Spark plasma and microwave sintering of Al6061 and Al2124 alloys

Despite the importance of aluminum alloys as candidate materials for applications in aerospace and automotive industries, very little work has been published on spark plasma and microwave processing of aluminum alloys. In the present work, the possibility was explored to process Al2124 and Al6061 alloys by spark plasma and microwave sintering techniques, and the microstructures and properties were compared. The alloys were sintered for 20 min at 400, 450, and 500℃. It is found that compared to microwave sintering, spark plasma sintering is an effective way to obtain homogenous, dense, and hard alloys. Fully dense (100%) Al6061 and Al2124 alloys were obtained by spark plasma sintering for 20 min at 450 and 500℃, respectively. Maximum relative densities were achieved for Al6061 (92.52%) and Al2124 (93.52%) alloys by microwave sintering at 500℃ for 20 min. The Vickers microhardness of spark plasma sintered samples increases with the increase of sintering temperature from 400 to 500℃, and reaches the values of Hv 70.16 and Hv 117.10 for Al6061 and Al2124 alloys, respectively. For microwave sintered samples, the microhardness increases with the increase of sintering temperature from 400 to 450℃, and then decreases with the further increase of sintering temperature to 500℃.     

Synthesis of glass ceramics from kaolin and dolomite mixture

Cordierite-and anorthite-based binary glass ceramics of the CaO-MgO-Al₂O₃-SiO₂ (CMAS) system were synthesized by mixing local and abundant raw minerals (kaolin and doloma by mass ratio of 82/18). A kinetics study reveals that the activation energy of crystallization (Ea) calculated by the methods of Kissinger and Marotta are 438 kJ·mol-1 and 459 kJ·mol-1, respectively. The Avrami parameter (n) is estimated to be approximately equal to 1, corresponding to the surface crystallization mechanism. X-ray diffraction (XRD) analysis shows that the anorthite and cordierite crystals are precipitated from the parent glass as major phases. Anorthite crystals first form at 850℃, whereas the μ-cordierite phase appears after heat treatment at 950℃. Thereafter, the cordierite allotropically transforms to α-cordierite at 1000℃. Complete densification is achieved at 950℃; however, the density slightly decreases at higher temperatures, reaching a stable value of 2.63 kg·m-3 between 1000℃ and 1100℃. The highest Vickers hardness of 6 GPa is also obtained at 950℃. However, a substantial decrease in hardness is recorded at 1000℃; at higher sintering temperatures, it slightly increases with increasing temperature as the α-cordierite crystallizes.     

Novel sintering behavior of polystyrene nano-latex particles in filming process

Filming process of polystyrene nano-latex (NPS) particles was studied by a combination of various methods. For a constant annealing time of 1 h, the AFM images showed that the deformation and sintering temperatures for NPS particles were ca. 90℃ and 100℃ respectively. In spin-lattice relaxation measurements of solid state NMR, it is found that T_1L, T_1S and I_1L/I₀ increased significantly after annealing at 90℃ and above. DSC results showed that there was an exothermic peak near T_g after annealing for 1 h at the selected temperatures below 95℃; otherwise, the exothermic peak disappeared after annealing at 100℃ or above. The apparent density of NPS increased suddenly in the temperature range. The results implied that the macromolecules in NPS particles are in a confined state with higher conformational energy and less cohensional interactions which are the drive force for the sintering at a lower temperature compared with the multichain PS particles and the bulk polymer.     

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

Spark plasma sintering was used to fabricate Al/diamond composites. The effect of sintering temperature on the microstructure and thermal conductivity (TC) of the composites was investigated with the combination of experimental results and theoretical analysis. The composite sintered at 550℃ shows high relative density and strong interfacial bonding, whereas the composites sintered at lower (520℃) and higher (580–600℃) temperatures indicate no interfacial bonding and poor interfacial bonding, respectively. High relative density and strong interfacial bonding can maximize the thermal conductivity of Al/diamond composites, and taking both effects of particle shape and inhomogeneous interfacial thermal conductance into consideration can give a fairly good prediction of composites’ thermal conduction properties.     

