Transmission Electron Microscope Study of Secondary Phases in Cr3+:LiCaAlF6 Single Crystals

Cr³⁺-doped LiCaAlF₆ single crystals, considered as promising laser materials, contain secondary phases of different sizes and shapes which can be observed as "needles" or "dust" by light microscopy. TEM investigations presented in this paper give evidence for precipitation as the reason for the so-called microscopic "dust". The elongated shape of the so-called "needles" seems to be a consequence of the microscopic growth of facets which become visible by the decoration of the facet boundaries with microscopic precipitates.     

On the Analysis of Hydrogen in as grown and Ion Implanted GaAs Single Crystals

Hydrogen detection and analysis was carried out on the undoped semi‐insulating (S.I.) gallium arsenide (GaAs) single crystal using conventional elastic recoil detection analysis (ERDA) technique with high energy, heavy ion beam. Presence of hydrogen (nearly 3 x 1020 atoms/cc) has been observed on the as‐grown samples and further high concentration of atomic hydrogen (total concentration of 7 x 1020 atoms/cc) was found at the surface and was found to be decreasing with depth after 100 nm. Further the low energy hydrogen and oxygen ions implanted separately in GaAs at room temperature were also analysed by ERDA technique. From the analysis, the projected range (Rp) of 100 keV hydrogen and oxygen ions in GaAs was determined to be 891 nm (with Δ Rp equal to 320 nm), 170 nm (with Δ Rp equal to 120 nm) respectively. The experimentally determined values of both Rp and Δ Rp are more as compared with the values obtained using the TRIM theoretical program. Low temperature (4K) photoluminescence (PL) measurements of un‐implanted and H⁺ implanted samples show the passivation of intrinsic deep level defect EL2 and shallow acceptor impurity carbon by the low energy implanted hydrogen ions. The low energy hydrogen implantation may be used as a method of hydrogenation for passivation.     

Influence of Host Lattice in Interstital Dopant Sites: EPR Studies on Cu (II) Doped Sarcosine Cadmium Bromide Single Crystals

EPR study of Cu(II) doped in sarcosine cadmium bromide single crystals are carried out at room temperature. The impurity ions occupy the interstitial position in this crystal lattice. Crystalline field around the Cu(II) ion in this low symmetry crystal is rhombic. The transitions arise from a single paramagnetic site with g_xx = 2.1082, g_yy = 2.0005, g_zz = 2.2071, and A_xx = ‐64 x 10^‐4 cm^‐1, A_yy = ‐23 x 10^‐4 cm^‐1, A_zz =‐185 x 10^‐4 cm^‐1. The ground state is an admixture of dx2‐y2 and dz2 states. The observed molecular orbital coefficient value a2 = 0.85 reveals a moderate covalency of the s bonding and b2 = 0.967 indicates the weak pi bonding. A strong interaction between Cu(II) and nitrogen ligands is found to exist.     

Overhauser Shift of the Conduction Electron Spin Resonance in (FA)2PF6 Single Crystals

The shift ΔB _ov of the ESR line due to saturation of the NMR of the hyperfine coupled nuclei (Overhauser shift) was measured for single crystals of the organic conductor (FA)₂PF₆. ΔB_ov , is proportional to [Abar] _tt , being the average hyperfine interaction between the conduction electrons and the protons in resonance, and the dynamic nuclear spin polarization (DNP), respectively. The DNP enhancement factor V was determined for the two orientations of the static magnetic field B _o , perpendicular (V _∥ = 525 ± 40) and parallel (V _∥ = 280 ± 25) to the needle axis a, respectively. The absolute value of the average hyperfine coupling is [Abar]^zz = –(1.16 ± 0.05) Gauss · g_e μ _B . Both, the temperature dependence and the anisotropy of the proton spin relaxation times T ₁ ^p and T ₁ ^p were measured from the time dependence of the Overhauser shift, ΔB_ov (t) after rf-pulses or after switching “on” and “off” the ESR saturation. Within the metallic phase of the crystal the proton relaxation is governed by a Korringa law. The experiments definitely show, that the electron spins, showing up in the ESR are those of the conduction electrons.     

