ZrC-Cu-C/C复合材料的烧蚀性能及烧蚀机制

为了提高炭/炭(C/C)复合材料的耐烧蚀性能,以孔隙率为38%的C/C复合材料为坯体,Zr-Cu混合粉末为熔渗剂,采用反应熔渗法制备了ZrC-Cu-C/C复合材料。通过氧-乙炔焰烧蚀实验,研究了熔渗剂成分对复合材料高温耐烧蚀性能的影响。利用XRD、SEM和EDS对烧蚀前后ZrC-Cu-C/C复合材料的相组成和微观结构进行了分析。结果表明:ZrC-Cu-C/C复合材料烧蚀前主要存在C、ZrC和Cu相,有微量Zr残余;烧蚀20s后表面主要存在炭基体、ZrO_2、CuO、Cu_2O及残余的ZrC和Cu。随熔渗剂中Zr含量增加,复合材料的线烧蚀率和质量烧蚀率均呈现先减小后增大的趋势,以60%Zr-Cu(质量分数)为熔渗剂制备的ZrC-Cu-C/C复合材料的抗烧蚀性能最佳,其线烧蚀率和质量烧蚀率分别为0.0018mm·s~(-1)和0.0013g·s~(-1)。ZrC-Cu-C/C复合材料的烧蚀机制为以C的升华、ZrO_2的熔化及Cu的蒸发和汽化为主的热物理烧蚀、ZrC和C氧化的热化学烧蚀以及高压热流冲刷引起的机械剥蚀的综合作用。     

Ablation behavior and mechanism of SiC/Zr–Si–C multilayer coating for PIP-C/SiC composites under oxyacetylene torch flame

To improve the ablation resistance of PIP-C/SiC composites, SiC/Zr–Si–C multilayer coating was prepared by chemical vapor deposition (CVD) using methyltrichlorosilane (MTS) and hydrogen as the precursors and molten salt reaction using KCl–NaCl, sponge Zr and K₂ZrF₆, then the ablation capability of the coated composites was tested under oxyacetylene torch flame. The linear and mass ablation rates were much lower than those of uncoated samples. The linear and mass ablation rates of the three coating coated samples reached 0.0452 mm/s and 0.031 g/s, decreased by 27.3% and 27.1%, respectively. Moreover, the linear and mass ablation rates of the five coating coated samples reached 0.0255 mm/s and 0.0274 g/s, decreased by 59.0% and 35.5%. The gases released during ablation could take away a lot of heat, which was also helpful to the protection of the composites.     

Ablation characteristics of mosaic structure ZrC-SiC coatings on low-density,porous C/C composites

Mosaic structure Zr C-SiC coatings were fabricated on low-density, porous C/C composites via thermal evaporation and an in-situ method. Zr C was packed in a typical lamellar mode, and the mosaic structure was formed by the deposition of Zr and Si atoms on the shallow surface of the porous C/C composites.Ablation analysis showed that the defects in the coatings originate from the boundary between the Zr C and holes created by the consumption of SiC at 2500?C. After ablation for 200 s at 3000?C, a dense ZrO_2 layer formed on the coating surface, and the defects were sealed owing to the continuous supply of ablative components. The mass and line ablation rates of the Zr C-SiC coatings were-0.46 ± 0.15 mg cm~(-2)·s~(-1) and-1.00± 0.04 μm s~(-1), respectively.     

Formation of Cu Nanodots on Diamond Surface to Improve Heat Transfer in Cu/D Composites

Diamond‐dispersed copper matrix (Cu/D) composite materials with different interfacial configurations are fabricated through powder metallurgy and their thermal performances are evaluated. An innovative solution to chemically bond copper (Cu) to diamond (D) has been investigated and compared to the traditional Cu/D bonding process involving carbide‐forming additives such as boron (B) or chromium (Cr). The proposed solution consists of coating diamond reinforcements with Cu particles through a gas–solid nucleation and growth process. The Cu particle‐coating acts as a chemical bonding agent at the Cu–D interface during hot pressing, leading to cohesive and thermally conductive Cu/D composites with no carbide‐forming additives. Investigation of the microstructure of the Cu/D materials through scanning electron microscopy, transmission electron microscopy, and atomic force microscopy analyses is coupled with thermal performance evaluations through thermal diffusivity, dilatometry, and thermal cycling. Cu/D composites fabricated with 40 vol% of Cu‐coated diamonds exhibit a thermal conductivity of 475 W m^?1 K^?1 and a thermal expansion coefficient of 12 × 10^?6 °C^?1. These promising thermal performances are superior to that of B‐carbide‐bonded Cu/D composites and similar to that of Cr‐carbide‐bonded Cu/D composites fabricated in this study. Moreover, the Cu/D composites fabricated with Cu‐coated diamonds exhibit higher thermal cycling resistance than carbide‐bonded materials, which are affected by the brittleness of the carbide interphase upon repeated heating and cooling cycles. The as‐developed materials can be applicable as heat spreaders for thermal management of power electronic packages. The copper‐carbon chemical bonding solution proposed in this article may also be found interesting to other areas of electronic packaging, such as brazing solders, direct bonded copper substrates, and polymer coatings.

