The influence of defects in the crystal structure on helium diffusion in quartz

The solubility and diffusion of helium in quartz crystals are investigated as functions of the distribution and density of structural defects. The types of defects in the crystals are identified and their distribution over growth sectors is determined by x-ray diffraction topography and phase radiography with a synchrotron radiation source. The effective solubility and effective diffusion coefficients for helium in quartz are estimated from the experimental data on the amount of helium extracted from samples with different contents of defects. It is revealed that the effective diffusion coefficient of helium depends on the number of dislocations.     

C60单晶的表面形貌与生长缺陷

用气相法生长出了毫米尺寸的具有规则晶面和金属光泽的高质量的纯C₆₀单晶.X射线衍射分析表明,C₆₀单晶在室温下具有面心立方(fcc)结构,晶格常数为α=1.4199(4)nm。用扫描电子显微镜和光学显微镜观察了C₆₀单晶的形貌,除观察到fcc结构的晶体所特有的{111}和{200}两种稳定晶面以及非常容易形成的孪晶之外,还发现了在{111}面上的树枝状、垄状和生长丘以及在{200}面上的树枝状、游泳池状和生长丘的生长缺陷。对C_{60 关键词：}     

Investigation of the phase transitions of ferroelectric KIO3 and KNbO3 crystals by optical diffraction

Optical diffraction is reviewed as a technique for investigation of the phase transitions in crystals with a multidomain structure. It has been used to study the phase transitions in KIO₃ and KNbO₃ single crystals. Strong optical diffraction bands resulted from electric domains in KNbO₃ crystals and their change with temperature were observed when a laser beam passed through the crystals. The diffraction patterns observed changed abruptly at 427°C, 223°C, and -50°C respectively, at which KNbO₃ crystals undergo structural phase transitions. It is considered that the change of the diffraction patterns with temperature is due to change of the electric domains in the crystals.     

Structural aspects of solid-state amorphization in Eu<Subscript>2</Subscript>(MoO<Subscript>4</Subscript>)<Subscript>3</Subscript> single crystals

X-ray diffraction studies of Eu₂(MoO₄)₃ single crystals were performed, which demonstrate that, in contrast to polycrystalline samples, these crystals do not exhibit amorphous-like diffraction patterns during the reverse transition from the high-pressure phase into the initial β phase; rather, the diffracted intensity in their diffraction patterns decreases significantly to the background. Such a diffraction pattern can be explained under the assumption that a single crystal is divided into small (nanoscopic) regions inside which the lattice parameters of the high-pressure phase and the initial β phase change continuously. The simultaneous recovery of the single-crystal state of the β phase from this intermediate state in all nanoscopic regions as the annealing temperature increases indicates that nanocrystals in this state are structurally correlated with each other. This result suggests that the halo-type diffraction patterns of polycrystalline samples reflect an intermediate state between the high-pressure phase and the β phase in every initial crystallite (as in the single crystals) rather than being caused by an amorphous structure of the sample. In this case, the total diffraction pattern of differently oriented crystallites gives an amorphous-like diffraction pattern reflecting the contributions from numerous various crystallographic planes involved in diffraction.     

Spectral,electron microscopic and chemical investigations of gamma-induced purple color zonings in amethyst crystals from the Dursunbey-Balıkesir region of Turkey

