Mechanical properties and microstructure of Fe3Al intermetallics fabricated by mechanical alloying and spark plasma sintering

Fabrication technology and mechanical properties of the Fe3Al based alloys were studied by spark plasma sintering from elemental powders （Fe-30Al, volume fraction, %） and mechanically alloying powders. The mechanically alloying powders were processed by the high-energy ball milling the elemental mixture powders with the milling time of 5, 8 and 10 min, respectively. The spark plasma sintering process was performed under the pressure of 50 MPa at 1 050 ℃ for 5 min. The phase identification by X-ray diffraction presents the Fe reacts with Al completely during the processing time. The samples are nearly full density （e.g. the relative density of sinter of raw powder is 99%）. The microstructure was observed by TEM. The mechanical properties were tested by three-point bending at room temperature in air. The results show that the mechanical properties are better （e.g. bend strength of 1 500 MPa ） than those of the ordinary Fe3Al casting.     

Mechanical properties of β-SiC fabricated by spark plasma sintering

The consolidation of SiC nanopowder synthesized by the mechanical alloying method was subsequently accomplished by spark plasma sintering of 1700 °C for 10 min under an applied pressure of 40 MPa. The SiC sintered compact with relative density of 98% consisted of nano-sized particles smaller than 100 nm. This phenomenon resulted in the ordering process of stacking disordered structure formed by mechanical alloying. In this work, the effect of grain size and relative density on the mechanical properties were studied. The mechanical properties of sintered compacts were evaluated and compared with the reference samples fabricated from the commercial SiC powder (β-SiC, 0.3 μm, IBIDEN Co., Gifu, Japan) with sintering additive (B–C mixture). The Vickers hardness and bending strength of those sintered compacts increased with the increment of the density. However, the mechanical properties were lower than those of reference samples in case of lower density, even though the mechanical property was close to that of reference sample in case of higher density. This phenomenon was considered for the difference of bond strength between grains because those sintered compacts were fabricated without any sintering additives, while those reference samples were fabricated by accelerating the grain bonding with a sintering additive of B–C mixture. In other words, those results indicated that the effect of sintering additive affected on mechanical properties directly. This paper was presented at the International Symposium on Manufacturing, Properties, and Applications of Nanocrystalline Materials sponsored by the ASM International Nanotechnology Task Force and TMS Powder Materials Committee on October 18–20, 2004 in Columbus, OH.     

放电等离子烧结Ti-43Al-9V合金显微组织和力学性能(英文)

采用机械合金化和放电等离子烧结工艺制备细晶Ti-43Al-9V合金,研究不同烧结温度与显微组织和力学性能之间的关系。结果表明:机械球磨后粉末形状规则,尺寸在5～30μm之间,烧结所得块体材料主要由γ-TiAl、α2-Ti3Al和少量B2相组成。烧结温度为1150°C时,获得的等轴晶粒尺寸为300nm～1μm。烧结温度升高到1250°C时,等轴晶粒的尺寸明显增大,显微硬度从HV592降低到HV535,抗弯强度从605降低到219MPa,压缩断裂强度从2601降低到1905MPa,压缩率从28.95%降低到12.09%。     

放电等离子烧结合成晶化相增强的块状Ti66Nb18Cu6.4Ni6.1Al3.5细晶复合材料

基于改进的非晶形成合金体系,选取Ti66Nb18Cu6.4Ni6.1Al3.5合金为研究对象,通过放电等离子烧结机械合金化制备的非晶合金粉末,结合非晶晶化法,合成以高Nb含量的晶化β-Ti(Nb)延性相为基体的块状细晶复合材料.利用X射线衍射(XRD)、差示扫描量热仪(DSC)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)和万能材料试验机等手段对合成的非晶合金粉末和细晶复合材料进行表征分析.结果表明球磨60h后,初始混合粉末绝大部分转变成了非晶相,其玻璃转变温度、晶化温度、晶化峰值温度和熔化温度分别为750K、830K、847K和1422K,表明Nb含量的增加显著提高合金体系的热稳定性.另外,合成的块状钛基细晶复合材料的显微结构为β-Ti延性相包围(Cu,Ni)-Ti2相,其相区尺寸均大于1μm.当升温速率为167K/min、烧结温度为1373K时,合成的复合材料密度、屈服强度、断裂强度和断裂应变分别为5.64g/cm3、1705.8MPa、2126.4MPa和5.4%.     