Mn_4N固相合成反钙钛矿型Mn_3MN(M∶Cu,Ge)的机理研究

以Mn4N、Cu和Ge粉末为原料,在N2气氛下固相烧结合成了反钙钛矿结构的锰基氮化物Mn3MN(M:Cu, Ge).利用热重-差热分析(TG-DSC),X射线衍射(XRD),扫描电镜(SEM)等技术研究了合成Mn3MN(M:Cu, Ge)的固相反应机理及制备的工艺条件.固相反应的主要机理是Cu(或Ge)原子通过固溶扩散置换出Mn4N立方结构中顶点的Mn原子形成反钙钛矿结构;置换出来的Mn与多余的Cu反应形成Mn3Cu固溶相, 在N2气氛中氮化再次生成反钙钛矿Mn3CuN相.以Mn4N制备纯的反钙钛矿结构的Mn3MN需要严格控制原料的配比,且需要在高真空高纯N2保护气氛中进行烧结.     

Deformation Modes and Structure Evolution in Laser‐Shock‐Loaded Molybdenum Single Crystals of High Purity

This paper reports on the microstructural changes occurring within molybdenum single crystals after shock treatment with an excimer laser‐system in a confined ablation mode with different number of impacts. Using different complementary investigation methods (optical microscopy, scanning electron microscopy and transmission electron microscopy) it is found that slip and twinning are active modes of deformation during the shock‐induced plastic deformation. After laser treatment with a single laser pulse slip bands on {112} planes containing several microscopic twins are the dominating microstructural feature, whereas further laser‐shock‐processing leads to the formation of a homogeneous arrangement of screw dislocations, tangles and loops. Deformation modes and microstructure in laser shocked samples prove to be quite similar to those of explosive shocked specimens although the laser‐induced peak pressure is about an order of magnitude lower than that during explosive loading.It is shown that the laser shock‐induced hardening increases with increasing number of impacts in the range from 1 to 6 impacts. This shock‐induced strengthening is correlated with the overall dislocation density.     

Si modified Ge10 cluster: the preparation and characterization of single crystal Na4(Ge,Si)9O20

A Si modified Ge₁₀ cluster with structure Na₄(Ge,Si)₉O₂₀ (denoted as HUT‐1) was synthesized by hydrothermal synthesis at 160 °C with a sodium silicate source. The compound was characterized by single crystal, powder X‐ray diffraction and TGA‐DSC analysis. HUT‐1 crystallizes in space group I4₁ (80) with calculated unit cell (a=14.966(5) Å, c=7.343(2) Å, V=1644.8(9) ų), which has the same structure as Na₄Ge₉O₂₀. HUT‐1 has a high Si/Ge ratio with an approximate formula of Na₄Ge_7.68Si_1.32O₂₀. Single crystal X‐ray structure refinements together with results from X‐ray powder diffraction (XRPD) confirm the occupancy of Si at two tetrahedral sites. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

以磷化铁为添加剂沿(111)面生长磷掺杂金刚石大单晶

掺杂是调控金刚石性能的一种重要手段。本文采用温度梯度法,在5.6 GPa、1 312 ℃的条件下,选用Fe₃P作为磷源进行磷掺杂金刚石大单晶的合成。金刚石样品的显微光学照片表明,随着Fe₃P添加比例的增加,金刚石晶体的颜色逐渐变深,包裹体数量逐渐增加,晶形由板状转变为塔状直至骸晶。金刚石晶形的变化表明Fe₃P的添加使生长金刚石的V形区向右偏移,这是Fe₃P改变触媒特性的缘故。红外光谱分析表明,Fe₃P的添加使金刚石晶体中氮含量上升,这说明磷的进入诱使氮原子更容易进入金刚石晶格中。激光拉曼光谱测试表明,随着Fe₃P添加比例的增加,所合成的掺磷金刚石的拉曼峰位变化不大,其半峰全宽(FWHM)值变大,这说明磷的进入使得金刚石晶格畸变增加。XPS测试结果显示,随着Fe₃P添加比例的增加,金刚石晶体中磷相对碳的原子百分含量也会增加,这意味着添加Fe₃P所合成的金刚石晶体中有磷存在。     

Study of the Nature and Distribution of Elementary Steps on the (100) Cleavage Faces of MgO Single Crystals by Atomic Force Microscopy

Some observations made on the nature and distribution of monolayer (elementary) steps on the (100) cleavage faces of MgO single crystals by atomic force microscopy are presented and discussed. The following types of patterns of monolayer steps are described: (1) trains of steps, (2) steps terminating on the cleaved surface at the emergence points of screw dislocations, and (3) localized pinning of advancing steps at random sites (probably at the emergence points of edge dislocations). It is shown that: (1) the origins of emergence points of monolayer steps are devoid of hollow cores due to a small Burgers vector of dislocations and (2) the minimum distance between two emerging steps due to screw dislocations and between two pinning centres due to edge dislocations depends on their sign, and is determined by the mutual interaction between neighbouring dislocations.     

