添加ZrO2的Pd/Al2O3催化剂及其催化蒽醌加氢性能

以四氯合钯（II）酸（H2PdCl4）为前体,活性氧化铝（Al2O3）为载体,硝酸锆（Zr（NO3）4）为添加组分,采用不同方式的分步浸渍法制备了添加ZrO2的Pd/Al2O3催化剂。考察了制备方法和反应条件对催化剂蒽醌加氢催化性能的影响,发现催化剂活性与制备方法有关。当对添加锆的载体进行适当焙烧,控制Pd负载量为0.3%,还原温度低于300℃时,催化剂的蒽醌加氢活性较高,与未添加ZrO2的催化剂相比提高了约20%。X射线衍射（XRD）、氮气物理吸附（BET）、透射电镜（TEM）、X光电子能谱（XPS）和程序升温还原（TPR）等表征对催化剂物相结构、比表面积、表面形貌及组分间相互作用的分析表明,ZrO2的掺杂提高了载体Al2O3的高温稳定性,改善了催化剂中活性组分Pd与载体间的相互作用,促进了Pd在载体表面的分散,从而提高了催化活性。     

Na2O-MgO-Al2O3-SiO2建筑装饰微晶玻璃的研究

利用浇铸法制备了MgO-Al2O3-SiO2微晶玻璃。采用示差扫描量热法(DSC)、X射线衍射(XRD)、扫描电子显微镜(SEM)等分析方法,研究NMAS微晶玻璃玻璃组成中Al2O3/SiO2对微晶玻璃的析晶和性能的影响。结果表明:玻璃中析出的主晶相为镁橄榄石。随Al2O3/SiO2的减小,镁橄榄石的衍射峰强度逐渐减弱,次晶相为a-堇青石。C3、C4中还有很少量-6-1的顽辉石相。微晶玻璃热膨胀系数逐渐升高,抗折强度和硬度逐渐减小。C1在600℃时的热膨胀系数为7.01×10K,抗折强度为115MPa,硬度达为8.0GPa。     

BaO-Al2O3-B2O3-SiO2系微晶玻璃低温共烧陶瓷研究

采用烧结法制备了BaO-Al2O3-B2O3-SiO2系微晶玻璃低温共烧陶瓷。通过差热分析仪、影像式烧结点试验仪、X射线衍射仪等方法研究了玻璃组成以及烧结制度对微晶玻璃结构和性能的影响。结果表明:随着B2O3替代Al2O3量的增加,玻璃转变温度和烧结温度逐渐降低,析晶能力增强,有利于重硅酸钡晶体的析出,但不利于钡长石晶体的析出。烧结制度对析出晶体的种类和数量有很大影响。在850℃烧结2 h,微晶玻璃低温共烧陶瓷的气孔率低于1%,热膨胀系数在(7.05～12.78)×10-6/℃之间变化。     

Al2O3-ZrO2负载Ni2P催化剂加氢脱硫脱氮活性

采用浸渍-沉淀法制备Al2O3-ZrO2复合氧化物,通过程序升温还原法制备Ni2P/Al2O3-ZrO2催化剂。运用X射线衍射、N2吸附-脱附、X射线光电子能谱技术对载体和催化剂进行表征,并以噻吩加氢脱硫、吡啶加氢脱氮反应为探针考察复合氧化物对Ni2P催化剂加氢活性的影响。结果表明,在Al2O3表面引入少量ZrO2,既保持了γ-Al2O3大比表面积的结构优势,又减少了P或Ni与Al2O3表面的接触,促进Ni2P的形成。载体中ZrO2质量分数20%的Ni2P/Al2O3-ZrO2催化剂活性最高,载体焙烧温度过高会导致催化剂活性下降。     

MoO3掺杂对高纯Zr0.84Y0.16O1.92体系结构和电性能的影响

采用溶胶-凝胶法合成高纯(SiO2<50 mg/kg)Zr0.84Y0.16O1.92+x MoO3(0.00≤x≤0.07)固溶体,研究MoO3的掺杂量对Zr0.84Y0.16 O1.92体系结构和电性能的影响。通过X射线衍射(XRD)和场发射扫描电子显微镜(FE-SEM)对材料进行表征,交流阻抗谱(AC)测试材料的电性能。结果表明,掺入MoO3后,体系仍保持立方莹石型结构;MoO3掺杂于Zr0.84Y0.16O1.92固体电解质的最佳掺量为0.05%;MoO3具有降低体系烧结温度、促进晶粒生长和提高体系致密度的作用,掺入MoO3的Zr0.84Y0.16O1.92体系晶界电导率和总电导率提高。     