Microstructural evolution and sintering kinetics during spark plasma sintering of Fe and Al blended powder

The reaction diffusion between Fe and Al during spark plasma sintering (SPS) was studied. Microstructural evolution was investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM) and the sintering kinetics was disclosed. The main interphase of the SPS sample was Fe₂Al₅ at 773–873 K. Ball-milling enabled a large number of lattice defects and grain boundaries thus the reaction kinetics was accelerated, although the direct current can also promote those defects. After milling, the phase transformation kinetics was improved from 0.207 before mill to 4.56×10^?3. Besides, this work provided more details for the generation of Joule heating. The resistance offered to the electric path was considered to be the source of Joule heating, and particularly the resistance offered by the different contact interfaces of die, punch, graphite foil and the sample played a leading role for the generation of Joule heating during spark plasma sintering.     

Mechanical alloying and characteristics of spark plasma sintering of Ti-A1 composite powders

The mechanical alloying process of Ti-Al composite powders were carried out by use of high energy ball-milling machine. Structure variations of powder mixtures during mechanical alloying and characteristic of spark plasma sintering were investigated. The results show that during milling, TiAl, Ti3Al and Ti2Al phase intermetallic compounds are formed, simultaneously with powder refinement for the （TiH2-45Al-0.2Si-SNb） and （TiH2-45Al-0.2Si-7Nb） mixtures. The particle sizes of two powder mixtures are less than 300 nm after milling for 30 h. Sintering process of the milled powder can be completed in a short time by spark plasma sintering, and the sintering microstructure is composed of fine and homogeneous TiAl and Ti3Al phase.     

放电等离子烧结-非晶晶化法合成Ti7oNb7.8Cu8.4Ni7.2Al6.6复合材料

采用机械合金化制备不含和含2%(体积分数)B4C的钛基非晶合金粉末,随后采用放电等离子烧结-非晶晶化法合成不含／含(TiB+TiC)的Ti7oNb7.8Cu8.4Ni7.2Al6.6超细晶／细晶钛基复合材料;运用X射线衍射分析(XRD)、差示扫描量热分析(DSC)、扫描电子显微镜(SEM)和万能材料试验机等对制备的钛基非晶粉末和超细晶／细晶钛基复合材料进行表征.结果表明高能球磨80h的钛基粉末中主要为非晶相,B4C颗粒的加入对钛基粉末的玻璃转变温度、晶化温度和晶化焓有显著的影响.另外,不含／含(TiB+TiC)的复合材料的显微硬度分别为5.47和5.33GPa;以50K/min升温到1223K并保温10min获得的Ti70Nb7.8Cu8.4Ni7.2Al6.6块体试样的断裂强度和断裂应变分别为2098MPa和11.5%.     

双步球磨和放电等离子烧结TiAl基合金的显微组织和力学性能(英文)

采用双步球磨法和放电等离子烧结技术制备细晶Ti-45Al-2Cr-2Nb-1B-0.5Ta-0.225Y(摩尔分数,%)合金,并研究烧结温度、显微组织和力学性能之间的关系。结果表明:双步球磨粉末的颗粒形状较规则,其颗粒尺寸为20～40μm,主要由TiAl和Ti3Al相组成。放电等离子烧结后的块体由主相TiAl、少量的Ti3Al相及Ti2Al和TiB2相组成。当烧结温度为900°C时,烧结块体获得的主要组织是等轴晶组织,等轴晶粒尺寸大多数在100~200nm的范围内,合金的压缩断裂强度为2769MPa,压缩率为11.69%,抗弯强度为781MPa;当烧结温度为1000°C时,等轴晶粒明显长大,TiB2相明显增多,合金的压缩断裂强度为2669MPa,压缩率为17.76%,抗弯强度为652MPa。随着烧结温度的升高,合金的维氏硬度由658降低到616。压缩断口形貌分析表明,合金的断裂方式为沿晶断裂。     

Fabrication and mechanical properties of WC-Co-Al2O3 nanocomposites by spark plasma sintering

Small amounts of nanocrystalline Al2O3 particles were doped in WC-Co nanocrystalline powders to study their reinforcing effects, and spark plasma sintering technique was used to fabricate the WC-Co-Al2O3 nanocomposites. Experimental results show that the use of Al2O3 nanoparticles as dispersions to reinforce WC-Co composites can increase the hardness, especially the transverse rupture strength of the WC-Co hardmetal. With addition of 0.5%(mass fraction) Al2O3 nanoparticles, the spark plasma sintered WC-TCo-0. 5Al2O3 nanocomposites exhibit hardness of 21.22 GPa and transverse rupture strength of 3 548 MPa. The fracture surface of the WC-TCo-0.5Al2O3 nanocomposites mainly fracture with transcrystalline rupture mode. The reinforcing mechanism is maybe related to the hindrance effect of microcracks propagation and the pinning effect for the dislocations movement, as well as the residual compressive strength due to the Al2O3 nanoparticles doped.     

