金核/铂壳纳米粒子的光化学合成及电催化活性

在含不同摩尔比的Au(Ⅲ)和Pt(Ⅳ)离子的PEG(聚乙二醇)-丙酮溶液中,采用光化学共还原法合成了一组Au@Pt复合纳米粒子,并以炭黑分别对其负载制成Au@Pt/C催化剂。借助于UV-Vis、TEM和HR-TEM的表征,证实复合纳米粒子为球形的核/壳结构;分别以XPS、EDS和电化学方法分析了复合粒子的化学状态、结构特点和Au@Pt/C催化剂的催化性质。结果表明,不同Au:Pt摩尔比的Au@Pt/C催化剂对甲醇氧化反应具有良好的催化活性和稳定性,其中Au:Pt=1:1时形成的Au@Pt/C催化剂电催化活性最高,约为商品Pt/C催化剂的4倍。简要讨论了核/壳结构产生高催化活性的主要原因。     

脉冲电沉积法制备双贵金属催化剂及其电化学性能研究

目的 制备对偏二甲肼具有良好电催化活性响应的复合催化剂。方法 运用脉冲电沉积法在玻碳电极上制备了AuPd、AuPt、PdPt催化剂,研究了占空比、上下限电位、脉冲频率、沉积时间等条件的影响,采用扫描电镜、X射线衍射仪表征了其表面形貌和晶体结构,采用电化学循环伏安法研究了催化剂氧还原反应(ORR)活性和对偏二甲肼(UDMH)电催化氧化活性。结果 3种催化剂的双金属均已合金化,AuPd催化剂为纳米晶枝状结构,AuPt催化剂为纳米球状结构。当占空比为1∶10,上下限电位分别为0.7、0.3 V,沉积频率为10 Hz,沉积时间为20 min时,AuPd催化剂的ORR活性达到最佳;当占空比为1∶30,上下限电位分别为1.1、‒0.1 V,沉积频率为0.05 Hz时,PdPt催化剂的ORR活性达到最佳;当占空比为1∶10,上下限电位分别为1.3、‒0.2 V,沉积频率为0.5 Hz,沉积时间为10 min时,AuPt催化剂的ORR活性达到最佳。AuPd、AuPt催化剂对UDMH具有明显的电催化响应,AuPd的氧化峰积分高达0.23 mAV/cm²,AuPt高达0.25 mAV/cm²。结论 脉冲电沉积法制备的Au基AuPd、AuPt复合催化剂相较于PdPt催化剂和商业Pt/C催化剂对UDMH有更高的电催化活性。     

Ti/Co3O4/RuO2-IrO2纳米结构阳极电催化析氧研究

目的 研发含纳米结构Co3O4中间层的Ti/Co3O4/RuO2-IrO2阳极,并对其电化学析氧性能进行研究,以提升Ti/RuO2-IrO2金属氧化物阳极的电化学析氧性能。方法 在Ti基底上电沉积制备Co(OH)2,烧结形成Co3O4纳米片结构,随后采用热分解工艺在Ti/Co3O4表面制备RuO2-IrO2电催化层,从而构建了Ti/Co3O4/ RuO2-IrO2复合阳极。使用透射电子显微镜(TEM)、扫描电子显微镜(SEM)、X-射线衍射仪(XRD)和电化学工作站对涂层的微观表面形貌、物相组成、电化学性能等进行观察与分析。结果 SEM显示出Ti/Co3O4纳米片上RuO2-IrO2的负载量随涂刷次数增加逐渐增多,最终完全遮盖Co3O4纳米片中间层。且随着RuO2- IrO2前驱体溶液涂覆次数的增加,XRD观察到RuO2-IrO2衍射峰强度在逐渐增大。TEM测试显示Co3O4中间层是由纳米颗粒堆叠组成且具有多孔结构。电化学极化曲线测试表明,涂覆三次RuO2-IrO2层的含Co3O4中间层阳极析氧电位最低,当电流密度达到10 mA/cm²时,析氧电位仅为1.326 V(vs. SCE),低于无中间层的Ti/RuO2-IrO2阳极(1.413 V)。循环伏安测试表明,Ti/Co3O4/RuO2-IrO2阳极的伏安电量达到62.83 mC/cm²,相较于Ti/RuO2-IrO2阳极的23.65 mC/cm²提高了166%。稳定性能试验表明,在经过1 000次循环稳定性试验后,加入Co3O4纳米片中间层的复合阳极的伏安电量降低了35.94%,低于无中间层阳极48.88%的伏安电量损耗率。循环极化试验后的Ti/Co3O4/RuO2-IrO2复合阳极的电化学活性仍明显优于循环极化试验前的Ti/RuO2-IrO2阳极。结论 Co3O4纳米片中间层的加入使得Ti/Co3O4/RuO2-IrO2阳极的电催化析氧性能和稳定性都得到了提升。     