第二金属对Ni/Al2O3·SiO2催化重整制氢的影响

本文以尿素作为沉淀剂采用沉积-沉降法制备出NiM/Al2O3.SiO2（M=La,Co,Zr和Y）催化剂。研究第二金属La,Co,Zr和Y的添加对Ni/Al2O3.SiO2催化剂上乙醇水蒸气重整制氢性能的影响,结果表明：Co、La或Y能有效的提高Ni/Al2O3.SiO2催化剂的性能。TPR得出：添加La、Y或Zr能促使活性组分分散到载体中。XPS得出：La,Co的添加能极大地提高还原后催化剂表面单质Ni的含量。     

添加B2O3对Y掺杂BaZrO3烧结性及电导率的影响

研究了加入不同量氧化硼（B2O3）对 Y 掺杂 BaZrO3（BaY0.1Zr0.9O2.95）质子导体烧结性及电导率的影响。研究表明：加入适量 B2O3（质量分数为0.5%～0.75%）可以使 Y 掺杂 BaZrO3的烧结温度降低到 1500 ℃,保温时间缩短到 4～6h,相对密度可达 95%左右,远大于不加 B2O3试样的。与未掺入 B2O3的 Y 掺杂 BaZrO3试样相比,该体系材料的电导率没有明显降低。过量 B2O3（1.0%）的加入将使其以第二相形式存在于烧结体中,从而降低材料的电导率。     

铜改性镍基催化剂制备及其催化联苯加氢性能

采用共浸渍法制备了一系列Cu改性的Ni基催化剂(x Ni-y Cu/Al2O3,x,y分别为Ni和Cu的含量,以Al2O3的质量为基准,下同),用于联苯催化加氢制备环己基苯(CHB)。通过X射线粉末衍射(XRD)、BET、XPS及透射电子显微镜(TEM)对催化剂进行了表征。考察了催化剂50%Ni-10%Cu/Al2O3用量、H2压力、反应温度对联苯加氢制备环己基苯的影响。结果表明:Cu晶粒在催化剂表面优先析出,使表面Ni活性中心稀释、Ni晶粒尺寸变小,从而提高了CHB的选择性。当联苯为1.5 g,m(50%Ni-10%Cu/Al2O3)=0.5 g,以环己烷为溶剂、p(H2)=2.2 MPa、200℃反应4 h时,联苯的转化率可达94.7%,CHB的选择性达到99.8%。催化剂50%Ni-10%Cu/Al2O3循环使用9次后,联苯的转化率稍有降低,CHB的选择性几乎不变。     

镍包覆Al2O3纳米颗粒对氧化铝陶瓷与铝之间润湿性的影响

采用Ni(NO3)2·6H2O前驱体液相包覆技术对纳米Al2O3颗粒进行金属化处理,经过干燥、加热分解和高温氢气还原处理后,前驱体完全转化为金属Ni晶体,从而获得镍涂覆的Al2O3颗粒。X射线衍射、透射电子显微镜和能谱分析结果表明:金属镍包覆在纳米Al2O3颗粒表面。包覆的纳米Al2O3颗粒经过热压烧结制备的陶瓷体与金属铝之间的润湿角为72.5°,明显改善了陶瓷与金属之间的润湿性。     

Al2O3/Cu70Ti25Zr5/Nb界面结构及强度

本研究选用Cu70Ti25Zr5活性钎料钎焊Al2O3/Nb,通过对Al2O3/Cu70Ti25Zr5/Nb界面结构及接头性能研究,旨在进一步揭示Al2O3/含Ti活性钎料间界面反应机制,并为指导工程应用提供最佳工艺参数。借助扫描电镜,能谱,X射线衍射探讨了Al2O3/Cu70Ti25Zr5/Nb钎焊接头界面结构,并采用拉剪试验评价了接头强度,研究结果表明,时间0.6ks,温度小于1223K,界面产生了3种新相：Cu2Ti4O,Ti0.5Zr0.5O0.19,CuTi,界面结构为Al2O3/Cu2Ti4O Ti0.5Zr0.5O0.19/CuTi/Cu固溶体＋CuTi,温度大于1293K,界面产生了Cu2Ti4O,Ti,CuTi3种新相,界面结构为Al2O3/Cu2Ti4O/Ti固溶体／CuTi/Cu固溶体＋CuTi,在1293K,0.6ks条件下,接头剪切强度最高达到162MPa,温度大于或小于1293K,强度下降。     

