PIP工艺制备C_f/SiC复合材料孔隙结构及其传热传质特性研究
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摘要
先驱体浸渍—裂解(PIP)工艺制备的C_f/SiC复合材料内部孔隙率可达10～20vol.%,孔隙是除纤维、基体、界面外C_f/SiC复合材料的又一重要组分,直接影响材料的力学、抗氧化、传热、传质等性能,并赋予复合材料许多潜在功能。本文以PIP-C_f/SiC复合材料孔隙结构为对象,开展孔隙表征、控制及应用技术研究。旨在建立一套适合其特点的综合表征体系,实现对孔隙结构的准确、全面描述;探明工艺因素对孔隙形成的影响规律,总结行之有效的控制方法;并以主动冷却防热结构为背景,建立孔隙结构与PIP-C_f/SiC复合材料传热、传质性能间的本构关系与预测模型,为深化PIP-C_f/SiC复合材料理论研究,拓展其应用领域奠定基础。
根据PIP-C_f/SiC复合材料的孔隙结构及使用特点,对多孔介质已有表征手段进行筛选、改进,首次建立了适合PIP-C_f/SiC复合材料的一套表征方法,即综合压汞(MIP)、等温吸附(BET)、扫描电镜(SEM)及气泡法等手段表征PIP-C_f/SiC复合材料的孔隙率、比表面、孔隙形貌、孔隙尺寸及分布、孔隙拓扑结构(分形特征)等特征,建立了孔隙结构物理模型。
通过研究三维编织物(3D)、“二维半”编织物(2.5D)及二维叠层碳布(2D)增强的PIP-C_f/SiC复合材料孔隙结构发现,各织构复合材料的孔隙存在若干共性特征,如主体结构呈“孔道/喉—孔腔”二元模式,纳米微孔在各类材料中普遍存在,贯通孔仅占全部孔隙的一部分等;但在孔隙尺寸、形状、含量、连通性等方面,纤维增强体的织构方式具有决定性影响:例如在孔隙率方面,2.5D-C_f/SiC的最高,三维四向编织物(3D4d)次之,三维五向织物(3D5d)最低,而二维碳布叠层(2D)复合材料介于两种三维编织物之间。孔隙空间结构方面,3D-C_f/SiC复合材料内部孔隙呈三维网络,主要包括百微米级纤维束间孔腔(pore chambers),几微米至几十微米的纤维束间孔道(pore channels/throats)以及纳米级微孔(micro-pores/cracks)等三类,纤维束间孔道不但沟通了各个孔腔,也连接了更小的纳米微孔。2.5D-C_f/SiC与2D-C_f/SiC复合材料孔隙呈现二维层状特征,其连通性具有明显的各向异性特征。此外,织构上的差别还导致3D4d-C_f/SiC、3D5d-C_f/SiC、2.5D-C_f/SiC及2D-C_f/SiC复合材料内的孔腔、孔道、纳米孔及贯通孔含量存在较大差异。对表面特征研究表明,不同织构PIP-C_f/SiC复合材料比表面均不高,属非多孔固体的水平,但与吸附质(N_2)作用较大,且由于孔尺寸分布范围广泛,吸附等温线均呈Ⅱ类反S型,上述特征均与复合材料内部纳米微孔含量及分布密不可分。
通过对不同制备周期中间体的跟踪表征,首次研究了PIP-C_f/SiC复合材料的孔隙结构随制备进行的演化过程,发现SiC基体优先在3D复合材料的纤维束间孔道填充,但当致密度达到一定水平后,孔道体积未继续下降,而以孔腔填充为主;相反,2.5D和2D-C_f/SiC复合材料在经纬纱交叠处的孔隙尺寸在制备初期既已形成,两者的层间孔腔是后续基体填充的主要对象,孔隙空间连通性也随制备相应演化;受所含纳米微孔含量变化影响,各类复合材料的比表面演化情况也不同,但其孔隙表面粗糙程度基本接近,均由织物表面覆盖的SiC颗粒所贡献。
系统研究了浸渍工艺参数(浸渍液类型、浸渍压力、时间等)对孔隙结构的影响。结果表明,以硅油(PSO)为代表的具有低粘度、良好浸润性及受热交联的浸渍液体系填充增强体织物内部空间的能力较强,致密化效率高于聚碳硅烷(PCS)/Xylene/SiC_p(泥浆)、PCS/DVB及PCS/Xylene体系,制得复合材料的孔隙率低于5%,孔隙以20～0.1μm的基体内微裂纹为主。浸渍压力对浸渍不同尺寸孔隙的促进效果是不同的,对于0.1μm以下微裂纹,需要对浸渍液施加较高的外界压力(4MPa以上)方能实现克服浸渍阻力,提高浸渍效率的目的。目前使用的PCS/Xylene,PCS/Xylene/SiC_p,PCS/DVB以及PSO浸渍液体系均能与碳纤维织物较好的浸润,保持现有浸渍时间,各类浸渍液均能够深入织物内部,对织物内主要孔隙进行充分填充。
通过气体透过法研究了PIP-C_f/SiC复合材料的渗流传质特性。结果显示,气体(N_2)在各类织构C_f/SiC复合材料中渗流时的流态包括层流、非层流及滑流,流态转变的临界压力受材料致密度、增强体织构、浸渍液类型等因素影响。
