活化天然矿石选择性还原二氧化碳为无定形碳

Natural magnetite formed by the isomorphism substitutions of transition metals, including Fe, Ti, Co, etc., was activated by mechanical grinding followed by H₂ reduction. The temperature-programmed reduction of hydrogen (H₂-TPR) and temperature-programmed surface reaction of carbon dioxide (CO₂-TPSR) were carried out to investigate the processes of oxygen loss and CO₂ reduction. The samples were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and energy-dispersive X-ray spectroscopy (EDS). The results showed that the stability of spinel phases and oxygen-deficient degree significantly increased after natural magnetite was mechanically milled and reduced in H₂ atmosphere. Meanwhile, the activity and selectivity of CO₂ reduction into carbon were enhanced. The deposited carbon on the activated natural magnetite was confirmed as amorphous. The amount of carbon after CO₂ reduction at 300°C for 90 min over the activated natural magnetite was 2.87wt% higher than that over the natural magnetite.     

Atomic model of liquid pure Fe

Using a θ-θ X-ray diffractometer, the liquid structure of pure Fe was investigated and the diffraction intensity, structure factor, pair distribution function as well as the coordination number and atomic distance were obtained. The experimental results showed that there was also a pre-peak on the curve of the structure factor of liquid pure Fe. The pre-peak is a mark of medium-range order in melts. According to the characteristics of pre-peak, an atomic model of liquid pure Fe is constructed, namely, the structure of liquid pure Fe is a combination of clusters consisting of bcc cells with shared vertexes and other atoms with random dense atom distribution.     

Fe3O4@SiO2磁性纳米粒子的制备及表征

用多元醇还原法制备出平均粒径为6.0 nm的Fe3O4磁性纳米粒子,并用盐酸溶液(1 mol/L)对其进行酸化处理,然后利用反相微乳液法,在Op-10/正丁醇/环己烷/浓氨水反相微乳体系中制备出Fe3O4@SiO2磁性纳米复合粒子.利用X射线衍射(XRD)仪,透射电子显微镜(TEM),傅立叶-红外光谱仪(FT-IR)和...     

用于散热器的冷轧钢板耐蚀性

利用化学浸泡及电化学方法研究了４种钢制散热器材质在不同含氧量和氯离子浓度下的腐蚀速度及耐蚀性，并用Ｘ射线衍射对锈蚀物进行了结构分析。实验结果表明，钢材腐蚀速度主要取决于供热水系统中的溶氧量。在脱氧条件下则形成Ｆｅ３Ｏ４保护膜，此时氯离子将加速材料的腐蚀。腐蚀极化电阻则随残余应力的增加而下降。     

硅源加入方式对Fe3O4/SiO2核壳结构制备的影响及磁性能研究

表面包覆惰性层是解决四氧化三铁(Fe3O4)粒子团聚、易氧化、亲水性差等问题的一种有效方法,但惰性层的引入一般会导致包覆后样品磁性能下降,从而限制了Fe3O4的应用.以正硅酸乙酯(TEOS)和氨水为原料,制备了具有良好磁响应性的Fe3O4/SiO2核壳结构.样品的结构、形貌、尺寸和表面吸附官能团采用X-ray粉末衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)和红外光谱(FTIR)等测试手段进行了表征.研究发现,TEOS加入方式影响SiO2层生长过程,从而影响包覆的均匀程度.Fe3O4/SiO2核壳结构表现出顺磁性和良好的磁响应性(52emu/g).     

金属掺杂TiO2粉体的光催化性能研究

采用溶胶凝胶法制备了TiO2和掺杂Ag+,Zn 2+ ,Cu 2+ ,Fe 3+ 和Eu 3+ 的TiO2纳米粉体.用XRD, SEM、及EDS对它们进行了表征,通过表征说明TiO2的晶型为锐钛矿,同时也表明金属离子成功的掺杂到TiO2晶型中.通过对罗丹明B的降解,研究了光催化剂的性能,结果表明:Ag+掺杂的TiO2纳米粉体具有较高的光催化活性.     

Crystalline ribonuclease A loses function below the dynamical transition at 220 K.

