Si_3N_4/Fe,Si_3N_4/Fe_3Al界面的固相反应(英文)

用扫描电子显微镜、电子能谱仪、X射线衍射等研究了在Ar气氛中,经1150℃,10h等温热处理后,Si3N4/Fe,Si3N4/Fe3Al平而偶界面固相反应区的形貌、成分分布、显微结构及相组成.结果表明:Si3N4/Fe界面固相反应形成约120μn厚的反应区,Fe含量从Si3N4侧到Fe侧逐渐增加,反应区中的Si成分约为5%(原子分数),反应区主要由Fe(Si)固溶体构成,其中均匀地分御着细小的孔洞:Si3NdFe3Al界面固相反应形成约3μm厚的反应区,反应区具有比Fe3Al高得多的Al含量,反应区由FeAl,Fc(Al,Si)固溶体及三元化合物AlgFeSi3构成.Si3NdFe3Al具有比Si3N4/Fe高得多的 界面化学相容性.     

电泳沉积-烧结两步法制备C/SiC复合材料

采用电泳沉积法在石墨基体上制备厚度可控的Si涂层,考察了电泳沉积参数(电压、沉积时间、固含量及添加剂量)对涂层沉积量的影响。所制备的Si涂层通过烧结与石墨基体发生在位反应形成SiC涂层。涂层成分的XRD分析表明烧结后生成β-SiC。用SEM观察涂层烧结前后的形貌,烧结后Si渗入基体内部。孔径分布数据表明所形成的SiC涂层导致石墨孔径变小。1200℃的抗氧化实验表明涂层起到了良好的防护作用。实验提供了一种制备C/SiC复合材料的新方法。     

铜构件磁控溅射多层膜及其耐蚀性

先在铜基体上电镀Ni层,接着溅射沉积Ni–Cr和Ni–Cr–Al–Si合金薄膜.对比了Ni层、Ni/Ni–Cr复合膜层和Ni/Ni–Cr/Ni–Cr–Al–Si复合膜层的相结构、微观形貌和耐蚀性.结果表明,Ni电镀层表面光滑,Ni/Ni–Cr复合膜层和Ni/Ni–Cr/Ni–Cr–Al–Si复合膜层表面都由致密、连续的...     

SiCp/Al复合材料的自发熔渗机理

以Mg为助渗剂,采用液态铝自发熔渗经氧化处理的SiC粉体压坯的方法,制备出高增强体含量的SiCp/Al复合材料.通过考察铝液在SiC粉体压坯中的渗入高度与温度、时间的关系来研究铝液的熔渗机理,并对SiCp/Al复合材料进行X射线衍射、能量散射谱和金相分析.结果表明:在熔渗前沿发生的液-固界面化学反应促进两相润湿,毛细管力导致铝液自发渗入到SiC多孔陶瓷中;熔渗高度与时间呈抛物线关系.熔渗激活能为166 kJ/mol,这表明渗透过程受界面反应控制.经氧化处理的SiC粉体均匀地分布在金属基体中,其轮廓清晰.在SiCp/Al复合材料中未发现Al4C3的存在.     

热压合成Ti3Si0.9Al0.3C1.95固溶体材料

以单质的Ti,Si,Al粉和石墨粉为原料,用热压烧结法原位合成了单一相的Ti3Si0.9Al0.3C1.95层间固溶体材料.研究了合成温度和原料配比对合成产物相组成的影响,并对Ti3Si0.9Al0.3C1.95晶粒的超结构现象及其转变进行了讨论.结果表明:合成单一相Ti3Si0.9Al0.3C1.95固溶体的最佳原料摩尔配比为该相理论配比,相应的最佳热压烧结温度为1 600℃.Ti3Si0.9Al0.3C1.95晶粒具有与Ti3SiC2类似的板状晶外形,但各个晶面的X射线衍射(X-raydiffraction,XRD)峰的2θ与Ti3SiC2相比向小角度方向偏移.块体材料中Ti3Si0.9Al0.3C1.95晶粒的Si(Al)原子层存在原子无序排列的超结构现象,其XRD谱中没有或只有微弱的(OOI)晶面的衍射峰存在,但取自于同一块材料的粉末,其晶粒的Si(Al)原子层发生有序化转变,超结构现象消失.     