PIP-C_f/SiC复合材料内的贯通孔结构是控制气体渗流关键因素。气泡法能够测定这些渗流的通道的分布函数α(D),结合并联(或串联)毛细管模型能够有效预测C_f/SiC复合材料的气体渗透系数K。不同织构C_f/SiC复合材料的K与其总孔隙率Φ间并无直接联系,各类C_f/SiC复合材料按其渗透能力高低排列为:3D4d-C_f/SiC＞2D-C_f/SiC＞3D5d-C_f/SiC＞2.5D-C_f/SiC,其中3D4d-C_f/SiC的K值可达10~(-14)m~2,但织构一定的条件下,致密度提高能够有效降低复合材料的渗透系数。此外,浸渍PSO,PCS/DVB,PCS/Xylene/SiC_p及PCS/Xylene体系制备的3D复合材料的按其渗透系数大小可排序为:C_f/SiC/Si-O-C＜C_f/SiC/C＜C_f/SiC/SiC_p＜C_f/SiC,3D-C_f/SiC/Si-O-C的气体渗透系数仅为10~(-18)m~2左右。
采用有效当量法研究了PIP-C_f/SiC复合材料的热物理性能。室温下,3D-C_f/SiC复合材料的比热容为0.74J/(g·K),随温度升高而升高;热扩散系数为0.0183cm~2/s,随温度升高线性降低;有效导热系数K_(eff)室温时为2.45W/(m·K),且随温度正向变化;半球全发射率为0.75(80～90℃)。有效导热系数K_(eff)反映了C_f/SiC复合材料固体骨架(纤维,基体)的声子导热及孔隙的辐射换热的综合传热效果,特别在高温下,后者的传热贡献能够弥补导热量下降,导致PIP-C_f/SiC复合材料的K_(eff)随温度提高反而增大。
通过研究PIP-C_f/SiC热物理性能的影响因素发现,先驱体转化SiC基体的有效导热系数不高(1.56～1.47 W/m/K,RT～700℃)是导致C_f/SiC复合材料整体传热水平不高的重要原因之一,这与其内部裂纹缺陷及晶体结构发育不完全有关。此外,增强体织构决定了固体骨架及孔隙排布,对C_f/SiC复合材料内导热及辐射换热机制具有显著影响。对于本文C纤维热导率远高于SiC基体的情况,C_f/SiC复合材料在某一方向的有效导热系数与织物在该向纤维体积含量成正比。由于孔隙辐射换热的差异,致密度对各类织构C_f/SiC复合材料的传热性能影响各不相同,如对3D复合材料而言,孔隙率降至15%以下,继续致密化非但不能提高导热系数,反而使其略有下降;而2.5D织物增强复合材料的K_(eff)却随致密度持续提高。
由H-J模型计算的PIP-C_f/SiC复合材料界面接触热阻与文献报道值吻合,但高于CVI-C_f/SiC。界面接触热阻与增强体织构、纤维种类关系不大,而主要受制备工艺的影响,升温能使界面间隙部分愈合,导致热阻有所降低。
Besides fiber,matrix and their interface,pore is another important component of carbon fiber reinforced silicon carbide(C_f/SiC) composites fabricatd via precursor infiltration and pyrolysis(PIP).Typical porosity of PIP-C_f/SiC composites amounts to 10～20%.These unignorable pores have considerable influence on the mechanical properties,oxidation behaviour;mass and heat transfer of the composites,and provide them some potential functions.In this dissertation,the PIP-C_f/SiC's porous microsturcture characterization techniques were investigated.The pore structure's evolution during fabrication was tracked,its relationship with processing factors was discussed,and the control means were concluded consequently.Aiming at the application of active-cooled aerospace thermal components,the PIP-C_f/SiC's porous structure's effects on its thermal properties and permeability were also researched.
Through evaluating and improvig the general porous media's measuring techniques,an integrated characterization procedure was established,including the MIP, BET,SEM and bubble point method etc.,then applied to research the PIP-C_f/SiC's porous characters successfully,e.g.porosity,morphology,pore size distribution, topology and so on.Based on the results,a detailed physical model was constructed.
