A new synthesis reaction of Ti3SiC2 through pulse discharge sintering Ti/SiC/TiC powder

Ti₃SiC₂ was synthesized by pulse discharge sintering 4Ti/2SiC/TiC mixture powder in a temperature range of 1250–1450 °C. The purity of Ti₃SiC₂ was improved to 92 vol% at a sintering temperature of 1350 °C. The microstructure in the synthesized samples was controlled to be fine, coarse and duplex grains, depending on the sintering temperature and time.     

Growth kinetics and oxidation behavior of WSi2 coating formed by chemical vapor deposition of Si on W substrate

The growth kinetics of WSi₂ coating formed by chemical vapor deposition (CVD) of Si on a W substrate at temperatures between 1000 and 1200 °C using SiCl₄–H₂ gas mixtures was investigated and its isothermal oxidation resistance in 80% Ar–20% O₂ atmosphere was evaluated at temperatures between 800 and 1300 °C. WSi₂ coating grew with a parabolic rate law after an initial incubation period, indicating the diffusion-controlled growth. The activation energy for growth of WSi₂ coating was about 42.5 kcal/mol. The isothermal oxidation rate of WSi₂ coating increased with increasing oxidation temperature but rapidly decreased at 1300 °C. The oxidation product of WSi₂ coating was composed of the WO₃ particles embedded in the amorphous SiO₂ matrix at below 1200 °C but consisted of only SiO₂ phase at 1300 °C. The fast oxidation behavior of WSi₂ coating at below 1200 °C was attributed to the formation of many cracks and pores, i.e. short-circuit diffusion path of oxygen, within the oxide scale, which resulted from the internal stress generated both by the large volume expansion caused by the oxidation reactions of WSi₂ and by the evaporation of WO₃ phase. The slow oxidation behavior of WSi₂ coating at 1300 °C was due to the exclusive formation of a slow-growing continuous SiO₂ scale by the rapid evaporation of WO₃ phase.     

Effects of TiC addition on formation of Ti3SiC2 by self-propagating high-temperature synthesis

Formation of Ti₃SiC₂ was conducted by self-propagating high-temperature synthesis (SHS) from both the elemental powder compacts of Ti:Si:C = 3:1:2 and the TiC-containing samples compressed from powder mixtures of Ti/Si/C/TiC with TiC content ranging from 4.3 to 33.3 mol%. The effect of TiC addition was studied on combustion characteristics and the degree of phase conversion. For the elemental powder compacts, with the progress of combustion wave the sample experiences substantial deformation, including axial elongation and radial contraction. The extent of sample deformation and flame-front propagation velocity were considerably reduced for the samples with TiC addition, because the dilution effect of TiC lowered the reaction temperature. Two reaction mechanisms were adopted to explain the formation of Ti₃SiC₂, one involving the reaction of a Ti–Si liquid phase with solid reactants for the elemental powder compact and the other dominated by the interaction of solid-phase species for the TiC-containing sample. For all products synthesized in this study, the XRD analysis identifies formation of Ti₃SiC₂ along with a major impurity TiC and a small amount of Ti₅Si₃. The resulting Ti₃SiC₂ is typically elongated grains. Based upon the XRD profile, the Ti₃SiC₂ content at a level of 71.5 vol.% was obtained in the product from the elemental powder compact. With the addition of TiC, an improvement in the yield of Ti₃SiC₂ was observed and an optimal conversion reaching 85 vol.% was achieved by the sample with 20 mol% of TiC. However, further increase of the TiC amount led to a decrease in the Ti₃SiC₂ content, because of the low reaction temperature around 1150 °C.     

Reactions between Ti and Ti3SiC2 in temperature range of 1273-1573 K

The reactions of Ti₃SiC₂ and Ti in the temperature range of 1 273–1 573 K under a pressure of 20 MPa were investigated. The results confirm that Ti reacts with Ti₃SiC₂ above 1 273 K and new phases like TiC_x, Ti₅Si₃ and TiSi₂ are identified. The reactions are closely related to temperature and content of Ti₃SiC₂ in Ti. During the reaction process, Ti₃SiC₂ decomposes in two different modes. The first is caused by the de-intercalation of Si from it and the TiC_x is formed by the remained titanium and carbon; the second is that the carbon is separated from the Ti₃SiC₂ and reacts with titanium furthermore. The diffusing of silicon is believed to be the determinant ingredient of the reaction.     

