Microstructural control of and mechanical properties of mechanically alloyed tungsten heavy alloys

93W-5.6Ni-l.4Fe tungsten heavy alloys with controlled microstructures were fabricated by mechanically alloying of elemental powders of tungsten, nickel and iron by two different process routes. One was the full mechanical alloying of blended powders with a composition of 93W-5.6Ni-l.4Fe, and the other was the partial mechanical alloying of blended powders with a composition of 30W-56Ni-14Fe followed by blending with tungsten powders to form a final composition of 93W-5.6Ni-l.4Fe. The raw powders were consolidated by die compaction followed by solid state sintering at 1300°C for 1 hour in a hydrogen atmosphere. The solid state sintered tungsten heavy alloys were subsequently liquid phase sintered at 1445∼1485°C for 4-90 min. The two-step sintered tungsten heavy alloy using mechanically alloyed 93W-5.6Ni-l.4Fe powders showed tungsten particles of about 6-15 μm much finer than those of 40 um in a conventional liquid phase sintered tungsten heavy alloy. An inhomogeneous distribution of the solid solution matrix phase was obtained in the two-step sintered tungsten heavy alloy using partially mechanically alloyed powders. The two-step sintered tungsten heavy alloy using mechanically alloyed 93W-5.6Ni-l.4Fe powders showed larger elongation of 16% than that of 1% in the solid state sintered tungsten heavy alloy due to the increase in matrix volume fraction and decrease in W/W contiguity. Dynamic torsional tests of the two-step sintered tungsten heavy alloys showed reduced shear strain at maximum shear stress than did the sintered tungsten heavy alloys using the conventional liquid phase sintering.     

Impact and dynamic deformation behavior of mechanically alloyed tungsten heavy alloy

93W-5.6Ni-l.4Fe tungsten heavy alloy was fabricated by mechanical alloying process using elemental powders of tungsten, nickel and iron, followed by sintering at temperatures of 1445~1485°C under hydrogen atmosphere. The tungsten heavy alloy sintered using mechanically alloyed powders showed finer tungsten particles about 5~18 μm with high density above 99% at shorter sintering time than that fabricated by conventional liquid-phase sintering process. Charpy impact energy of mechanically alloyed tungsten heavy alloy increased with increasing the matrix volume fraction and with decreasing the W/W contiguity. The high strain rate dynamic deformation behavior of tungsten heavy alloys using torsional Kolsky bar test exhibited different fracture modes dependent on microstructure. While the brittle intergranular fracture mode was dominant when the tungsten particles were contiguously interconnected in tungsten heavy alloys solid-state sintered below 1460°C, the ductile shear fracture mode was dominant when the tungsten particles were surrounded by ductile matrix phase in tungsten heavy alloys liquid-phase sintered above 1460°C.     

Microstructure and properties of liquid-phase sintered tungsten heavy alloys by using ultra-fine tungsten powders

The microstructure and properties of liquid-phase sintered 93W-4.9Ni-2.1Fe tungsten heavy alloys using ultra-fine tungsten powders (medium particle size of 700 nm) and original tungsten powders (medium particle size of 3um) were investigated respectively. Commercial tungsten powders (original tungsten powders) were mechanically milled in a high-energy attritor mill for 35 h. Ultra-fine tungsten powders and commercial Ni, Fe powders were consolidated into green compacts by using CIP method and liquid-phase sintering at 1465℃ for 30 rain in the dissociated ammonia atmosphere. Liquid-phase sintered tungsten heavy alloys using ultra-fine tungsten powders exhibit full densification (above 99% in relative density) and higher strength and elongation compared with conventional liquidphase sintered alloys using original tungsten powders due to lower sintering temperature at 1465℃ and short sintering time. The mechanical properties of sintered tungsten heavy alloy are found to be mainly dependent on the particles size of raw tungsten powders and liquid-phase sintering temperature.     

Effects of ThO2 on the solid-state sintering behavior of W-Ni-Fe alloy

Dilatometric analyses were employed to investigate the influence of ThO₂ particles on the sintering behavior of W-Ni-Fe alloys up to 1450 °C which is below the liquid formation temperature. The activation energies were obtained by analyzing by the shift of the iso-density points as a function of the linear-heating rate. It is well known that the dominant sintering mechanism of tungsten particles is grain-boundary diffusion in the solid-state. The activation energies were 304.00-467.39 kJ/mol for W-Ni-Fe and 519.10-2949.60 kJ/mol for the thoria doped alloy, respectively. The results for the non-added alloy are in agreement with the values reported in the literature. The possibility that the much higher energies for the doped alloy reflect a retardation of sintering due to the presence of thoria particles at the surface of the tungsten is discussed.     

