In-Situ Characterization of SiC–AlN multiphase ceramics

AlN and SiC can react and form a solid solution at temperatures above 1800 °C, a result that may be beneficial for sintering silicon carbide ceramics. The pressureless sintered AlN–SiC multiphase ceramics have reached high density at a temperature of 2100 °C for 1 hr in Ar. Analytical scanning transmission electron microscopy was then used to determine the grain boundary, fracture surface, and the local compositions. Because AlN has a higher solid vaporization pressure than SiC, the vaporization rate of the AlN solid would far exceed that of SiC at a sintering temperature. The vaporizing AlN was deposited on the surface of SiC powder; SiC grains then elongated in a random arrangement. The form of elongated rod crystals of 4H SiC is 5 to 8 m in length and 1 m in width. It resulted in the sample fracture section producing pulling-out and a strong tearing-open effect. The bending strength and the fracture toughness of the material obtained are 420 MPa and 4.40 MPa × m^1/2, respectively.     

Fabrication and Properties of SiB6-B4C with Phenolic Resin as a Carbon Source

Si-B-C ceramic composites were synthesized using SiB6, B4C, and phenolic resin as a carbon source by pressureless sintering in an Ar atmosphere. Then, the Si-B-C ceramic composites were fabricated to determine their potential for applications as high hardness and high temperature composites. The X-ray diffraction patterns of sintered bodies of SiB6-B4C with carbonized phenolic resin can be seen that SiB6 and C changed to B4C and SiC. In this study, it is obtained that carbonized phenolic resin is good addition material as a reaction material comparing to carbon powder at 1683 K for 1 h by pressureless sintering in an Ar atmosphere.     

高性能SiC—AlN复相陶瓷

采用热压烧结工艺,通过合理的组成设计和烧结温度控制,制备出了高性能SiC-AlN复相陶瓷,在较佳条件下,复合材料的室温强度、断裂韧性、显微硬度分别高达1130MPa、6．2MPa·m^1/2、28．6GPa．显微结构研究表明,随着AlN的加入,复合材料的晶粒尺寸明显细化,并呈多层次效应,即由固溶体的形成所引起的一次晶粒细化和晶内亚晶界所引起的二次晶粒细化．     

Effects of Cation Impurities on Thermal Conductivity of Yttria-Doped Aluminum Nitride

Effects of cation impurities such as Fe and Si on thermal conductivity of yttria-doped aluminum nitride were investigated. Two types of aluminum nitride powders, Tokuyama F-grade and Denka AP-10, were compared. The powders have similar contents of oxygen but different levels of cation impurities. Since the thermal conductivity of sintered aluminum nitride is virtually affected by the residual oxygen contents in the grains, effects of yttria additions and prolonged firing time are also investigated. The resultant thermal conductivity is thought to be influenced by the sample size of sintering bodies because extracting oxygen from the aluminum nitride lattice in larger samples requires longer time resulting from a longer diffusion path. In comparing the AlN powders, impurity contents of Fe and Si are somewhat higher in Denka powder than Tokuyama powder. These impurity elements degrade the thermal conductivity of sintered aluminum nitride. Degradation effects in thermal conductivity due to presence of Fe and Si are evaluated by artificially introducing these elements to Tokuyama AlN powder. The difference in the thermal conductivity resulting from the two types of powders is discussed.     