Au-Pt双金属纳米粒子的制备及其电催化性质

在PEG10000/Vc/HAuCl4体系中,用Vc还原HAuCl4制备金纳米粒子,以所制备的金纳米粒子为晶种,通过控制HAuCl4与H2PtCl6的质量比,制备不同Pt/Au比的双金属纳米粒子,并进一步研究其对H2O2电化学氧化的催化作用。紫外-可见光谱(Uv-vis)、透射电子显微镜(TEM)、选区电子衍射(SAED)、X射线粉末衍射(XRD)等实验结果表明：Au-Pt双金属纳米粒子为面心立方结构的合金。用循环伏安法对Au-Pt双金属纳米粒子修饰的玻碳电极的电化学性能进行测试,结果表明：Au-Pt双金属纳米粒子对H2O2电化学氧化有一定的催化作用。催化效率随Au-Pt双金属粒子中Pt含量的增加而增加。     

化学还原法制备铂及铂合金催化剂及其性能

采用混合水溶液浸渍,硼氢化钠还原的方法制备了微型直接甲醇燃料电池用电催化剂,包括碳载铂、碳载铂基合金电催化剂.XRD、SEM、EDX测试结果表明催化剂的粒度达纳米级,且分散性好、原子摩尔配比合理.将Pt/C、Pt合金/C分别作为电池的阴极和阳极电催化剂,通过电池的极化曲线和功率密度曲线筛选出最佳的催化剂组成.在室温下,甲醇浓度为2mol/L时,阴极采用30wt%Pt的Pt/C,阳极采用n(Pt)∶n(Ru)∶n(Ir)∶n(Mo) = 2∶1∶2∶3的PtRuIrMo/C电催化剂,其电池的性能最好.     

含石墨烯IrO_2-Ta_2O_5涂层钛阳极性能改进研究

采用热分解的方法制备了不同含量石墨烯(graphene)的IrO_2-Ta_2O_5涂层钛阳极(Ti/IrO_2-Ta_2O_5-G),并运用场发射扫描电子显微镜(FESEM)、能谱仪(EDS)等分析手段和循环伏安(CV)、阳极极化及电化学阻抗谱(EIS)等测试方法对阳极的微观结构和电化学性能进行研究。结果表明:Ti/IrO_2-Ta_2O_5-G阳极表面凹凸不平,裂纹细而小,为析氧反应提供了更多的活性中心,电化学活性表面积增大,析氧电催化活性增强;加有不同量石墨烯的Ti/IrO_2-Ta_2O_5-G阳极的电化学性能有一定差别,其中加入0.4 g·L~(-1)石墨烯阳极的电化学性能提高最明显。     

纳米结构ZrO_2的阳极氧化制备

采用电化学阳极氧化法在Zr-4板表面上制备了一层结构规整的纳米结构ZrO2。考察了阳极氧化电压对纳米结构氧化锆形貌和尺寸的影响。利用扫描电子显微镜(SEM)和X射线衍射(XRD)分析纳米结构的氧化锆的形貌和相组成。结果表明,阳极氧化电压是影响ZrO2纳米结构形貌和尺寸的重要因素,即在5V条件下为枝状结构;10V条件下为花朵状结构;20V条件下为纳米管阵列结构。并讨论了ZrO2纳米结构的形成机制。     

纳米SiO2粒子/镍基复合镀层腐蚀行为

将纳米SiO2粒子通过超声分散引入到化学镀Ni-P合金镀液中,在碳钢基体表面共沉积得到纳米SiO2粒子/镍基复合镀层。通过X射线衍射(XRD)、扫描电镜(SEM)对Ni-P镀层和纳米SiO2粒子/镍基镀层的微观结构形貌进行了分析;采用失重法和电化学方法研究了纳米SiO2粒子/镍基复合镀层在3.5%NaCl溶液中的腐蚀行为。结果表明,纳米SiO2粒子/镍基复合镀层仍是非晶态,纳米SiO2粒子的加入提高了镀层的致密性,提高了镀层的耐腐蚀性能。     

