多孔钯块材的脉冲烧结制备及其气体载氘行为(英文)

钯材的高速载氘对金属-氢同位素系统和氢能应用领域的研究具有重要的意义.本文研究了以海绵钯粉为原料通过脉冲烧结制备多孔钯块材的新工艺,用SEM和XRD分析了制备的多孔钯块材的微观结构形貌和相组成,并进一步研究了多孔钯块材的气体载氘行为.结果表明,采用脉冲烧结工艺可制备出孔隙率为81.6%的纯净多孔钯块材,氘在该钯材中的初始载入速度较高但迅速降低,80 s内即可完成约90%氘的载入;载氘开始约10 s后,氘的载入速度下降到较低的水平并缓慢衰减.     

多层陶瓷电容器中的Ag─Pd系内电极浆料

从银钯化合物混合溶液中共沉淀中间体，再还原得到Ａｇ─Ｐｄ合金粉。其粒度随Ｐｄ量增加而降低。预氧化处理合金粉，得到表面为氧化钯和银而中心为Ａｇ─Ｐｄ合金的内电极粉。所配制的浆料可用于制备性能达到规定标准的多层陶瓷电容器。     

多层陶瓷电容器中的Ag—Pd系内电极浆料

从银钯合物混合溶液中共沉淀中间体，再还原得到Ａｇ－Ｐｄ合金粉。其粒度随Ｐｄ量增加而降低。预氧化处理合金粉，得到表面为氧化钯和银而中心为Ａｇ－Ｐｄ合金的内电极粉。所配制的浆料可用于制备性能达到规定标准的多层陶瓷电容器。     

金修饰纳米多孔Pd催化剂对甲酸氧化的电催化活性

以水热法制备出纳米多孔网状钯催化剂(nanoPd),采用电位扫描在其上沉积金,制成金修饰纳米钯电极(Au/nanoPd),运用循环伏安法(CV)、线性扫描(LSV)和交流阻抗谱(EIS)比较nanoPd和Au/nanoPd电极对甲酸氧化反应的电催化活性。CV和LSV结果表明:金在nanoPd表面的沉积促进钯对甲酸氧化的电催化活性,起始电位提前,电流密度更高。EIS研究结果也表明:在Au/nanoPd电极上,甲酸氧化反应的电荷传递电阻更低。结果表明:金修饰纳米钯电极(Au/nanoPd)对甲酸氧化具有较高的电催化活性。     

钯锰纳米多孔材料对乙醇的电催化氧化

采用熔体快淬结合去合金化法制备了钯锰纳米多孔材料(NP-PdMn)。用X射线衍射(XRD)、X射线光电子能谱分析(XPS)、扫描电子显微镜(SEM)和透射电子显微镜(TEM)对材料进行了表征,并研究了其在碱性条件下对乙醇氧化的电催化活性。表征显示,NP-Pd Mn为具有三维双连续纳米多孔结构的棒状材料;锰取代了晶格中部分钯的位置使得晶面间距变小;部分钯和锰在材料表面以氧化态存在。催化性能分析表明,与商业Pd/C相比,NP-PdMn/C催化剂具有优于商业Pd/C的催化活性和稳定性。     

多孔不锈钢基体上钯膜沉积的制备研究

分别采用化学镀法、电镀法以及两者相结合的方式在孔径为5μm的多孔不锈钢基体上进行了致密钯膜的制备。采用SEM、EDS、XRD等对多孔不锈钢表面钯膜进行了表征。结果表明:以0.1 g/L的PdCl_2盐酸溶液对完成前处理的多孔不锈钢进行化学镀预镀后,再使用钯含量为17 g/L钯氨溶液进行电镀可制备出成分纯净的钯膜,此时,钯膜表面形貌平整致密且均匀,无明显坑洞和裂缝,膜厚10～20μm。     

利用纳米钯的受热收缩性制备高洁净度多孔钯材料

采用纳米钯黑做造孔剂并与海绵钯混合进行等离子脉冲放电烧结(SPS)的方法制备多孔钯块体材料。结果表明,纳米钯黑材料在500~550℃受热后会产生明显的收缩,具有良好的造孔效果。由于采用该方法不引入任何杂质,故可在550℃时制备出洁净度与孔隙率(87.88%)高、力学性能好的多孔钯块体材料。该方法也可为其它高洁净度多孔金属材料的制备提供有价值的借鉴。     