电子和空穴注入对氮掺杂SnO2材料光电性能的影响

采用基于密度泛函理论的线性缀加平面波(FLAPW)方法研究了电子、空穴对N掺杂SnO2光电性能的影响,结果表明注入空穴比注入电子的Sn16O31N体系禁带宽度减小了0.02 eV,比未注入电子、空穴的Sn16O31N体系变窄了0.04 eV,导带也相对展宽,体系呈现出半金属特性,SnO2材料导电性能有所提高.注入空穴的体系光学特性也发生了较大的变化,其吸收系数、能量损失函数及折射率在低能区域低于本征和电子注入体系,整个体系的态密度向低能方向移动发生了红移,吸收边变宽,体系的光学响应增大.     

Electron Paramagnetic Resonance of VO2+ in M2Zn(SeO4)2 · 6H2O(M=K,Rb) Single Crystals

The EPR spectrum of VO²⁺ has been studied in single crystals of K₂Zn(SeO₄)₂ · 6H₂O and Rb₂Zn(SeO₄)₂ ∼ 6H₂O at ∼9.45 GHz. VO²⁺ substitutes for Zn²⁺ have preferential orientations in the lattice. The V = O of the intense vanadyl center is nearly along the longest Zn H₂O direction. Spin-Hamiltonian parameters have been evaluated from single crystal as well as from powder spectra.     

Controllable synthesis,characterization and optical properties of Ag@AgCl coaxial core‐shell nanocables

Core‐shell structures often exhibit improved physical and chemical properties. Developing a relatively general, facile, and low temperature synthetic approach for core‐shell structures with complex compositions is still a particularly challenging work. Here we report a general chemical conversion route to prepare high quality Ag@AgCl coaxial core‐shell nanocables via the redox reaction between Ag nanowires and FeCl₃ in solution. The powder X‐ray diffraction of the Ag@AgCl coaxial core‐shell nanocables shows additional diffraction peaks corresponding to AgCl crystals apart from the signals from the Ag nanowire cores. Scanning electron microscopy and transmission electron microscopy images of the Ag@AgCl coaxial core‐shell nanocables reveal that the Ag nanowires are coated with AgCl nanoparticles. The effect of the molar ratio of Fe:Ag on the morphology and optical absorption of the Ag@AgCl coaxial core‐shell nanocables is systematically investigated. The result shows that the optical absorption of Ag nanowires decreases gradually and that of AgCl nanoparticles improves gradually with the increase of the molar ratio of Fe:Ag. The formation process of the Ag@AgCl coaxial core‐shell nanocables has been discussed in detail. The present chemical conversion approach is expected to be employed in a broad range of applications to fabricate innovative core‐shell structures with different compositions and shapes for unique properties. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

弛豫铁电单晶(PMNT)中负离子配位多面体结晶方位与工程化畴

本文从晶体中负离子配位多面体结构基元结晶方位及其形变的论点讨论了PMNT晶体工程化畴的形成机理,认为晶体工程化畴的形成是在电场作用下,当A位离子沿着晶体a、b、c轴孔道发生位移导致B八面体中的B离子位移和B八面体形变,两者相互制约所致,三方和四方晶系的晶体中畴的形成都是沿着B八面体的对角线方向分布.     

Structure and thermal stability of MOCVD ZrO2 films on Si (1 0 0)

The structure and thermal stability of ZrO₂ films grown on Si (1 0 0) substrates by metalorganic chemical vapor deposition have been studied by high-resolution transmission electron microscopy, selected area electron diffraction and X-ray energy dispersive spectroscopy. As-deposited films consist of tetragonal ZrO₂ nanocrystallites and an amorphous Zr silicate interfacial layer. After annealing at 850°C, some monoclinic phase is formed, and the grain size is increased. Annealing a 6 nm thick film at 850°C in O₂ revealed that the growth of the interfacial layer is at the expense of the ZrO₂ layer. In a 3.0 nm thick Zr silicate interfacial layer, there is a 0.9 nm Zr-free SiO₂ region right above the Si substrate. These observations suggest that oxygen reacted with the Si substrate to grow SiO₂, and SiO₂ reacted with ZrO₂ to form a Zr silicate interfacial layer during the deposition and annealing. Oxygen diffusion through the tetragonal ZrO₂ phase was found to be relatively easier than through the monoclinic phase.     