When the dynamic properties of many different proteins are plotted as a function of temperature, biphasic behaviour is observed, with a broad transition centred around 220 K. Atomic mean-square displacements from X-ray crystallography and M?ssbauer scattering show this behaviour, as do electron transfer rates and dynamic information from inelastic neutron scattering. Molecular dynamics simulations over a range of temperatures also exhibit a transition at about 220 K: high-temperature atomic fluctuations are dominated by anharmonic collective motions of bonded and nonbonded groups of atoms, but below 220 K the predominant dynamic behaviour is harmonic vibration of individual atoms. Here we show by high-resolution X-ray diffraction that crystalline ribonuclease A does not bind substrate or inhibitor at 212 K but will bind either rapidly at 228 K. Once bound at the higher temperature, inhibitor cannot be washed off after the enzyme is cooled to below the transition temperature. These results suggest that enzyme flexibility is required for catalytic function.     

低温高效催化降解刚果红染料的Fe/CeO2催化剂

有机染料废水成为目前世界公认的主要工业污染源之一,对有机染料的降解越来越引起人们的重视.采用溶胶-凝胶法(sol-gel)和浸渍法制备掺杂Fe的催化剂Fe/CeO2,以X-射线衍射(XRD)和N2物理吸附-脱附对催化剂的结构进行了表征,并对其催化降解有机染料刚果红的性能进行了研究.结果表明,在CeO2中添加过渡金属Fe未改变CeO2晶相结构,且Fe物种在CeO2上处于高分散状态.采用催化湿式过氧化氢氧化法(CWPO)处理10 mg/L偶氮染料刚果红,在低温(5~35℃)范围内,质量分数为2.0%Fe/CeO2催化剂均能表现出高的催化活性.室温25℃时,当催化剂和氧化剂(质量分数为30%H2O2)投加量分别为0.05 g和0.02 mol/L,处理40 min后刚果红降解率可达96%.同时,催化剂重复性实验结果表明催化剂具有良好的稳定性.     

铋系超导体的57Fe穆斯堡尔谱效应

对铋系超导体的正常态和超导态之间的转换进行了与温度相关的穆斯堡尔谱、X－射线衍射、磁化系数ac和电阻率的测量。铋系超导体的穆斯堡尔谱测量显示出两个通常的四极劈裂峰值，表明材料的组成成分是2223相。^57Fe占位的讨论采用点电荷模型。与温度相关的^57Fe穆斯堡尔谱和X－射线衍射研究晶格振动的动力学信息都是从77K到室温的范围。实验结果表明在120K和200K附近时，Cu-O层中出现了晶格软化。在Tc以上温度出现晶格软化是超导转变的先驱效应。     

Imaging ultrafast molecular dynamics with laser-induced electron diffraction

Establishing the structure of molecules and solids has always had an essential role in physics, chemistry and biology. The methods of choice are X-ray and electron diffraction, which are routinely used to determine atomic positions with sub-?ngstr?m spatial resolution. Although both methods are currently limited to probing dynamics on timescales longer than a picosecond, the recent development of femtosecond sources of X-ray pulses and electron beams suggests that they might soon be capable of taking ultrafast snapshots of biological molecules and condensed-phase systems undergoing structural changes. The past decade has also witnessed the emergence of an alternative imaging approach based on laser-ionized bursts of coherent electron wave packets that self-interrogate the parent molecular structure. Here we show that this phenomenon can indeed be exploited for laser-induced electron diffraction (LIED), to image molecular structures with sub-?ngstr?m precision and exposure times of a few femtoseconds. We apply the method to oxygen and nitrogen molecules, which on strong-field ionization at three mid-infrared wavelengths (1.7, 2.0 and 2.3?μm) emit photoelectrons with a momentum distribution from which we extract diffraction patterns. The long wavelength is essential for achieving atomic-scale spatial resolution, and the wavelength variation is equivalent to taking snapshots at different times. We show that the method has the sensitivity to measure a 0.1?? displacement in the oxygen bond length occurring in a time interval of ～5?fs, which establishes LIED as a promising approach for the imaging of gas-phase molecules with unprecedented spatio-temporal resolution.     