TC4合金表面微弧氧化膜SiO_2溶胶凝胶封孔后抗氧化性能研究（英文）

为提高TC4合金的高温抗氧化能力,采用二步法在其表面制备了一种复合涂层。采用微弧氧化工艺在偏铝酸钠电解液中于合金表面原位沉积多孔膜层,然后采用溶胶凝胶提拉浸渍工艺在微弧氧化膜层表面进行封孔处理,并进行后续热处理。SEM和EDS结果表明,膜层总厚度为6μm,封孔层厚度约为1μm。高温氧化实验结果表叫,随着氧化时问的延长,封孔后样品的抗氧化能力也随之提高,与未封孔样品相比,其氧化增重大大降低。微弧氧化膜的表面多孔状态为封孔的溶胶层提供了天然锚固接触点,从而能够起到良好的密封作用。     

小牛血清润滑下钛基多孔陶瓷膜层的摩擦学性能

利用微弧氧化法在纯钛材及大变形纯钛材表面制备多孔陶瓷膜层。采用扫描电镜、X射线能谱仪、非接触三维轮廓仪和纳米压痕仪考察了多孔陶瓷膜层的微观形貌、粗糙度和硬度,并用UMT型多功能摩擦磨损试验机评价了多孔陶瓷膜层在小牛血清润滑条件下的摩擦学行为。结果表明,随载荷增加,摩擦系数减少。膜层磨损机制主要为粘着磨损和磨粒磨损。与纯钛材多孔陶瓷膜层相比,大变形纯钛材多孔陶瓷膜层的摩擦系数更低且波动更平稳,耐磨性能更优,这归因于大变形纯钛材多孔陶瓷膜层表面孔隙率更高,硬度更强,硬弹比(H/E)更大。     

基于冷喷涂的多孔钛与钛合金的制备与表征

基于冷喷涂技术的优点,结合喷涂后热处理开发了一种新的多孔钛与钛合金制备工艺.研究了热处理对所制备多孔钛与钛合金块材的组织与结合强度的影响.结果表明,所得多孔块材的气孔率与粉末本身及喷涂条件有关,气孔率在10%～50%之间变化.热处理态的气孔率代表了冷喷涂制备块材的实际气孔率.所得多孔块材喷涂态的结合强度在10～30 MPa之间变化.热处理后粒子间接触界面通过扩散达到冶金结合,多孔块材的结合强度均明显增加(超过55 MPa).     

放电等离子烧结制备多孔镍催化材料

研究以球形雾化镍粉为原料通过放电等离子烧结(SPS)制备多孔镍块体催化材料的新工艺,用SEM、氮吸附和XRD分析制备的多孔镍块材的微观结构和相组成,并进一步研究多孔镍材对甲烷部分氧化法(POM)制取合成气反应的高流速催化性能。结果表明,采用SPS工艺可制备出孔隙率大于70%的纯净多孔镍材,850 ℃保温120 s制备的镍材可应用于流速达2.70 L/min的POM反应,经其催化的CH4转化率高于80%     

Nanoindentation of porous bulk and thin films of La0.6Sr0.4Co0.2Fe0.8O3−δ

In this paper we show how reliable measurements on porous ceramic films can be made by appropriate nanoindentation experiments and analysis. Room-temperature mechanical properties of the mixed-conducting perovskite material La_0.6Sr_0.4Co_0.2Fe_0.8O_3?δ (LSCF6428) were investigated by nanoindentation of porous bulk samples and porous films sintered at temperatures from 900 to 1200 °C. A spherical indenter was used so that the contact area was much greater than the scale of the porous microstructure. The elastic modulus of the bulk samples was found to increase from 33.8 to 174.3 GPa and hardness from 0.64 to 5.32 GPa as the porosity decreased from 45% to 5% after sintering at 900–1200 °C. Densification under the indenter was found to have little influence on the measured elastic modulus. The residual porosity in the “dense” sample was found to account for the discrepancy between the elastic moduli measured by indentation and by impulse excitation. Crack-free LSCF6428 films of acceptable surface roughness for indentation were also prepared by sintering at 900–1200 °C. Reliable measurements of the true properties of the films were obtained by data extrapolation provided that the ratio of indentation depth to film thickness was in the range 0.1–0.2. The elastic moduli of the films and bulk materials were approximately equal for a given porosity. The 3-D microstructures of films before and after indentation were characterized using focused ion beam/scanning electron microscopy tomography. Finite-element modelling of the elastic deformation of the actual microstructures showed excellent agreement with the nanoindentation results.     