放电等离子烧结时间对高密度W-7Ni-3Fe合金组织性能的影响

利用放电等离子烧结技术制备高密度W-7Ni-3Fe合金,研究了烧结保温时间对合金致密度、物相、显微组织以及力学性能的影响。结果表明,在1200℃烧结5~14 min后,合金均能实现充分致密化,保温时间对相对密度影响较小。合金中的W晶粒随保温时间的延长开始尺寸变化不大,烧结11 min以上才明显长大,但大多数W晶粒尺寸仍小于5μm。烧结时间超过8min,合金中新出现一种灰色的富W组织。随保温时间延长,合金的洛氏硬度下降不大,然而抗弯强度却明显上升。合金弯曲断口形貌在较短保温时间以沿晶断裂为主,粘结相的延性撕裂和W晶粒的解理断裂随烧结时间延长逐渐增多。     

高分数GNFs/6061Al基复合材料的放电等离子体烧结制备及其显微组织与性能

采用放电等离子体烧结(SPS)工艺在610℃制备30％～50％(质量分数)纳米石墨片(GNF)/6061Al基复合材料,研究烧结压力及GNF含量对复合材料显微组织和力学、热学性能的影响.结果表明,SPS有效抑制GNFs/6061Al基复合材料中Al4C3等界面反应产物的生成.随着GNF含量的增加,GNFs团聚程度增加,...     

Mechanical and corrosion properties of Ti-35Nb-7Zr-xHA composites fabricated by spark plasma sintering

To improve the bioactivity of Ti-Nb-Zr alloy, Ti-35Nb-7Zr-xHA (hydroxyapatite, x=5, 10, 15 and 20, mass fraction, %) composites were fabricated by spark plasma sintering. The effects of the HA content on microstructure, mechanical and corrosion properties of the composites were investigated utilizing X-ray diffraction (XRD), scanning electron microscope (SEM), mechanical tests and electrochemical tests. Results show that all sintered composites are mainly composed of β-Ti matrix, α-Ti and metal–ceramic phases (CaO, CaTiO₃, CaZrO₃, Ti_xP_y, etc). Besides, some residual hydroxyapatites emerge in the composites (15% and 20% HA). The compressive strengths of the composites are over 1400 MPa and the elastic moduli of composites ((5%–15%) HA) present appropriate values (46–52 GPa) close to that of human bones. The composite with 15% HA exhibits low corrosion current density and passive current density in Hank's solution by electrochemical test, indicating good corrosion properties. Therefore, Ti-35Nb-7Zr-15HA composite might be an alternative material for orthopedic implant applications.     

放电等离子烧结制备Fe75Zr3Si13B9磁性材料

采用机械合金化技术制备Fe75Zr3Si13B9非晶合金粉体,利用SPS放电等离子烧结技术在不同烧结温度下将非晶合金粉体制备成d20 mm×7 mm的块体非晶纳米晶合金。采用XRD和DSC分析了Fe75Zr3Si13B9非晶合金粉体的相组成、玻璃转变温度Tg、开始晶化温度Tx和晶化峰温度Tp。然后利用XRD、SEM、Gleeble3500、VSM分析不同烧结温度下块体的相转变、微观形貌、力学性能和磁性能。研究表明,在500 MPa的烧结压力下,随着烧结温度的升高,非晶相开始晶化形成非晶纳米晶双相结构,同时,样品的致密度、抗压强度、微观硬度、饱和磁化强度均显著提高。最后在500 MPa的烧结压力和863.15 K的烧结温度下,获得密度6.9325 g/cm3、抗压强度1140.28 MPa、饱和磁化强度1.28 T的非晶纳米晶磁性材料。     

Microstructure,sintering behavior and mechanical properties of SiC/MoSi2 composites by spark plasma sintering

SiC/MoSi₂ composites were synthesized at different temperatures by spark plasma sintering using Mo, Si and SiC powders as raw materials. The phase composition, microstructure and mechanical properties of the as-prepared composites were investigated and the sintering behavior was also discussed. Results show that SiC/MoSi₂ composites are composed of MoSi₂, SiC and trace amount of Mo_4.8Si₃C_0.6 phase and exhibit a fine-grain texture. During the synthesis process, there was an evolution from solid phase sintering to liquid phase sintering. When sintered at 1600 °C, the SiC/MoSi₂ composites present the most favorable mechanical properties, the Vickers hardness, bending strength and fracture toughness are 13.4 GPa, 674 MPa and 5.1 MPa·m^1/2, respectively, higher 44%, 171%, 82% than those of monolithic MoSi₂. SiC can withstand the applied stress as hard phase and retard the rapid propagation of cracks as second phase, which are beneficial to the improved mechanical properties of SiC/MoSi₂ composites.     