Three dimensional braided(3D) fabrics,two and a half dimensional braided(2.5D) fabrics,and carbon cloth laminates(2D) reinforced C_f/SiC composites' pore structures were investigated respectively.It is found that there are some common features of pores in C_f/SiC despite the reinforcements architectures' differences,e.g.the "chamber-throat/channel" binary pattern of the most pores,the existence of nanopores, and the small fraction of the fully-open pores etc..Nevertheless,the reinforcements have decisive effects on porous structures,e.g.from the aspect of porosity,2.5D-C_f/SiC＞3 dimesional,4 directional(3D4d)-C_f/SiC＞2D-C_f/SiC＞3 dimensional,5 directional (3D5d)-C_f-/SiC.As for the configuration,3D-C_f/SiC's pores are three-dimensional network style,composed of some hundreds of microns inter-bundle pore chambers, dozens of microns inter-bundle pore throats/channels,and nano-micropores.The channels communicate such chambers and micropores,integrating all pores inside. While the pores in 2.5D- and 2D-C_f/SiC have a laminar structure,whose topology is obviously anisotropic.Surface characterization indicates the specific surface areas of the aforementioned C_f/SiC are much lower than traditional porous media's,the isotherm sorption curve isⅡstyle,which are all determinated by the nano-micropores' contents and size distributions.
By tracing the structural variations of the semi-articles before finally produced,the porous structure's evolution is recognized during the PIP fabrication.It is found that the SiC matrix keeps filling the inter-bundle channels of the 3D-C_f/SiC firstly,and changes to fill the pore chambers as the densification reachs some level.On the contrary,the channels at the warp-weft crossply of 2.5D and 2D-C_f/SiC have come into being at the fabrication beginning,the laminar pore chambers are the matrix filling targets all along, and the pores' connectivity evolutes consequently.Owing to the fractions of nano-micropores,the aforementioned C_f/SiC's specific areas develop differently; however,their surfacial toughness is similar,which is due to the covering SiC matrix on the surfaces of pores.
