Effect of processing parameters on the microstructure and thermal conductivity of diamond/Ag composites fabricated by spark plasma sintering

Diamond/metal composites with 50 vol.% diamond have been produced by spark plasma sintering (SPS) using pure Ag as a matrix and diamond particles as reinforcement. Three kinds of powder mixing processes were used to prepare the mixture of diamond/Ag powders: dry mixing without milling medium, wet mixing and magnetic blending. Subsequently, they were all consolidated by SPS at various processing parameters to produce bulk diamond/Ag composites. Then samples were heat treated in order to obtain a higher thermal conductivity. The effect of processing parameters on the morphologies of the mixed powders, the microstructure and the thermal conductivity of the composites were investigated by comparing the experimental data. It reveals that particles were easy to agglomerate and the distribution of mixed powders was inhomogeneous by dry mixing method, and wet mixing method is too complex. The most favorable mixing process is magnetic blending by which the powders can be homogenously mixed and the composites prepared by optimized SPS processing parameters can obtain the highest relative density and the best thermal conductivity among the composites prepared by different processes. The magnetic blending diamond/Ag composites even have a 23% increase in thermal conductivity compared with pure silver sintered by SPS.     

Effect of particle size on the microstructure and thermal conductivity of Al/diamond composites prepared by spark plasma sintering

Spark plasma sintering (SPS) was used to fabricate Al/diamond composites. The influence of diamond particle size on the microstructure and thermal conductivity (TC) of composites was investigated by combining experimental results with model prediction. The results show that both composites with 40 μm particles and 70 μm particles exhibit high density and good TC, and the composite with 70 μm particles indicates an excellent TC of 325 W·m⁻¹·K⁻¹. Their TCs lay between the theoretical estimated bounds. In contrast, the composite with 100 μm particles demonstrates low density as well as poor TC due to its high porosity and weak interfacial bonding. Its TC is even considerably less than the lower bound of the predicted value. Using larger diamond particles can further enhance thermal conductive performance only based on the premise that highly dense composites of strong interfacial bonding can be obtained.     

放电等离子烧结法制备Cu/金刚石复合材料的性能与显微组织

由于具备较高的热导率,铜/金刚石复合材料已成为应用于电子封装领域的新一代热管理材料。采用放电等离子烧结工艺（SPS）成功制备含不同金刚石体积分数的Cu/金刚石复合材料,研究复合材料的相对密度、微观结构均匀性和热导率（TC）随金刚石体积分数（50%、60%和70%）和烧结温度的变化规律。结果表明：随着金刚石体积分数的降低,复合材料的相对密度、微观结构均匀性和热导率均升高;随着烧结温度的提高,复合材料的相对密度和热导率不断提高。复合材料的热导率受到金刚石体积分数、微观结构均匀性和复合材料相对密度的综合影响。     

体积分数和烧结温度对(AlSiTiCrNiCu)p/6061Al复合材料的热导率的影响

高熵合金具有高硬度、高强度、耐磨、耐腐蚀、高温热稳定等优异性能,源于金属-金属间天然的界面结合特性,高熵合金与铝合金有良好的界面润湿性。本文采用AlSiTiCrNiCu高熵合金颗粒作为增强相增强铝合金,研究高熵合金体积分数与烧结温度对复合材料导热性能的影响。结果表明,(AlSiTiCrNiCu)p/6061Al复合材料的导热率随着AlSiTiCrNiCu颗粒体积分数的增大而降低,20 vol.% (AlSiTiCrNiCu)p/6061Al复合材料的导热率为61.59 W/(m?K),相比于基体6061Al合金降低了52 %。当体积分数为10%时,随着烧结温度的升高,复合材料的导热率降低,烧结温度为540℃时,复合材料的导热率为65.80 W/(m?K)。TEM分析,高熵合金与铝合金的界面为扩散性界面,没有发生界面发应,有助于导热率的降低。     

Influence of powder characteristics on structure and properties of Ni3Al fabricated by spark plasma sintering

Three kinds of Ni and Al powder mixtures with nominal composition Ni75Al25 were employed to prepare Ni3Al alloys by spark plasma sintering（SPS） process. The raw powders include fine powder, coarse powder and mechanically-alloyed fine powder. The effects of powder characteristics and mechanical alloying on structure and properties of sintered body were investigated by scanning electron microscopy（SEM）, X-ray diffraction（XRD）, bending test and Vickers hardness measurements. For all mixture powders near fully dense Ni3Al alloys （relative density〉99.5%） are obtained after sintering at 1150℃ for 5 min under 40 MPa. However a small fraction of Ni can be reserved for alloy from coarse powders. The results reveal that grain size is correlated with particle character of raw powder. Ni3Al alloy made from mechanically-alloyed fine powder has finer and more homogenous microstructure. The hardness of all alloys is similar varying from HV470 to 490. Ni3Al alloy made from mechanically-alloyed fine powder exhibites higher bending strength （1 070 MPa） than others.     