Bulk amorphous Al_（85）Ni_（10）Ce_5 composite fabricated by cold hydromechanical pressing of partially amorphous powders

Gas atomized Al85Ni10Ce5 partially amorphous alloy powders were successfully consolidated into bulk alloy specimens with high relative density at room temperature by cold hydromechanical pressing. The consolidated specimens have a high fracture strength of up to 1.1 GPa. Two densification mechanisms are proposed to explain the consolidation process. The viscous flow of the amorphous phase because of local heating facilities the elimination of residual pores.     

Interfacial behavior of Fe76Si9B10P5/Zn0.5Ni0.5Fe2O4 amorphous soft magnetic composite during spark plasma sintering process

Fe_(76)Si_9B_(10)P_5/Zn_(0.5)Ni_(0.5)Fe_2O_4 amorphous composite with micro-cellular structure and high electrical resistivity was prepared by spark plasma sintering(SPS) at 487 °C. XRD and SEM results showed that the Fe_(76)Si_9B_(10)P_5 alloy powders remained the amorphous state and the composite was dense. A fusion zone at interface of Fe_(76)Si_9B_(10)P_5 cell body and Zn_(0.5)Ni_(0.5)Fe_2O_4 cell wall was observed by TEM, which also indicates the formation of local high temperature. The interface bonding based on the formation of local high temperature in SPS process was observed. It is believed that the tip effect of Zn_(0.5)Ni_(0.5)Fe_2O_4 nanoparticles promotes the local discharging and plasmas creation in the gaps, and the discharging energy forms an instantaneous local high temperature to complete the local sintering and the densification of Zn_(0.5)Ni_(0.5)Fe_2O_4 particles at a low nominal sinter temperature. Simultaneously, the local high temperature stimulates the adjacent gaps discharging, thus facilitate the continuous formation of new discharging path. Finally, sintering and densification of the amorphous composite is complete.     

MgCo2-D2 and MgCoNi-D2 systems synthesized at high pressures and interaction mechanism during the HDDR processing

MgCo_2 and MgNiCo crystallize with hexagonal Laves type intermetallic structures of the C14 type and do not form hydrides at ambient hydrogen pressures. However, applying high hydrogen pressures in the GPa range forces the hydrogen absorption and leads to the formation of multi-phase compositions, which contain approximately 2.5 atoms H per formula unit of MgCo_2 or MgNiCo and remain thermally stable under normal conditions.The hydrogenation of MgCo_2 resulted in its decomposition to a ternary Mg_2CoD_5 deuteride and metallic cobalt. Phase-structural transformations accompanying the vacuum desorption of deuterium in the temperature range of 27–500 °C were studied using in situ neutron powder diffraction. The investigation showed a complete recovery of the initial MgCo_2 intermetallic via a Hydrogenation-Disproportionation-Desorption-Recombination process. At 300°C, the Mg_2CoD_5 deuteride first decomposed to elementary Mg and hexagonal Co. At 400°C, a MgCo phase was formed by interaction between Mg and Co. At the highest processing temperature of 500°C, a solid-state interaction of MgCo and Co resulted in the recovery of the initial MgCo_2.The interaction of MgNiCo with deuterium under the synthesis conditions of 2.8 GPa and 200 °C proceeded in a more complex way. A very stable ternary deuteride MgNi_2D_3 was leached away while Co was separated in the form of Mg_2CoD_5 and the remaining nickel formed a solid solution with Co with the approximate composition Ni_(0.7)Co_(0.3).The thermal desorption of deuterium from MgCo_2D_(2.5) and from MgNiCoD_(2.5) has been studied by Thermal Desorption Spectroscopy with deuterium released into a closed volume. The observed effects nicely correlate with changes in the phase structural composition of the hydrides formed.MgCo_2 is a new example of the hydrogen storage alloy, in which a successful HDDR processing results in the reversible formation of the initial intermetallic at much lower temperatures than in the equilibrium phase diagram of the Mg-Co system.     

