Effects of the TiC and sintering process on the TiC-steel composite

In this paper, the composite of low alloy steel reinforced with TiC particles was prepared by conventional powder metallurgy process. The effects of the combined carbon content of TiC powder, sintering temperature and heating rate on the composite were studied. The results showed that the selected TiC powder has a combined carbon content of 17.91?wt-% and the optimal sintering process is heating from 600 to 1440°C at a rate of 1°C?min^?1 and holding for 1?h at 1440°C. The composite after heat treatment has excellent mechanical properties with density of 6.45?g?cm^?3, hardness of 68–69 HRC and TRS of 1763?MPa, respectively, and will be used as wear-resistant parts, assembly fixtures, moulds, etc.     

Effect of powder reactivity on microwave sintering of alumina

Effect of the reactivity of starting alumina powder of varying crystallinity on the sintering behavior in microwave process was studied. From X-ray amorphous to highly crystalline alumina, powders were obtained by conventional heating of compacts made of the precursor amorphous powder by heating it at different temperatures from 800 to 1500 °C. These samples were then sintered in a multimode microwave field of 2.45 GHz for 10 min at 1500 °C. The microwave effect on densification of the various alumina powders was evaluated by comparing the microwave and conventional sintering data. The results show significant microwave enhancement in the densification of the samples without any pretreatment. This enhancement became less significant as the temperature of the pretreatment increased and finally diminished. Since the pretreatment at elevated temperatures made the powder more stable thermodynamically, this study indicates that the sintering enhancement of a ceramic material in microwave is a metastability-related phenomenon.     

Reactive sintering mechanism of Ti + Mo<Subscript>2</Subscript>C and Ti + VC powder compacts

TiC reinforced Ti-matrix composites have been synthesized successfully by reactive sintering of Ti-1.5%Fe-2.25%Mo (wt%) powder compacts with addition of Mo₂C and VC particles. The reactions for the formation of TiC particles start at 600 °C, but the distribution of TiC particles and the densification behavior in the two compacts are significantly influenced by the metal carbides (Mo₂C or VC). The compact with addition of Mo₂C has a relative density of 98% after sintering at 1300 °C for 1.5 h, but TiC particles are agglomerated in the Ti matrix. The compact with addition of VC has a relative density of about 91% after sintering at 1300 °C for 1.5 h, but TiC particles distribute more homogenously in the Ti matrix. Different TiC particle distribution and densification behaviors are attributed to the reaction rates between Ti and metal carbides and the subsequent diffusion process.     

A new synthesis reaction of Ti3SiC2 from Ti/TiSi2/TiC powder mixtures through pulse discharge sintering (PDS) technique

Ti/TiSi₂/TiC powder mixtures with molar ratios of 1:1:4 (M1) and 1:1:3 (M2) were first employed for the synthesis of Ti₃SiC₂ through pulse discharge sintering (PDS) technique in a temperature range of 1100–1325 °C. It was found that Ti₃SiC₂ phase began to form at the temperature above 1200 °C and its purity did not show obvious dependence on the sintering temperature at 1225–1325 °C. The TiC contents in M2 samples is always lower than that of the M1 samples, and the lowest TiC contents in the M1 and M2 samples were calculated to be about 7 wt% and 5 wt% when the sintering was conducted at the temperature near 1300 °C for 15 minutes. The relative density of the M1 samples is always higher than 99% at sintering temperature above 1225 °C, indicating a good densification effect produced by the PDS technique. A solid-liquid reaction mechanism between Ti-Si liquid phase and TiC particles was proposed to explain the rapid formation of Ti₃SiC₂. Furthermore, it is suggested that Ti/TiSi₂/TiC powder can be regarded as a new mixture to fabricate ternary carbide Ti₃SiC₂. Received: 5 September 2001 / Accepted: 11 September 2001     

Enhanced microwave absorption properties of polymer-derived SiC/SiCN composite ceramics modified by TiC