Solid state reactions in highly dispersed praseodymium oxide–SiO2 system

This paper reports results of studies on the interaction of praseodymium oxide nanocrystals with an amorphous silica. Nano-sized (3–4 nm) amorphous precursor of praseodymium oxide synthesized using a microemulsion technique were supported onto a high surface SiO₂ or occluded into SiO₂ matrix. Solid state reactions occurring in these binary systems upon heat treatment in air, argon or hydrogen at 800–1100 °C were studied by TEM, XRD, FT-IR and UV–vis spectroscopy. It has been found that morphology of the sample as well as annealing atmosphere influence greatly the phase evolution. At temperatures above 900 °C, nanocrystalline praseodymium silicates of various morphology and crystal structure were obtained. In particular, a new polymorph of Pr₂Si₂O₇, isostructural with I-type Ln₂Si₂O₇ (Ln₆[Si₄O₁₃][SiO₄]₂) Ln = Ce, La, has been identified.     

Ti3 SiC2 复合材料耐磨性能研究

Ti₃SiC₂是一种六方晶体结构的特殊陶瓷材料,兼具金属与陶瓷的优异性能,拥有优良的高温强度、抗氧化性及可加工性等优点,广泛应用于耐磨润滑材料。本文综述其同金属和SiC、金刚石、TiC、Al₂O₃等复合后的优异性能和广阔应用,并展望其在和金属、陶瓷、金刚石等材料复合领域的研究方向。      

Synthesis of iron（Ⅲ）-doped nanostructure TiO2/SiO2 and their photocatalytic activity

Iron(Ⅲ)-doped nanostructure TiO2-coated SiO2 (TiO2/SiO2) particles were prepared using the layer-by-layer assembly technique and their photocatalytic property was studied. TiO2 colloids were synthesized employing the sol-gel method with TiCl4 as a precursor. The samples were characterized by Fourier transform infrared spectroscopy (FTIR), SEM, EDS, XPS, and XRD. The experimental results show that TiO2 nanopowders on the surface of SiO2 particles are well distributed, the amount of TiO2 is increased with the adding of coating layers, the pure anatase-TiO2 coating layers are synthesized at 500℃, and the photocatalytic activity of Fe3 -doped TiO/SiO2 is higher than tnat of undoped TiO2/SiO2.     

Synthesis and characterization of 0.3 Vf TiC–Ti3SiC2 and 0.3 Vf SiC–Ti3SiC2 composites

In this work, two composite compositions—one with 30% (v/v) SiC, the other with 30% (v/v) TiC, balance Ti₃SiC₂—were synthesized and characterized. Fully dense samples were fabricated by hot isostatically pressing Ti, SiC and C powders for 8 h at 1500 or 1600 °C and a pressure of 200 MPa. Both TiC and SiC lower grain boundary mobility in Ti₃SiC₂. Coarsening of the SiC particles was also observed. At comparable grain sizes, all composites tested were weaker in flexure than the unreinforced Ti₃SiC₂ matrix, with the reduction in strength being the worst for the SiC composites. This reduction in strength is most probably due to thermal expansion mismatches between the matrix and reinforcement phases. The composite samples were exceptionally damage tolerant; in one case a 100 N Vickers indentation (in a 1.5-mm thick bar) did not reduce the flexural strength as compared to an unindented or as-fabricated samples. The same is true for thermal shock resistance; quenching samples from 1400 °C in room temperature water, resulted in strength reductions that were 12% at best and 50% at worst. In the 25–1000 °C temperature range, the thermal expansion coefficients of the two composites were indistinguishable at 8.2×10⁻⁶ K⁻¹. The Vickers hardness values depended on load; at 100 N, the hardnesses were ≈15 GPa; at 300 N, they asymptote to 7–8 GPa. For the most part, very few cracks emanate from the corners of the Vickers indents even at loads as high as 500 N. In the few cases where cracks did initiate, fracture toughness values were crudely estimated to lie in the 5–7.5 MPa √m range.     