The influences of infiltration conditions on the pore structure were researched systematically concerning infiltrate types,pressures,and holding time etc.The results indicate low-viscosity,good wettability,and heat-cure capacities are preferable for infilates to fill the reinforcements' inner spaces efficiently.Thus,polysiloxane(PSO) has higher densification efficiency than polycarbosilane(PCS)/Xylene/SiC_p(slurry), PCS/Xylene,and PCS/DVB.The composites infiltrated by PSO have a much lower porosity(less than 5%),and contain 0.1～20μm micro-cracks mainly.To overcome the resistance and accelerate the infiltrates penetrating,various pressure levels are required for different sized pores,e.g.1atm is sufficient for the pores above 1μm,while at least 4MPa additional pressure are necessary for micropores below 0.1μm.Attributing to the good wettability of aforementioned infiltrates on the carbon fibers,present infiltration time esures all inliltrate permeate into the fabrics deeply.
The mass transfer features were evaluated by measuring the gas permeability of PIP-C_f/SiC.The flowrate-pressrue curves indicate that gas(N_2) flows through the C_f/SiC in three different modes,i.e.laminar,non-laminar,and slipping flow.The flowmode conversion pressures are affected by the densification level,reinforcements' architectures,and infiltrates types et al.
It is found that the full-open pores' characters are the crucial factor determining the gas permeability of C_f/SiC,because they provide the flowing channels for the fluids. Through the bubble point method,their size distribution functionα(D) is obtained. Insertingα(D) into the parrell or series capillary model is able to predict the composites' permeabilities accurately.There are no direct relationship between the permeabilities and porosities of C_f/SiC reinforced by different fabrics,and the relative ranking of their permeabilities is 3D4d-C_f/SiC＞2D-C_f/SiC＞3D5d-C_f/SiC＞2.5D-C_f/SiC,in which the level of 3D4d-C_f/SiC is 10~(-14)m~2.However,the increase of densification can deduce the composite's permeability effectively,for each C_f/SiC above.Moreover,infiltrating PSO, PCS/DVB,PCS/Xylene/SiC_p,and PCS/Xylene produced 3D composites are able to be ranked as:C_f/SiC/Si-O-C＜C_f/SiC/C＜C_f/SiC/SiC_p＜C_f/SiC,according to their permeabilities.And the lowest one of 3D-C_f/SiC/Si-O-C is only 10~(18)m~2.
The equivalent concept was adopted in studying the thermal properties of PIP-3D-C_f/SiC. At room temperature,the specific heat(C_p) is 0.74 J/g/K,thermal diffusivity (TD) is 0.0183 cm~2/s,effective thermal conductivity(K_(eff)) is 2.45 W/m/K,and total emssivity is 0.75(80～90℃).With the temperature inceasing,the C_p and K_(eff) both present positive temperature dependence,while the TD shows negative one over the full temperature range.The K_(eff) values reflect the exact mechanisms of the PIP-C_f/SiC's heat transfer,which involves the solide skeleton(fiber,matrix) thermal conduction via phonons and the radiation contribution of pores inside.Moreover,it is supposed that the latter mechanism is capable of compensating the decrease of thermal conduction occurred at high temperatures,which results in the positive temperature dependence of K_(eff).
The influencing factors of PIP-C_f/SiC's thermal properties are also discussed.Due to the inherent micro-cracks and low crystalline,the SiC presents low K_(eff)(1.56～1.47 W/m/K,from RT to 700℃) derived from PCS,which is the main reason of relatively low heat transfer capacity of PIP-C_f/SiC.Besides the matrix,the reinforcements' architectures determine the configuration of solide skeleton and pore,thus have inevitably great effects on the thermal conduction and radiation,e.g.the K_(eff) is direct proportion to the fiber fraction of fabrics along some direction.There is no fixed correlationship between the densifcation levels and thermal properties of C_f/SiC.For instance,as the porosity of 3D-C_f/SiC decease below 15%,following densification process can not make K_(eff) increase continuously,but cause it deduce a little,while for 2.5D-C_f/SiC,this inceasing trend is lasting in spite of the densification level.The diversity of radiation capacity accounts for this phenomenon,deriving from the different pores' configurations.