碳纤维增强Si-C-N陶瓷基复合材料的氧化行为

采用化学气相浸渗(chemical vapor infiltration,CVI)法制备了以热解碳为界面的碳纤维增强碳氮化硅陶瓷基(carbon fiber reinforced siliconcarbonitride ceramic,C/Si-C-N)复合材料.用热重法研究了无涂层C/Si-C-N在空气环境中的氧化行为.研究表明:由950℃ CVI沉积的Si-C-N基体所制备的C/Si-C-N复合材料的氧化行为与碳纤维增强SiC陶瓷基(carbon fiber reinforced silicon carbide ceramic,C/SiC)复合材料的完全不同.在600～1 200℃,C/Si-C-N的氧化速率随温度的升高而持续增加,其抗氧化能力在600℃明显高于C/SiC复合材料;在900℃,抗氧化能力与C/SiC复合材料基本相当;在1 200℃,抗氧化能力则低于C/SiC复合材料.C/Si-C-N复合材料所表现出来的氧化行为主要与Si-C-N基体较低的热膨胀系数有关.     

Fe2O3对天然原料合成Al4SiC4/Al4O4C复合耐火材料的影响（英文）

以焦宝石、活性炭和铝粉为原料并添加Fe2O3后制备了Al4SiC4/Al4O4C复合耐火材料。利用化学分析、X射线衍射和扫描电镜研究了Fe2O3对所制备复合材料的物相组成和显微结构的影响。结果表明：在烧结过程中,从1400℃开始,Fe2O3转变为低熔点物相Fe3Si,产生液相促进Al4SiC4成核、细化晶粒,同时包裹Al4SiC4。此外,未添加Fe2O3的样品中生成的Al4O4C短纤维,Fe2O3的加入使得Al4O4C相变为细小的晶粒。

Abstract：

Al4SiC4/Al4O4C composite refractory was synthesized by using flint clay,activated carbon and aluminum powders as the raw materials and Fe2O3 as the additive. The effects of Fe2O3 on the phase composition and microstructure of Al4SiC4/Al4O4C composite refractory were investigated by chemical analysis,X-ray diffraction and scanning electron microscopy. The results show that Fe2O3 transforms into a low melting point phase of Fe3Si above 1 400 ℃,which leads to generate liquid phase and promote the nu-cleation and grain refinement of Al4SiC4 phase. Fe3Si also could coat Al4SiC4 grains. Moreover,the morphology of Al4O4C in Al4SiC4/Al4O4C composite refractory without addition of Fe2O3 is short fibrous-like structure,but changes into fine granules structure after adding Fe2O3.     

Evolution of Phase Composition and Microstructure of Al_2O_3-Si-Al Composite at High Temperatures in Reducing Atmosphere

Al2 O3-Si-Al composite specimens with the size of 25 mm × 25 mm × 125 mm were prepared using fused alumina （as aggregates and fines）,ultra-fine α-Al2O3,Si and Al powders as starting materials,liquid phenol formaldehyde resin as the binder,pressing and heating at 800-1 500 ℃ for 3 h under carbon embedded condition.Evolution of phase composition and microstructure of Al2 O3-Si-Al composite during heating from 800 to 1 500 ℃ under carbon embedded condition were studied.The results show that：（1） Al4 C3,AlN and SiC are initially formed at 800-900 ℃ due to reactions of Al and Si with C or CO and N2 ; （2） at 1 000-1 300 ℃,the amounts of Al4C3,AlN and SiC increase with temperature rising and their crystals grow; （3） at 1 400-1 500 ℃,Al4 C3 and AlN disappear,and minor SiAlON crystals are observed; the nonoxide crystals develop well and they are interlaced in the corundum skeleton structure,which creates strengthening and toughening     