退火温度对挤压态细晶钨合金性能及组织演变的影响

采用稀土微合金化和液相强化烧结技术制备细晶93W-4.9Ni-2.1Fe+0.03%Y合金。研究在快速热挤压形变强化后,时效热处理对挤压态细晶93W-4.9Ni-2.1Fe+0.03%Y合金显微硬度和组织演变的影响,并与相应条件的传统钨合金进行对比。结果表明,随着退火温度的升高,2种钨合金钨相的显微硬度大大降低。EDS分析表明,随着退火温度的升高,钨合金粘结相中钨含量逐渐增加,其中细晶钨合金经过1200 ℃退火处理后,粘结相钨含量高达26.11%,而传统钨合金在1350 ℃退火处理后含量最高,达到28.14%。显微组织观察表明,退火有利于降低W-W连接度和细化钨颗粒;与传统钨合金相比,高温退火后,细晶钨合金的粘结相体积比更高且分布更为均匀     

An investigation on the solid state sintering of mechanically alloyed nano-structured 90W–Ni–Fe tungsten heavy alloy

In this study, 90W–7Ni–3Fe heavy alloy was investigated for its microstructure development, mechanical properties and fracture behavior after solid state sintering. The nano-sized powders were synthesized by mechanical alloying (MA). The microstructure of solid state sintered heavy alloys consisted of tungsten matrix. The average tungsten grain size in the range of 1.7–3.0 μm was obtained. It was found that the grain size largely affected the mechanical properties. Tensile strength more than 1200 MPa was achieved at a sintering temperature of 1350 °C. Fracture mechanisms based on microscopical observations on the fracture surfaces were studied. Matrix failure, tungsten-intergranular cleavage and tungsten–matrix interfacial separation were found to be the possible failure mechanisms.     

Tensile behavior change depending on the varying tungsten content of W–Ni–Fe alloys

Tungsten heavy alloys (WHAs) are metal–metal composites consisting of nearly pure spherical tungsten particles embedded in a Ni–Fe–W or Ni–Co–W or Ni–Cu–W ductile matrix. In this dual phase alloy, there are several complicated relations between the ductile matrix and hard tungsten particles. The aim of this research was to examine the effect of varying tungsten content on the microstructure and mechanical properties of tungsten heavy alloys. The microstructural parameters (grain size, connectivity, contiguity and solid volume fraction) were measured and were found to have a significant effect on the mechanical properties of tungsten-based heavy alloys. The result shows that the binding strength between the W and the matrix phase has a major influence on the ductility of tungsten-based alloys. The larger this binding force is, the better the ductility is.     

Microstructure and hardness of Mg-based composites reinforced with Mg2Si particles

Magnesium powders were mechanically alloyed with SiO2 powder particles having different particle sizes using high-energy ball milling techniques under Ar atmosphere for 1 h. The powders were consolidated with cold pressing under 560 Mpa. They were then sintered at 550℃ for 45 min under Ar atmosphere. The composites obtained on the Mg-SiO2 system were investigated using the Archimedes principle, a differential scanning calorimeter, X-ray diffraction, optic microscopy, and scanning electron microscopy. For the mechanically alloyed powders, the solid-state reaction of the synthesis of Mg2Si and MgO progressed further during sintering of the materials. The results showed that the strengthening mechanisms were dependent on dispersion hardening of fine Mg2Si and MgO particulates dispersed homogeneously in the matrix.     

放电等离子体烧结制备钨-钒-铬合金及性能表征

利用机械球磨、放电等离子体烧结法制备了质量分数(%,下同)为W-(10~30)V-(10~30)Cr的三元合金,对烧结后的合金进行了显微结构和室温力学性能研究。结果表明,采用放电等离子体烧结可以制得相对密度为99.7%的W-30V-20Cr合金,其实际密度比烧结纯钨降低了49.74%;显微结构分析表明V、Cr可以很好地合金化,形成塑性连续相,包裹在钨分散相的周围,很好地改善了钨合金的力学性能,W-30V-20Cr的抗弯强度为437.13 MPa,比烧结纯钨增加了25%,HV硬度为6154 MPa;W-30V-20Cr合金具有较高的断裂韧性值,为15.51 MPa·m1/2。     

Effect of microstructural parameters on the properties of W-Ni-Fe alloys

The aim of this research was to examine the effect of microstructural parameters on the tensile properties of dif- ferent compositions of tungsten heavy alloys. The microstructural parameters (grain size, connectivity, contiguity, and solid volume fraction) were measured and were found to have a significant effect on the tensile properties of tungsten-based heavy alloys. The microstructural parameters of W-Ni-Fe alloys are sufficiently different to present a range of me- chanical properties. It is concluded that the mechanical properties of tungsten heavy alloys largely depend on the micro- structural parameters and their ductility is particularly harmed when grains are contiguous.     