Porous SiCN(Ti) composite ceramics with good microwave absorbing performance were fabricated by pyrolysis of solid polysilazane modified by tetrabutyl titanate. The introduction of Ti not only acted as active filler to react with free carbon in the matrix to form TiC, but also played the role as catalyst to promote the formation of SiC nanowires. Finally, SiCN(Ti) composite ceramics formed a microstructure containing multi-nanophases and multi-nano heterogeneous interfaces when annealing temperature reached 1500 °C. The complex microstructure annealed at 1500 °C made composite ceramics have good matching impedance, as well as greatly increase the interfacial polarization loss and dipole polarization loss. As a result, the TiC/SiC/SiCN composite ceramics showed the excellent performance of electromagnetic wave absorption in X band. The minimum reflection loss (RL) of samples was ??17.1 dB at the thickness of 1.9 mm, and the maximum effective absorption bandwidth (EAB) of composite ceramics was 3.2 GHz when the thickness of sample was 2.1 mm, which exhibited a promising prospect as a structural and microwave absorbing integration material.

     

Mechanical properties of hydroxyapatite–zirconia compacts sintered by two different sintering methods

Microwave sintering is traditionally employed to reduce the sintering temperature required to densify powder compacts. The effect of microwave heating on hydroxyapatite (HA)–zirconia (ZrO₂) green bodies has been investigated in order to understand how microwave energy may affect the physical and mechanical properties of the resultant densified composites. Laboratory synthesised nano-sized HA and a commercial nano-sized ZrO₂ powder have been ball milled to create mixtures containing 0–5 wt% ZrO₂ loadings. Compacts were microwave sintered at either 700, 1000 or 1200°C with a 1 h hold time. Comparative firings were also performed in a resistive element furnace using the same heating profile in order to assess the differences between conventional and microwave heating on the physical, mechanical and microstructural properties of the composites. Samples sintered at 700°C show little sign of densification with open porosities of approximately 50%. Composites conventionally sintered at 1000°C were between 65 and 75% dense, whereas the samples microwave sintered at this temperature were between 55 and 65% dense. Samples sintered at 1200°C showed the greatest degree of densification (>80%) with a corresponding reduction in open porosities. TCP generation occurred as a consequence of sintering at 1200°C, even with 0 wt% ZrO₂, and increased degradation of the HA phase to form significant amounts of TCP occurred with increasing additions of ZrO₂, along with increasing open porosity. Nanosized ZrO₂ prevents the densification of the HA matrix by effectively pinning grain boundaries and this effect is more pronounced in the MS materials. Similar strengths are achieved between the microwave and conventionally sintered samples. Greater amount of open porosity and pore interconnectivity are seen in the MS samples, which are considered to be useful for biomedical applications as they can promote osteo-integration.     

Low temperature synthesis of Ti3 SiC2 from Ti/SiC/C powders

Abstract

Ternary carbide Ti₃ SiC₂ was first synthesised through a pulse discharge sintering (PDS) technique from mixtures of Ti, SiC, and C with different molar ratios. Sintering processes were conducted at 1200 – 1400°C for 15 – 60 min at a pressure of 50 MPa. The phase constituents and microstructures of the synthesised samples were analysed by X-ray diffraction (XRD) technique and observed by scanning electron microscopy (SEM). The results showed that, for samples sintered from 3Ti/SiC/C powder at 1200 – 1400°C, TiC is always the main phase and only little Ti₃ SiC₂ phase is formed. When the molar ratios Ti : SiC : C were adjusted to 3 : 1.1 : 2 and 5 : 2 : 1, the purity of Ti₃ SiC₂ in the synthesised samples was improved to about 93 wt-%. The optimum sintering temperature for Ti₃ SiC₂ samples was found to be in the range 1250 – 1300°C and all the synthesised samples contain platelike grains. The relative density of Ti₃ SiC₂ samples was measured to be higher than 99% at sintering temperatures above 1300?C. It is suggested that the PDS technique can rapidly synthesise ternary carbide Ti₃ SiC₂ with good densification at lower sintering temperature.     