     

C/C复合材料Ta2O5-TaC/SiC抗氧化抗烧蚀涂层研究

采用包埋法和低压化学气相沉积(CVD)法在碳/碳(C/C)复合材料表面依次制备了Ta2O5-TaC内涂层和SiC外涂层,用X射线衍射分析(XRD)、扫描电镜(SEM)及电子能谱(EDS)对涂层的相组成、微观形貌和元素组成进行了分析,研究了涂覆涂层后C/C复合材料在1 500℃静态空气中的防氧化性能及在氧-乙炔烧蚀中的抗烧蚀性能。结果表明:采用两步法制得的Ta2O5-TaC/SiC复合涂层结构致密,该复合涂层有效提高了C/C复合材料的抗氧化和抗烧蚀性能;Ta2O5-TaC/SiC复合涂层在1 500℃静态空气环境下可对C/C复合材料有效保护100 h以上;涂层试样在氧乙炔烧蚀环境中烧蚀60 s表明涂层可将C/C复合材料的线烧蚀率降低47.07%,质量烧蚀率降低29.20%。     

真空铸造高强度C/Mg复合材料

本文介绍用真空铸造法制造抗拉强度超过1000MPa的高强度C/Mg复合材料。将T300纤维经C-Si-O梯度涂层处理后单向排布于型腔内,在真空下注入ZM-5合金液,凝固后即得C/Mg复合材料零件或试样。试样的抗拉强度在纤维体积分数为0.35时达1050MPa。本文讨论C-Si-O梯度涂层对获得高强度复合材料的作用。     

Fe基高温合金涂层封填C/C-ZrC-SiC复合材料的制备及抗烧蚀机制

为了改善C/C-ZrC-SiC复合材料在高超声速飞行器热防护领域的使用性能,采用低压悬浮浸渗法制备出Fe基高温合金涂层封填C/C-ZrC-SiC复合材料。利用XRD、SEM、EDS等手段研究氧乙炔焰烧蚀前后Fe基高温合金涂层封填C/C-ZrC-SiC复合材料表层微观结构演变规律,阐明了Fe基高温合金涂层对C/C-ZrC-SiC复合材料烧蚀行为的影响。结果表明:C/C-ZrC-SiC复合材料在1 650℃的大气环境下并通过低压悬浮浸渗法浸渗2 h后,其表层形成一层均匀、致密、且结合紧密的Fe基高温合金涂层。在2 500℃下烧蚀180 s后,改性后的C/C-ZrC-SiC复合材料表面出现较小的烧蚀坑,质量烧蚀率相比未表面改性的试样降低了8%,线烧蚀率降低了35%。且表面生成一层均匀致密的Fe₂O₃-ZrO₂复合氧化物保护层,大大降低了表面裂纹、孔洞等缺陷的产生,从而降低了氧的扩散速率及缺陷带来的应力集中。最终Fe基高温合金覆盖层提高了C/C-ZrC-SiC复合材料的高温抗氧化性和抗机械剥蚀性能。      

Ablation property of a C/C-Cu composite prepared by pressureless infiltration

Using Ti addition to improve the wettability between molten Cu and a C/C composite with a density of 1.60 g·cm^− 3, a C/C-Cu composite was obtained by pressureless infiltration. The Cu filled the pores of the C/C composite, while elemental Ti, being distributed between the carbon and Cu, reacted with carbon to form TiC which covered the carbon. During the ablation process under an O₂-C₂H₂ flame, the ablation of the infiltrated Cu and TiC in the composite was prior to the mechanical denudation of the C/C composite. The composite showed a better ablation performance in terms of short-term anti-ablation than a widely used C/C composite.     

Preparation for 2D–C/C composites with pure RL textures and its characteristic

在沉积温度为1080--1200℃、沉积总压力为10 kPa和气体滞留时间为0.01 s的条件下, 以天然气为碳源, 以氮气为载气, 使用新型ICVI工艺对预制体初始密度为0.43 g/cm$^{3}$(纤维体积分数25%)的2D针刺整体炭毡进行致密化,
在150 h内制备出表观密度为1.75 g/cm³的C/C复合材料. 用偏光显微镜和高分辨扫描电镜观察了热解碳基体的微观组织结构, 分析了三点弯曲试样的断口形貌. 结果表明: 制备的C/C复合材料具有粗糙层(RL)组织结构, 试样的弯曲强度为164.77 MPa、模量为21.34 GPa, 表现为阶梯式失效, 断裂行为呈现出明显的假塑性.     