Amethyst crystals on matrix specimens from the Dursunbey-Bal?kesir region in Turkey have five representative purple color zonings: dark purple, light purple, lilac, orchid, and violet. The purple color zonings have been analyzed with optical absorption spectra in the visible wavelength region, chemical full trace element analyses (inductively coupled plasma-atomic emission spectroscopy and inductively coupled plasma-mass spectroscopy), and scanning electron microscopic images with high magnification. It can be proposed that the production of the purple color in amethyst crystals is due to three dominant absorption bands centered at 375, 530, and 675 nm, respectively. In addition, the purple color zonings are also due to four minor absorption bands centered at 435, 480, 620, and 760 nm. X-ray diffraction graphics of the investigated amethyst crystals indicate that these crystals are composed of a nearly pure alpha-quartz phase and do not include any moganite silica phase and/or other mineral implications. Trace element analyses of the amethyst crystals show five representative purple color zonings, suggesting that the absorption bands can be mainly attributed to extrinsic defects (chemical impurities). However, another important factor that influences all structural defects in amethyst is likely to be the gamma irradiation that exists during amethyst crystallization and its inclusion in host materials. This gamma irradiation originates from the large underlying intrusive granitoid body in the region of amethyst formation. Irradiation modifies the valence values of the impurity elements in the amethyst crystals. It is observed that the violet-colored amethyst crystals have the most stable and the least reversible coloration when exposed to strong light sources. This situation can be related to the higher impurity content of Fe (2.50 ppm), Co (3.1 ppm), Ni (38 ppm), Cu (17.9 ppm), Zn (10 ppm), Zr (3.9 ppm), and Mo (21.8 ppm).     

邻苯二甲酸氢钾(KAP)的同步辐射截面形貌术

本文叙述邻苯二甲酸氢钾(KAP)晶体内部不完整性(滑移位错等)的同步辐射截面形貌图的衬度研究工作。有关缺陷象衬度随波长增加而提高的实验事实同引用均匀畸变动力学的理论所引入的平均应变梯度参数β和βt_eff的理论计算结果,相当符合,它为应用同步辐射源来清晰显示单晶中有关缺陷,提供一个波长选择的依据。 关键词：     

氘化对KH2PO4晶体微观缺陷影响的正电子湮没研究

采用传统降温法从不同程度氘化(x=0, 0.51, 0.85)的生长溶液中生长氘化KH₂PO₄(KDP) 晶体, 利用正电子湮没技术(正电子寿命谱和多普勒展宽谱)、结合X射线衍射谱(XRD) 结构分析, 对KDP晶体氘化生长的微观缺陷进行了研究, 讨论了氘化程度对晶体内部微观结构特性、缺陷类型和浓度的影响. XRD结果显示晶胞参数a, b值随氘含量的增加而增加, c值无明显变化; 正电子寿命谱结果发现随着氘化浓度的提高, KDP晶体内部中性填隙缺陷以及氧缺陷不断增加, 引起晶体晶格畸变; 氢空位、K空位、杂质替位缺陷不断发生缔合反应形成复合缺陷, 缺陷浓度不断减少; 团簇、微空洞等大尺寸缺陷也在不断发生聚合反应, 缺陷浓度表现为不断减少. 多普勒实验结果表明随着氘化程度的提升, 晶体内部各类缺陷表现为同步变化. 实验结果表明, KDP晶体在低浓度氘化生长(50%以内)下缺陷反应较弱, 而在高浓度氘化(50%以上)下的缺陷反应显著增强.     

位错的会聚束电子衍射研究

从硅位错附近得到的会聚束电子衍射图样表明高阶劳厄带线和菊池线分裂,晶体学等效的衍射显示不同的分裂或不分裂,这些结果可以用晶体缺陷的衍衬理论来解释,不分裂的衍射相当于位错的不可见,即g·b=0,会聚束电子衍射提供了强有力的研究缺陷的高空间分辨率手段。 关键词：     

Structural investigations on YbRh2Si2: from the atomic to the macroscopic length scale

YbRh2Si2 has advanced to a prototype material for investigating physics related to the Kondo effect. An optimization of the synthesis resulted in single crystals of extraordinary crystalline quality. At the atomic scale, we utilize scanning tunneling microscopy to study the topography of cleaved single crystals. A structural and chemical analysis was conducted by highly accurate x-ray diffraction and wavelength dispersive x-ray spectroscopy measurements. The latter indicate a homogeneity range of the YbRh2Si2 phase between approximately 40.0–40.2 at.% Rh. For our high-quality samples the number of defects found on the atomic scale (of the order of 0.3% of the visible lattice sites) is in quantitative agreement with a very small off-stoichiometry within this homogeneity range. Comparing our results for these samples allows an assignment of the structural defects observed at the cleaved surfaces to Rh occupying Si sites and, even less numerous Si in Rh sites. Such an analysis is hampered for samples of lesser quality, but there seem to be numerous empty Si-sites. Based on these observations the results of scanning tunneling spectroscopy can be analyzed in further detail and provide insight into the Kondo physics.     