Effects of copper addition on the sintering behavior and mechanical properties of powder processed Al/SiC<Subscript><Emphasis Type="Bold">p</Emphasis></Subscript> composites

The effect of copper addition on powder processed Al-10 vol% SiC composites was studied in regards to their sintering responses. Copper was mixed with aluminum powder either as elemental powders or as the coated layer on SiC particles. After sintering at 600°C for 1 h, Al-SiC composites with no copper addition showed little densification. It also demonstrated very low bend strengths of 49 and 60 MPa, indicating poor bonding between the powders in the sintered composite. The addition of 8% copper to the Al/SiC system effectively improved the sintering response, producing over 95% theoretical density, a bend strength of 231 MPa with the copper coated SiC, and a 90% density with over 200 MPa bend strength with the admixed copper.The as-sintered microstructures of the Al–SiC composites clearly revealed particle boundaries and sharp pores, indicating that only a limited neck growth occurred during sintering. In the case of Al–Cu–SiC composites, however, a liquid phase was formed and spread through particle boundaries filling the interfaces or voids between SiC particles and the matrix powders. The coated copper on SiC particles produced a somewhat better filling of the interface or voids, resulting in a little more densification and better sintered strength. Since the solubility of copper in aluminum is less than 2% at the sintering temperature, the alloying of copper in the aluminum matrix was limited. Most of the copper added was dissolved in the liquid phase during the sintering and precipitated as CuAl₂ phase upon cooling.     

Pressureless-sintered and HIPed SiC-TiB2 composites from SiC-TiO2-B4C-C powder compacts

Dense SiC-TiB₂ composites with prescribed compositions were obtained through pressureless sintering of SiC-TiO₂-B₄C-C powder compacts. During the process, TiO₂, B₄C and C reacted to form TiB₂, followed by the consolidation of SiC matrix with the aid of excess B₄C and C. The effects of the composition of the starting powders on the final density were investigated and the mechanical properties of the composite were evaluated. The sintered body with additional HIPing at 1900 °C exhibited the average four-point flexural strength of more than 700 MPa at both 20 and 1400 °C.     

Study of the sintering properties of plasma synthesized ultrafine SiC powders

A study on the sintering of ultrafine SiC powders synthesized from elemental Si and CH₄ using radio frequency (r.f.) induction plasma technology is reported. The powder had a particle size in the range of 40 to 80 nm and was composed of a mixture of α and β-SiC. It was subjected to pressureless sintering in an induction furnace in the presence of different sintering aids. With the addition of B₄C (2.0 wt% B) by mechanical mixing, the powders could only be partially densified, with the highest value of 84.5% of theoretical density being achieved at 2170 °C for 30 min. Through the use of “in-flight” boron doping of the powder during the plasma synthesis step (1.65 wt % B), the ultrafine powder obtained could be densified to above 90% of its theoretical density at 2050 °C for 30 min. The addition of oxide sintering aids (7.0 wt % Al₂O₃ + 3.0 wt % Y₂O₃) by mehanical mixing produced sintered pellets of 95% of theoretical density at 2000 °C for 75 min. The Vicker’s microhardness of the sintered pellets in this case was as high as 31.2 GPa. In order to improve our understanding of the basic phenomena involved, extensive microstructural (scanning electron energy microscopy: SEM), physical (shrinkage, weight loss, porosity, hardness) as well as chemical analysis (prompt gamma neutron activation analysis (PGNAA), energy dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA)) was carried out. This helped establish a relationship between the properties of the as-synthesized powder and their sintering properties. The influences of sintering temperature, sintering time, additive concentration, and powder purity on the densification behaviour of the plasma-synthesized powders was investigated. The results were compared with data obtained using commercial powder. This revised version was published online in November 2006 with corrections to the Cover Date.     

Carbon/ceramics composites — Preparation and properties

Fabrication methods for carbon/ceramics composites were established by using two different processes of hot-pressing and pressureless sintering without any binder phase. In the hot pressing method, some boron compounds were found to be an effective aid for sintering and graphitization of coke powder above 2000°C under some pressure. When the content of boron compound such as B₄C was high, graphite/B₄C composites could be fabricated. If some other ceramic powder such as NbC, TiC or TaC was mixed in addition to the B₄C, three component composites with graphite matrix could be obtained. In pressureless sintering method, raw coke carbon powder was ground for a long time to be transformed in to a sinterable and non-graphitizing-type carbon powder. From a mix of ceramic powders such as SiC or B₄C with the ground coke powder, the composites of carbon/SiC or carbon/SiC/B₄C systems could be fabricated by heat-treatment under normal pressure.Some properties of the graphite samples and carbon/ceramic composites were investigated. It was found that their mechanical properties were much better than those of conventional graphite samples and the resistance to oxidation and corrosion was also excellent. It is suggested that the composites could be applied as bearing or mechanical seals both for use in high temperature environments and as machine parts in contact with some molten metals.     

