FeCrAlNbTiRE电热合金相结构研究

用Ｘ射线衍射法和模拟粉晶衍射图的程序ＰＯＷＤ１２，研究了掺稀土的ＦｅＣｒＡｌＮｂＴｉＲＥ电热合金淬火和缓冷状态的相结构，所得结果如下：它们分别是ａ－Ｆｅ型无序固溶体和（Ｆｅ、Ｒｍ）３（Ｃｒ、Ａｌ）有序固溶体，因而前者相结构是体心立方点阵，后者出现超点阵峰，是简单立方点阵，而且后者的晶胞参数和体积分别是前者的２和８倍。     

CuO／CeO_2／γ－Al_2O_3催化剂的结构及氧物种

应用ＸＲＤ、ＥＳＲ及ＸＰＳ方法研究了ＣｕＯ／ＣｅＯ２／γ－Ａｌ２Ｏ３催化剂的体相及表面结构，并对催化剂表面氧物种进行了表征．实验结果表明，ＣｅＯ２使Ｃｕ２＋还原为低价钢离子和增加钢化合物的分散性．催化剂中ＣｅＯ２含量高时，表面有Ｏ２－和Ｏ－物种，而ＣｅＯ２含量低时，只有Ｏ２－物种．     

含氨茂铁异核金属配合物合成和性质研究

Ｐｄ（Ⅱ）、Ｐｔ（Ⅱ）ＤＭＡＦ配合物已合成，并已定结构。本文采用ＭＸ２（Ｍ－Ｎｉ（Ⅱ），Ｃｏ（Ⅱ），Ｚｎ（Ⅱ）、Ｃｕ（Ⅱ）；Ｘ＝Ｃｌ，Ｂｒ，Ｉ）在ＣＨ２Ｃｌ２中和ＤＭＡＦ作用合成［ＭＸ２．２ＤＭＡＦ］型配合物。由ＮｉＣｌ２．２ＤＭＡＦ．Ｃ７Ｈ８晶胞参数推知属于对称链状四配位结构。ＩＲ谱表明，该化合物化学式为ＭＸ２．２ＤＭＡＦ。ＣＶ表明配合物中Ｍ（Ⅱ）和Ｆｅ（Ⅱ）存在。由于金属离子互相影响。Ｅｐ／２     

NOVEL OXIDATION OF HEXABENZYLHEXAAZA－ISOWURTZITANE BY Me_2CHNO_2／CuCl／Py／O_2

ＮＯＶＥＬＯＸＩＤＡＴＩＯＮＯＦＨＥＸＡＢＥＮＺＹＬＨＥＸＡＡＺＡ－ＩＳＯＷＵＲＴＺＩＴＡＮＥＢＹＭｅ_２ＣＨＮＯ_２／ＣｕＣｌ／Ｐｙ／Ｏ_２ＸｉａｏＰｅｉＧＵＡＮ；ＨｏｎｇＹＡＮ；ＪｉａｎＧｕａｎｇＳＵＮ；ＹｏｎｇＺｈｏｎｇＹＵ（ＳｃｈｏｌｏｆＣｈｅ?..     

铈在Fe-28Al合金中的作用

以稀土元素Ｃｅ为微合金化元素，研究了Ｃｅ对Ｆｅ３Ａｌ二元合金（Ｆｅ２８Ａｌ）室温力学性能的影响，采用光学显微镜、扫描电镜、透射电镜、Ｘ射线光电子能谱仪、等离子耦合光谱、Ｘ射线衍射仪以及俄歇能谱仪等现代微观分析手段，探讨了Ｃｅ微合金化对Ｆｅ３Ａｌ合金组织结构和力学性能影响的作用机制。研究结果表明，Ｃｅ的加入改善了合金的室温塑性和强度，并在合金中起到了脱硫、脱氧、改变夹杂物形态、细化晶粒以及表面改性等作用。此外还对富Ｃｅ相颗粒在合金中的形态分布作了分析。     