A study on the microstructure of D023 Al3Zr and L12 (Al+12.5 at.% Cu)3Zr intermetallic compounds synthesized by PBM and SPS

The spark plasma sintering (SPS) of L1₂ phase Al₃Zr and (Al+12.5 at.% Cu)₃Zr powders with a nanocrystalline microstructure has been studied to produce bulk intermetallic compounds which maintain metastable structures such as L1₂ structure and nanocrystalline microstructure. The powders were prepared by 10 h planetary ball milling (PBM). Full-density L1₂ (Al+12.5 at.% Cu)₃Zr intermetallic compounds were obtained by SPS for 0 min at 600 °C. The specimens prepared with a longer holding time than 0 min at 600 °C or a higher temperature than 600 °C had local melting areas where micro-cracks were found. They had a lower relative density than the specimen SPS sintered at 600 °C for 0 min. The smallest grain size was obtained in the specimen prepared at 600 °C for 0 min, which was 20–30 nm as confirmed by TEM observation. This was the smallest grain size ever reported in the trialuminide specimens processed by various consolidations of nanocrystalline powders. Accordingly, the highest micro-hardness, 989.5 H_V, was obtained in the specimen and this value was three times higher than those of the specimens with micro grain sizes. Full density Al₃Zr intermetallics were prepared by SPS at 700 °C for 0 min. However, their crystal structure was D0₂₃ and micro-hardness was 778.1 H_V. By using SPS, the sintering time can be reduced within 10 min. It was thought that the decrease in sintering temperature for the PBM Al₃Zr and (Al+12.5 at.% Cu)₃Zr powders by 200–300 °C compared with the conventional sintering temperature resulted in the refinement of microstructure to the nano-size level.     

Oxidation behavior of porous Ti3SiC2 prepared by reactive synthesis

High-purity porous Ti₃SiC₂ with a porosity of 54.3% was prepared by reactive synthesis and its oxidation behavior was evaluated under air in the temperature range from 400 to 1000 °C. Thermogravimetric analysis and differential scanning calorimetry (TG-DSC), scanning electron microscope (SEM), X-ray diffractometometry (XRD), energy dispersive spectrometer (EDS), Raman spectrum, BET surface area analysis, and pore-parameter testing were applied to the studies of the oxidation kinetics, phase composition, micro morphology, and porous structure parameters of porous Ti₃SiC₂ before and after oxidation. The results showed that the formation of TiO₂ oxidized products with different modifications was the primary factor influencing the oxidation resistance and structural stability of porous Ti₃SiC₂. Cracks were observed in the samples oxidized in the full temperature range of 400-1000 °C because of the growth stress and thermal stress. At 400-600 °C, anomalous oxidation with higher kinetics and the aberrant decrement in pore size and permeability were attributed to the occurrence of severe cracking caused by the formation of anatase TiO₂. At raised temperatures over 600 °C, the cracking phenomena were alleviated by the formation of rutile TiO₂, but the outward growth of the oxide scales detrimentally decreased the connectivity of porous Ti₃SiC₂.     

Microstructures and mechanical properties of TiAl alloy prepared by spark plasma sintering

A fine-grained TiAl alloy with a composition of Ti-47%Al(mole fraction) was prepared by double mechanical milling(DMM) and spark plasma sintering(SPS). The relationship among sintering temperature, microstructure and mechanical properties of Ti-47%Al alloy was studied by X-ray diffractometry(XRD), scanning electron microscopy(SEM) and mechanical testing. The results show that the morphology of double mechanical milling powder is regular with size of 20?40 μm. The main phase TiAl and few phases Ti₃Al and Ti₂Al were observed in the SPS bulk samples. For samples sintered at 1000 °C, the equiaxed crystal grain was achieved with size of 100?250 nm. The samples exhibited compressive and bending properties at room temperature with compressive strength of 2013 MPa, compression ratio of 4.6% and bending strength of 896 MPa. For samples sintered at 1100 °C, the size of equiaxed crystal grain was obviously increased. The SPS bulk samples exhibited uniform microstructures, with equiaxed TiAl phase and lamellar Ti₃Al phase were observed. The samples exhibited compressive and bending properties at room temperature with compressive strength of 1990 MPa, compression ratio of 6.0% and bending strength of 705 MPa. The micro-hardness of the SPS bulk samples sintered at 1000 °C is obviously higher than that of the samples sintered at 1100 °C. The compression fracture mode of the SPS TiAl alloy samples is intergranular fracture and the bending fracture mode of the SPS TiAl alloy samples is intergranular rupture and cleavage fracture.     