Microstructure and hardness of Mg-based composites reinforced with Mg<Subscript>2</Subscript>Si particles

Magnesium powders were mechanically alloyed with SiO₂ powder particles having different particle sizes using high-energy ball milling techniques under Ar atmosphere for 1 h. The powders were consolidated with cold pressing under 560 MPa. They were then sintered at 550°C for 45 min under Ar atmosphere. The composites obtained on the Mg-SiO₂ system were investigated using the Archimedes principle, a differential scanning calorimeter, X-ray diffraction, optic microscopy, and scanning electron microscopy. For the mechanically alloyed powders, the solid-state reaction of the synthesis of Mg₂Si and MgO progressed further during sintering of the materials. The results showed that the strengthening mechanisms were dependent on dispersion hardening of fine Mg₂Si and MgO particulates dispersed homogeneously in the matrix.     

Effect of heating mode and sintering temperature on the consolidation of 90W-7Ni-3Fe alloys

The present study compares the sintering response of 90W-7Ni-3Fe alloys consolidated in a 2.45 GHz microwave furnace and a conventional furnace. The W-Ni-Fe compacts were sintered in a temperature range of 1200-1500 °C corresponding to solid-state as well as liquid phase sintering. The compacts were successfully sintered in a microwave furnace with about 80% reduction in the overall processing time. For both the heating modes, the W-Ni-Fe alloys exhibited significant densification prior to melt formation through solid-state sintering. The in situ dilatometric studies revealed that the contribution to densification from solid-state sintering is higher at lower heating rates. In comparison to conventional sintering, microwave sintered compacts showed relatively refined microstructure and higher hardness and flexural strength.     

Transient Liquid-Phase Sintering Characteristic of W-Ni-Fe Alloy via Microwave-Assisted Heating

研究了W-Ni-Fe合金在2.45 GHz微波炉中瞬时液相烧结的致密化行为和力学性能。结果表明:微波辅助热场下的93W-Ni-Fe合金显示出优异的力学性能和快速的致密化过程,其压缩试样在1500℃下烧结5 min后,拉伸强度、延伸率、相对密度和硬度(HRC)分别是1200 MPa,16.6%,98.6%和42.0;在微波辅助热场下,试样烧结可以减少80%的烧结时间;微波辅助热场下的瞬时液相烧结有利于减少烧结时间,加快致密化过程,并且有利于钨晶粒的细化,获得组织均匀和综合性能高的W-Ni-Fe合金。     

Solid state and liquid phase sintering of mechanically activated W–20 wt.% Cu powder mixture

W–20 wt.% Cu powder mixture was mechanically alloyed by high-energy ball milling for various times and the effect of mechanical alloying (MA) on the sintering response of the composite compacts was investigated. The densification, microstructure, hardness and electrical conductivity after solid phase sintering (SPS) and liquid phase sintering (LPS) were examined. It was shown that the microstructure of mechanically alloyed powder profoundly influence the sintering response, i.e. a meaningful relationship between the sintering kinetics and the milling time was observed. It is suggested that MA disintegrates the W–W particle networks and increases the contribution of solid phase sintering (SPS) of nanostructured Cu and W particles on the densification. Higher hardness and conductivity were achieved by prolonged MA and SPS, indicating a lower W–W contiguity of the milled powders compared with the conventionally prepared W–Cu composite. On the other hand, depression of the melting temperature of copper up to 145 °C was noticed by affording a prolonged MA. The lower melting temperature and finer distribution of the Cu particles in the W matrix enhanced the densification during LPS and improved the homogeneity and properties of the final product.     

Preparation and properties of W–Cu–Zn alloy with low W–W contiguity

The W–Cu–Zn alloy with a-brass matrix and low W–W contiguity was prepared by method of electroless copper plating combined with spark plasma sintering(SPS) method.The effects of process and parameters on the microstructure and mechanical properties of the alloy were investigated.The W–Cu–Zn alloy with a relative density of 96 % and a W–W contiguity of about 10 % was prepared by original fine tungsten particles combined with wet mixing method and SPS solid-state sintering method at 800 °C for 10 min.The microstructure analysis shows that Cu–Zn matrix consists of nano-sized a-brass grains,and the main composition is Cu_3Zn electride.The nano-sized Cu was coated on the surface of tungsten particles by electroless copper plating method,and the fairly low consolidation temperature and short solid-state sintering time result in the nano-sized matrix phase.The dynamic compressive strength of the W–Cu–Zn alloy achieves to1000 MPa,but the alloy shows poor ductility due to the formation of the hard and brittle Cu_3Zn electrides.The fine-grain strengthening and the solution strengthening of the Cu–Zn matrix phase are responsible for the high Vickers microhardness of about 300 MPa for W–Cu–Zn alloy.     