TC4合金表面扩散渗硅涂层的高温氧化行为和失效机制

为提高钛合金的高温抗氧化性能,采用固体粉末扩散渗方法在其表面制备了扩散渗硅涂层,研究了涂层的组织结构、高温氧化行为和失效机制。结果表明,所制备涂层具有致密的多层梯度组织结构,主要由TiSi₂外层,TiSi中间层和Ti₅Si₄+Ti₅Si₃内层组成。高温氧化实验结果表明,涂层在850℃空气中氧化时表面形成了由SiO₂和TiO₂混合组成的保护膜,高温抗氧化性能优良;氧化过程中,涂层与基体合金中Si和Ti的互扩散引起氧化膜内TiO₂含量增加及Si源不足,导致氧化膜保护性变差;氧化产物与涂层之间较高的P-B比、氧化膜与涂层组织间热膨胀系数不匹配导致了氧化膜开裂和剥落。     

High temperature oxidation of an oxide-dispersion strengthened NiAl

The oxidation behavior of an oxide-dispersion strengthened (ODS) NiAl has been studied between 900 and 1100°C in air. The dispersoids of mostly Al₂O₃ in fine-grained β-NiAl were incorporated by mechanical alloying (MA) in an argon atmosphere and hot pressing. It was found that excessive amounts of dispersoids and voids within the matrix had serious negative effects on the oxidation resistance of β-NiAl, by allowing for a more rapid formation of oxide scales and by providing fast diffusion paths for oxygen. Below the thin surface oxide scales consisted of -Al₂O₃, NiAl₂O₄ and Ni₂O₃, an internal oxidation zone was formed deep into the matrix. No metastable transient aluminas were formed during oxidation. The oxide ridge structure began to evolve after oxidation at 1100°C at the oxide–gas interface.     

Low temperature oxidation of Cr-alloyed MoSi2

Cr-alloyed MoSi2 was compared with monolithic MoSi2 with respect to oxidation at 450℃ for 456 h. Phases formed on Cr-alloygd MoSi2 after exposure are Cr2（MoO4）3, MOO3, and cristobalite （SiO2） according to X-ray diffraction results. Monolithic MoSi2 forms MoO3 and mainly amorphous SiO2. X-ray photoelectron spectroscopy indicates that the main oxidation product on the outermost surface is SiO2 for all studied samples. The samples form a relatively loose oxide but the oxide adherence improves with increasing Cr content. It is indicated that Cr addition can benefit pesting control in MoSi2.     

Preparation and luminescent properties of europium-activated YInGe2O7 phosphors

Effects of precursor milling on phase evolution and morphology of mullite (3Al₂O₃·2SiO₂) processed by solid-state reaction have been investigated. Alumina and silica powders were used as starting materials and milling was taken place in a medium energy conventional ball mill and a high-energy planetary ball mill. Milling in a conventional ball mill although decreases mullite formation temperature by 200 °C, but does not considerably change mullite phase morphology. Use of a planetary ball mill after 40 h of milling showed to be much more effective in activating the oxide precursors, and mullitization temperature was reduced to below 900 °C. Whisker like mullite was formed after sintering at 1450 °C for 2 h and volume fraction of this structure was increased by increasing the milling time. XRD results showed that samples mechanically activated for 20 h in the planetary ball mill were fully transformed to mullite after sintering at 1450 °C, whereas Al₂O₃ and SiO₂ phases were still detected in the samples milled in the conventional ball mill for 20 h and then sintered at the same conditions.     