Chemical reactivities of hafnium and its derived boride, carbide and nitride compounds at relatively mild temperature

MB₂/SiC composites are materials of choice for ultra-high-temperature structural applications, primarily in the aerospace arena. These composites are processed in a hot-press operation at a temperature range of 1900 to 2200°C. This article assesses potential mild-temperature (below 1500°C) chemical reactions that may lead to structures and coatings made of HfB₂/SiC under pressureless or mild-pressure conditions. The reactions are anticipated to be involved in reactive and shape-forming processes, where ceramic precursors and/or reactive powders are incorporated. This article pays special attention to exothermic reactions as well as to formers of a liquid phase; both can aid the desired phase formation, microstructure development, and sintering of the composite under milder conditions than currently practiced. Reactions between loosely mixed powders with melting points significantly above 1500°C were detected by X-ray diffraction (XRD) analyses. Significant solid-phase reactions of the loose powder mixtures were observed at this mild temperature in powder form. Preliminary microstructural studies using scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy-dispersive X-ray Spectroscopy (EDX) techniques have confirmed the presence of unique reaction mechanisms between the loosely connected particles.Good examples are the reactions between Hf powder and powders of BN or B₄C, all having melting points above 2200°C, which form at 1500°C, or below HfB₂/HfN and HfB₂/HfC crystalline domains, respectively. These reactions are less intuitive than the reaction with B₂O₃, which forms HfB₂/HfO₂, potentially via molten or gaseous phases of boron oxide.     

Interfacial reactions between SiC and aluminium during joining

Reactions between SiC and liquid aluminium were studied. Transmission electron microscopy (TEM) showed that aluminium carbide (Al₄C₃) phase was formed at the interface between pressureless sintered SiC and aluminium. In contrast, the Al₄C₃ phase was not detected at the reaction sintered SiC-Al interface. This difference in microstructures results in the change in bending strength of the joints. Mixtures of SiC and aluminium powders were heated to react in vacuum in the temperature range 973 to 1473 K and the reaction products were examined using X-ray powder diffraction. It was confirmed that Al₄C₃ and silicon were formed, and that the extent of reaction between SiC and aluminium was decreased by the addition of silicon into aluminium.     

Densification of ultrafine SiC powders

Recent results on the densification behaviour of ultrafine SiC powders (below 20 nm) are presented and compared with results on the densification of ultrafine silicon-based ceramic powders given in the literature. A study of different powder processing routes and their influence on the pore-size distribution is given. Pressureless sintered green bodies having pore sizes of about 20 nm show extreme coarsening without significant densification. The results indicate a significant influence of green density on shrinkage. Encapsulated hot isostatic pressing (HIPing) led to a reduction of pore size and to considerable density increase at temperatures below 1600 °C. But even then full density without extensive grain growth was difficult to achieve. The applied method to determine grain sizes (X-ray diffraction measurements, XRD, using the Scherrer formula, scanning electron microscopy, SEM, and transmission electron microscopy, TEM) gave similar results for TEM and SEM but lower values for XRD. A possible explanation is presented. Density and grain growth both during pressureless sintering and HIPing showed significant differences between samples with and without sintering additives (B and C). Whether or not the use of sintering agents is favourable in reaching high densities and fine grain sizes, is discussed. HIP densification was modelled assuming diffusion to be the dominant mechanism. Grain growth according to a t ^1/4 dependence and an activation energy of 6.8 eV was introduced into the model. Results on the properties (hardness, also at elevated temperatures, fracture toughness, bending and compression tests, thermal conductivity) of the hot isostatically pressed samples, are presented.     