Microstructure and properties of ultra-fine tungsten heavy alloys prepared by mechanical alloying and electric current activated sintering

The microstructure and properties of the 93W-4Ni-2Co-1Fe(mass fraction,%) tungsten heavy alloys prepared by mechanical alloying and electric current activated sintering from mixed elemental powders were investigated.After 15 h milling,the average W grain size in the powders is decreased to 120 nm.For the powders milled for 15 h,the density,hardness and transverse rupture strength of the alloys sintered only by an intensive pulse electric current are the maximum.When the total sintering time keeps constant,t...     

Sintering of a nano-crystalline tungsten heavy alloy powder

A nano-crystalline Tungsten heavy alloy powder was obtained by mechanical alloying of elemental powders in a jar mill with a high ball to powder ratio. The chemical composition of the primary powder was 93 W-4.9Ni-2.1Fe (wt%). The mechanically alloyed powder had 22 nm sized tungsten crystallites distributed in an amorphous nickel base phase. Mechanical alloying reduced particle size of powders and also yielded to more uniform particles size distribution. Sintering behavior and microstructural development of that powder were studied and compared with a conventionally mixed powder. Mechanically stored energy and better distribution of primary elements in Nano-crystalline powder had decreased motivation energy of sintering and that powders showed more densification at relatively lower sintering temperatures. Sintering at low temperatures can depress grain growth during sintering and provide desirable properties. A transient intermetallic phase was formed in the nano-crystalline powder during sintering that has not been seen in conventionally mixed powders.     

粉末冶金FeCoNiCu0.4Al0.4高熵合金的热处理组织与性能

采用机械合金化(MA)与放电等离子烧结(SPS)相结合的方法制备出FeCoNiCu0.4Al0.4高熵合金,研究不同热处理温度对合金显微组织与力学性能的影响规律。结果表明:机械合金化后,FeCoNiCu0.4Al0.4高熵合金形成了单相的FCC固溶体,经1100℃SPS烧结后的块体组织仍为单相FCC结构,其压缩屈服强度、塑性应变和显微硬度分别为1165.1 MPa、45.2%和356.9 HV。经过热处理后,合金组织中生成了新的BCC相,且BCC相的含量随热处理温度的升高先增多后减少,500、600和700℃热处理后BCC相的含量分别为7%、30%和21%(体积分数)。退火态FeCoNiCu0.4Al0.4高熵合金的屈服强度随热处理温度的升高先升高后降低。当BCC相含量增多时,材料的屈服强度和硬度相应地提高,而塑性却显著降低。     

The effect of contiguity on growth kinetics in liquid-phase sintering

Experimental and mathematical consideration of microstructural coarsening during liquid-phase sintering has resulted in kinetic laws which define grain size to the third power as being proportional to the isothermal sintering time. Despite thoseprior efforts, the situations typical to liquid-phase sintering are poorly treated by the current models because the models assume a structure consisting of widely separated spherical grains (zero contiguity). No experiment had been completed to quantify the effect of contiguity on the growth kinetics. In order to do this, the contiguity and growth rates of tungsten grains in a liquid matrix at 1,750K were measured in sintered heavy alloys of 78,83, 88,93 and 98 wt.% Wbalanced with 70Ni-30Fe. The observed grain growth rates were compared with the theoretical predictions of the LSW theory and volume fraction modified theories. By modifying the volume fraction effect with a contiguity term, a model was produced that closely followed the experimental results.     

On structure property correlation in high strength tungsten heavy alloys

Detailed structure-property correlation has been carried out in high strength tungsten heavy alloys. Alloys of compositions 90W-6Ni-2Fe-2Co, 89W-6Ni-2Fe-3Co, 89.5W-6Ni-2Fe-2Co-0.5Mo, 89.75W-6Ni-2Fe-2Co-0.25Mo, 90W-6Ni-1.5Fe-2.5Co and 90W-6Ni-1Fe-3Co have been prepared by liquid phase sintering followed by large deformation during thermo mechanical processing and studied for microstructure and mechanical properties. Despite differences in composition, higher volume fraction of matrix and lower W-W contiguity in the microstructure result in superior tensile strength and impact toughness. Increasing W content in the matrix enhances mechanical properties by imparting solid solution strengthening, increasing the matrix volume fraction and reducing W-W contiguity. The alloy 90W-6Ni-1Fe-3Co shows superior balance of properties with ultimate tensile strength of 1600 MPa and average impact toughness of 121 J/cm².