热处理对金刚石/2024Al复合材料微观组织和热物理性能的影响

采用挤压铸造法制备粒径为5μm、体积分数为50%的金刚石/2024Al 复合材料。退火处理后对其金相组织界面反应、界面结合情况以及金刚石颗粒的内部缺陷进行观察与分析,并对其热物理性能进行测试与研究。结果表明,金刚石/2024Al 复合材料的组织致密,无明显的气孔、夹杂等缺陷;颗粒为不规则多边形,有棱角,分布比较均匀。透射电镜观察表明,部分金刚石颗粒内部有位错和层错存在,而2024Al 基体中的位错密度较大,金刚石/2024Al界面处有较多的界面反应物生成,可能为Al2Cu。复合材料在20~100°C温度区间内的平均热膨胀系数为8.5×10-6°C-1,退火处理的复合材料其热膨胀系数有一定程度的降低;随着温度的升高,复合材料的平均热膨胀系数也呈现增加的趋势。复合材料的热导率约为100 W/（m·K）,退火处理能够提高复合材料的热导率。     

Predicted interfacial thermal conductance and thermal conductivity of diamond/Al composites with various interfacial coatings

The interfacial thermal conductance (ITC) and thermal conductivity (TC) of diamond/Al composites with various coatings were theoretically studied and discussed. A series of predictions and numerical analyses were performed to investigate the effect of thickness, sound velocity, and other parameters of coating layers on the ITC and TC. It is found that both the ITC and TC decline with increasing coating thickness, especially for the coatings with relatively low thermal conductivity. Nevertheless, if the coating thickness is close to zero, or quite a small value, the ITC and TC are mainly determined by the constants of the coating material. Under this condition, coatings such as Ni, TiC, Mo 2 C, SiC, and Si can significantly improve the ITC and TC of diamond/Al composites. By contrast, coatings like Ag will exert the negative effect. Taking the optimization of interfacial bonding into account, conductive carbides such as TiC or Mo 2 C with low thickness can be the most suitable coatings for diamond/Al composites.     

Microstructures and mechanical properties of the in situ TiB-Ti metal-matrix composites synthesized by spark plasma sintering process

In situ synthesized TiB reinforced titanium matrix composites have been synthesized by spark plasma sintering (SPS) process at 950-1250 °C, using mixtures of 15 wt% TiB₂ and 85 wt% Ti powders. The effects of the sintering temperature on densification behavior and mechanical properties of the TiB-Ti composites were investigated. The results indicated that with rising sintering temperatures, relative densities of the composites increase obviously, while the in situ TiB whiskers grow rapidly. As a result, bending strength of the TiB-Ti composites increases slowly at the combined actions of the factors referred above. Fracture toughness of the composites is improved remarkably due to the large volume fraction of Ti matrix, the crack deflection, pull-out and the micro-fracture of the needle-shaped TiB grains. The results also suggested that TiB-Ti composite sintered at 1250 °C by SPS process exhibits the highest relative density of 99.6% along with bending strength of 1161 MPa and fracture toughness of 13.5 MPa m^1/2.     

Al2O3p/Al复合材料中颗粒粒径与形态对组织和性能的影响

选用 5 .0和 0 .15 μm两种粒径的Al2 O3 颗粒 ,制备了Al2 O3 体积分数为 40 %的铝基复合材料。利用透射电镜对两种复合材料拉伸前后的组织进行观察 ,结果表明 :5 μm尖角形Al2 O3 颗粒增强复合材料的铸态组织中存在高密度的位错 ,这主要是由于热错配应力引起的 ;0 .15 μm椭球形Al2 O3 颗粒增强复合材料的铸态组织中几乎观察不到位错 ,这与颗粒细小且为等轴状、分布弥散、界面附近应力分布均匀等因素有关。对拉伸断口附近显微组织的观察表明 ,前者基体中位错进一步增殖 ,后者则存在明显的位错环。室温拉伸结果表明亚微米Al2 O3p/Al复合材料中的这种微观组织有利于材料强度和塑性的提高     

SiC_p/2024铝合金复合材料粉末混合半固态挤压法制备

研究了SiCp/ 2 0 2 4铝合金复合材料的粉末混合 半固态挤压成形工艺及所制备材料的组织和界面特征。不同温度下半固态挤压的挤压力与位移曲线表明 ,半固态挤压过程的成形力低且稳定。SEM和TEM电镜观察结果表明 ,该工艺可以获得增强颗粒分布均匀、基体组织致密、界面结合良好且无界面反应的复合材料型材。分析了半固态挤压后复合材料的力学性能 ,结果表明 :与基体合金相比 ,复合材料的弹性模量、屈服强度、抗拉强度均有很大提高 ;与其它工艺生产的该复合材料相比 ,所制备的复合材料的塑性相对较高。     

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.     