Thermal conductivity of diamond/Ag composites with chromium carbide coated diamonds for the building materials of high power modules

Abstract

This paper reports on a study of the preparation and characterisation of diamond/Ag composites for the building materials of high power modules. The Cr₇C₃ coated diamond particles are utilised to improve the interfacial bonding between the Ag and diamond and composites are prepared by hot pressing technique. The characteristics of Cr₇C₃ coating layers were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The results show that the Cr₇C₃ coatings on the diamonds result in a strong interfacial bonding and a greatly enhanced thermal conductivity of the composites. A largely enhanced thermal conductivity of 768 W m^?1 K^?1 is obtained in Cr₇C₃ coated composites, which increases 168% relative to that of uncoated composites at 65% diamond volume fraction. The measured thermal conductivity agrees reasonably well with the predictions by a differential effective-medium (DEM) model.     

C/C复合材料SiC-MoSi2-TiSi2涂层的设计与性能

为了提高C/C复合材料的高温抗氧化性能,设计了网状的SiC填充高性能的MoSi2和微量的TiSi2涂层。用包埋法制备了C/C复合材料SiC-MoSi2-TiSi2复相陶瓷单层涂层,对制备涂层的化学形成机理进行了分析。结果表明,在选择的实验条件下,制备设计的涂层是完全可行的,实验制备的涂层在1773K有氧环境下具有良好的抗氧化性能。涂层抗氧化性能的提高是因为在高温氧化下涂层表面产生了致密、连续、稳定的玻璃质氧化物。     

反应熔渗制备ZrC-SiC/(C/C)复合材料组织结构及耐烧蚀性能

采用反应熔渗法（RMI）制备出密度为3.288 g/cm3的ZrC-SiC/（C/C）复合材料,采用SEM-EDS、XRD和TEM等分析手段研究了ZrC-SiC/（C/C）复合材料的微观组织结构。结果表明:陶瓷相填充充分且均匀分布在C/C复合材料基体中,其内部组织主要由ZrC、SiC、热解炭（PyC）和碳纤维（CF）组成。熔渗剂反应充分,复合材料内部未检测到残余未反应金属Zr、Si。采用氧乙炔烧蚀设备检测ZrC-SiC/（C/C）复合材料在2 500℃下,烧蚀时间分别为30 s、60 s和90 s的烧蚀性能,其质量烧蚀率分别为5.667 mg/s、2.907 mg/s和3.030 mg/s,线烧蚀率分别为1.001 μm/s、4.662 μm/s和4.450 μm/s。试验结果表明,在高温烧蚀过程中,ZrC-SiC/（C/C）复合材料烧蚀中心区陶瓷相逐渐氧化生成ZrO₂和SiO₂;生成的ZrO₂和SiO₂混合物保护并填充复合材料烧蚀孔隙,阻止氧化反应向材料内部进行,有效提高了材料的烧蚀性能。      

C/C-Cu复合材料等离子体烧蚀性能

为了研究渗铜对C/C复合材料烧蚀性能的影响,利用化学气相渗透(CVI)和液态压力浸渗工艺制备了C/C-Cu复合材料,并采用等离子体烧蚀装置对C/C-Cu复合材料进行烧蚀,研究其烧蚀性能。结果表明: Cu的加入有效缩短了材料的制备周期;Cu均匀分布在C/C坯体内,呈连续的网状结构;在烧蚀前30 s阶段,Cu通过熔化吸热降低了C/C-Cu试样的升温速度,C/C-Cu复合材料的线烧蚀率低于C/C复合材料,耐烧蚀性能优异;随着烧蚀时间的延长,C/C-Cu复合材料表层的Cu液被火焰带走,表层变为多孔低密度的C/C层,C/C-Cu复合材料的线烧蚀率迅速增加并超过C/C复合材料,耐烧蚀性能降低。     

用气相反应法制备C/C复合材料的梯度SiC涂层

本文采用化学气相反应法（CVR）制备了C/C复合材料的梯度SiC涂层,对该梯度涂层的形成机理及抗氧化性能进行了试验研究.研究结果表明：Si渗入基体的速率对梯度涂层的形成产生直接的影响,当采用体密度较高的C/C基体时,得到了完整致密的梯度SiC涂层,生成的SiC为β-SiC,该涂层具有较好的高温抗氧化能力,在1500℃静态空气气氛中,氧化26小时后失重不超过2%.     