金刚石表面形成Ti3SiC2的反应机理

采用Ti、Si、TiC、金刚石磨料为原料,通过放电等离子烧结(SPS),制备了Ti3SiC2陶瓷结合剂金刚石材料.研究结果表明,Ti-Si-2TiC试样经SPS加热的过程中位移、位移率和真空度在1200℃时发生明显变化,表明试样发生了物理化学变化.XRD分析结果表明1200℃时试样发生化学反应生成了Ti3SiC2.随着温度升高,试样中Ti3SiC2含量逐渐增加.当烧结温度为1200℃、1300℃、1400℃和1500℃时,产物中Ti3SiC2含量分别为65.9%、79.97%、87.5%和90.1%.在Ti/Si/2TiC粉料中添加适量的金刚石5%和10%进行烧结,并未抑制Ti3SiC2的反应合成.SEM观察表明,金刚石与基体结合紧密,同时其表面生长着发育良好的Ti3SiC2板条状晶粒.提出了一种金刚石表面形成Ti3SiC2的机制,即金刚石表面的碳原子首先与周围的Ti反应生成TiC,然后TiC再与Ti-Si相发生化学反应,生成Ti3SiC2.     

Sintern von TiO2 im Mikrowellenfeld

Sintering of Titania under Microwave-Conditions A microwave sintering device was implemented at the Technical Institute of the Friedrich-Schiller-Universität Jena equipped with an applicator combining conventional high frequency with microwave heating. Additionally a dilatometer was integrated to measure shrinkage or expansion respectively. The device allows a reliable comparison of the materials behaviour treated under conventional and microwave conditions. Titania was used to prove that coupling and sinter behaviour can be assessed reproducible via measuring temperature and shrinkage. Titania samples with a green density of about 60% of theoretical density accept efficiently microwave energy above 940°C, heating rates of more than 300 K/min were measured. At 1360°C final densities of 98% TD were achieved within 40 minutes. Compared to conventional sintered titania (1400°C, 3 hours) microwave heating resulted in a significant smaller grain size.     

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.     

Effect of sintering temperature and heating mode on consolidation of Al–7Zn–2·5Mg–1Cu aluminum alloy

Densification behaviour, phase transformation, microstructural evolution and hardness values of microwave sintered Al?C7Zn?C2·5Mg?C1Cu (7775) aluminum alloy were investigated and compared with conventionally sintered samples. Microwave sintering was performed in 2·45?GHz multimode microwave furnace at temperatures ranging from 570?C630 °C. Microwave sintering at a heating rate of as high as 22°C/min resulted in ~55% reduction of processing time as compared to conventional sintering. A lower sintered density observed in the case of microwave processed samples was attributed to the inhomogeneity in microstructure and phase distribution. The X-ray diffraction results of conventionally sintered samples showed the presence of MgZn₂, Mg₂Zn₁₁ and CuMgAl₂, while only MgZn₂ and CuMgAl₂ phases were found in the case of microwave sintered samples and in lesser amount. Higher hardness and high standard deviation values were noticed for microwave sintered samples as compared to conventional counterparts.     

微波烧结Al2O3/SiC纳米复合陶瓷的研究

以分析纯Al(NO3)3.9H2O·NH3.H2O和50 nm的SiC粉体为原料,采用溶胶-凝胶法制备干凝胶,经热处理合成Al2O3/SiC纳米复合粉体。利用微波烧结制备Al2O3/SiC纳米复合陶瓷,并与常规烧结比较,分析了两种烧结方法对制备试样的力学性能影响。结果表明,与常规烧结相比,微波烧结可以提高Al2O3/SiC纳米复合陶瓷的强度和韧性,改善材料的显微结构,促进致密化和晶粒生长。     

A developed method for producing in situ TiC/Al composites by using quick preheating treatment and ultrasonic vibration

