Sequential ion-electron irradiation of zirconium carbide ceramics: Microstructural analysis

Zirconium Carbide (ZrC_x) was irradiated with 10 MeV Au³⁺ ions to a dose of 10 displacements per atoms (dpa) and subsequently with 100 and 300 keV electrons in a transmission electron microscope (TEM). After ion irradiation, dislocation loops were observed in the microstructure and an increase in the number of carbon vacancies was revealed by Raman spectroscopy. Grazing incidence X-ray diffraction (GIXRD) analysis showed that neither amorphization nor oxidation occurred during ion irradiation of the specimen. Subsequent electron irradiation of the pre-implanted ZrC_x foil led to formation of nanosized tetragonal ZrO₂ precipitates (5−10 nm diameter) on the surface of the TEM lamella. The formation of the new oxide phase was not related to the electron beam-induced heating of the specimen, but to electron stimulated oxidation caused by the residual oxygen inside the transmission electron microscope. Changes in size and density of ZrO₂ crystallites were observed between the pristine and ion irradiated ZrC_x regions following electron irradiation, suggesting that the initial microstructure of the ZrC_x substrate played a key role in the nucleation and growth of the oxide islands. The obtained results provide insights into the microstructural response of ZrC_x to different types of radiation and the inadvertent effects of the electron beam during TEM analysis of in-situ and ex-situ ion irradiated ZrC_x. Additionally, the findings of this work suggest a method to prepare local ZrO₂ nanoprecipitates within ZrC_x grains by selective electron beam irradiation.     

原位合成ZrC颗粒增强锆基非晶复合材料及力学性能

利用zr与TiC粉末之间的原位反应经铜模铸造方法制备了zrC颗粒增强zr41Til4Cul2.5Ni10Be22．5块状非晶复合材料结果表明：原位合成的ZrC颗粒尺寸细小、形状规整并均匀地分布在非晶基体上．与锆非晶合金相比，复合材料的压缩强度得到提高，塑性得到改善．对ZrC颗粒原位合成及强化机理进行了讨论．     

液中脉冲放电沉积ZrC陶瓷涂层的强化工艺及涂层性能的研究

采用特殊设计的专用脉冲电源液中放电表面强化设备,以硬质金属Zr为电极、45号钢为基体,进行了放电沉积ZrC陶瓷涂层的强化试验.研究了电参数、放电时间与涂层性能之间的关系,同时还研究了强化层形貌、物相结构及强化层的耐磨损性能.试验结果表明：强化层主要成分是ZrC;单个脉冲能量越大,形成的强化层就越厚;当放电时间超过25min时,强化层厚度基本不再增加;强化层具有良好的抗磨损性能.     

Spark plasma sintering of oxides and carbide dispersed zirconia inert matrix fuels

Zirconia-based inert matrix fuels reinforced by ZrC were synthesized via spark plasma sintering (SPS). Composites with full density were obtained. In order to prevent the oxidation introduced by dispersed ZrC in the bulk composite, SiC and ZrB₂ were later added into the composite and their capability to improve oxidation resistance was examined. SiC was found to form an oxidation layer which could enhance the oxidation resistance. In addition, micro hardness was improved attributing to effective sintering facilitated by silica flow and distribution of ZrC. With an optimum sintering condition and the addition of SiC, thermal conductivity was improved at higher temperature with the help of unoxidized ZrC reinforcement in the bulk composite.     

Co-reinforcing of ZrB2–SiC ceramics with optimized ZrC to Cf ratio

Characteristics of ZrB₂–SiC ultrahigh temperature ceramic matrix composites (UHTCMCs) reinforced with ZrC and carbon fiber (C_f) were investigated in this article. Spark plasma sintering (SPS) process was utilized to fabricate the samples at 1800 °C for 5 min under 30 MPa punch pressure and vacuumed atmosphere. In all samples, the volume ratio of ZrB₂: SiC was equal to 4:1, and the summation of ZrC and C_f reinforcements was 7.5 vol% with different ZrC: C_f ratios. Field emission scanning electron microscopy (FE-SEM), energy dispersive spectroscopy (EDS), densitometry, flexural strength, and hardness measurements were employed for characterization of the prepared samples. Microstructural inspection revealed the formation of SiC sheath around the carbon fibers due to several reactions in the surface SiO₂ layers existed on the SiC particles. Optimal flexural strength (628.4 MPa) and hardness (20.8 GPa) values were achieved for the sample co-reinforced with 6.5 vol% ZrC and 1 vol% C_f, with a relative density of 97.7%.     