The interfacial contact thermal resistance is coincident with the literature reported value of PIP-C_f/SiC calculated by H-J model.The interfacial thermal resistance is insensitive to the reinforecements' architectures and fiber types,but is determined by fabrication process,e.g.the PIP-C_f/SiC value is obviously higher than the CVI one.Due to some interfacial cracks' closure,temperature increasing make the thermal resistance fall off a bit.
根据PIP-C_f/SiC复合材料的孔隙结构及使用特点,对多孔介质已有表征手段进行筛选、改进,首次建立了适合PIP-C_f/SiC复合材料的一套表征方法,即综合压汞(MIP)、等温吸附(BET)、扫描电镜(SEM)及气泡法等手段表征PIP-C_f/SiC复合材料的孔隙率、比表面、孔隙形貌、孔隙尺寸及分布、孔隙拓扑结构(分形特征)等特征,建立了孔隙结构物理模型。
通过研究三维编织物(3D)、“二维半”编织物(2.5D)及二维叠层碳布(2D)增强的PIP-C_f/SiC复合材料孔隙结构发现,各织构复合材料的孔隙存在若干共性特征,如主体结构呈“孔道/喉—孔腔”二元模式,纳米微孔在各类材料中普遍存在,贯通孔仅占全部孔隙的一部分等;但在孔隙尺寸、形状、含量、连通性等方面,纤维增强体的织构方式具有决定性影响:例如在孔隙率方面,2.5D-C_f/SiC的最高,三维四向编织物(3D4d)次之,三维五向织物(3D5d)最低,而二维碳布叠层(2D)复合材料介于两种三维编织物之间。孔隙空间结构方面,3D-C_f/SiC复合材料内部孔隙呈三维网络,主要包括百微米级纤维束间孔腔(pore chambers),几微米至几十微米的纤维束间孔道(pore channels/throats)以及纳米级微孔(micro-pores/cracks)等三类,纤维束间孔道不但沟通了各个孔腔,也连接了更小的纳米微孔。2.5D-C_f/SiC与2D-C_f/SiC复合材料孔隙呈现二维层状特征,其连通性具有明显的各向异性特征。此外,织构上的差别还导致3D4d-C_f/SiC、3D5d-C_f/SiC、2.5D-C_f/SiC及2D-C_f/SiC复合材料内的孔腔、孔道、纳米孔及贯通孔含量存在较大差异。对表面特征研究表明,不同织构PIP-C_f/SiC复合材料比表面均不高,属非多孔固体的水平,但与吸附质(N_2)作用较大,且由于孔尺寸分布范围广泛,吸附等温线均呈Ⅱ类反S型,上述特征均与复合材料内部纳米微孔含量及分布密不可分。
通过对不同制备周期中间体的跟踪表征,首次研究了PIP-C_f/SiC复合材料的孔隙结构随制备进行的演化过程,发现SiC基体优先在3D复合材料的纤维束间孔道填充,但当致密度达到一定水平后,孔道体积未继续下降,而以孔腔填充为主;相反,2.5D和2D-C_f/SiC复合材料在经纬纱交叠处的孔隙尺寸在制备初期既已形成,两者的层间孔腔是后续基体填充的主要对象,孔隙空间连通性也随制备相应演化;受所含纳米微孔含量变化影响,各类复合材料的比表面演化情况也不同,但其孔隙表面粗糙程度基本接近,均由织物表面覆盖的SiC颗粒所贡献。
系统研究了浸渍工艺参数(浸渍液类型、浸渍压力、时间等)对孔隙结构的影响。结果表明,以硅油(PSO)为代表的具有低粘度、良好浸润性及受热交联的浸渍液体系填充增强体织物内部空间的能力较强,致密化效率高于聚碳硅烷(PCS)/Xylene/SiC_p(泥浆)、PCS/DVB及PCS/Xylene体系,制得复合材料的孔隙率低于5%,孔隙以20～0.1μm的基体内微裂纹为主。浸渍压力对浸渍不同尺寸孔隙的促进效果是不同的,对于0.1μm以下微裂纹,需要对浸渍液施加较高的外界压力(4MPa以上)方能实现克服浸渍阻力,提高浸渍效率的目的。目前使用的PCS/Xylene,PCS/Xylene/SiC_p,PCS/DVB以及PSO浸渍液体系均能与碳纤维织物较好的浸润,保持现有浸渍时间,各类浸渍液均能够深入织物内部,对织物内主要孔隙进行充分填充。
通过气体透过法研究了PIP-C_f/SiC复合材料的渗流传质特性。结果显示,气体(N_2)在各类织构C_f/SiC复合材料中渗流时的流态包括层流、非层流及滑流,流态转变的临界压力受材料致密度、增强体织构、浸渍液类型等因素影响。