Quick preheating treatment of Al–Ti–C was introduced in the fabrication of in situ TiC/Al metal matrix composites in our research. Al–Ti–C pellets were preheated in the furnace at 750 °C, in which the pure aluminum was melted. After adding the preheated pellets into the molten aluminum, the thermal explosion reaction of Al–Ti–C took place in a short time. In situ TiC particles synthesized in the pure molten aluminum were spherical in morphology and most of which were smaller than 1 μm in size. The synthesizing temperature of in situ TiC/Al composites was decreased significantly by using the quick preheating treatment, at least 150 °C lower than those used in the conventional methods. In addition, high-intensity ultrasonic vibration was applied into the melt to disperse TiC particle-reinforcement into the matrix and degas the melt as well. In situ TiC particles were distributed uniformly in the matrix, and the porosity in the composites was below 1% due to the effect of ultrasonic vibration. Furthermore, the microhardness test indicated that a homogeneous microstructure of in situ TiC/Al composite was obtained.     

Processing and Characterization of In Situ (TiC–TiB2)p/AZ91D Magnesium Matrix Composites

In this paper, a practical and cost‐effective processing route, in situ reactive infiltration technique, was utilized to fabricate magnesium matrix composites reinforced with a network of TiC–TiB₂ particulates. These ceramic reinforcement phases were synthesized in situ from Ti and B₄C powders without any addition of a third metal powder such as Al. The molten Mg alloy infiltrates the preform of (Ti_p + B₄C_p) by capillary forces. The microstructure of the composites was investigated using scanning electron microscope (SEM)/energy dispersive X‐ray spectroscopy (EDS). The compression behavior of the composites processed at different conditions was investigated. Also, the flexural strength behavior was assessed through the four‐point‐bending test at room temperature. Microstructural characterization of the (TiB₂–TiC)/AZ91D composite processed at 900 °C for 1.5 h shows a relatively uniform distribution of TiB₂ and TiC particulates in the matrix material resulting in the highest compressive strength and Young's modulus. Compared with those of the unreinforced AZ91D Mg alloy, the elastic modulus, flexural and compressive strengths of the composite are greatly improved. In contrast, the ductility is lower than that of the unreinforced AZ91D Mg alloy. However, this lower ductility was improved by the addition of MgH₂ powder in the preform. Secondary scanning electron microscopy was used to investigate the fracture surfaces after the flexural strength test. The composites show signs of mixed fracture; cleavage regions and some dimpling. In addition, microcracks observed in the matrix show that the failure might have initiated in the matrix rather than from the reinforcing particulates.     

Changes in γ-TiC stoichiometry during heat treatment of TiC reinforced Ti composites

Abstract

A liquid phase technique (casting) has been successfully employed for the production of Ti/TiC in situ metal matrix composites. The γ-TiC phase produced by this process is highly substoichiometric. Changes in chemistry of the TiC phase in these composites are noted during annealing at elevated temperatures. The degree of stoichiometry of TiC increases during annealing at 1050°C and further during post-annealing aging at 750°C. This increase in the degree of stoichiometry (C/Ti atomic ratio) is accompanied by lattice expansion and reduction in microhardness values of the TiC particles. The change in TiC stoichiometry is accompanied by the precipitation of soft Ti particles within the TiC phase. The results are compared with those obtained from composites fabricated by a powder metallurgy route where the carbide chemistry is insensitive to heat treatment.     

Microwave synthesis and sintering characteristics of CaCu<Subscript>3</Subscript>Ti<Subscript>4</Subscript>O<Subscript>12</Subscript>

CaCu₃Ti₄O₁₂ (CCTO) was synthesized and sintered by microwave processing at 2·45 GHz, 1·1 kW. The optimum calcination temperature using microwave heating was determined to be 950°C for 20 min to obtain cubic CCTO powders. The microwave processed powders were sintered to 94% density at 1000°C/60 min. The microstructural studies carried out on these ceramics revealed the grain size to be in the range 1–7 μm. The dielectric constants for the microwave sintered (1000°C/60 min) ceramics were found to vary from 11000–7700 in the 100 Hz–00 kHz frequency range. Interestingly the dielectric loss had lower values than those sintered by conventional sintering routes and decreases with increase in frequency.     