Quadrupole transitions revealed by Borrmann spectroscopy

The Borrmann effect-a dramatic increase in transparency to X-ray beams-is observed when X-rays satisfying Bragg's law diffract through a perfect crystal. The minimization of absorption seen in the Borrmann effect has been explained by noting that the electric field of the X-ray beam approaches zero amplitude at the crystal planes, thus avoiding the atoms. Here we show experimentally that under conditions of absorption suppression, the weaker electric quadrupole absorption transitions are effectively enhanced to such a degree that they can dominate the absorption spectrum. This effect can be exploited as an atomic spectroscopy technique; we show that quadrupole transitions give rise to additional structure at the L(1), L(2) and L(3) absorption edges of gadolinium in gadolinium gallium garnet, which mark the onset of excitations from 2s, 2p(1/2) and 2p(3/2) atomic core levels, respectively. Although the Borrmann effect served to underpin the development of the theory of X-ray diffraction, this is potentially the most important experimental application of the phenomenon since its first observation seven decades ago. Identifying quadrupole features in X-ray absorption spectroscopy is central to the interpretation of 'pre-edge' spectra, which are often taken to be indicators of local symmetry, valence and atomic environment. Quadrupolar absorption isolates states of different symmetries to that of the dominant dipole spectrum, and typically reveals orbitals that dominate the electronic ground-state properties of lanthanides and 3d transition metals, including magnetism. Results from our Borrmann spectroscopy technique feed into contemporary discussions regarding resonant X-ray diffraction and the nature of pre-edge lines identified by inelastic X-ray scattering. Furthermore, because the Borrmann effect has been observed in photonic materials, it seems likely that the quadrupole enhancement reported here will play an important role in modern optics.     

溶剂热法制备纳米Fe3O4粉体

通过溶剂热法,以FeOOH作为前驱体,以油酸作为表面活性剂,以十八烯为溶剂,制备了纳米Fe3O4颗粒,研究了油酸和FeCl3用量、反应时间对纳米Fe3O4粒子的大小以及分散性的影响.结果显示,FeCl3用量的增加和反应时间的延长均可使Fe3O4粒子粒径增大,油酸用量的增加会导致Fe3O4粒子粒径先减小再增大.利用XRD、TEM等手段对所制备颗粒的结构、形貌进行了表征,结果表明,所制备的纳米Fe3O4粒子属于反尖晶石结构.FeCl3用量为0.003mol,油酸用量为13.5mL时(即Fe3+/油酸约为1/15),在230℃反应12h得到结晶度较高,分散性良好,平均粒径比较小的纳米Fe3O4粒子.     

低温自蔓延燃烧法制备纳米Sm2O3

将溶胶-凝胶法（sol—gel）和低温燃烧技术（LCS）相结合，成功开发了一种以溶胶-凝胶为前驱体的燃烧合成Sm2O3纳米粉体的技术．利用XRD，TEM，AFM等方法对合成产物进行了表征，并考察了制备条件对Sm2O3纳米粉体尺寸和形貌的影响．     

An inverse transition of magnetic domain patterns in ultrathin films

Inverse freezing and inverse melting are processes where a more symmetric phase is found at lower temperatures than at higher temperatures. Such inverse transitions are very rare. Here we report the existence of an inverse transition effect in ultrathin Fe films that are magnetized perpendicular to the film plane. The magnetization of these films is not uniform, but instead manifests itself as stripe domains with opposite perpendicular magnetization. Predictions relating to the disordering of this striped ground state in the limit of monolayer film thicknesses are controversial. Mean-field arguments predict a continuous reduction of the stripe width when the temperature is increased; other studies suggest that topological defects, such as dislocations and disclinations, might penetrate the system and induce geometrical phase transitions. We find, from scanning electron microscopy imaging, that when the temperature is increased, the low-temperature stripe domain structure transforms into a more symmetric, labyrinthine structure. However, at even higher temperatures and before the loss of magnetic order, a re-occurrence of the less symmetric stripe phase is found. Despite the widespread theoretical and experimental work on striped systems, this phase sequence and the microscopic instabilities driving it have not been observed before.     