银金修饰TiO2纳米管阵列光阳极的制备及其光伏性质

采用阳极氧化法,以金属钛箔为原料制备了TiO2纳米管阵结构染料敏化纳米晶太阳能电池(DSSC)光阳极,并用电沉积、光沉积和真空蒸发法对其表面分别进行金属Ag和Au修饰。对金属修饰前后的光阳极用扫描电子显微镜(SEM)和X射线衍射分析仪(XRD)表征发现:阳极氧化法制备的TiO2纳米管阵列结构规整有序;经过化学沉积后,其表面均覆盖有一层致密的金属粒子薄膜。测量光电流密度-电压(J-V)曲线和电化学阻抗谱(EIS)发现:相比纯TiO2纳米管阵列,经过Ag修饰后的TiO2阵列其短路电流密度和开路电压最大可以分别提高到前者的4.9和1.7倍,并且其电化学阻抗出现显著降低。研究表明:金属Ag修饰改善了TiO2纳米管之间的连通性,提高了TiO2光阳极中电子的传输效率,并通过等离子共振激发出光电子,同时与TiO2相互作用,使其在可见光区域也能够促进电子-空穴对的分离。     

碳载Pd-Co-Au合金纳米粒子的制备及其电催化性能

采用乙二醇还原法并进一步热处理制备碳载Pd-Co-Au(Pd-Co-Au/C)三元合金纳米电催化剂,通过旋转圆盘和环盘电极等技术评价催化剂对氧气还原反应的电催化活性,并分析氧气还原的机理.结果表明:合成Pd-Co-Au/C催化剂中Pd和Au两相面心立方(fcc)结构共存,且随着热处理温度的提高,对应于Au的衍射峰强度减弱,而Pd衍射峰强度增强:当温度高于800℃时,形成具有Pd单相fcc结构的三元合金纳米催化剂.氧气还原反应的动力学表明:氧气在Pd-Co-Au/C三元合金催化剂上按4e路径还原为水.电化学表征表明,在酸性介质中,经800℃热处理的Pd7Co<<2>Au1/C催化剂对氧气还原的电催化活性最高,接近于商业化Pt/C的性能;而在含甲醇的酸性介质中,Pd-Co-Au/C催化剂电催化氧气还原的活性显著高于Pt/C.因此,Pd-Co-Au/C是一种高抗甲醇的新型氧气还原反应电催化剂.     

Peculiarities of the precipitation of nanosized ε-phase copper particles in ferrite plates of lamellar pearlite

The fine structure of pearlite in alloys with the structure of gray cast iron that contain 1.6 and 10.8 wt% copper has been studied using transmission electron microscopy. Peculiarities of the formation of the nanosized particles of the ε-phase in ferrite lamellae of the pearlite have been determined and their influence on the character of the dislocation structure in the ferrite constituent of the pearlite has been demonstrated. It has been found that the Kurdyumov–Sachs orientation relationship is established between the particles of the ε and α phases. In the investigated cast irons, the formation of nanosized ε-copper particles results in the growth of pearlite hardness by 35 HV and 84 HV, respectively.     

尖晶石型CoAl_2O_4纳米粉体的超声波化学法合成及表征(英文)

在超声波辐射下前躯体法合成了尖晶石型CoAl2O4纳米粉体。超声波辐射硝酸钴、硝酸铝和脲的水溶液制得前躯体。前躯体在1000℃下焙烧6h得到粒径约27nm,比表面积约108m2·g-1的纳米CoAl2O4粉体。纳米CoAl2O4及其前躯体用热重(TG)分析、差示量热扫描(DSC),傅里叶转换红外光谱(FT-IR),X射线衍射仪(XRD),透射电镜(TEM)和比表面测试仪(BET)进行了测试分析。     

具有大比例表面界面原子的纳米SnO2的合成与表征

采用络合沉淀法制备了纳米四方相SnO2颗粒,并对制备机理和颗粒结构和性质进行了实验研究.结果表明,反应过程中由于加入和释放出的有机物在纳米颗粒形核时起到了空间位阻的作用,避免了颗粒的迅速长大和团聚,而且在纳米SnO2形核时造成了缺氧环境,导致沉淀产物配位数不足,表面界面原子在颗粒原子总数中比例较高.XRD和TEM结果显示,纳米SnO2颗粒分布均匀.拉曼散射研究结果表明,10 nm的颗粒只有表面界面原子的贡献,未发现有体相原子的贡献.     