Effect of heating mode and temperature on sintering of YAG dispersed 434L ferritic stainless steel

This study examines the effect of heating mode, sintering temperature, and varying yttria alumina garnet (YAG) addition (5 and 10 wt%) on the densification and properties of ferritic (434L) stainless steel. The straight 434L stainless steel and 434L–YAG composites were sintered in a conventional and a 2.45 GHz microwave furnace. The composites were sintered to solid-state as well as supersolidus sintering temperature at 1200 and 1400 °C, respectively. Both 434L and 434L–YAG compacts coupled with microwaves and underwent rapid heating (∼45 °C/min). This resulted in about 85% reduction in the processing time. For all compositions microwave sintering results in greater densification. As compared to conventional sintering, microwave sintered compacts exhibit a more refined microstructure, thereby, resulting in higher bulk hardness. The mechanical properties and sliding wear resistance of 434L stainless steel is shown to be sensitive both to the sintering condition as well as YAG addition and has been correlated to the effect of heating mode on the pore morphology.     

微波烧结制备MAX-cBN复合材料及其反应机理研究

采用Ti3SiC2与Ti3AlC2粉体和cBN粉体为原料,通过微波烧结制备Ti3SiC2与Ti3AlC2结合剂cBN复合材料,同时研究cBN的含量对该复合材料的物相组成与显微形貌的影响。结果表明,Ti3SiC2-cBN试样烧结后得到了SiC、TiSi2、TiC、TiO、TiO2、SiO2。cBN添加量为10%的复合材料中Ti3SiC2分解较为严重。试样烧结后基体组织比较细小,只有几微米。当原料中cBN含量为20%时,cBN表面会形成凹凸不平的组织。Ti3AlC2-cBN试样烧结后得到了Ti2AlC、TiC、Ti、Al、Al2O3,Ti3AlC2材料分解完全。cBN含量较高时,它可以与Ti3AlC2或其分解产物充分反应,形成相应的氮化物或碳氮化物。     

Preparation of NixTiy compound via Ni plating followed by thermal treatment of Ti powder

In this research, Ni_xTi_y compound was prepared by thermal treatment of Ni-plated Ti powder. For this purpose, Ti powder was plated in an electroless Ni bath for various times (120, 225, 300, and 720?min). Hydrazine hydrate was used as a reductant for the deposition of pure Ni on the Ti particles. The plated powder (225?min) was heat treated under argon atmosphere to achieve Ni_xTi_y powder. Finally, the heated/plated powder was pressed by CIP followed by sintering at 980°C for prepare the Ni_xTi_y bulk sample. The plated powders as well as sintered one were characterized using scanning electron microscopy, energy dispersive spectrometer, X-ray fluorescence, X-ray diffraction and differential scanning calorimetric. The NiTi₂, NiTi, and Ni₃Ti phases were detected in the XRD patterns of heated/plated Ti powder. According to DSC data, the heated/plated Ti powder showed reversible martensitic transformation at temperature range of ?38.0°C to +38.1°C, while sintered/heated/plated Ti powder displayed reversible transformation at temperature range of 16.0°C–15.4°C.     

Microwave hybrid synthesis of silicon carbide nanopowders

Nanosized silicon carbide powders were synthesised from a mixture of silica gel and carbon through both the conventional and microwave heating methods. Reaction kinetics of SiC formation were found to exhibit notable differences for the samples heated in microwave field and furnace. In the conventional method SiC nanopowders can be synthesised after 105 min heating at 1500 °C in a coke-bed using an electrical tube furnace. Electron microscopy studies of these powders showed the existence of equiaxed SiC nanopowders with an average particle size of 8.2 nm. In the microwave heating process, SiC powders formed after 60 min; the powder consisted of a mixture of SiC nanopowders (with two average particle sizes of 13.6 and 58.2 nm) and particles in the shape of long strands (with an average diameter of 330 nm).