NiFe2O4-M金属陶瓷惰性阳极成分设计的热力学分析

NiFe2O4-M金属陶瓷惰性阳极由氧化物陶瓷相和金属相组成.多数美国专利认为Fe,Ni,Cu,Co,Ti,Cr,Mn,Al,Pd,Ag,V,Zr,Y,La,Ta,Nb,Sc,Hf,Ca,Sn,Zn等21种金属均适合作为上述阳极的金属相成分.但文中的热力学详细分析计算结果表明:在上述前8种金属中,仅有Cu,Ni 2种适...     

Structural characterization of iron-based bulk metallic glass alloys produced by centrifugal casting

In this study bulk metallic glass alloys in the Fe-Zr-B-M (M=Al, Co, Cu, Mo, Ni, W) systemwere produced by using a centrifugal casting method. The thickness ofthe samples that could be produced with an almost completely amorphousstructure was found to be as high as ～2 mm for alloy Fe60Co8Zr10Mo5W2B15. Alloying element additions or replacements have resulted in a considerable effect on glass-forming ability. Among others, Al and Cu were found to have the most deteriorative effects. The ternary alloy Fe70Zr10B20, from which bulk metallic glass alloys can be formed by cleverly implementing several alloying elements, was seen to have a different phase transformation behavior when compared to alloy Fe60Co8Zr10Mo5W2B15. For the latter alloy, the phase transformation process and microstructure evolution were found to be extremely sensitive to variation of the cooling rate.     

化学沉淀-水热法合成高矫顽力碳纳米管磁性复合材料

采用化学沉淀-水热法成功的合成了一种新颖的Ni0.75Zn0.25Fe2O4纳米晶包覆多壁碳纳米管(Ni0.75Zn0.25Fe2O4-CNTs)磁性复合材料.采用透射电镜、X射线衍射、红外光谱和振动样品磁强计等方法对制备的样品进行了表征.透射电镜结果表明Ni0.75Zn0.25Fe2O4纳米晶包覆在碳纳米管表面,纳米晶的大小为8～15 nm.X射线衍射结果表明:200℃是制备纳米Ni0.75Zn0.25Fe2O4包覆碳纳米管复合材料较好的反应条件,比合成单相Ni0.75Zn0.25Fe2O4纳米晶的温度要低.磁性复合材料中Ni0.75Zn0.25Fe2O4晶体的大小约为16.0nm.红外结果表明NiZn的特征峰在590cm-1和414cm-1处.磁滞回线结果表明室温下复合材料具有较高的矫顽力(Hc=27 244.3 kA/m).     

高分散纳米Y型分子筛负载Ni_2P催化剂的制备及其加氢脱硫性能

以无模板剂法合成的纳米Y型分子筛(35 nm左右)为载体,采用低温还原法制备了高分散Ni_2P/NY催化剂,同时制备了普通Y型分子筛担载的Ni_2P/Y催化剂作为对比。采用X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)和X射线光电子能谱(XPS)等手段对载体和催化剂进行了表征,并在固定床反应器中考察了不同催化剂对4,6-二甲基二苯并噻吩(4,6-DMDBT)的加氢脱硫反应性能。结果表明,该催化剂的高活性来自纳米Y型分子筛上Ni_2P分散度的提高和高活性中心的暴露。在反应温度为340℃,反应压力为3.0 MPa的条件下,以Ni_2P/NY为催化剂,4,6-DMDBT的转化率达到了96.0%,高于CoMoS/Al_2O_3商业催化剂(77.2%)和Ni_2P/Y催化剂(67.0%)。     

Oxidation Behavior of Silver- and Copper-Based Brazing Filler Metals for Silicon Nitride/Metal Joints

The oxidation behavior of reactive-element-containing brazing filler metals at 600°C was studied. Weight-gain measurements coupled with scanning electron microscopy and energy dispersive X-ray analysis indicated the formation of a nonprotective oxide on the following three ternary alloys: (i) Cu-80%, Sn-10%, Ti-10%; (ii) Ag–Cu eutectic + 5% Ti; and (iii) Ag–Cu eutectic + 5% Zr. Additions of Ni and Si to these alloys failed to reduce spallation. However, a protective oxide was formed by adding Al. The resultant quaternary alloys possessed excellent flow properties on silicon nitride.     