Effect of sintering temperature on the preparation of Cu–Ti3SiC2 metal matrix composite

Ti3SiC2 has the potential to replace graphite as reinforcing particles in Cu matrix composites for applications in brush,electrical contacts and electrode materials.In this paper the fabrication of Cu-Ti3SiC2 metal matrix composites prepared by warm compaction powder metallurgy forming and spark plasma sintering(SPS) was studied.The stability of Ti3SiC2 at different sintering temperatures was also studied.The present experimental results indicate that the reinforcing particles in Cu-Ti3SiC2 composites are not stable at and above 800℃.The decomposition of Ti3SiC2 will lead to the formation of TiC and/or other carbides and TiSi2.If purity is the major concern,the processing and servicing temperatures of the Cu-Ti3SiC2 composite should be limited to 750℃ or lower.The composites prepared by warm compaction forming and SPS sintering at 750℃ have lower density when compared with the composites prepared by SPS sintering at 950℃,but their electrical resistivity values are very close to each other and even lower.     

Effect of boehmite sol on the crystallization behavior and densification of mullite formed from a sol–gel precursor

Hybrid mullite sol was synthesized from an aqueous solution of aluminum nitrate (AN), aluminum isopropoxide (AIP) and tetraethylorthosilicate (TEOS), doped with boehmite sol with different ratios. Pressureless sintering of the xerogel was carried out at different temperatures in the presence of boehmite doping. The xerogel and sintered powder were characterized by FTIR, TG-DSC, XRD, SEM and bulk density. The addition of boehmite caused the formation of metaphase spinel (6Al2O3·SiO2) crystal before the appearance of mullite phase, which could lead to the formation of amorphous phase and suppress the premature formation of mullite. Both of these effects improve the densification of mullite. A maximum density about 98% of the theoretical density (TD, 3.01 g/cm3 ) of mullite could be obtained for 5 wt% boehmite addition at 1200 1C pressureless sintering.     

Low temperature spark plasma sintering of TC4/HA composites

Ti6Al4V/hydroxyapatite composites(TC4/HA) have been prepared by high energy ball milling and low temperature spark plasma sintering at 600 °C, 550 °C, 500 °C and 450 °C, respectively. The sintering temperature of the composites was sharply decreased as the result of the activation and sur fi cial modi fi cation effects induced from high energy ball milling. The decomposition and reaction of hydroxyapatite was successfully avoided, which offers the composites superior biocompatibility. The hydroxyapatite in the composites was distributed in gap uniformly, and formed an ideal network structure. The lowest hardness, compressive strength and Young's modulus of the composites satisfy the requirements of human bone.     

Studies on the effects of pre-firing and sintering temperature on NSDC nanocomposite electrolytes

Solid oxide fuel cells (SOFCs) technology, with fuel flexibility, is one of the most promising power generation technology. However, the high operating temperature of SOFCs has hindered their commercial applications. As a crucial requirement to enhance its performance, SOFCs electrolytes should operate at a low temperature. Carbonate/ceria composites are developed as electrolytes for low operating temperature SOFCs, and a better understanding of the mechanism of its ionic conductivity serves this purpose. In this work, ceria-carbonate composite electrolyte, Na₂CO₃/samarium doped ceria (NSDC) were synthesized by the co-precipitation method. The synthesized electrolytes were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and UV–Vis spectroscopy. The XRD and SEM results showed that the sintered NSDC nanocomposite comprised a single-phase dense electrolyte structure. The crystallite size of the NSDC nanocomposite was greatly affected by the different pre-firing temperatures and different sintering temperatures. Also, the ionic conductivity of the prepared NSDC nanocomposite electrolytes was strongly dependent on the pre-firing and sintering temperatures. The NSDC nanocomposite electrolytes were pre-fired at 950 ?°C and 650 ?°C and sintered at 1200 ?°C and 900 ?°C respectively, had ionic conductivity in H₂ and air high as 0.36 ?S/cm and 0.3 ?S/cm.     