Thermal conductivity behavior of SPS consolidated AIN/Al composites for thermal management applications

AIN/Al composites are a potentially new kind of thermal management material for electronic packaging and heat sink applications.The spark plasma sintering(SPS)technique was used for the first time to prepare the AIN/Al composites,and attention was focused on the effects of sintering parameters on the relative density,microstructure and,in particular,thermal conductivity behavior of the composites.The results showed that the relative density and thermal conductivity of the composites increased with increasing sintering temperature and pressure.The composites sintered at 1550℃ for 5 min under 70 Mpa showed the maximum relative density and thermal conductivity,corresponding to 99% and 97.5 W·m-1·K-1,respectively.However,the thermal conductivity of present AIN/Al composites is still far below the theoretical value.Possible reasons for this deviation were discussed.     

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.     

Process optimization,microstructures and mechanical/thermal properties of Cu/Invar bi-metal matrix composites fabricated by spark plasma sintering

An orthogonal experiment scheme was designed to investigate the effects of the Cu content, compaction pressure, and sintering temperature on the microstructures and mechanical and thermal properties of (30–50)wt.%Cu/ Invar bi-metal matrix composites fabricated via spark plasma sintering (SPS). The results indicated that as the Cu content increased from 30 to 50 wt.%, a continuous Cu network gradually appeared, and the density, thermal conductivity (TC) and coefficient of thermal expansion of the composites noticeably increased, but the tensile strength decreased. The increase in the sintering temperature promoted the Cu/Invar interface diffusion, leading to a reduction in the TC but an enhancement in the tensile strength of the composites. The compaction pressure comprehensively affected the thermal properties of the composites. The 50wt.%Cu/Invar composite sintered at 700 °C and 60 MPa had the highest TC (90.7 W/(m·K)), which was significantly higher than the TCs obtained for most of the previously reported Cu/Invar composites.     

Thermal conductivity behavior of SPS consolidated AlN/Al composites for thermal management applications

AlN/Al composites are a potentially new kind of thermal management material for electronic packaging and heat sink applications.The spark plasma sintering (SPS) technique was used for the first time to prepare the AlN/Al composites,and attention was focused on the effects of sintering parameters on the relative density,microstructure and,in particular,thermal conductivity behavior of the composites.The results showed that the relative density and thermal conductivity of the composites increased with increasing sintering temperature and pressure.The composites sintered at 1550 ℃ for 5 min under 70 MPa showed the maximum relative density and thermal conductivity,corresponding to 99% and 97.5 W m-1 K-1,respectively.However,the thermal conductivity of present AlN/Al composites is still far below the theoretical value.Possible reasons for this deviation were discussed.     

Ti2SnC质量分数对铜基复合材料显微组织及性能的影响

为了制备强度高导电性能优异的铜基复合材料,以三元层状导电陶瓷Ti2SnC作为增强相,通过直热法粉末烧结技术制备Ti2SnC/Cu复合材料。研究了在烧结温度800℃、成型压力45MPa、保温时间30min、真空度50Pa的成型条件下,质量分数分别为0、5%、8%、10%的Ti2SnC增强相对复合材料的显微结构、硬度、抗拉强度、抗冲击韧性和导电率等性能的影响。结果表明:Ti2SnC的质量分数为5%时,综合性能最优,致密度和导电率分别达到94%、39%IACS,抗拉强度248MPa,硬度为88.7HBS,可适用于受电弓滑板。     

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.     

微波烧结工艺对Ti-Mg复合材料组织和性能的影响

为了确定制备Ti-Mg复合材料的最佳微波烧结工艺,采用微波烧结制备了Ti-15Mg复合材料。采用扫描电镜、差热分析、X射线衍射、光学显微镜、压缩试验以及耐腐蚀性测试等系统性地研究了烧结温度、保温时间对复合材料微观组织、力学性能和耐腐蚀性能的影响。结果表明,烧结温度为540~600 ℃,随着烧结温度的升高,复合材料的致密化程度提高,孔隙率降低,抗压强度增强,耐腐蚀性增强;烧结温度为600 ℃时,镁均匀地分布在钛基体中,复合材料的性能最佳,满足作为医用材料的性能要求;烧结温度继续升高则会导致复合材料中镁的大量挥发,孔隙率增加,复合材料的强度下降。微波烧结制备Ti-15Mg复合材料具有快速、稳定烧结的特点,因此保温时间对复合材料性能的影响不明显。