一氧化碳高效吸附剂CuCl／分子筛

利用自发单层分散原理，将ＣｕＣｌ分散在载体表面制备高效的ＣＯ吸附剂，将ＣｕＣｌ与γ－Ａｌ２Ｏ３，４Ａ，１３Ｘ，ＮａＹ，ＣｕＹ分子筛等高比表在载体混合，在３５０℃焙烧数小时，ＸＲＤ和ＥＸＡＦＳ研究证明ＣｕＣｌ可在载体表面达到原子水平的分散由于Ｃｕ＾＋可与ＣＯ生成配位键。由此可制得对ＣＯ有高吸附容量和选择性的吸附剂，其中ＣｕＣｌ／ＮａＹ和ＣｕＣｌ／Ｃｕ＾＋Ｙ吸附剂的吸附容量在２０℃，ＣＯ分压为６０ｋＰ     

铁钴镍铜锌镉铝在聚乙二醇—硫酸铵—茜素S体系中萃取分离

本文用茜素Ｓ作萃取剂，研究了Ｆｅ，Ｃｏ，Ｎｉ，Ｃｕ，Ｚｎ，Ｃｄ，Ａｌ在聚乙二醇－硫酸铵－茜素Ｓ体系中的非有机溶剂萃取行为。实验结果表明，在ｐＨ５的ＨＡｃ－ＮａＡｃ缓冲溶液中，Ｆｅ，Ａｌ与茜素Ｓ的络合物可被ＰＥＧ相几乎完全萃取，Ｃｕ，Ｎｉ部分被萃取，而Ｃｏ，Ｚｎ，Ｃｄ则不被萃取，从而实现了Ｆｅ与Ｃｏ，Ｚｎ，Ｃｄ及Ａｌ与Ｃｏ，Ｚｎ，Ｃｄ混合离子间的定量分离。     

易潮解化合物AlCl3和FeCl3在载体表面的分散状态及分散量

易潮解化合物ＡｌＣｌ３和ＦｅＣｌ３在载体表面的分散状态及分散量宗越潘晓民段连运＊谢有畅（北京大学物理化学研究所，北京１００８７１）关键词氯化铝，氯化铁，氧化铝，分散状态，分散阈值，Ｘ射线衍射无水ＡｌＣｌ３和无水ＦｅＣｌ３同属Ｌ酸，在酸催化中起着重要的...     

含氮茂铁异核金属配合物的合成和性质研究

Ｐｄ（Ⅱ）、Ｐｔ（Ⅱ）ＤＭＡＦ配合物已合成，并已定结构［１］．本文采用ＭＸ２（Ｍ＝Ｎｉ（Ⅱ），Ｃｏ（Ⅱ），Ｚｎ（Ⅱ），Ｃｕ（Ⅱ）；Ｘ＝Ｃｌ，Ｂｒ，Ⅰ）在ＣＨ２Ｃｌ２中和ＤＭＡＦ作用合成［ＭＸ２·２ＤＭＡＦ］型配合物．由ＮｉＣｌ２·２ＤＭＡＦ·Ｃ７Ｈ８晶胞参数推知属于对称链状四配位结构．ＩＲ谱表明，该化合物化学式为ＭＸ２·２ＤＭＡＦ．ＣＶ表明配合物中Ｍ（Ⅱ）和Ｆｅ（Ⅱ）存在．由于金属离子互相影响，Ｅｐ／２随Ｍ（Ⅱ）性质呈规律性变化．     

CuCl/γ-Al2O3上NO脱除过程研究

设计了一系列的对比实验,利用ＸＲＤ,ＸＰＳ,ＴＰＲ,ＥＸＡＦＳ等技术,系统研究了ＣｕＣｌ／γ－Ａｌ２Ｏ３上的ＮＯ脱除反应过程。结果发现,ＣｕＣｌ／γ－Ａｌ２Ｏ３样品暴露在空气中,表面被部分氧化生成ＣｕＣｌ２及ＣｕＯ等,在高温处理和反应过程中,造成样品表面氯的损失,同时生成更多的ＣｕＯ,因而得新还原处理后测活性时,得到高分散的金属铜,使样品的ＮＯ分解活性提高,但由于ＮＯ对低价铜有很强的氧化作用,ＮＯ     

