高固含量低粘度碳化硅陶瓷浆料的制备与性能研究

采用两种粒径SiC颗粒(11.31μm和3.82μm)、石油焦粉为原料,研究分析不同比例SiC颗粒级配对SiC陶瓷浆料粘度的影响,制备高固含量(≥50vol%)、低粘度(≤1Pa·s)的碳化硅陶瓷浆料,利用注浆成型方法成型SiC陶瓷素坯,反应烧结制备高纯致密SiC陶瓷材料。     

复杂结构碳化硅陶瓷制备工艺的研究进展

碳化硅陶瓷具有高强度、高热导率、良好化学稳定性等特点,广泛应用于航空航天、石油化工、集成电路等领域,但碳化硅陶瓷的硬度高、脆性大,在加工过程中易产生缺陷,从而制约了复杂结构碳化硅陶瓷的应用.介绍了复杂结构碳化硅陶瓷的制备工艺,并分析了目前常用的冷等静压成型结合无压烧结制备技术、凝胶注模成型结合反应烧结制备技术、注浆成型...     

反应烧结碳化硅表面改性的初步研究

应用电子束蒸发硅,霍尔离子源电离甲烷,并辅助沉积的方法在反应烧结碳化硅(RB SiC)基底上沉积了碳化硅(SiC:H)改性薄膜.X射线衍射(XRD)测试表明制备的碳化硅改性薄膜为α相.通过控制沉积速率,制备了硬度为9.781～13.087GPa,弹性模量为89.344～123.413GPa的碳化硅改件薄膜.比较同样条件下镀制银膜的抛光良好微晶玻璃和经过精细抛光的改性 RB SiC,结果表明两者反射率相近;附着力实验表明,制备的薄膜和基底结合良好;在温度冲击实验下,制备的薄膜无龟裂和脱落.     

霍尔离子源辅助制备碳化硅改性薄膜的初步研究

应用电子枪蒸发硅,霍尔离子源电离甲烷,并辅助沉积的方法在反应烧结碳化硅（Reaction Bonded Silicon Carbide: RB SiC）基底上沉积了碳化硅（SiC:H）改性薄膜。XRD测试表明制备的碳化硅改性薄膜为α相。通过控制沉积速率,制备了硬度从9.781 GPa-13.087 GPa,弹性模量89.344 GPa-123.413 GPa的碳化硅改性薄膜。比较同样条件下都镀制银膜的抛光良好微晶玻璃和经过精细抛光的改性反应烧结碳化硅,两者有相近的反射率。附着力实验表明制备的薄膜和基底有良好的结合。在温度冲击实验下,制备的薄膜无龟裂和脱落。     

固体碳源在碳化硅浆料中的分散

碳化硅固相烧结必须添加C、B烧结助剂,才能促进碳化硅的致密。而烧结助剂在碳化硅粉体中间的分散是影响碳化硅陶瓷结构是否均匀以及能否提高其力学性能的关键。本文研究3种固体碳源材料石油焦、碳黑和石墨粉末在固含量为15%的碳化硅浆料中的分散行为。用沉降实验数据比较无分散剂、加入分散剂焦磷酸钠或Darven C3种不同分散条件下,固体碳源粉体的分散性。实验结果表明:分散剂的加入对SiC浆料分散效果有很大影响,3种碳源中碳黑分散最好;最佳分散组合为碳黑加入Darven.C。     

大尺寸轻型碳化硅质镜体的制造与材料性能测试

利用凝胶注模(gel-casting)成型工艺制备了620 mm和700 mm×300 mm的碳化硅(SiC)轻型反射镜素坯,经过脱模、干燥、脱脂和反应烧结等工艺,制备了反应烧结SiC(RB-SiC)镜体。镜体经过加工和测试,结果表明:制备的RB-SiC内部结构均匀致密;力学性能和热学性能优异,抗弯强度、断裂韧性和热膨胀系数分别达到了350 MPa、 4.1 MPa·m^1/2和2.67×10^－6/K;镜体经抛光后的表面粗糙度RMS值可优于3 nm,适合用于制备空间用大尺寸轻型反射镜。     

空间用碳化硅反射镜的设计制造与测试

碳化硅由于其优异的机械性能和热物理性能而成为颇具吸引力的反射镜材料。采用反应烧结碳化硅(RB-SiC)材料制备了空间用反射镜体,用化学气相沉积(CVD)工艺在镜体镜面沉积一层致密的碳化硅薄膜,反射镜采用蜂窝状背面开放式轻量化结构。对直径为250 mm反射镜的组织、性能做了一系列研究测试。结果表明:反射镜体为Si/SiC两相组织,薄膜为单相SiC,反射镜的机械、热性能优异,薄膜与基体结合强度为345.5 MPa,研磨后镜面表面粗糙度达到1.487 nm rms。采用本文工艺方法有能力制备米级直径的空间用碳化硅反射镜。     