PIP-C_f/SiC复合材料内的贯通孔结构是控制气体渗流关键因素。气泡法能够测定这些渗流的通道的分布函数α(D),结合并联(或串联)毛细管模型能够有效预测C_f/SiC复合材料的气体渗透系数K。不同织构C_f/SiC复合材料的K与其总孔隙率Φ间并无直接联系,各类C_f/SiC复合材料按其渗透能力高低排列为:3D4d-C_f/SiC＞2D-C_f/SiC＞3D5d-C_f/SiC＞2.5D-C_f/SiC,其中3D4d-C_f/SiC的K值可达10~(-14)m~2,但织构一定的条件下,致密度提高能够有效降低复合材料的渗透系数。此外,浸渍PSO,PCS/DVB,PCS/Xylene/SiC_p及PCS/Xylene体系制备的3D复合材料的按其渗透系数大小可排序为:C_f/SiC/Si-O-C＜C_f/SiC/C＜C_f/SiC/SiC_p＜C_f/SiC,3D-C_f/SiC/Si-O-C的气体渗透系数仅为10~(-18)m~2左右。
采用有效当量法研究了PIP-C_f/SiC复合材料的热物理性能。室温下,3D-C_f/SiC复合材料的比热容为0.74J/(g·K),随温度升高而升高;热扩散系数为0.0183cm~2/s,随温度升高线性降低;有效导热系数K_(eff)室温时为2.45W/(m·K),且随温度正向变化;半球全发射率为0.75(80～90℃)。有效导热系数K_(eff)反映了C_f/SiC复合材料固体骨架(纤维,基体)的声子导热及孔隙的辐射换热的综合传热效果,特别在高温下,后者的传热贡献能够弥补导热量下降,导致PIP-C_f/SiC复合材料的K_(eff)随温度提高反而增大。
通过研究PIP-C_f/SiC热物理性能的影响因素发现,先驱体转化SiC基体的有效导热系数不高(1.56～1.47 W/m/K,RT～700℃)是导致C_f/SiC复合材料整体传热水平不高的重要原因之一,这与其内部裂纹缺陷及晶体结构发育不完全有关。此外,增强体织构决定了固体骨架及孔隙排布,对C_f/SiC复合材料内导热及辐射换热机制具有显著影响。对于本文C纤维热导率远高于SiC基体的情况,C_f/SiC复合材料在某一方向的有效导热系数与织物在该向纤维体积含量成正比。由于孔隙辐射换热的差异,致密度对各类织构C_f/SiC复合材料的传热性能影响各不相同,如对3D复合材料而言,孔隙率降至15%以下,继续致密化非但不能提高导热系数,反而使其略有下降;而2.5D织物增强复合材料的K_(eff)却随致密度持续提高。
由H-J模型计算的PIP-C_f/SiC复合材料界面接触热阻与文献报道值吻合,但高于CVI-C_f/SiC。界面接触热阻与增强体织构、纤维种类关系不大,而主要受制备工艺的影响,升温能使界面间隙部分愈合,导致热阻有所降低。
Besides fiber,matrix and their interface,pore is another important component of carbon fiber reinforced silicon carbide(C_f/SiC) composites fabricatd via precursor infiltration and pyrolysis(PIP).Typical porosity of PIP-C_f/SiC composites amounts to 10～20%.These unignorable pores have considerable influence on the mechanical properties,oxidation behaviour;mass and heat transfer of the composites,and provide them some potential functions.In this dissertation,the PIP-C_f/SiC's porous microsturcture characterization techniques were investigated.The pore structure's evolution during fabrication was tracked,its relationship with processing factors was discussed,and the control means were concluded consequently.Aiming at the application of active-cooled aerospace thermal components,the PIP-C_f/SiC's porous structure's effects on its thermal properties and permeability were also researched.