低压化学气相沉积制备ZrC涂层：原位溴化工艺

本研究设计了一种溴化装置,用于合成并稳定控制ZrBr4蒸汽的流量。采用低压化学沉积技术,以Zr-Br2-C3H6-H2-Ar为体系,1200°C在石墨基底上制备了ZrC涂层。研究了气体组分(源气C/Zr比)对ZrC涂层微观形貌及生长机制的影响。源气C/Zr比为1.5时,涂层的沉积过程为由表面反应机制为主,ZrC涂层较为疏松。源气C/Zr比为0.5~1时,扩散动力学是涂层的主要生长机制,所制备的ZrC涂层具有致密均匀ZrC涂层,并沿(200)晶面择优取向。同时,源气C/Zr比为0.5时,制备的ZrC涂层无自由碳存在并具有近化学计量比。     

20Mn2钢晶粒超细化及性能

借鉴超塑预处理细化晶粒的思路，在20Mn2钢中加入与其液态(1650℃）密度相同、且不溶于钢的ZrC粒子，使其成为钢在热轧时的形变核心和奥氏体及形变诱导铁素体的再结晶核心。并综合引入形变强化、相变强化、第二相弥散强化效应及细晶强化效应，使两种状态试验钢晶粒尺寸均细化到1—2μm。与20Mn2钢相比，淬火态试验钢σ0.2和σb分别提高187．0％和131．8％。同时，延伸率也有所提高；油淬态试验钢的σ0.2和σb分别提高为39．9％和34．2％，与20Mn2钢的塑性指标相比，油淬及低温回火态延伸率分别提高了90％和111％。     

High-repetition rate pulsed laser deposition of ZrC thin films

ZrC thin films were grown on (100) Si substrates by the pulsed laser deposition (PLD) technique using a high-repetition rate excimer laser working at 40 Hz. The substrate temperature during depositions was set at 300 °C and the cooling rate was 5 °C/min. X-ray diffraction investigations showed that the films were crystalline. Films deposited under residual vacuum or 2 × 10^− 3 Pa of CH₄ atmosphere exhibited a (200)-axis texture, while those deposited under 2 × 10^− 2 Pa of CH₄ atmosphere were found to be equiaxed. The surface elemental composition of as-deposited films, analyzed by Auger electron spectroscopy (AES), showed the usual high oxygen contamination of carbides. Once the topmost − 3-5 nm region was removed, the oxygen concentration rapidly decreased, being around 3-4% only in bulk. Scanning electron microscopy (SEM) investigations showed a smooth, featureless surface morphology, corroborating the roughness values below 1 nm (rms) obtained from simulations of the X-ray reflectivity (XRR) curves. From the same simulations we also estimated films mass density values of around 6.32-6.57 g/cm³ and thicknesses that correspond to a deposition rate of around 8.25 nm/min. Nanoindentation results showed a hardness of 27.6 GPa and a reduced modulus of 228 GPa for the best quality ZrC films deposited under an atmosphere of 2 × 10^− 3 Pa CH₄.     

ZrCl4蒸汽沉积法制备高温气冷堆包覆燃料颗粒ZrC涂层

采用ZrCl₄蒸汽、H₂和C₃H₆作为化学反应体系,以Ar为载气,在流化床沉积炉中制备高温气冷堆包覆燃料颗粒ZrC涂层。对所制备涂层进行了分析表征,结果显示：ZrC涂层剖面均匀光滑,无明显孔洞;与内致密热解炭层的界面清晰,厚度约为35μm;涂层主要成分为Zr和C,Zr/C摩尔比接近化学计量比1∶1,其主要相组成为面心立方的ZrC;晶粒生长无明显的择优取向。     

Phase transition,thermodynamic and elastic properties of ZrC

First principles calculation and quasi-harmonic Debye model were used to obtain more physical properties of zirconium carbide under high temperature and high pressure. The results show that the B1 structure of ZrC is energetically more favorable with lower heat of formation than the B2 structure, and that mechanical instability and positive heat of formation induce the inexistence of the B2 structure at normal pressure. It is also found that the B1 structure would transform to the B2 structure under high pressure below the critical point of V/V₀=0.570. In addition, various thermodynamic and elastic properties of ZrC are obtained within the temperature range of 0–3000 K and the pressure range of 0–100 GPa. The calculated results not only are discussed and understood in terms of electronic structures, but also agree well with corresponding experimental data in the literature.