Effect of Carbon Source on Crystal Morphology of SiC in-situ Formed in AI2O3-Si-C Matrix

Three kinds of Al2O3- Si- C matrix specimens were prepared using tabular corundum powder and Si powder as starting materials,ultrafine flake graphite,nano carbon black,and carbon nanotubes as carbon sources,respectively,to research the effect of micro or nano carbon materials on structure and morphology of formed Si C crystals. The specimens were fired at 1 000,1 200 and 1 400℃ for 3 h in carbon-embedded condition,respectively.The phase composition was studied by XRD and the crystal morphology of Si C was investigated by FESEM. The results show that:( 1) the amount of Si C increases with the firing temperature rising;( 2) the in-situ reaction mechanism and the formed Si C crystal morphology vary with carbon source: carbon nanotubes are generally converted into Si C whiskers by carbon nanotubes-confined reaction; Si and nano carbon black react to nucleate quickly,and the nucleated Si C crystals grow evenly in all directions forming Si C particles; Si C whiskers are produced from edge to internal of ultrafine flake graphite.     

特大尺寸轻型碳化硅镜坯烧结工艺研究

本文分析了反应烧结过程中温度场分布对碳化硅(SiC)镜坯的影响,提出安全升降温速率与陶瓷坯体尺寸的平方成反比关系;测试了SiC素坯热膨胀系数、导热系数与温度的关系,在此基础上讨论了镜坯中的热应力与安全升降温参数的确定;同时通过对固态、液态硅(Si)以及Si固液态转变的特性分析,确定了最佳硅熔渗温度;最后分析了反应烧结SiC(RBSiC)中残余应力的产生机理,提出了解决办法.     

Selectivity of Silicon Carbide/Stainless Steel Solid-State Reactions and Discontinuous Decomposition of Silicon Carbide

Solid-state reactions of SiC with a multicomponent system, stainless steel, have been studied at 1125°C. Four-layered reaction products consisting of modulated carbon precipitation zone, random carbon precipitation zone, four-phase mixture zone, and grain-boundary precipitation zone were formed in the reaction zone. The carbon precipitates were embedded in a matrix of complex metal silicides. In addition, extensive interfacial melting was noted. Carbon atom was found to diffuse faster than Si and selectively reacted with Cr to form Cr carbide(s) along the grain boundaries of stainless steel. No Fe carbides or Ni carbides were ever detected. Among the consituents existing in stainless steel, Ni atoms have the highest affinity for Si. An uphill diffusion of Ni toward the SiC reaction front was observed. While the diffusion of Cr and Fe toward SiC followed a downhill concentration gradient, very small amounts of Cr reached the SiC interface. The selective reactions of Si and C with Ni, Fe, and Cr are discussed on the basis of Gibbs free energy of formation of various compounds. The diffusion kinetics of C and Si atoms in selected metal/SiC reactions are discussed on the basis of their chemical affinities for respective metals. The modulation of carbon precipitation is correlated with previous results from Ni/SiC, Ni₃Al/SiC, Fe/SiC, Co/SiC, and Pt/SiC, reactions. A general model describing discontinuous decomposition of SiC is proposed to explain the origin of carbon modulation.     

Load-assisted SHS joining of NiAl to Ni

The joining of NiAl to Ni substrates was carried out through load-assisted SHS reaction. The process of bonding between liquid reaction products and Ni substrate was studied. A transition layer at the NiAl/Ni interface was found to form mainly due to the diffusion of Al. The components of Ni-rich phases were found to undergo diffusion into the reaction products. Microstructural observations showed the formation of excellent bonding at the NiAl/Ni interface.     

