1.8T1.2) underwent a series of heat treatments, the TRS value was obviously enhanced to 2007?±?17?MPa after quenching, and sub-zero and tempering heat treatments. Moreover, the sub-zero and heat treatments improved the distribution of MC carbides, which effectively enhanced the strength of sintered V4 Extra composites.