烧结温度对铜基粉末冶金摩擦材料性能的影响

为了探究烧结温度对铜基粉末冶金摩擦材料性能的影响,通过四种温度(825、850、875、900 ℃)热压烧结,成功制备了铜基粉末冶金摩擦材料。研究了材料的微观组织、密度、硬度、抗压强度、摩擦性能,由此得到材料的较佳烧结温度。结果表明,在四种烧结温度下,材 料中的各元素能均匀地分布在Cu基体中。随着烧结温度的升高,密度、硬度、抗压强度和摩擦因数都先增大后减小,而孔隙率和磨损量先减小后增大。Cr能改善Cu与C之间的湿润性,提高金属基体与非金属组元之间的结合强度,从而使材料的密度增大;Ni、Mn能向Cu中扩散,形成固溶体,阻碍位错运动,提高材料的硬度。铜基粉末冶金摩擦材料较佳烧结温度为850 ℃,此时的密度为6.17 g/cm³,孔隙率为8.62%,维氏硬度为81.2,抗压强度为172.8 MPa,摩擦因数为0.37,磨损量为0.074 g。     

Effect of sintering parameters on the microstructure and thermal conductivity of diamond/Cu composites prepared by high pressure and high temperature infiltration

Pure Cu composites reinforced with diamond particles were fabricated by a high pressure and high temperature (HPHT) infiltration technique. Their microstructural evolution and thermal conductivity were presented as a function of sintering parameters (temperature, pressure, and time). The improvement in interfacial bonding strength and the maximum thermal conductivity of 750 W/(m·K) were achieved at the optimal sintering parameters of 1200℃, 6 GPa and 10 min. It is found that the thermal conductivity of the composites depends strongly on sintering pressure. When the sintering pressure is above 6 GPa, the diamond skeleton is detected, which greatly contributes to the excellent thermal conductivity.     

Microwave sintering effects on the microstructure and mechanical properties of Ti-51at%Ni shape memory alloys

Ti-51at%Ni shape memory alloys (SMAs) were successfully produced via a powder metallurgy and microwave sintering technique. The influence of sintering parameters on porosity reduction, microstructure, phase transformation temperatures, and mechanical properties were investigated by optical microscopy, field-emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), differential scanning calorimetry (DSC), compression tests, and microhardness tests. Varying the microwave temperature and holding time was found to strongly affect the density of porosity, presence of precipitates, transformation temperatures, and mechanical properties. The lowest density and smallest pore size were observed in the Ti-51at%Ni samples sintered at 900℃ for 5 min or at 900℃ for 30 min. The predominant martensite phases of β2 and β19' were observed in the microstructure of Ti-51at%Ni, and their existence varied in accordance with the sintering temperature and the holding time. In the DSC thermograms, multi-transformation peaks were observed during heating, whereas a single peak was observed during cooling; these peaks correspond to the presence of the β2, R, and β19' phases. The maximum strength and strain among the Ti-51at%Ni SMAs were 1376 MPa and 29%, respectively, for the sample sintered at 900℃ for 30 min because of this sample's minimal porosity.     

Densification behavior of mechanically milled Cu–8 at% Cr alloy and its mechanical and electrical properties

Synthesis and consolidation behavior of Cu–8 at%Cr alloy powders made by mechanical alloying with elemental Cu and Cr powders,and subsequently,compressive and electrical properties of the consolidated alloys were studied.Solid solubility of Cr in Cu during milling,and subsequent phase transformations during sintering and heat treatment of sintered components were analyzed using X-ray diffraction,scanning electron microscopy and transmission electron microscopy.The milled powders were compacted applying three different pressures(200 MPa,400 MPa and 600 MPa)and sintered in H2atmosphere at 900 1C for 30 min and at 1000 1C for 1 h and 2 h.The maximum densification(92.8%)was achieved for the sample compacted at 600 MPa and sintered for 1000 1C for 2 h.Hardness and densification behavior further increased for the compacts sintered at 900 1C for 30 min after rolling and annealing process.TEM investigation of the sintered compacts revealed the bimodal distribution of Cu grains with nano-sized Cr and Cr2O3precipitation along the grain boundary as well as in grain interior.Pinning of grain boundaries by the precipitates stabilized the fine grain structure in bimodal distribution.     