Influence of crystal synthesis on the incommensurate phase and lock-in transition of Rb2ZnCl4 crystals

A comparative study of several crystals of Rb₂ZnCl₄, obtained by different crystal growing methods, has allowed us to determine the influence of growth defects on the incommensurate phase and on the lock-in transition of these samples. X-ray diffraction has allowed us to complete previous dielectric measurements realized on the same samples and to relate the crystalline quality to the evolution of the modulation as a function of the temperature. The principal influence of an increasing defect density seems to be a stronger pinning of the modulated phase and this induces a lower lock-in temperature and a wider hysteresis.     

磷酸铝(AlPO4)晶体中缺陷的X射线形貌研究

用X射线衍射形貌法研究了AlPO₄晶体中的微观缺陷。在所研究的晶体中,主要晶体缺陷是生长层,沉淀物和位错。位错密度在晶体表面附近最大,晶体中部较低。位错主要起源于热应力和由沉淀物或生长层所造成的晶格畸变。多数位错的柏氏矢量是b=(a+c)<1123>型,部分的是b=a[2110]。分析了晶体缺陷与生长条件之间的关系。控制生长过程中的温度波动,特别是晶体出炉时的冷却速度,对提高晶体完美性是重要的。 关键词：     

Mechanism of crystallization of the Ni70Mo10B20 alloy above the glass transition temperature

The phase transformations occurring in the Ni₇₀Mo₁₀B₂₀ alloy in the course of heating above the glass transition temperature are investigated using x-ray diffraction, transmission electron microscopy, high-resolution electron microscopy, and differential scanning calorimetry. It is shown that annealing of the alloy above the glass transition temperature leads to segregation of the amorphous phase into regions enriched with and depleted in molybdenum and/or boron. An increase in the temperature or time of annealing is accompanied by primary crystallization in regions of each type. Crystallization of the regions enriched with molybdenum results in the formation of face-centered cubic crystals of a molybdenum solid solution in nickel (phase 2). Nickel boride crystallizes in the regions enriched with boron. The face-centered cubic phase (phase 1), which is similar to pure nickel, crystallizes in the regions depleted in molybdenum and boron. Nanocrystals of phase 1 are free of defects. Nanocrystals of phase 2 with larger sizes contain a great number of defects.     

Super deformability and thermoelectricity of bulk γ-InSe single crystals

Indium selenide, a III–V group semiconductor with layered structure, attracts intense attention in various photoelectric applications, due to its outstanding properties. Here, we report super deformability and thermoelectricity of γ-In Se single crystals grown by modified Bridgeman method. The crystal structure of In Se is studied systematically by transmission electron microscopy methods combined with x-ray diffraction and Raman spectroscopy. The predominate phase of γ-In Se with dense stacking faults and local multiphases is directly demonstrated at atomic scale. The bulk γ-In Se crystals demonstrate surprisingly high intrinsic super deformative ability which is highly pliable with bending strains exceeding12.5% and 264% extension by rolling. At the meantime, In Se also possesses graphite-like features which is printable,writable, and erasable. Finally, the thermoelectric properties of γ-In Se bulk single crystals are preliminary studied and thermal conductivity can be further reduced via bending-induced defects. These findings will enrich the knowledge of structural and mechanical properties' flexibility of In Se and shed lights on the intrinsic and unique mechanical properties of In Se polytypes.     