粉末中C抑制FeAl熔滴氧化机制及其对等离子喷涂层组织与性能的影响*

大气等离子喷涂（APS）金属时,熔滴不可避免地发生氧化是难以获得粒子间结合充分的致密涂层的主要原因。以FeAl金属间化合物为例,提出一种在粉末中添加亚微米金刚石颗粒引入碳源,以期利用碳在高温下优先氧化的特性抑制等离子喷涂飞行粒子中Fe、Al元素的氧化,获得无氧化物的高温熔滴从而制备低氧含量（质量分数）、粒子间充分结合的FeAl金属间化合物涂层的新方法。采用APS制备Fe Al涂层,研究金刚石的添加对涂层氧含量、碳含量、涂层内粒子间结合质量与硬度的影响规律,探讨FeAl熔滴飞行中的氧化行为。采用商用热喷涂粒子诊断系统测量APS喷涂中的粒子温度,通过SEM与XRD表征了涂层的组织结构,并表征涂层的结合强度与硬度。结果表明,在等离子射流的加热和Fe、Al元素放热反应的联合作用下,飞行中FeAl熔滴的表面温度可达2 000℃以上,满足C原位脱氧的热力学条件。与不含碳的传统Fe Al涂层中的氧含量随喷涂距离的增加而显著增加的规律完全不同,用Fe/Al/2.5C粉末喷涂时涂层中的氧含量随距离的增加而减小,表明飞行中熔滴的氧化得到抑制,实现了C原位脱氧抑制金属元素氧化的自清洁氧化物的效应。FeAl/...     

Effect of pore size on the high temperature oxidation of Ni-Fe-Cr-Al porous metal

This study investigated the effect of the pore size of Ni-22.4%Fe-22%Cr-6%Al porous metal on its hightemperature oxidation. Two types of open porous metals with pore sizes of 800 μm and 580 μm were used. A 24-hour isothermal oxidation test was conducted at three different temperatures of 900 °C, 1000 °C, and 1100 °C under a 79% N₂ + 21% O₂ atmosphere. The results of the BET analysis revealed that the specific surface area increased as the pore size decreased from 800 μm to 580 μm. The high-temperature oxidation results showed that porous metals exhibited far lower levels of oxidation resistance compared with bulk metals, and that the oxidation resistance of porous metals decreased with a decreasing pore size. According to the microstructural observations of the oxide layers, the 900 °C and 1000 °C oxidation layer contained Ni, Cr, and Al oxides mainly on the strut. The 800 μm porous metal strut exhibited similar oxidation behavior at 1100 °C to that found at lower temperatures. In contrast, the 580 μm porous metal strut was found to consist of Ni and Fe oxides in the upper layer and Ni, Cr, and Al oxides in the lower layer, representing a low oxidation resistance. For powders affixed to the strut inside the porous metal, a different oxide-forming behavior from that of the strut was observed. In addition, the Ni-Fe-Cr-Al porous metal high-temperature oxidation microscopic mechanism is also discussed.     

等离子体球化处理和放电等离子烧结制备钡钨阴极多孔钨基体

采用等离子体球化处理和放电等离子烧结(SPS)相结合的方法制备了钡钨阴极多孔钨基体。研究了等离子体球化处理工艺参数对钨粉的球化率和性能的影响规律,以及SPS制备的多孔钨基体的微观组织和相应钡钨阴极的发射性能。结果表明:当喂粉速率和载气流量分别为2.4 g/min和4.0 L/min时,可得到球化率大于98%,且表面光滑、球形度高的球形钨粉;经球化处理后,钨粉的松装密度和流动性显著提高。与原料钨粉相比,采用球形钨粉制备得到的多孔钨基体的孔隙结构和分布均得到显著改善,且开孔率由18.3%提高至19.7%;相应的钡钨阴极在1050℃下的饱和脉冲发射电流密度由8.7 A/cm~2提高至11.2 A/cm~2。