Microstructural evolution of some MgO–TiO2 and MgO–Al2O3 powder mixtures during high-energy ball milling and post-annealing studied by X-ray diffraction

High-energy dry ball-mill and post-anneal processing were applied to synthesize MgTiO₃ and Mg₂TiO₄ single crystalline phases from the predetermined compositions of MgO–TiO₂ powder mixtures. Also, the experiments were performed to show that it is possible to prepare MgAl₂O₄ single crystalline phase from the predetermined composition of MgO–Al₂O₃ powder mixture only by employing high-energy dry ball milling, i.e. without post-annealing the milled samples. In contrast, fully developed single crystalline powders of MgTiO₃ and Mg₂TiO₄ were obtained after post-annealing the milled samples for 1 h at 900 and 1200 °C, respectively.     

Sm0.5Sr0.5CoO3 cathode material from glycine-nitrate process: Formation, characterization, and application in LaGaO3-based solid oxide fuel cells

Cathode material Sm_0.5Sr_0.5CoO₃ (SSC) with perovskite structure for intermediate temperature solid oxide fuel cell was synthesized using glycine-nitrate process (GNP). The phase evolution and the properties of Sm_0.5Sr_0.5CoO₃ were investigated. The single cell performance was also tested using La_0.9Sr_0.1Ga_0.8Mg_0.2O_3−δ (LSGM) as electrolyte and SSC as cathode. The results show that the formation of perovskite phase from synthesized precursor obtained by GNP begins at a calcining temperature of 600 °C. The single perovskite phase is formed completely after sintering at a temperature of 1000 °C. The phase formation temperature for SSC with complete single perovskite phase is from 1000 to 1100 °C. The SrSm₂O₄ phase appeared in the sample sintered at 1200 °C. It is also found that the sample sintered at 1200 °C has a higher conductivity. The electrical conductivity of sample is higher than 1000 S/cm at all temperature examined from 250 to 850 °C, and the highest conductivity reaches 2514 S/cm at 250 °C. The thermal expansion coefficient of sample SSC is 22.8 × 10⁻⁶ K⁻¹ from 30 to 1000 °C in air. The maximum output power density of LSGM electrolyte single cell attains 222 and 293 mW/cm² at 800 and 850 °C, respectively.     

Preparation of neodymium sulphides by the reaction of Nd2(So4)3 with carbon disulphide

The reaction to synthetize neodymium sulphides from neodymium sulphate octahydrate in a stream of carbon disulphide gas was studied. The dehydration of the octahydrate in vacuum was finished at 300 °C. At 1050–1100 °C in air neodymium oxysulphide, Nd₂O₂SO₄, was formed. Neodymium oxysulphide, Nd₂O₂S, was formed upon heating with a reducing agent such as annealed carbon. The reaction of neodymium sulphate with carbon disulphide commenced at 500–600 °C, resulting in formation of the disulphide, NdS₂. The crystal structure of NdS₂ heated at 500 °C was, however, different from that of the sample heated at 600 °C. In the temperature range 800–900 °C -Nd₂S₃ was obtained as a single phase after heating for at least 3 h in high flow rates of gas mixtures of nitrogen and high concentrations of carbon disulphide. The sesquisulphide, γ-Nd₂S₃ (or Nd₃S₄), was formed at temperatures as high as 1100 °C. The reaction conditions for the compounds mentioned above are discussed together with the analysis of their crystal structures by X-ray powder diffractometry.     

Deformation behaviour and oxidation resistance of single-phase and two-phase L21-ordered Fe–Al–Ti alloys

Single-phase Fe–Al–Ti alloys with the Heusler-type L2₁ structure and two-phase L2₁ Fe–Al–Ti alloys with MgZn₂-type Laves phase or Mn₂₃Th₆-type τ₂ phase precipitates were studied with respect to hardness at room temperature, compressive 0.2% yield stress at 20–1100 °C, brittle-to-ductile transition temperature (BDTT), creep resistance at 800 and 1000 °C and oxidation resistance at 20–1000 °C. At high temperatures the L2₁ Fe–Al–Ti alloys show considerable strength and creep resistance which are superior to other iron aluminide alloys. Alloys with not too high Ti and Al contents exhibit a yield stress anomaly with a maximum at temperatures as high as 750 °C. BDTT ranges between 675 and 900 °C. Oxidation at 900 °C is controlled by parabolic scale growth.     