Through evaluating and improvig the general porous media's measuring techniques,an integrated characterization procedure was established,including the MIP, BET,SEM and bubble point method etc.,then applied to research the PIP-C_f/SiC's porous characters successfully,e.g.porosity,morphology,pore size distribution, topology and so on.Based on the results,a detailed physical model was constructed.
Three dimensional braided(3D) fabrics,two and a half dimensional braided(2.5D) fabrics,and carbon cloth laminates(2D) reinforced C_f/SiC composites' pore structures were investigated respectively.It is found that there are some common features of pores in C_f/SiC despite the reinforcements architectures' differences,e.g.the "chamber-throat/channel" binary pattern of the most pores,the existence of nanopores, and the small fraction of the fully-open pores etc..Nevertheless,the reinforcements have decisive effects on porous structures,e.g.from the aspect of porosity,2.5D-C_f/SiC＞3 dimesional,4 directional(3D4d)-C_f/SiC＞2D-C_f/SiC＞3 dimensional,5 directional (3D5d)-C_f-/SiC.As for the configuration,3D-C_f/SiC's pores are three-dimensional network style,composed of some hundreds of microns inter-bundle pore chambers, dozens of microns inter-bundle pore throats/channels,and nano-micropores.The channels communicate such chambers and micropores,integrating all pores inside. While the pores in 2.5D- and 2D-C_f/SiC have a laminar structure,whose topology is obviously anisotropic.Surface characterization indicates the specific surface areas of the aforementioned C_f/SiC are much lower than traditional porous media's,the isotherm sorption curve isⅡstyle,which are all determinated by the nano-micropores' contents and size distributions.
By tracing the structural variations of the semi-articles before finally produced,the porous structure's evolution is recognized during the PIP fabrication.It is found that the SiC matrix keeps filling the inter-bundle channels of the 3D-C_f/SiC firstly,and changes to fill the pore chambers as the densification reachs some level.On the contrary,the channels at the warp-weft crossply of 2.5D and 2D-C_f/SiC have come into being at the fabrication beginning,the laminar pore chambers are the matrix filling targets all along, and the pores' connectivity evolutes consequently.Owing to the fractions of nano-micropores,the aforementioned C_f/SiC's specific areas develop differently; however,their surfacial toughness is similar,which is due to the covering SiC matrix on the surfaces of pores.
The influences of infiltration conditions on the pore structure were researched systematically concerning infiltrate types,pressures,and holding time etc.The results indicate low-viscosity,good wettability,and heat-cure capacities are preferable for infilates to fill the reinforcements' inner spaces efficiently.Thus,polysiloxane(PSO) has higher densification efficiency than polycarbosilane(PCS)/Xylene/SiC_p(slurry), PCS/Xylene,and PCS/DVB.The composites infiltrated by PSO have a much lower porosity(less than 5%),and contain 0.1～20μm micro-cracks mainly.To overcome the resistance and accelerate the infiltrates penetrating,various pressure levels are required for different sized pores,e.g.1atm is sufficient for the pores above 1μm,while at least 4MPa additional pressure are necessary for micropores below 0.1μm.Attributing to the good wettability of aforementioned infiltrates on the carbon fibers,present infiltration time esures all inliltrate permeate into the fabrics deeply.
