镍镀层中微量六方晶格镍的存在与稳定性研究

对由含糖精的Watts液得到的镍镀层(含硫镍)和Watts镍镀层(无硫镍)进行透射电镜观察及选区电子衍射实验,结果表明无硫镍镀层呈粒状结构,晶粒尺寸在100～500nm之间,属面心立方结构；含硫镍镀层为层状结构,层间距在700～1500nm之间,每层又由许多宽约200～300nm的小层组成,晶粒尺寸约20～30nm,大部分属面心立方结构,在层与层交界处发现有少量六方结构镍晶体,差示扫描量热法实验表明,在约180℃左右六方结构镍转化为更稳定的面心立方结构。     

快淬Sm(CobalFe0.1 Cu0.16Zr0.04)7.0的微波晶化及硬磁性

研究了Sm（CobalFe0.1Cu0.16Zr0.04）7.0快淬带在微波场作用下晶化处理后的微结构及磁性能。结果表明,Sm（CobalFe0.1Cu0.16Zr0.04）7.0在传统晶化处理后晶粒尺寸约为500-1500 nm,FeCo软磁性相异常长大。微波场作用下,合金在700℃处理4 min时晶粒尺寸约为10 nm,磁体的Ms为1.192 T,Hci为14.8 kA.m-1;在650-700℃处理4-30 min均获得了晶粒尺寸为20 nm的单一球形颗粒,磁体主要由1∶7主相和少量Sm2Co7相构成。在650℃晶化处理30 min后,合金具有方形度较好的平滑磁滞回线,Hci为542.6 kA.m-1,剩磁比达0.86。微波场可细化晶粒尺寸并抑制FeCo软磁性相的生成,使磁体具有良好的交换耦合作用。     

压力、温度和晶粒尺寸对Fe-N合金的合成及结构的影响

在 1× 1 0 - 3 Pa～ 4 GPa的压力和 5 80～ 930 K温度范围内 ,利用高压技术并结合机械球磨 ,研究了压力、温度和晶粒尺寸对α-Fe与非晶 BN的固态反应的影响 .发现高压和晶粒细化可以极大地促进α-Fe和非晶 BN的固态反应过程 ,α-Fe与非晶 BN发生固态反应的临界晶粒尺寸约 8nm.压力和温度对反应产物及其晶体结构有明显影响 .2 GPa和 80 0 K时 ,反应产物为具有正交结构的 Fe-N新相 ;在 3～ 4 GPa和 690～80 0 K时 ,可形成单一ε-Fex N合金相 ;而在 4 GPa和 930 K以上 ,反应产物由 Fe-N合金相转变为 Fe3B相     

铌酸锂、钽酸锂晶体的结构特征

从铌酸锂和钽酸锂晶体的结晶学数据出发,分析其结构特征和组成化学键的结合情况.对于这两个晶体的结晶学格位占有情况和阳离子的位移进行了理论上的分析.作者首次明确地给出了铌酸锂和钽酸锂晶体中与晶体组成有关的阳离子位移趋势.     

Pechini 方法制备铌酸锂薄膜的研究

采用Pechini方法，以柠檬酸为配位剂与金属离子配位，在Pt/Ti/SiO₂/Si基片上制备了多晶铌酸锂(LiNbO₃)薄膜。以13C核磁共振、拉曼光谱和红外光谱分析研究了柠檬酸与金属离子的配位情况，提出了一种Nb-柠檬酸配合物可能的分子结构，即柠檬酸作为三齿配体，以端羧基、-OH和中间羧基与Nb离子配位。以TG-DTA对Li-Nb凝胶前驱体的热分解历程进行分析，以拉曼光谱和XRD分析了LiNbO₃薄膜在不同温度下热处理的相组成和结构。结果表明，600 ℃下退火2 h可得到单相多晶LiNbO₃薄膜，薄膜表面致密、平整，晶粒的平均尺寸为50 nm。     

锂掺杂ZnO陶瓷靶材制备及其掺杂引起的缺陷

采用燃烧合成和放电等离子烧结方法制备锂掺杂ZnO陶瓷靶材. 利用XRD, SEM, TEM和激光粒径分析等手段分析合成粉体与陶瓷的显微结构. 结果表明, 锂掺杂ZnO粉体与陶瓷均为纤锌矿结构, 无其他相存在; 粉体的粒径分布为0.18-1.7 μm, 烧结体致密度较高, 晶粒尺寸为1-3 μm. 此外, 分析锂元素在烧结过程中引起掺杂缺陷变化, 锂元素由ZnO晶格的间隙位置转移为替代锌晶格位置, 实现受主掺杂, 为实现p型ZnO薄膜的制备奠定基础.     