Interconnected SiC–Si network reinforced Al–20Si composites fabricated by high pressure solidification

The microstructures and mechanical properties of the interconnected SiC–Si network reinforced Al–20Si composites solidified under high pressures were investigated. The results demonstrate that the complete interconnected SiC–Si network can be obtained by high pressure solidification, and the connected micron-sized pores are uniformly distributed in the interconnected SiC–Si network. The compressive strength and microhardness of the SiC/Al–20Si composites solidified under 3 GPa were 723 MPa and 229 HV_0.05, respectively. Furthermore, the fracture process of SiC/Al–20Si composites was studied by in situ TEM tensile testing. The result shows that the crack first initiated and propagated at the Al/Si interface under an external load, and the SiC particles in the interconnected SiC–Si network can effectively hinder the crack propagation, thus enhancing the strength.     

Catalytic graphitization of carbons by various metals

A study was made of the catalytic graphitization of carbons by 22 kinds of metals. Heat treatments were carried out at 2600°C for 1 hr and 3000°C for 10 min under argon atmosphere. In graphitizing 3,5-dimethylphenol-formaldehyde resin carbon powder with which 20w/o metal powder (Al, Cr, Mn, Fe, Co, Ni, Ca, Ti, V, Mo and W) was mixed, graphitic carbon was catalytically formed. The first six metals, which belong to the carbon dissolution-precipitation mechanism, gave large graphitic crystal flakes at an early stage of the reaction; the other metals resulted in fine crystals through the carbide formation-decomposition mechanism. For the non-graphitizing phenol formaldehyde resin carbon in which 10w/o metal powder was dispersed, Mg, Si, Ca, Cu and Ge catalyzed formation of only graphitic carbon; and Al, Ti, V, Cr, Mn, Fe, Co, Ni, Mo and W formed both graphitic and turbostratic carbons. Except for Al and Cu, the former effect was exerted by non-transition metals and the latter effect by transition metals. Boron alone markedly accelerated homogeneous graphitization of both kinds of carbon; and Zn, Sn, Sb, Pb and Bi had no catalytic effect. On the basis of these results, the relationships between some properties of the metals, their catalytic abilities and the kind of catalytic effects are discussed.     

Thermodynamic Brazing Alloy Design for Joining Silicon Carbide

Using solution thermodynamic theory, a Ni-Cr Si alloy, based on the Ni/Cr ratio of AWS BNi-5 (Ni-18Cr-19Si (atom%)), was designed for brazing SiC ceramics. The optimum thermodynamic composition was computed to be Ni-14.3Cr-36Si (atom%). Brazing experiments were conducted to assess the effect of changing the Si content away from this composition on the joint microstructures. For alloys containing less than 36 atom% Si, an excessively vigorous joining reaction occurred, resulting in the formation of a porous reaction zone at the brazing alloy/SiC interface, the amount of porosity decreasing as the brazing alloy composition approached the thermodynamically predicted optimum. It was found that the most likely mechanism for the formation of the porous zone was CO evolution during the SiC decomposition reaction. The best microstructures were attained for 40 atom% Si alloy joints, closely agreeing with the thermodynamic model, whereas higher Si content alloys exhibited localized debonding of the brazing alloy from the SiC.     

Effect of Interfacial Reaction on the Thermal Conductivity of Al–SiC Composites with SiC Dispersions

The effect of interfacial reactions between Al and SiC on the thermal conductivity of SiC-particle-dispersed Al-matrix composites was investigated by X-ray diffraction and transmission electron microscopy (TEM), and the thermal barrier conductance ( h _c) of the interface in the Al–SiC composites was quantified using a rule of mixture regarding thermal conductivity. Al–SiC composites with a composition of Al (pure Al or Al–11 vol% Si alloy)–66.3 vol% SiC and a variety of SiC particle sizes were used as specimens. The addition of Si to an Al matrix increased the thermal barrier conductance although it decreased overall thermal conductivity. X-ray diffraction showed the formation of Al₄C₃ and Si as byproducts in addition to Al and SiC in some specimens. TEM observation indicated that whiskerlike products, possibly Al₄C₃, were formed at the interface between the SiC particles and the Al matrix. The thermal barrier conductance and the thermal conductivity of the Al–SiC composites decreased with increasing Al₄C₃ content. The role of Si addition to an Al matrix was concluded to be restraining an excessive progress of the interfacial reaction between Al and SiC.     