Phase evolution in ultra-fine TiC0.7N0.3-based cermet during sintering

Ultra-fine TiC_0.7N_0.3-based cermet is prepared and the phase evolution and microstructure are studied by XRD and SEM. The results show that in ultra-fine cermet, solid state reactions take place more readily than in common cermets at 900 °C; liquid phase forms at about 1230 °C in ultra-fine cermets, which is at a lower temperature than what has been reported; denitridation occurs during sintering of both cermets in vacuum, and they had better be sintered in N₂ to preserve the C/N atomic ratio of TiC_0.7N_0.3.     

Study on phase formation and sintering kinetics of BaTi0.6Zr0.4O3 powder synthesized through modified chemical route

BaTi_0.6Zr_0.4O₃ powder was prepared from barium oxalate hydrate, zirconium oxy-hydroxide and titanium dioxide precursors. Barium oxalate hydrate and zirconium oxy-hydroxide were precipitated from nitrate solution onto the surface of suspended TiO₂. Phase formation behaviour of the materials was extensively studied using XRD. BaTiO₃ (BT) and BaZrO₃ (BZ) start forming separately in the system upon calcinations in the temperature range 600–700 °C. BT–BZ solid solution then forms by diffusion of BT into BZ from 1050 °C onwards. The precursor completely transforms into BaTi_0.6Zr_0.4O₃ (BTZ) at 1200 °C for 2 h calcination. The activation energy (AE) of BT (134 kJ mol⁻¹) formation was found to be less than that of BZ (167.5 kJ mol⁻¹) formation. BTZ formation requires 503.6 kJ mol⁻¹ of energy. The sintering kinetics of the powder was studied using thermal analyzer. The mean activation energy for sintering was found to be 550 kJ mol⁻¹.     

NiCrAlY/Al-Al2O3/Ti2AlNb高温抗氧化和力学性能研究

采用电弧离子镀技水在NiCrAlY涂层与O相Ti₂AlNb合金之间沉积不同Al:Al₂O₃比例的Al-Al₂O₃薄膜作为扩散阻挡层.研究了900℃下恒温氧化500 h后NiCrAlY/Al-Al₂O₃/Ti₂AlNb体系中Al-Al₂O₃层阻挡合金元素互扩散的行为,以及对涂层氧化动力学曲线的影响.结果表明,没有添加扩散阻挡层的NiCrAlY/Ti₂AlNb体系,涂层和基体之间的元素互扩散十分严重,涂层丧失抗氧化能力;而添加扩散阻挡层的材料体系,涂层和基体之间的元素互扩散受到抑制,涂层的长期抗高温氧化性能得到提高.对于3Al-Al₂O₃,1Al-Al₂O₃和0Al-Al₂O₃ 3种扩散阻挡层,综合比较材料体系的抗氧化性能、阻挡层阻挡涂层和基体元素互扩散能力、以及涂层和基体之间结合力,当1Al-Al₂O₃薄膜作为扩散阻挡层时,材料性能最优异.同时,本文利用扩散阻挡系数简洁定量地表示出不同Al:Al₂O₃比例阻挡层的阻挡扩散能力.     

ZrO2–SiO2 gradient multilayer oxidation protective coating for SiC coated carbon/carbon composites

In order to eliminate the mismatch of thermal expansion coefficient between the ZrO₂ outer layer and the internal bonding SiC layer, ZrO₂–SiO₂ composition-gradient transition layers were prepared by a sol–gel technique using tetraethoxysilane (TEOS) and zirconyl chloride as source materials. Energy dispersive spectroscopy (EDS) analysis displays that the gradient composition ZrO₂–SiO₂ outer coating could be obtained by immersing the SiC precoated carbon/carbon (C/C) composites into the gradient composition zirconia-silica sols (ZS sol) in turn. Oxidation test shows that, after 10 h oxidation in air at 1773 K, the weight loss of the gradient ZrO₂–SiO₂ coating coated SiC-C/C is only 1.97%.