碳化硅零件的激光选区烧结及反应烧结工艺

为了获得高密度、高性能、复杂结构的碳化硅陶瓷件,提出采用机械混合法制备含有黏结剂和乌洛托品固化剂的碳化硅复合粉体,对复合粉体进行激光选区烧结（SLS）形成陶瓷素坯,并对素坯进行气氛烧结和渗硅处理,使其与基体发生反应烧结,最终形成复杂陶瓷异形件。实验证明：若激光功率为8.0 W、扫描速率为2 000 mm/s、扫描间距为0.1 mm、单层厚度为0.15 mm,获得的 SLS 陶瓷样品密度和强度最好。对SLS试样进行合理的中温碳化和高温渗硅,所得碳化硅陶瓷烧结体的抗弯强度最高可达 81 MPa,相对密度大于86%。     

轻型碳化硅质反射镜坯体的制造工艺

研究了轻型碳化硅质反射镜坯体制造技术,讨论了制备工艺中的关键环节.提出了一种先进的消失模技术用于制备性能更加优异的背部半封闭式轻量化结构.针对制备大尺寸复杂形状陶瓷的难点,研究了SiC陶瓷素坯凝胶注模成型及成型过程中高固相含量低黏度SiC浆料的配置、浆料固化时间控制及大尺寸复杂形状SiC湿坯的液体干燥工艺等.测试分析了...     

反应烧结制备Ti3SiC2材料

分别以粉末钛、硅、石墨和钛、碳化硅、石墨为原料,采用反应烧结工艺制备Ti3SiC2材料.结果表明:当以钛、硅、石墨单质粉料为原料时,在1200~1400℃温度范围内能够合成出高纯度的Ti3SiC2块体材料,且其纯度随着硅含量的增加而提高;当原料摩尔比为3:1.3:2和3:1.4:2时,该材料中只有Ti3SiC2相而无其他相存在;而以钛、碳化硅、石墨粉末为原料时,在1200~1400℃温度范围内很难合成出高纯度的Ti3SiC2块体材料.     

Microstructural studies of the temperature-dependence of deformation structures around hardness indentations in ceramics

Various light microscopy and SEM techniques have been used to study the temperature dependence of deformation structures around hardness indentations in highly brittle ceramics (including single crystals of silicon and silicon carbide and polycrystalline forms cf SiC, Si₃N₄ and B₄C). Nomarski differential interferometry has enabled slip steps to be resolved around high-temperature indentations, allowing identification of the dominant slip systems and measurement of the extent of surface plasticity as a function of temperature. The occurrence of indentation fracture as a function of both temperature and specimen microstructure was studied by SEM methods (including stereo imaging), Nomarski differential interferometry and polarized reflection light microscopy. Generally, radial and lateral crack sizes increased with increasing temperature, due to increasing residual stresses around indentations caused by increasing indentation plasticity. Examples of microstructural control of crack paths are given for various single crystal and polycrystalline materials.     

On material selection for ultra-high accuracy and high-speed machine table for applications such as E-beam lithography

The selection of the right material for the mechanical stage of an electron beam lithography system is an important step in achieving the high accuracy required for submicron lithography. The material must be nonmagnetic, vacuum compatible, and strong enough for operation. It must possess mechanical properties to reduce static errors and dynamic errors, as well as electrical properties to minimize the E-beam deflection errors. After comparison of the most promising materials, silicon carbide is concluded to be the best material for an E-beam stage because of its low coefficient of thermal expansion, very high elastic modulus, light weight, and excellent hardness. Being semiconductive, it resolves both electric charge-up problems and beam deflection errors due to eddy current.     

The effect of a weak W/SiC interface on the strength of Sigma silicon carbide monofilament

Fractography studies have shown that the strength-determining flaws in silicon carbide monofilaments are generally at the core/silicon carbide interface or in the vicinity of the outside, carbon-based coating. In tungsten-cored monofilaments like DERA Sigma, the W/SiC flaws primarily determine the strength. Fracture is accompanied by brittle failure of the tungsten. The crack propagates simultaneously outwards through the silicon carbide, inwards through the tungsten and also around the W/SiC interface before being deflected into the tungsten or out through the silicon carbide. Experiments depositing boundary layers between the tungsten and silicon carbide have resulted in significantly different fracture behaviour. The tungsten fails in a ductile manner and the strength-determining flaws are located predominantly at the outside surface of the silicon carbide. This behaviour is discussed in terms of models proposed by E. Martin and W. Curtin. It is thought that the work will ultimately lead to a significantly stronger, tungsten-based monofilament.     