Ag/Au Alloy LSPR Engineering by Co‐deposition of RF‐Sputtering and RF‐PECVD

Silver‐Gold alloy/diamond like carbon (Ag‐Au/DLC) nanocomposite films were prepared by co‐deposition of RF‐sputtering and RF‐PECVD on glass substrates by using acetylene gas and silver‐gold target. The deposition process was carried out at room temperature in one minute with the variable parameters of initial pressures and RF powers. X‐ray diffraction analysis demonstrated the formation of Ag/Au alloy nanoparticles with a face‐centered cubic (FCC) structure. Localized surface plasmon and optical properties of Ag‐Au alloy nanoparticles were studied by UV‐visible spectrophotometry which showed that increasing RF power and initial pressure cause a redshift in all samples. Moreover, the effect of RF power and initial pressure on the size and shape of nanoparticles were studied by 2D Atomic force microscopy images. Energy dispersive X‐ray spectroscopy revealed the formation of Ag‐Au/DLC nanoparticles and the percentages of C, Ag, Au and O in all samples. The applied method for Ag/Au alloy preparation is the one step and low‐cost method which makes the samples ready for sensing application.     

原位担载型煤直接液化催化剂的表征

 通过原位担载法将铁系催化剂担载于煤表面,考察了催化剂前驱体的相态、配位环境以及在载体表面的分散状态．采用X射线吸收精细结构和X射线衍射法对原位担载型铁系催化剂前驱体进行了表征．结果表明,催化剂前驱体在煤表面以非晶态、高分散的形式存在,其化学组成主要为FeOOH,且催化剂前驱体的分散程度与载体煤的物理化学性质有关．     

XPS and SEM study of calcite bearing rock powders in the case of reactivity measurement with HCl solution

The dissolution of seven natural limestones and calcareous rocks in hydrochloric acid solution was examined to investigate their capability for wet flue gas desulphurisation. All samples were crushed, ground and sieved to a size‐fraction of 150–250 µm. Thereafter they were subjected to a dissolution experiment utilising stepwise titration with hydrochloric acid. The dissolution rates of three calcareous rocks were found to be controlled by reaction kinetics, while the limestones showed mass transfer control. The surface characterisation was implemented before and after dissolution experiments using X‐ray photoelectron spectroscopy and scanning electron microscopy. Additional characterisation was carried out with X‐ray diffraction, X‐ray fluorescence and polarizing microscope. Initial reactivities have been shown to decrease in the order limestone, calcareous rock with high calcium concentration, calcareous rock with low calcium concentration. Coarse grain structure is proposed to decrease the initial reactivity. Copyright © 2011 John Wiley & Sons, Ltd.     

Influences of acid and heat treatments on the structure and water vapor adsorption property of natural zeolite

Natural zeolite was first acid treated and then heat treated. The influences of acid and heat treatments on the structure and water vapor adsorption property of natural zeolite were investigated. X‐ray photoelectron spectroscopy (XPS), X‐ray diffraction (XRD), thermogravimetric analysis (TG), and Brunauer‐Emmett‐Teller (BET) surface areas were employed to investigate the structure changes of the zeolite samples. Water vapor adsorption property of the samples was investigated in order to determine wettability of the samples. The results showed that nitric acid treatment could remove Al from the structure, decrease relative crystallinity, and significantly increase specific surface area of the zeolite samples. Heat treatment could change or even destroy the structure, effectively remove water molecules from the surface/structure, and decrease the specific surface area of the zeolite samples. Water vapor adsorptions on the acid‐treated zeolite samples were significantly lower than that for the zeolite sample, and the adsorptions further reduced for the heat‐treated zeolite samples. The increase of Si/Al ratio, decreases of silanol groups, and specific surface area of the samples were major reasons related to the reductions of water vapor adsorptions on the zeolite samples.     