Effect of Rare Earth Sc Addition on Microstructure and Mechanical Properties of an Al-Cu-Mg-Ag Alloy

Al-5.3Cu-0.8Mg-0.6Ag alloys containing 0, 0.1, 0.3 and 0.5 (mass. %) Sc were prepared by ingot metallurgy and thermomechanical treatment. The effect of Sc addition on the precipitation and microstructure of the alloys has been investigated using mechanical testing, optical microscope, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). It has been shown that trace Sc element refines the grains of the casting alloys and the average grain size decreases from 85 μm to 30 μm. Increasi...     

Investigation of the processes of refining of ceramic articles in a plasma flow

Results of investigations of the process of dissipation of polydisperse particles in low-temperature plasma flow with the formation of ultrafine, including nanosized, particles are presented. A special method is proposed that can be used for producing polydisperse powders, including ultrafine and nanosized powders, with spherical particles and the amorphous, crystalline, or amorphous, crystalline structure.     

聚合-热解法制备Co0.2Zn0.2Mn0.6Fe2O4纳米颗粒及其表征

采用聚合-热解法制备了Co0．2Zn0．2Mn0．6Fe2O4磁性纳米颗粒，借助热重分析法（TG）、X射线衍射（XRD）、透射电镜（TEM）和振动样品磁强计（VSM）对产物进行了表征．结果表明，产物具有尖晶石结构，无杂相，粒径分布范围在8-15nm之间．常温下该材料的剩磁强度和矫顽力分别为0．516和2．388kA／m．     

Synthesis of bulk nanostructured aluminum alloy component through vacuum plasma spray technique

The benefits of large-size engineering components with nanocrystalline structure (providing improved strength) are yet to be realized due to processing difficulties and associated grain growth problems. In this work, a free-standing bulk nanocrystalline structure of hypereutectic aluminum alloy (Al–21wt.%Si) has been fabricated through the vacuum plasma spray (VPS) forming technique using micron-size powder feedstock. Optical microscopy, scanning electron microscopy and transmission electron microscopy have been used to investigate the evolution of multi-scale microstructure as the result of rapid solidification in VPS forming process. The characterization implies the presence of nanosized eutectic Al–Si grains (25–100 nm) with uniformly distributed ultrafine primary silicon particles of submicron size. The effect of microstructural evolution on mechanical properties has been studied by tensile testing and microhardness measurement. A considerable improvement in ultimate tensile strength and hardness of the sprayed deposit has been observed in comparison with conventionally cast hypereutectic Al–17wt.%Si alloys.     

Synthesis of ultrafine/nanocrystalline W-(30-50)Cu composite powders and microstructure characteristics of the sintered alloys

Ultrafine/Nanocrystalline W-Cu composite powders with various copper contents (30, 40 and 50 wt.%) have been synthesized by sol-spray drying and a subsequent hydrogen reduction process. The powders were consolidated by direct sintering at temperatures between 1150 and 1260 °C for 90 min. The powder characteristics and sintering behavior, as well as thermal conductivity of the sintered alloys were investigated. The results show that the synthesized powders exist in ultrafine composite particles containing numerous nanosized particles, and the composition distributed very homogeneously. As the copper contents increase, the grain size of the powders decreases. The subsequent sintered parts show nearly full density with the relative density more than 99% at the temperature of 1250 °C. The sintered parts have very fine tungsten grains embedded in a bulk matrix. With increased copper contents, the tungsten grain size decreases and the microstructural homogeneity of the sintered alloys improves further. The thermal conductivity properties, while a little lower than that of the theoretical value, depend on the copper contents.     

Effects of nanosized metallic palladium loading and calcination on characteristics of composite silica

1　INTRODUCTIONThemotivationfortheresearchoncolloidalmet alparticlesstemmedfromtheiruniqueelectro opticalandelectrochemicalproperties[13] .Duringthe pastfew years,aflurryofactivityhasbeendirectedto wardsthepreparationofnanosizedmetallicparticlesduetolargeenhancementinthephysicalpropertiesofnanostructuredcompositescomparedtothebulk[4 6 ] .Therefore ,size dependentchangesinband gapener gy ,excited stateelectronicbehaviorandopticalspec traaregenerateddrasticallyfromthoseknownforthemolecularan…