炭／炭复合材料SiC／Mo（Six，Al1-x）2涂层形成机理与抗高温氧化性能

采用高温包渗技术在炭／炭复合材料表面制备了SiC／Mo（Six,Al1-x）2复合涂层,采用两步反应法研究了复合涂层的生成机理。发现复合涂层是由Si、Al2O3、SiC、MoSi2原始粉末材料与基体炭材料经过复杂化学反应生成的SiC、Mo（SixAl1-x）2以及微量Mo4．8Si3C0．6固溶体组成。在较低温度下（〈1750℃）,单质硅与基体碳的液-固相反应,经过2小时后可以在炭／炭复合材料表面和内部孔隙表面生成致密的SiC过渡涂层;在较高温度下（≤2000℃）,SiC、Al2O3和MoSi2间的反应较为复杂,其主要过程为SiC与Al2O3间生成液体硅、液体铝和气态SiO、Al2O的多相反应,该反应生成的液体铝能够与MoSi2颗粒发生置换反应,生成熔点降低的Mo（Six,Al1-x）2转移涂层;同时,生成的液体硅与CO反应生成晶须状β—SiC,并与Mo（Six,Al1-x）2形成增强型复合涂层。本文还研究了过量单质Si和SiC对Mo（Six,Al1-x）2的还原反应,化学反应推论与实验结果相吻合。以新提出的涂层生成机理为指导,以粉末原料质量组成为Si10％,Al2O3 10％,SiC54％和MoSi226％时所制得了致密并且无粘结的复合涂层材料,并研究了封孔处理后复合材料的抗氧化性能。     

In Situ TiC Ceramic Particles Locally Reinforced Al‐Si Matrix Composites Prepared by SHS‐Casting Method from the Al‐Si‐Ti‐C System

Using Al‐Si‐Ti‐C powder mixtures, TiC grains locally reinforced Al‐Si matrix composites were produced through self‐propagating high‐temperature synthesis and casting method. The formation of TiC could be ascribed to the dissolution–reaction–precipitation mechanism. The TiC grains were uniformly distributed in the locally reinforced regions of the Al‐Si matrix. With increasing Al‐Si content, the size of TiC grains decreased. No pores and cracks were present at the interface between the Al‐Si matrix and the reinforced regions. Wear resistance of the locally reinforced regions is significantly improved compared with that of the Al‐Si matrix.     

Abnormal mechanical hysteresis behavior of Tyranno-ZMI SiC/SiC containing Ti3Si(Al)C2

This work studied the effect of tough phase Ti₃Si(Al)C₂ on the mechanical hysteresis behavior of SiC/SiC. Different from continuous fibers reinforced brittle ceramic matrix composites, the mechanical hysteresis behavior of SiC/SiC containing Ti₃Si(Al)C₂ shows some abnormal phenomena: as peak applied stress increases during cyclic loading-unloading-reloading tests, the thermal residual stress values exhibit highly dispersion and the thermal misfit relief strain shows abnormally slow growth. These abnormal phenomena are caused by the reduction of transvers cracks (perpendicular to loading fibers) and the generation of hoop cracks (parallel to loading fibers). The plastic deformations of Ti₃Si(Al)C₂ prevents the transverse cracking of modified matrix, while promoting the hoop cracking of SiC matrix prepared by chemical vapor infiltration (CVI-SiC). Hoop cracking occurs within the transition zone containing amorphous SiO₂ layer and carbon layer in CVI-SiC matrix. The combination of weak transition zone and strong modified matrix finally leads to the occurrence of hoop cracking.