Carbon Fiber-reinforced (YMAS) Glass-Ceramic Matrix Composites. II. Structural Changes in the Matrix with Temperature

With the overall aim to study a specific family of carbon-reinforced glass-ceramic matrix composites, the structural and textural changes occurring within a glass belonging to the Mg–Al–Si–Y–O chemical system were investigated. Investigation techniques were mainly transmission electron microscopy, but also scanning electron microscopy, polarized light optical microscopy, X-ray diffraction, and thermal analysis. Some differences between the carbon (fiber)-containing material and the carbon-free material are revealed, mainly through local oxygen-depletions due to a reduction effect by carbon. Mainly, the way that the various phases allowed by the starting stoichiometry crystallize during an increasing heat-treatment is observed, i.e. magnesium aluminum silicate as indialite, yttrium silicate, magnesium aluminum oxide as spinel, in addition to corundum. Phases transformations, crystallized phase morphologies, and textural relationships between phases are among the features described.     

The preparation and properties of zirconia-doped Y–Si–Al–O–N oxynitride glasses and glass-ceramics

Two series (N-9 and N-18 series) of zirconia-doped Y–Si–Al–O–N oxynitride glasses and glass-ceramics were designed. Nominal compositions of the glass samples in equivalent percent (eq%) are xZr: (24–0.25x)Y: (15–0.25x)Al: (61–0.5x)Si: 91O: 9 N and xZr: (24–0.25x)Y: (15–0.25x)Al: (61–0.5x)Si: 82O: 18 N (x=0, 2, 4, 6), respectively. The obtained samples were characterized by differential thermal analysis (DTA), X-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). Densities, Vickers hardness, fracture toughness, glass transition temperature, and thermal expansion coefficient data were established for each sample. Effect of Zr and N content on glass network structure, thermal and mechanical properties was investigated. It was found that the addition of zirconia is effective in preparing Y–Si–Al–O–N oxynitride glasses with lower glass transition temperature and higher hardness.     

Effect of Composition on Crystallization of Y/Yb–Si–Al–O–N B-Phase Glasses

The effect of a partial or full replacement of yttrium by ytterbium on the crystallization of an oxynitride B-phase parent glass with composition (e/o) 35Y/Yb:45Si:20Al:83O:17N has been investigated by thermal analysis, X-ray diffractometry and analytical transmission electron microscopy. Single B-phase formation was extended to higher temperatures by low ytterbium:yttrium ratios, while a full replacement resulted in a two-phase B- and J-phase glass–ceramic. The B-phase crystals took up a substantial range of composition that was dependent on the substitution level, and yttrium/ytterbium was always clearly anti-correlated with silicon. Some aluminum was accommodated in the dendritic J-phase crystals, and their yttrium/ytterbium content varied between 64 and 79 cation%.     

A study of the oxidation behavior of CrN and CrZrN ceramic thin films prepared in a magnetron sputtering system

CrN and CrZrN ceramic thin films were produced by a planar type reactive sputtering system on glass and stainless steel substrates. We investigated oxidation resistance of CrN and CrZrN ceramic thin films with different Zr contents. The structure of the films at different thermal-annealing temperatures was investigated by X-ray diffraction (XRD), atomic force microscopy (AFM) and scanning electron microscopy (SEM). The mechanical properties of the films at different thermal-annealing temperatures were measured by nano-indentation. The results of this study showed that the addition of few amount of Zr (0.4 at%), can improve thermal stability of CrZrN ceramic thin film and increase the oxidation temperature of the film from 600 °C to 800 °C. The relatively good oxidation resistance (800 °C) and high hardness of the film with the lowest Zr content, indicates that this film is a good candidate for high temperature applications.     

溶剂热法合成YAG：Ce粉体及其表征

本文以Al（NO3）3·9H2O、Ce（NO3）3·6H2O和Y2O3为原料,碳酸氢铵为沉淀剂制备反应前驱体,乙二胺作为反应介质,采用溶剂热法在230℃下保温10h合成了YAG：Ce粉体。利用X射线衍射（XRD）、透射电子显微镜（TEM）和红外光谱分析（FT～IR）等测试手段,对所制备样品的结构和形貌进行了表征。