Microstructures and mechanical properties of TiAl alloy prepared by spark plasma sintering

A fine-grained TiAl alloy with a composition of Ti-47%Al(mole fraction) was prepared by double mechanical milling(DMM) and spark plasma sintering(SPS). The relationship among sintering temperature, microstructure and mechanical properties of Ti-47%Al alloy was studied by X-ray diffractometry(XRD), scanning electron microscopy(SEM) and mechanical testing. The results show that the morphology of double mechanical milling powder is regular with size of 20?40 μm. The main phase TiAl and few phases Ti₃Al and Ti₂Al were observed in the SPS bulk samples. For samples sintered at 1000 °C, the equiaxed crystal grain was achieved with size of 100?250 nm. The samples exhibited compressive and bending properties at room temperature with compressive strength of 2013 MPa, compression ratio of 4.6% and bending strength of 896 MPa. For samples sintered at 1100 °C, the size of equiaxed crystal grain was obviously increased. The SPS bulk samples exhibited uniform microstructures, with equiaxed TiAl phase and lamellar Ti₃Al phase were observed. The samples exhibited compressive and bending properties at room temperature with compressive strength of 1990 MPa, compression ratio of 6.0% and bending strength of 705 MPa. The micro-hardness of the SPS bulk samples sintered at 1000 °C is obviously higher than that of the samples sintered at 1100 °C. The compression fracture mode of the SPS TiAl alloy samples is intergranular fracture and the bending fracture mode of the SPS TiAl alloy samples is intergranular rupture and cleavage fracture.     

Influence of process control agents on the performance of Ni3Al by mechanical alloying

The influence of process control agents (PCAs) on the mechanical properties of Ni3Al intermetallic compounds by mechanical alloying was in- vestigated in order to develop oxide deposition reinforced intermetallics. The PCAs in mechanical alloying were pure ligroin, 75 vol.% ligroin 25 vol.% alcohol, 50 vol.% ligroin 50 vol.% alcohol, 25 vol.% ligroin 75 vol.% alcohol, and pure alcohol. The normal composition is Ni-22.9at.%Al-0.5at.%B, the ball-to-powder weight ratio is 10:1, and the milling time is 30 min. Then, the powders were sintered by spark plasma sintering under 40 MPa for 5 min at 1000°C. The results show that a higher bending strength and a higher hardness were obtained when the PCAs were 75% ligroin 25% alcohol in mechanical alloying. The bending strength is about 2700 MPa and the hardness (HV) is more than 6 GPa.     

放电等离子体烧结技术制备过共晶Al-Si-Fe粉末冶金合金的显微组织和压缩变形行为

Al-Si-Fe基铝合金材料由于具有高耐磨性、低密度以及低热膨胀性能,因而主要用于汽车发动机部件。利用气体雾化粉末,采用放电等离子体烧结技术制备Al-17Si-5Fe-2Cu-1Mg-1Ni-1Zr合金。所制备材料的晶粒尺寸为530nm,并且观察到细等轴晶粒和均匀分布的析出物。研究了放电等离子体烧结技术制备的材料在不同温度和应变速率下的压缩变形行为。结果表明,所有的真应力一真应变曲线在达到峰值应力后呈稳态流动趋势,随着测试温度的升高和应变速率的降低,峰值应力呈下降趋势。在变形样品中,观察到了等轴晶粒和等轴晶粒中的位错结构。这些现象说明,合金在高温变形过程中发生了动态再结晶。     

Consolidation and properties of ultrafine binderless cemented carbide by spark plasma sintering

Owing to the absence of metal binder, binderless cemented carbides have higher wear, corrosion, and oxidation resistance. WC-0.3VC-0.5Cr3C2 powders with an average particle size of 200nm and a little amount of active element were consolidated by spark plasma sintering. The sintered microstructure revealed that the average WC grain size was 0.24μm, which was almost consistent with the initial fine powder. The results of XRD showed that W2C phase was formed. Nearly complete densification of ultrafine binderless cemented carbide was achieved by sintering at 1400℃ for 120s under 50MPa. The resulting hardness and the fracture toughness were 28.18 GPa and 6.05MPa·m1/2, respectively.