静电纺丝法制备SrTiO3多晶微纳米纤维

应用静电纺丝法并结合Sol-gel 技术制备了SrTiO3微纳米纤维. SEM, TEM及电子衍射分析结果显示, 于900 ℃煅烧获得的纤维直径分布在50~400 nm之间, 其典型直径约为280 nm. XRD分析结果表明, 纤维由立方结构的SrTiO3晶粒组成, 平均晶粒尺寸为33 nm.     

以纳米微晶纤维素为模板的酸催化水解法制备球形介孔TiO_2

以纳米微晶纤维素(NCC)为模板剂,采用酸催化水解法制备了球形介孔TiO2(SP-TiO2).并采用扫描电镜、透射电镜、X射线衍射、紫外-可见漫反射光谱和低温N2吸附-脱附等手段对其进行了表征.结果表明,所制SP-TiO2为直径100～200nm的规整球形颗粒,单个球形颗粒由粒径为10～20nm的TiO2小晶粒组成.其介孔孔径为8.2～13.5nm,且随焙烧温度的升高而增大.NCC长链结构之间羟基键合所形成的狭小空间构成的微反应器,可有效限制TiO2前驱体的生长和团聚,诱导其晶粒自组装成球形结构,并抑制由锐钛矿相向金红石相转变.600oC焙烧的SP-TiO2表现出最高的光催化活性,对苯酚降解率达89%.     

程序升温反应法由纳米氧化铁制备纳米氮化铁

先以廉价的无机铁盐为主要原料,采用沉淀法和溶胶凝胶法制备纳米氧化铁粒子,由此得到粒径大小在10～20nm,20～40nm和40～60nm的氧化铁,在此基础上,以纳米氧化铁为前体,在氨气气氛下由程序升温反应法制备纳米氮化铁.研究发现,纳米氧化铁经程序升温反应氮化后,可以制备出纳米尺度的氮化铁.不同大小的氧化铁纳米粒子氮化后尺寸存在明显的差异,在一定范围内,小粒径的纳米氧化铁氮化后更容易长大;对于大小相近的γ相与α相纳米氧化铁粒子,γ氧化铁纳米粒子氮化后尺寸增大更为显著.制得的氮化铁的形貌与其氧化铁前体保持一致.     

锂离子电池负极材料立方相氮化铌纳米材料的制备与性能(英文)

采用固相合成方法,在反应釜中350℃下合成了氮化铌纳米材料。X射线粉末衍射图表明所得氮化铌样品为立方相(空间群:Fm3m)。高分辨透射电子显微镜与场发射扫描电子显微镜显示所制得的氮化铌样品直径分布在30~300 nm之间。热重分析表明所得材料在空气中具有良好的抗氧化性能。将氮化铌与锂片组装成纽扣电池进行充放电测试,测试结果显示其首次充电比容量可达314 mAh.g-1。经50次充放电循环后,容量保持在228 mAh.g-1,具有较好的循环稳定性。     

Interface stoichiometry and structure in anodic niobium pentoxide

High-resolution transmission electron microscopy and electron energy loss spectroscopy (EELS) were performed on electrochemically anodized niobium and niobium oxide. Sintered anodes of Nb and NbO powders were anodized in 0.1 wt% H3PO4 at 10, 20, and 65 V to form surface Nb2O5 layers with an average anodization constant of 3.6 +/- 0.2 nm/V. The anode/dielectric interfaces were continuous and the dielectric layers were amorphous except for occurrences of plate-like, orthorhombic pentoxide crystallites in both anodes formed at 65 V. Using EELS stoichiometry quantification and relative chemical shifts of the Nb M4,5 ionization edge, a suboxide transition layer at the amorphous pentoxide interface on the order of 5 nm was detected in the Nb anodes, whereas no interfacial suboxide layers were detected in the NbO anodes.     