A Coprecipitation Coating Synthesis of SiC/YAG Composites

The α-SiC in 0.5μm size powders were coated with Al_2O_3 and Y_2O_3 by a coprecipitation coating (CPC) method forfabrication of SiC/YAG composites. The same powder preparation was carried out by conventional mechanical mixing(MM) method for comparison. Two kinds of SiC/YAG composites were manufactured by pressureless sintering usingthe different powders, named CPC composite and MM composite thereafter respectively. It is shown that the CPCcomposite has the advantages of homogeneous distribution of YAG phase and of being sintered to high density ata low temperature, 100℃ lower than that of MM composite. The strength (573 MPa) and hardness (23.3 GPa) ofthe CPC composite are significantly higher than those (323 MPa and 13.5 GPa) of the MM composite, respectively.     

Characterization of cemented Cu matrix composites reinforced with SiC

In this study, some properties of copper produced by cementation method and its composites reinforced with 1wt%, 2wt%, 3wt% and 5wt% SiC particles, produced by powder metallurgy method, were investigated. Composite powders were pressed by applying an uniaxial pressure of 280 MPa and sintered at temperatures of 700 °C for 2 h embedding in graphite powder. Scanning electron microscope (SEM-EDS), X-ray diffraction (XRD) techniques were used to characterize the Cu and SiC which are dominant components in the sintered composites. Microstructure studies revealed that SiC particles were located around the copper particles. The relative densities of Cu-SiC composites determined by Archimedes’ principle decreased from 98.11% to 90.93% with increasing reinforcement components. Measured hardness of sintered compacts varied from 127 to155 HVN. Maximum electrical conductivity of test materials ranged from 80.17% IACS to 57.76% IACS.     

Hot-pressed AlN-Cu metal matrix composites and their thermal properties

AlN-Cu metal matrix composites containing AlN volume fractions between 0.1 and 0.5 were fabricated firstly by liquid phase sintering of AlN using Y₂O₃ as a sintering aid and then by hot pressing the powder mixtures of sintered AlN and Cu at 1050°C with a pressure of 40 MPa under flowing nitrogen. With Y₂O₃ additions of 1.5 to 10 wt%, the densification of AlN could be achieved by liquid phase sintering at 1900°C for 3 h and subsequently slow cooling. The sintered AlN showed a maximum thermal conductivity of 166 W/m/K at a Y₂O₃ level of 6 wt%. Dense AlN-Cu composites with AlN contents up to 40 vol% were achieved by hot pressing. The thermal conductivity and the coefficient of the thermal expansion (CTE) of the composites decreased with increasing AlN volume fractions, giving typical values of 235 W/m/K and 12.6 × 10^–6/K at an AlN content of 40 vol%.     

Sintering of ultrafine SiC powders prepared by plasma CVD

Ultrafine SiC powders with a nanometre particle size were synthesized by r.f. plasma chemical vapour deposition (CVD) using a chemical system of SiH₄−C₂H₄−Ar. The powder was also ultrapure with a grade of 99.999% purity. The product was polytype 3C−SiC and black in colour, in spite of its high purity, because of its ultrafine size. Silicon carbide is a difficult ceramic to sinter; it is possible to sinter it to full density with the aid of sintering additives. Ultrafine and ultrapure SiC powders were hot-pressed without sintering additives in the present study, in order to investigate the sintering behaviour. The CVD powders proved sinterable to 88% theoretical density without sintering additives. The present experiments revealed that powder treatment before firing was a key technology when using ultrafine powders as starting materials in the sintering process. The sintering behaviour of the powder was characterized by a large shrinkage. Phase transformation was negligible after hot pressing at 2200°C for 30 min.     