p型Si上Ni—Pd薄膜的电化学制备及其表征

采用控电位沉积方式在ｐ型Ｓｉ上制备了Ｎｉ－Ｐｄ合金薄膜；考察了合金的阴极沉积和阳极溶出行为；研究了极化方式对膜组成、厚度、结构及形貌的影响．结果表明，在沉积初期，膜主要以层状方式生长，当膜增厚或阴极极化增强时，则以岛状形式生长．Ｘ射线衍射测试表明，Ｎｉ－Ｐｄ合金呈面心立方结构，其晶面间距随合金组成不同而变化．     

氮自掺杂暴露（001）晶面TiO2微米片的可见光光催化CO2还原性能增强

化石能源的使用可产生大量CO2,带来严重的温室效应。光催化CO2还原生产太阳燃料技术既有望缓解温室效应,又可以将低能量密度的太阳能转化为高能量密度的化学能储存起来方便使用。高效光催化材料的开发是发展光催化技术的关键。迄今,在已开发的所有半导体光催化材料中, TiO2仍是广泛研究的明星材料。在实际使用中, TiO2的光催化效率仍受限于其极弱的可见光利用率和较高的电子-空穴复合几率。近年来,越来越多的研究表明TiO2的结构与形貌特征极大地影响其光催化效率。尤其, TiO2的外露晶面设计与晶面效应研究引起了广泛关注。由于具有较高表面能和较多表面不饱和键,起初大多数理论和实验研究认为锐钛矿TiO2(001)晶面是光催化活性晶面。后来,越来越多研究表明并非锐钛矿TiO2(001)晶面的暴露比例越高其光催化活性就越高。最近,我们发现锐钛矿TiO2(001)晶面与(101)晶面在调控光催化CO2还原性能上具有良好的协同效应。密度泛函理论计算表明,锐钛矿TiO2的(001)晶面与(101)晶面的能带结构有差异,(001)晶面的导带位置相对于(101)晶面而言较高,而(101)晶面的价带位置相对于(001)晶面而言较低。基于此我们提出,具有合适比例的锐钛矿TiO2的(001)晶面与(101)晶面的交界处可以形成最佳的表面异质结或晶面异质结。表面异质结的形成导致光生电子倾向于向(101)扩散,光生空穴倾向于向(001)扩散,从而促进光生电子-空穴分离,降低光生电子-空穴复合几率。在此工作基础上,我们直接以氮化钛为原料,氢氟酸为添加剂,通过简单的水热反应一步合成了氮自掺杂的TiO2微米片。利用X射线粉末衍射、扫描电镜、X射线光电子能谱、紫外-可见漫反射光谱、氮气吸附-脱附以及电化学阻抗谱等方法手段对所制备的光催化剂进行了基本结构与理化性质表征分析,并研究了其可见光光催化CO2还原性能。电镜照片结果表明,我们所制备的氮自掺杂锐钛矿TiO2微米片的(001)晶面与(101)晶面比例分别为65%和35%。基于我们前期研究结果, TiO2微米片的(001)晶面与(101)晶面可以形成表面异质结,具有良好的电荷分离效率,这也得到了电化学阻抗谱研究结果的证明。同时,由于N的原位掺杂,所制备的TiO2微米片具有优异的可见光捕获能力。由于可见光利用效率增强与光生电子-空穴分离效率提高这两方面的综合作用,所制备的氮自掺杂TiO2微米片具有非常好的可见光光催化CO2还原制甲醇性能,比商用P25及氮掺杂TiO2纳米粒子等参考样品的可见光光催化性能更优异。研究表明,通过原位自掺杂方法与晶面设计方法相结合,可以同时改善TiO2的可见光利用效率和光生电子-空穴分离效率,优化TiO2的可见光光催化性能,这也为后续开发新型高效光催化材料提供了新思路。     

Solid‐Solution Alloy Nanoparticles of the Immiscible Iridium–Copper System with a Wide Composition Range for Enhanced Electrocatalytic Applications