基于碳化硅器件的充电机偏磁抑制自动控制装置的研究

在轨道交通行业,碳化硅器件凭借其开关速度快、可实现高频化、低能耗等方面的优势,迅速得到了较为广泛的关注与应用。伴随着变换器的功率密度提高,与变换器配合的变压器更容易发生偏磁问题。该文对全碳化硅充电机进行主电路参数设计,并设计出具有变压器偏磁抑制功能的自动控制装置。通过试验,验证了该变压器偏磁抑制自动控制装置的有效性。     

Tribological Impact of SiC Encapsulation of Released Polycrystalline Silicon Microstructures

A method for coating released polysilicon microstructures with thin, uniform and conformal coatings of SiC derived from the single source precursor, 1,3-disilabutane (DSB) has been developed. This coating method has been successfully applied to micromechanical test devices which allow evaluation of friction and wear properties of the coating. Here, data on the coefficient of static friction of SiC coatings produced from DSB is presented. Also, a comparative wear study for devices which have been oxidized, treated with an anti-adhesion coating, and SiC coated is shown. Wear is examined by scanning electron microscopy (SEM) on devices which have been cycled repetitively under a nominal load. It is found that the application of a few nanometers-thin SiC coating provides exceptional wear resistance as well as significant reduction in friction on the microscale.     

高密度反应烧结SiC的耐化学腐蚀性能

考察了以SiC和碳粉为主要原料制备的不同密度和游离硅含量的反应烧结SiC陶瓷的耐酸碱腐蚀性能,结果表明:游离硅含量及其分布状况是决定SiC陶瓷耐化学腐蚀性能的主要因素。密度为3.16 g/cm3的反应烧结SiC耐化学腐蚀性能显著优于密度为3.07 g/cm3的材料。同等密度但含少量游离碳的高密度材料耐腐蚀性能更好,在98℃5%HF/5%HNO3(质量分数)中腐蚀30 h后失重量仅为中等密度材料的1/17.4。混酸腐蚀时反应烧结SiC初始1 h腐蚀量与材料中游离硅的体积含量呈线性关系,其后,高、低密度材料的腐蚀失重量的比值减小。     

碳化硅发热元件失效分析

对国产炉用碳化硅发热元件在1600℃空气中的高温失效行为进行了研究。结果表明：在900℃以下随温度升高，碳化硅发热元件电阻缓慢减小，超过900℃后随温度升高电阻增加较快；1600℃时随保温时间的增加，碳化硅发热元件的电阻缓慢增加，250min后，电阻急剧增加，直至发热元件断裂。失效表面分析表明，碳化硅发热元件表面以生成气相产物为主，断口处以生成玻璃相为主。     

碳化硅陶瓷液相烧结时的液相生成过程

使用高温实时观测设备对添加有Al2O3-Y2O3烧结助剂的碳化硅(SiC)陶瓷在烧结过程中的收缩情况进行了观测,获得了液相烧结SiC的收缩曲线;使用TG-DTA-MASS联用技术、原位X射线衍射技术对该SiC陶瓷在液相生成前后的质量损失(失重)情况及其在烧结过程中的物相变化进行了分析。结果表明:SiC表面SiO2的存在降低了Al2O3-Y2O3的共熔温度,使液相在远低于烧结助剂最低共熔温度时就已经生成;液相的生成造成了碳化硅试样的快速失重。     

Tribological behaviour of SiC?TiC?TiB2 composites under unlubricated sliding conditions

The friction and wear behaviour of eight different SiC TiC TiB₂ composite materials, with a practically constant SiC:TiC ratio of 1 and an increasing amount of TiB₂, was determined comparatively in oscillating sliding tests at room temperature under unlubricated conditions. The influence of the relative humidity (RH) of the surrounding air was investigated in tests in dry, normal, and moist air. All tests were performed against SiC balls and Al₂O₃ balls as counterbodies. The friction was affected by RH but barely at all by the composition of the composites. The wear resistance of the composites was found to be improved considerably by addition of TiB₂ in the range 20–60%. The highest wear resistance of the system was found when Al₂O₃ was used as the counterbody material.     

典型碳化硅光学材料的超光滑抛光试验研究

研究了三种典型的碳化硅光学材料CVD SiC、HP SiC以及RB SiC的材料去除机理与可抛光性,并对其进行了超光滑抛光试验。在分析各种材料制备方法与材料特性的基础上,通过选择合理的抛光工艺参数,均获得了表面粗糙度优于Rq=2nm（采样面积为0.71mm×0.53mm）的超光滑表面。试验结果表明：研磨过程中,三种碳化硅光学材料均以脆性断裂的方式去除材料,加工表面存在着裂纹以及材料脱落留下的缺陷;抛光过程中,CVD SiC主要以塑性划痕的方式去除材料,决定表面粗糙度的主要因素为表面微观划痕的深度;HP SiC同时以塑性划痕与晶粒脱落的形式去除材料,决定表面粗糙度的主要因素为碳化硅颗粒大小以及颗粒之间微孔的尺寸;RB SiC为多组分材料,决定其表面粗糙度的主要因素为RB SiC三种组分之间的去除率差异导致的高差。
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