Mechanical properties and friction behaviors of CNT/AlSi<Subscript>10</Subscript>Mg composites produced by spark plasma sintering

The mechanical properties and friction behaviors of CNT/AlSi₁₀Mg composites produced by spark plasma sintering (SPS) were investigated. The results showed that the densities of the sintered composites gradually increased with increasing sintering temperature and that the highest microhardness and compressive strength were achieved in the specimen sintered at 450℃. CNTs dispersed uniformly in the AlSi₁₀Mg matrix when the addition of CNTs was less than 1.5wt%. However, when the addition of CNTs exceeded 1.5wt%, the aggregation of CNTs was clearly observed. Moreover, the mechanical properties (including the densities, compressive strength, and microhardness) of the composites changed with CNT content and reached a maximum value when the CNT content was 1.5wt%. Meanwhile, the minimum average friction coefficient and wear rate of the CNT/AlSi₁₀Mg composites were obtained with 1.0wt% CNTs.     

Modulation structure stability of heat-treated Co/C and CoN/CN soft X-ray multilayers

Modulation structure stability of Co/C and CoN/CN soft X ray multilayers has been investigated by X ray diffraction and Raman spectroscopy. The graphitization of the amorphous carbon layers in Co/C multilayers causes a period expansion of 12% at annealing temperatures below 400℃. An enormous period expansion (～40%) induced by the crystallization and agglomeration of Co layers has been observed at 500℃. While the period expansion of CoN/CN multilayers is only 4% at 400℃. The interface pattern of the CoN/CN multilayers still exists even if they were annealed at 700℃. The relatively good thermal stability of CoN/CN multilayers can be attributed to the suppression of the formation of the sp 3 bonding and, at annealing temperatures higher than the phase transition temperature of 420℃ (from hcp to fcc), the coexistence of hcp and fcc Co structures through doping nitrogen.     

纳米结构碳化钽在超高压力下硬度的研究

通过利用国产DS6×800T铰链式六面顶压机装置高温高压烧结了纳米结构的碳化钽样品,研究和表征了纳米结构碳化钽在超高压力下的物性行为。样品在3 GPa/1 500℃下进行烧结,其相对密度为93%。实验结果表明超高压力更有利于样品的致密化,并且可以降低烧结温度。通过烧结实验,得到了纳米结构碳化钽在压力为3 GPa时的维氏硬度为17.2 GPa,平均断裂韧度为(5.0±0.2)MPa m1/2。     

Influence of sintering temperature on the structure and piezoelectric properties of ZnO-modified (Li, Na, K)NbO3 lead-free ceramics

ZnO-modified (Li, Na, K)NbO₃ lead-free ceramics with a nominal composition of Li_0.06(Na_0.535K_0.48)_0.94NbO₃+0.7mol% ZnO (LNKN-Z₇) was synthesized normally at 930?C1000°C. The Zn ions incorporated into the A-site at a higher sintering temperature, which changed LNKN-Z₇ to soft piezoelectric ceramics with the mechanical quality factor decreasing from 228 to 192. A phase transition from tetragonal to orthorhombic symmetry was identified by XRD analysis, and the corresponding calculation of lattice parameters was conducted at 970?C980°C. Because of such transitional behavior and fine microstructure, the optimized values of piezoelectric coefficient, planar electromechanical coupling coefficient, and relative dielectric constant were obtained.     

Microwave sintering of Ca<Subscript>0.6</Subscript>La<Subscript>0.2667</Subscript>TiO<Subscript>3</Subscript> microwave dielectric ceramics

Ca_0.6La_0.2667TiO₃ ceramics were prepared by conventional and microwave sintering techniques and their sinterability, microstructure, and microwave dielectric properties were investigated in detail for comparison. Densified Ca_0.6La_0.2667TiO₃ ceramics were obtained by microwave sintering at 1350°C for 30 min and by conventional sintering at 1450°C for 4 h. An unusual phenomenon was found that some larger grains (grain size range: 8–10 μm) inclined to assemble in one area but some smaller ones (grain size range: 2–4 μm) inclined to gather in another area in the microwave sintered ceramics. The microwave dielectric properties of Ca_0.6La_0.2667TiO₃ ceramics prepared by microwave sintering at 1350°C were as follows: dielectric constant (ɛ _r) = 119.6, quality factor (Qf) = 17858.5 GHz, and temperature coefficient of resonant frequency (τ _f) = 155.5 ppm/°C. In contrast, the microwave dielectric properties of the ceramics prepared by conventional sintering at 1450°C were ɛ _r = 117.4, Qf = 13375 GHz, and τ _f = 217.2 ppm/°C.