Investigation of the structure of solid solutions of elements of the IV. group (Si,Ge) in gallium antimonide

Precision measurements of the lattice parameter and the density of Si- and Ge-doped GaSb monocrystals were accomplished. The investigated crystals were Czochralski-grown from an equiatomic melt (with respect to its own components) and doped with 2 · 10¹⁷ to 4 · 10¹⁹ cm^–3 Si and 2 · 10¹⁷ to 4 · 10¹⁹ cm^–3 Ge, respectively. The concentrations of the dopants were determined spectroscopically. — Hall measurements at room temperature showed that Si as well as Ge in GaSb produce p-conduction.     

On the electronic transport properties of amorphous (Si,Ge) alloys: charged scattering centers and compositional disorder

The electronic transport properties of a-(Si,Ge):H alloys over the entire range of Ge content (0-100%) grown using low pressure, reactive ECR plasma deposition with high H dilution and subtle (sub-ppm) B-doping have been investigated in detail by employing the microwave photomixing technique. Strong evidence for the existence of long-range potential fluctuations in a-(Si,Ge):H alloys has been found from the measurements of electric field dependence of the drift mobility. It was observed for the first time that the film transport properties do not degrade monotonically with increasing Ge content; there exists a valley point near the middle of the composition range, where the strongest potential fluctuations occur as a result of a significant increase in the charged defect density. Beyond this point, the film quality increases again, but still much worse than that for the Si end. The effect of potential fluctuations can be enhanced by adding Ge or Si to the alloy system resulting in deterioration of the transport properties of a-(Si,Ge):H alloys. Our present results demonstrate that the increased charged scattering centers and compositional disorder upon adding Ge or Si to the alloys play an important role in the potential fluctuations.     

SEM,Chemical Etching and THz Wave Generation of 4-Dimethylamino-N-methyl-4-stilbazolium Tosylate (DAST) Single Crystals

Crystallography Reports - The 4-dimethylamino-N-methyl-4-stilbazolium tosylate (DAST) crystal which was candidate for generating and detecting terahertz (THz) wave was grown by slope nucleation...     

Atomic force microscopy studies on surface morphologies of CdHg(SCN)4 crystals grown in solutions containing excessive amount of Cd(II) cations

Surface morphologies of CdHg(SCN)₄ (CMTC) crystals grown from solutions with excessive amount of Cd(II) cations (5%, 20% and 50% in molar ratio) have been investigated by atomic force microscopy (AFM). [Cd(SCN)_n]^2‐n (n ≤ 4) complex anions formed by addition of excessive Cd(II) cations in the solutions have been found to act either as growth units or impurities during CMTC crystal growth. On the prismatic faces, incorporation of [Cd(SCN)_n]^2‐n (n ≤ 4) complex anions as growth units leads to the formation of well‐oriented protuberance trains at the step fronts, named as “locally anisotropic crystal growth”. These protuberances become fewer, less distinct and nearly disappeared with the increase of excessive Cd(II) cations in the solutions. The pyramidal face, however, varies from regular 2D nucleation growth at a low concentration of Cd(II) to much rougher growth surfaces at high concentrations, exhibiting typical surface morphologies where crystal growth is completely inhibited by impurities. Observations in this experiment provide a new picture of crystal growth.     

Tb2Fe17和Tb2（Fe,Si）17磁性单晶的生长和相图

利用磁悬浮冷坩埚提拉法技术生长了Tb2Fe17和Tb2(Fe,Si)17的单晶,并用差热分析等方法研究了材料的相图。研究结果表明：Tb2Fe17的相关系并非以往报道的包晶反应。而是同成分熔化。本文还给出了Tb2Fe17化合物附近的新相图。采用优化后的生长条件,获得了缺陷较少的Tb2Fe17和Tb2(Fe,Si)17高质量单晶,分析了Si替代对于化合物结构的影响,测量了Tb2Fe17单晶样品的基本磁性。从材料的一级磁化过程的测量可以看出,在理想配比条件下最容易获得缺陷密度低的单晶样品,这种磁性测量方法为了解单晶的完整性提供了一个有效的间接观察方法。