非化学计量对铁氧化物还原热力学平衡的影响

铁氧化物是具有非化学计量比的化合物,非化学计量对铁氧化物的还原过程带来一系列影响。本文采用Dieckmann缺陷模型和Weiss的浮氏体理想固溶体模型分别对非化学计量比的磁铁矿和浮氏体进行了热力学计算。同时根据电荷守恒和物质守恒,对铁氧化物固溶体的综合缺陷度δ与还原失重率和亚铁含量的关系进行了分析,以期对实验终产物的判定提供依据。通过理论分析与计算,最终明确了不同化学计量比的磁铁矿和浮氏体在不同温度下的平衡还原势PCO(H2),即相应的优势区图。在给定还原势的纯赤铁矿等温还原过程(未有金属Fe生成时),当失重率小于6%时,还原产物属于Fe3+占优势的磁铁矿区域;当失重率高于6%时,反应进入Fe2+占优势的浮氏体区域。     

(Fe Cr)_(83)B_(17)非晶合金结构及其晶化相变的研究

本文用DTA和X射线衍射技术,研究了(FeCr)_(83)B_(17)非晶合金晶化相变全过程。说明该非晶体系的晶化相变过程中,原子键力是晶化相变的驱动力。从“t-x”关系表明,在我们实验条件下(x=5％,15％,25％),高熔点的Cr含量(x)增大所引起晶化峰位向高温方向增大值具有良好的线性关系。实验指出,(Fe_(1-x)Cr_x)_(83)B_(17)非晶合金淬火态的结构单元是Fe_3B局域9原子多面体结构的原子团。     

过渡金属离子对介孔氧化硅粒子大小的影响

目的:考察过渡金属离子对表面活性剂诱导模板法合成的介孔氧化硅粒子大小的影响.方法:通过合成过程中加入不同浓度的Cr2+,Ni2+,Cu2+和Fe2+离子,制备不同粒径的介孔氧化硅.结果:通过X射线粉末衍射仪(XRD)确定所合成的氧化硅的介孔结构;通过透射电镜(TEM)和扫描电镜(SEM)观测合成的介孔氧化硅的形貌和粒子大小.结论:通过表面活性剂诱导模板法所合成的氧化硅具有有序的介孔结构,过渡金属离子的添加,使介孔氧化硅粒径变小,并且,随过渡金属离子浓度的增加,介孔氧化硅的粒径更小.同时,过渡金属离子的引入,还使介孔氧化硅粒子的表面粗糙度发生改变.     

One-pot synthesis of PVP-coated Ni<Subscript>0.6</Subscript>Fe<Subscript>2.4</Subscript>O<Subscript>4</Subscript> nanocrystals

Novel poly(N-vinyl-2-pyrrolidone) (PVP)-coated nickel ferrite nanocrystals were prepared by simultaneously pyrolyzing nickel(II) acetylacetonate (Ni(acac)₂) and iron(III) acetylacetonate (Fe(acac)₃) in N-vinyl-2-pyrrolidone (NVP). The PVP coating was formed in situ through polymerization of NVP. The crystalline structure of the resultant nickel ferrite was analyzed by high-resolution transmission electron microscopy, electron diffraction patterns, and powder X-ray diffraction. In addition, the valence state of Ni and the metal contents of Ni and Fe in different valence states were analyzed by X-ray photoelectron spectroscopy (XPS), atomic absorption and the phenanthroline method. The surface coating layer of PVP and its binding states were characterized by Fourier transform infrared spectroscopy in combination with XPS. Colloidal stability experiments revealed that the nanocrystals could be dispersed well in both phosphate-buffered saline and Dulbecco’s Modified Eagle Medium.     

Study of transport behavior for Fe-doping La(0.67)Ca(0.33)MnO3 perovskite manganese

Systematic studies of the transport properties of La0.67Ca0.33Mn1-xFexO3 (x=0-0.3) systems showed that with increasing Fe-doping content x the resistance increases and the insulator-metal transition temperature moves to lower temperature. For small doping content, the transport property satisfies metal transport behavior below the transition temperature, and above the transition temperature it satisfies the small polaron model. This behavior can be explained by Fe^3 doping, which easily forms Fe^3 -O^2- -Mn^4 channel, suppressing the double exchange Mn^3 -O^2- -Mn^4 channel and enhancing the spin scattering of Mn ions induced by antiferromagnetic clusters of Fe ions.