Preparation of Fe3AI based iron aluminides from elemental and prealloyed povvders

Abstract

Iron aluminides were prepared by a powder metallurgy process from elemental powders, mixtures of prealloyed and elemental powders, and prealloyed powder. The sintering behaviour of various powders was studied using scanning electron microscopy, optical microscopy, and density measurement. It was found that sintering of elemental powder involved two distinct processes, i.e. alloying and densification, but sintering of prealloyed powder involved densification alone. The addition of prealloyed powder to elemental powders was helpful in restraining the swelling of sintered samples, the degree of swelling of sintered samples being reduced as the amount of prealloyed powder increased. For samples made from Fe-25 at.-%Al prealloyed powder, remarkable shrinkage was measured after sintering at 1250°C for 1 h. Within the correct range, their density increased with sintering temperature and time, but prolonged sintering at high temperature resulted in the loss of aluminium and a two phase microstructure. The difference in sintering behaviour between the various powders was discussed on the basis of thermodynamics.     

SEM/EDS分析纳米TiN颗粒在SiC陶瓷中的分布状况

采用水基喷雾造粒技术制备SiC/纳米TiN复合粉体,并借助二步成型和无压烧结技术制备SiC/纳米TiN复合陶瓷,利用场发射扫描电镜结合能谱分析(SEM/EDS)研究了纳米TiN颗粒在SiC/纳米TiN复合粉体、素坯及烧结体过程中的分布状态,借此评价制备工艺。     

Influence of calcination temperature on the properties of spray dried alumina-zirconia composite powders

Alumina-zirconia composite powders containing 10, 12.5, 15 or 20 wt% zirconia were prepared by spray-drying the hydroxide gels. These powders were calcined at 650 and 950 °C. The spray-dried as well as the calcined powders were characterized by means of Coulter counter, Sorptometer, infrared spectroscopy (i.r.), scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and X-ray diffraction (XRD). Initially the spray-dried powders are amorphous and spherical in shape with a diameter of 6 m and crystallize after calcination treatment at 950 °C. Sintered density of the 950 °C calcined powder compacts was higher than 650 °C calcined powder compacts. Compacts made from 650 °C treated powders retained 100% tetragonal phase after sintering irrespective of composition. Some amount of tetragonal phase is transformed into monoclinic phase in the composites containing higher amount of zirconia in the sintered compacts made from 950 °C calcined powders.     

Synthesis of Cu-W nanocomposite by high-energy ball milling

The Cu-W bulk nanocomposites of different compositions were successfully synthesized by high-energy ball milling of elemental powders. The nanocrystalline nature of the Cu-W composite powder is confirmed by X-ray diffraction analysis, transmission electron microscopy, and atomic force microscopy. The Cu-W nanocomposite powder could be sintered at 300-400 degrees C below the sintering temperature of the un-milled Cu-W powders. The Cu-W nanocomposites showed superior densification and hardness than that of un-milled Cu-W composites. The nanocomposites also have three times higher hardness to resistivity ratio in comparison to Oxygen free high conductivity copper.     

Effect of Amount of Carbonyl Iron Powders on the Sintering Microstructure, and Mechanical Properties of Fe-4 Cu Alloy Synthesized Using Metal Injection Molding

An atomized iron powder used in conventional powder metallurgy, mixed with 4 wt.% Cu powders was injection molded with carbonyl iron powder and a sintering aid. The use of atomized iron powder can reduce cost, but decreases packing density and sintering rate. To improve the densification of atomized powders, 20-40 wt.% carbonyl iron powder was added for increasing packing density and promoting sintering. The sintered alloy was characterized by the bulk density, mechanical properties, and scanning electron microscope observations. The results of sintering for the samples added with 30 wt.% carbonyl powder show that the relative bulk density, hardness, tensile strength and elongation are up to 83.87%. HRF 92.2, 315.5 MPa and 4%, respectively. The proportion of carbonyl iron powders and sintering temperature were found to influence the relative bulk density and the mechanical properties of the specimens significantly.