The mass transfer features were evaluated by measuring the gas permeability of PIP-C_f/SiC.The flowrate-pressrue curves indicate that gas(N_2) flows through the C_f/SiC in three different modes,i.e.laminar,non-laminar,and slipping flow.The flowmode conversion pressures are affected by the densification level,reinforcements' architectures,and infiltrates types et al.
It is found that the full-open pores' characters are the crucial factor determining the gas permeability of C_f/SiC,because they provide the flowing channels for the fluids. Through the bubble point method,their size distribution functionα(D) is obtained. Insertingα(D) into the parrell or series capillary model is able to predict the composites' permeabilities accurately.There are no direct relationship between the permeabilities and porosities of C_f/SiC reinforced by different fabrics,and the relative ranking of their permeabilities is 3D4d-C_f/SiC＞2D-C_f/SiC＞3D5d-C_f/SiC＞2.5D-C_f/SiC,in which the level of 3D4d-C_f/SiC is 10~(-14)m~2.However,the increase of densification can deduce the composite's permeability effectively,for each C_f/SiC above.Moreover,infiltrating PSO, PCS/DVB,PCS/Xylene/SiC_p,and PCS/Xylene produced 3D composites are able to be ranked as:C_f/SiC/Si-O-C＜C_f/SiC/C＜C_f/SiC/SiC_p＜C_f/SiC,according to their permeabilities.And the lowest one of 3D-C_f/SiC/Si-O-C is only 10~(18)m~2.
The equivalent concept was adopted in studying the thermal properties of PIP-3D-C_f/SiC. At room temperature,the specific heat(C_p) is 0.74 J/g/K,thermal diffusivity (TD) is 0.0183 cm~2/s,effective thermal conductivity(K_(eff)) is 2.45 W/m/K,and total emssivity is 0.75(80～90℃).With the temperature inceasing,the C_p and K_(eff) both present positive temperature dependence,while the TD shows negative one over the full temperature range.The K_(eff) values reflect the exact mechanisms of the PIP-C_f/SiC's heat transfer,which involves the solide skeleton(fiber,matrix) thermal conduction via phonons and the radiation contribution of pores inside.Moreover,it is supposed that the latter mechanism is capable of compensating the decrease of thermal conduction occurred at high temperatures,which results in the positive temperature dependence of K_(eff).
The influencing factors of PIP-C_f/SiC's thermal properties are also discussed.Due to the inherent micro-cracks and low crystalline,the SiC presents low K_(eff)(1.56～1.47 W/m/K,from RT to 700℃) derived from PCS,which is the main reason of relatively low heat transfer capacity of PIP-C_f/SiC.Besides the matrix,the reinforcements' architectures determine the configuration of solide skeleton and pore,thus have inevitably great effects on the thermal conduction and radiation,e.g.the K_(eff) is direct proportion to the fiber fraction of fabrics along some direction.There is no fixed correlationship between the densifcation levels and thermal properties of C_f/SiC.For instance,as the porosity of 3D-C_f/SiC decease below 15%,following densification process can not make K_(eff) increase continuously,but cause it deduce a little,while for 2.5D-C_f/SiC,this inceasing trend is lasting in spite of the densification level.The diversity of radiation capacity accounts for this phenomenon,deriving from the different pores' configurations.
The interfacial contact thermal resistance is coincident with the literature reported value of PIP-C_f/SiC calculated by H-J model.The interfacial thermal resistance is insensitive to the reinforecements' architectures and fiber types,but is determined by fabrication process,e.g.the PIP-C_f/SiC value is obviously higher than the CVI one.Due to some interfacial cracks' closure,temperature increasing make the thermal resistance fall off a bit.
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