YTao4：Nb，Eu的发光性能研究

用高温固相反应法合成了铌酸根NbO^3-4和Eu^3 共掺杂的正钽酸盐化合物Y1－xEuxTa1-yNbyO4,研究该体系中紫外光和X射线激发下的发光性能,研究表明,在紫外光激发下,YTaO4:Nb,Eu是一种比较有效的红色发光材料,激发能可以通过NbO^3 4离子传递给Eu^3 ,随钽酸盐中NbO^3-4基团浓度的增中,化合物的结构从M'型YTaO4变成褐钇铌型YNbO4结构,它的发光性质也随之改变。     

Electronic and Optical Properties of KNbO3,NaNbO3 and K0.5 Na0.5 NbO3 in Paraelectric Cubic Phase：a Comparative First-principles Study

The structural,electronic and optical properties of KNbO 3 (KN),NaNbO3(NN)and K05 Na0.5NbO3(KNN) in paraelectric cubic phase were calculated employing the plane-wave pseudopotential method based on density functional theory (DFT).The calculated electronic structures of the three crystals show similar features in the valence bands and the lower conduction bands.However,the structures in higher conduction bands differ markedly due to the effect of Na and K atoms.The calculated optical properties reveal that the features of optical spectrum at low energy are dominated by the transitions from O2p valence bands to Nb 4d conduction bands and those at high energy are related to the transitions to K 4s4p and/or Na 3s3p states.Moreover,the optical constants of KNN are approximately the average of KN and NN at high energy.Therefore,the optical properties of KNN in high energy region can probably be altered by changing the ratio of Na/K.     

Electron microscopy studies of potassium sodium niobate ceramics.

Using electron microscopy, K0.5Na0.5NbO3 (KNN) ceramics sintered at 1030 degrees C for 8 h and 1100 degrees C for 2 and 24 h was studied. The scanning electron microscopy and X-ray spectrometry revealed that the materials consisted of a matrix phase in which the (Na+K)/Nb ratio corresponded closely to the nominal composition and a small amount of Nb-rich secondary phase. A bimodal microstructure of cube-shaped grains was revealed in the fracture and thermally-etched surfaces of the KNN. In the ceramics sintered at 1100 degrees C, the larger grains (up to 30 mum across), contained angular trapped pores. The transmission electron microscopy analysis revealed that the crystal planes of the grains bordering the intragranular pore faces were of the {100} family with respect to the simple perovskite cell. Ferroelectric domains were observed in the grains of this material.     

层状类钙钛矿结构新铌酸盐KSr2Nb3O10

A new niobate compound KSr₂Nb₃O₁₀ was synthesized for the first time. The chemical compositions, crystal structure, optical property, density and melting point of the new compound were characterized by EPMA, TEM, XRD, DTA and so on. KSr₂Nb₃O₁₀ crystallizes the orthorhombic system with unit cell parameters a=0.7816(1) nm, b=0.7764(2) nm, c=2.9995(2) nm, V=1.8114(4) nm³, and space group P2₁2₁2₁, Z=8. The structure may be described as treble perovskite sheets ［Sr₂Nb₃O₁₀］^- interleaved with K⁺. Further, it was found that KSr₂Nb₃O₁₀ has intercalation phenomenon. Na⁺, Li⁺, H⁺, NH⁺₄ could exchange the interlayer cations K⁺ of KSr₂Nb₃O₁₀, and n-hexylamine also could intercalate into the place between the layers of ［Sr₂Nb₃O₁₀］^-.     