For the first time, we synthesize solid‐solution alloy nanoparticles of Ir and Cu with a size of ca. 2 nm, despite Ir and Cu being immiscible in the bulk up to their melting over the whole composition range. We performed a systematic characterization on the nature of the Ir_xCu_1?x solid‐solution alloys using powder X‐ray diffraction, scanning transmission electron microscopy coupled with energy‐dispersive X‐ray spectroscopy and X‐ray photoelectron spectroscopy. The results showed that the Ir_xCu_1?x alloys had a face‐centered‐cubic structure; charge transfer from Cu to Ir occurred in the alloy nanoparticles, as the core‐level Ir 4f peaks shifted to lower energy region with the increase in Cu content. Furthermore, we observed that the alloying of Ir with Cu enhanced both the electrocatalytic oxygen evolution and oxygen reduction reactions. The enhanced activities could be attributed to the electronic interaction between Ir and Cu arising from the alloying effect at atomic‐level.     

In situ TREXS Observation of Surface Reduction Reaction of NiO Film with ∼2 nm Surface Sensitivity

X‐ray absorption fine structure (XAFS) spectroscopy is one of the most widely used methods at synchrotron radiation facilities. XAFS gives us information on chemical states and local structures. Fundamentally, XAFS is bulk sensitive, not surface sensitive. If a surface sensitive XAFS method was available, surface chemical reactions can be observed under realistic conditions. Here, we report the development and present status of a type of surface sensitive x‐ray spectroscopy, which is named total reflection x‐ray spectroscopy, TREXS.     

Influence of nitrogen partial pressure on the microstructure and morphological properties of sputtered RuN coatings

In this work, the production of RuN thin films using the reactive direct current magnetron sputtering technique is presented. Samples were grown with varying Ar/N₂ ratio with values of 60/40, 80/20, 85/15, 90/10, 95/5, and 100/0. X‐ray photoelectron spectroscopy was employed to determine the presence of RuN before and after a sputtering etching process. According to the high‐resolution of N1s spectra, 3 peaks were identified at 397.4 ± 0.3 eV, 398.3 ± 0.3 eV, and 398.8 ± 0.3 eV binding energies, corresponding to hybridizations of nitrogen with transition metals, oxynitrides, and oxycarbides. X‐ray diffraction analyses were performed, showing the coexistence of the RuN face‐centered cubic and Ru hexagonal compact packed phases. After the etching process, the samples grown at nitrogen flow rates greater than 15% continued to show the RuN face‐centered cubic phase. Atomic force microscope analyses showed that as the nitrogen concentration increased, the grain size and roughness also tended to increase.     

Surface composition of PdCuAu ternary alloys: a combined LEIS and XPS study

PdCuAu ternary alloy samples with different composition were synthesized on top of ZrO₂‐modified porous stainless steel disks by the sequential electroless deposition technique. The structure, morphology and bulk composition of the samples were characterized by X‐ray diffraction (XRD), scanning electron microscopy and energy dispersive X‐ray spectroscopy (EDX). Complete alloy formation with a pure fcc phase for the Pd₇₁Cu₂₆Au₃, Pd₇₀Cu₂₅Au₅ and Pd₆₇Cu₂₄Au₉ samples and a bcc structure for the Pd₆₂Cu₃₆Au₂ and Pd₆₀Cu₃₇Au₃ samples were obtained upon annealing at 500 °C for 120 h as revealed by XRD. A combination of low‐energy ion scattering (LEIS) and X‐ray photoelectron spectroscopy (XPS) was used to investigate the surface properties of the PdCuAu alloys. XPS results confirmed alloy formation under the annealing conditions. XPS analysis also revealed that the near‐surface regions of the alloys became enriched in Pd with respect to the bulk composition determined by EDX. In contrast, LEIS and angle‐resolved XPS analyses showed that the top‐most surface layers in all samples were copper‐rich compared with the bulk composition. This high Cu surface concentration could impart resistance to bulk sulfide formation to the PdCuAu alloy membranes. Copyright © 2015 John Wiley & Sons, Ltd.