碳／碳复合材料的宽温域自愈合抗氧化

在前期碳材料自愈合抗氧化研究的基础上,提出了通过多元陶瓷基体改性赋予碳／碳复合材料在较宽温度范围内实现自愈合抗氧化的基本原理和技术方案,分析了B4C—SiC、ZrC—SiC和ZrB2-ZrC—SiC等多元陶瓷的抗氧化机理,并采用新近合成的ZrB2-ZrC—SiC三元复相陶瓷有机前驱体,通过PIP技术制备了一系列超高温复相陶瓷改性的碳／碳复合材料,研究了该类复合材料在2200℃以下高速气流冲蚀环境中的协同抗氧化和抗烧蚀性能,发现材料表面生成的复合氧化物层能够在一定条件下赋予复合材料自愈合抗氧化能力。     

ZrB2-SiC复相陶瓷涂层制备及其保护C/C-SiC复合材料性能

为提高C/C-SiC复合材料的超高温抗烧蚀性能,通过浆料涂刷和高温烧结相结合的方法在C/C-SiC复合材料表面制备了ZrB₂-SiC复相陶瓷涂层,利用EDS、SEM对涂层的成分及微观形貌进行了分析。对涂层材料的力学性能和抗烧蚀性能进行了表征,结果表明：制备的ZrB₂-SiC复相陶瓷涂层保护C/C-SiC复合材料的拉伸强度、弯曲强度及剪切强度分别为147 MPa、355 MPa和21.9 MPa,与无涂层保护的针刺C/C-SiC复合材料的力学性能相比略有下降。涂层材料具有良好的抗氧化烧蚀性能,经过热流密度为3 200 kW/m²的氧乙炔火焰烧蚀600 s试验,其线烧蚀率和质量烧蚀率分别为0.001 mm/s和0.0006 g/s。     

涂层碳/碳复合材料氧化机理的研究

通过高温等温氧化实验,对自制涂层碳/碳复合材料的氧化机理进行了研究.研究结果表明,涂层碳/碳复合材料的等温氧化可分为4个阶段.氧化初期,涂层的表面开始氧化,氧化失重是一个受氧气和涂层的化学反应控制,表现为氧化增重;氧化中期,氧化失重受玻璃质的形成速度和蒸发速度控制,表现为缓慢的氧化失重,氧化失重与时间的关系为直线型;随后,涂层上出现裂纹的形成和愈合过程,涂层深层被氧化,表现为较快的氧化失重;最后,涂层被局部破坏,基体被部分氧化,氧化失重直线上升.     

MoSi2-SiC 抗氧化涂层对碳/碳复合材料弯曲性能的影响

在C/C 复合材料表面制备了MoSi₂-SiC 抗氧化涂层, 分析了涂层工艺对C/C 复合材料组织的影响, 测试了材料的室温弯曲力学性能。结果表明, 该工艺在C/C 复合材料表面生成抗氧化涂层的同时, 基材内部的层间和纤维束界面, 以及孔隙周围也被硅化。C/C 复合材料经涂层工艺处理后, 弯曲断裂行为发生改变, 弯曲强度明显升高,塑性有一定程度的降低。      

Microstructure and Processing of 3D Printed Tungsten Microlattices and Infiltrated W–Cu Composites

Tungsten is of industrial relevance due its outstanding intrinsic properties (e.g., highest melting‐point of all elements) and therefore difficult to 3D‐print by conventional methods. Here, tungsten micro‐lattices are produced by room‐temperature extrusion‐based 3D‐printing of an ink comprising WO₃–0.5%NiO submicron powders, followed by H₂‐reduction and Ni‐activated sintering. The green bodies underwent isotropic linear shrinkage of ≈50% during the thermal treatment resulting in micro‐lattices, with overall 35–60% open‐porosity, consisting of 95–100% dense W–0.5%Ni struts having ≈80–300 μm diameter. Ball‐milling the powders and inks reduced the sintering temperature needed to achieve full densification from 1400 to 1200 °C and enabled the ink to be extruded through finer nozzles (200 μm). Partial sintering of the struts is achieved when NiO is omitted from the ink, with submicron interconnected‐porosity of ≈34%. Several tungsten micro‐lattices are infiltrated with molten copper at 1300 °C under vacuum, resulting in dense, anisotropic W–Cu composites with 40–65% tungsten volume fraction. Partially sintered struts (containing nickel) with submicron open porosity are also infiltrated with Cu, resulting in co‐continuous W–Cu composites with wide W struts/Cu channels at the lattice scale (hundreds of micrometers), and fine W–Cu interpenetrating network at the strut scale (hundreds of nanometers) allowing for the design of anisotropic mechanical and electrical properties.

     

铸造高强度C/Al复合材料

本文介绍用铸造法制造抗拉强度超过750MPa的高强度C/Al复合材料。将国产高强度碳纤维经MSC涂层处理后以束状排布于精密铸造模壳内,在4000Pa的真空度和0.75MPa的空气压力下将356合金液浸渗入预热模壳内,凝固后获得C/Al复合材料零件或试样。试样的抗拉强度当纤维体积分数为0.35时达764MPa。论文讨论了纤维束状排布对浸渗过程和材料韧性的有利影响。