铌取代型杂多钨酸盐的合成、表征、生物活性及晶体结构

合成了铌、过氧化铌取代的钨硅、钨锗杂多配合物M     

Li(+) ion conductivity in rock salt-structured nickel-doped Li(3)NbO(4)

Two mechanisms of doping Li(3)NbO(4), which has an ordered, rock salt superstructure, have been established. In the "stoichiometric mechanism", the overall cation-to-anion ratio is maintained at 1:1 by means of the substitution 3Li(+) + Nb(5+) --> 4Ni(2+). In the "vacancy mechanism", Li(+) ion vacancies are created by means of the substitution 2Li(+) --> Ni(2+). Solid solution ranges have been determined for both mechanisms and a partial phase diagram constructed for the stoichiometric join. On the vacancy join, the substitution mechanism has been confirmed by powder neutron diffraction; associated with lithium vacancy creation, a dramatic increase in Li(+) ion conductivity occurs with increasing Ni content, reaching a value of 5 x 10(-4) Omega(-1) cm(-1) at 300 degrees C for composition x= 0.1 in the formula Li(3-2x)Ni(x)NbO(4). This is the first example of high Li(+) ion conductivity in complex oxides with rock salt-related structures.     

Synthesis of (K,Na)NbO3 particles by traditional hydrothermal method and high-temperature mixing method under hydrothermal�Csolvothermal conditions

Pure (K,Na)NbO₃ (KNN) powders have been successfully prepared by using traditional hydrothermal method and high-temperature mixing method (HTMM) under solvothermal and hydrothermal conditions. The products were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) to show the change of phase, morphology, and size of the as-prepared particles with the alkalinity of the starting solution. Compared with the traditional hydrothermal method, smaller particles with higher phase purity are prepared using HTMM under hydrothermal conditions. It is found that the alkalinity has significant effects on the crystal size. The KNN grain size first increases and then decreases with increasing alkalinity. Typical samples solvothermally synthesized in a mixed solvent with isopropanol/deionized water ratio of 50/50 by volume were made of well-crystallized single-crystalline nanoparticles with size of about 500 nm.     

Energy relationship and the polarization of C_(60) cage in the endohedral complexes (X@C_(60))

In this paper, we carry out the calculation on the system (X@C60)(X=Li, Na, K, Kb, Cs; F, Cl, Br, I), where the position of X changes along 5 typical symmetry directions. For the calculation of quantum chemistry we use EHMO/ASED method, for the calculation of molecular mechanics we use Buckingham potential (exp-6-1) function, and for the calculation of thermo-chemical cycle we use individually isolating the processes such as the structure variation, charge transfer and charge distribution, and their interactions etc. The calculation results show that (1) In the region of radius r≈0.2 nm of the Ceo cage, the potential field is nearly spherical; (2) Except for Li and Na, the systems are the most stable with minimum energies at the center of C60 cage. For Li and Na, the systems are the most stable with minimum energies at r≈0.16 nm and r≈0.13 nm, respectively. In view of the interactive region of chemical bonds, the interactions between X and the C60 cage do not belong to the classical chemical bonds; (     

93Nb NMR and DFT investigation of the polymorphs of NaNbO3

Sodium niobate (NaNbO(3)) has a particularly complex phase diagram, with a series of phase transitions as a function of temperature and pressure, and even at room temperature a number of different structural variations have been suggested. Recent work has demonstrated that bulk powders of NaNbO(3), prepared using a variety of synthetic approaches, contain a mixture of perovskite phases; the commonly reported Pbcm phase and a second, polar phase tentatively identified as belonging to space group P2(1)ma. The two phases exhibit very similar (23)Na MAS NMR spectra, although high-resolution MQMAS spectra were able to distinguish between them. Here, we investigate whether different perovskite polymorphs can be distinguished and/or identified using a variety of (93)Nb NMR methods, including MAS, MQMAS and wideline experiments. We compare the experimental results obtained for these more common perovskite materials to those for the metastable ilmenite polymorph of NaNbO(3). Our experimental results are supported by first-principles calculations of NMR parameters using a planewave pseudopotential approach. The calculated NMR parameters appear very different for each of the phases investigated, but high forces on the atoms indicate many of the structural models derived from diffraction require optimisation of the atomic coordinates. After geometry optimisation, most of these perovskite phases exhibit very similar NMR parameters, in contrast to recent work where it was suggested that (93)Nb provides a useful tool for distinguishing NaNbO(3) polymorphs. Finally, we consider the origin of the quadrupolar coupling in these materials, and its dependence on the deviation from ideality of the NbO(6) octahedra.