Determination of the Space-Charge Field Amplitude by the Phase Modulation Method

Results of experimental and theoretical investigations into the conversion of the phase modulation of light into its intensity modulation in photorefractive crystals are presented. Based on the vector diffraction theory, an analytical expression describing a phase demodulation in crystals in an external electric field applied in an arbitrary direction is derived. The phase demodulation is used to determine the space-charge field amplitude in cubic crystals. It is demonstrated that the space-charge magnitude measured in GaP and Bi₁₂TiO₂₀ crystals is less than that predicted by the Kukhtarev single-level model.     

Formation of nanodefects in LiF crystals under gamma irradiation

The absorption spectra, photoluminescence spectra, and microhardness of LiF crystals exposed to gamma radiation from a shutdown reactor and a ⁶⁰Co source at a dose rate of 7.65 Gy/s are investigated. The structure of these crystals is determined using x-ray diffraction analysis. It is revealed that the Li sublattice contains not only point and complex radiation-induced defects but also 28-nm LiOH particles induced by gamma radiation. It is shown that the formation of defects occurs more efficiently upon exposure to radiation from a shutdown reactor than from a ⁶⁰Co source.     

层状晶体层错的会聚束电子衍射研究

用会聚束电子衍射得到了石墨和辉钼矿的底面横向层错的带轴图样。带轴图样显示了层错引起的变化,对称性降低和部分衍射分裂,本文首先指出衍射分裂或不分裂可以用晶体缺陷衍射衬度理论来解释,这对应于缺陷的可见和不可见,这结果对缺陷的研究有普遍性意义。这方法为研究晶体缺陷提供了强有力的手段。 关键词：     

Order—Disorder phase transformation in ZrS2 single crystals

Order-disorder phase transformation has been observed in ZrS₂ single crystals on annealing them at a temperature of 400 ± 10°C. Loss of sulphur, resulting in its deficiency, on annealing of crystals is thought to be the cause of the observed phase transformation. Evidence in its support, based on X-ray and electron diffraction results, is advanced.     

Compound synthesis in TiO2 implanted with Rubidium

Rubidium ions, with energy in the range 0.1 MeV, 2.0 MeV have been implanted in TiO₂ single crystals at RT and LNT.

Defects induced by implantation have been studied by optical spectroscopy, X-ray diffraction, RBS, TEM and electrical conductivity.

During implantation, the implanted samples are blue colored after irradiation. This coloration is due to an optical absorption band localized at 900 nm which corresponds to optical transition of intrinsic defects identified as Ti³⁺. These defects are induced by a chemical reaction between the implanted ions and the oxygen of the lattice as in the case of D⁺, H⁺, Li⁺, Na⁺ and K⁺ implanted in rutile.^1-3

The synthesis of a new phase in heavily implanted rutile is exhibited by using a thermal treatment and by combining techniques such as RBS, TEM and X-ray diffraction at glancing angle in the temperature range 300°C-700°C.

This compound does not correspond to metallic precipitates of rubidium which are observed in MgO implanted with Rb ions.

Planar defects have been observed in the implanted area. A correlation is exhibited between these defects and the precipitates of the new phase. From X-ray diffraction measurements and TEM observations, the composition of the synthetized compound is likely Rb₂TiO₃.     

Phase transformations during the growth of paracetamol crystals from the vapor phase

Phase transformations during the growth of paracetamol crystals from the vapor phase are studied by differential scanning calorimetry. It is found that the vapor-crystal phase transition is actually a superposition of two phase transitions: a first-order phase transition with variable density and a second-order phase transition with variable ordering. The latter, being a diffuse phase transition, results in the formation of a new, “pretransition,” phase irreversibly spent in the course of the transition, which ends in the appearance of orthorhombic crystals. X-ray diffraction data and micrograph are presented.     

Degree of structural perfection of icosahedral quasicrystalline grains investigated by synchrotron X-ray diffractometry and imaging techniques

A study of the structural perfection of icosahedral quasicrystalline grains of various alloys (Al-Pd-Mn, Zn-Mg-RE (RE L rare earth) and Al-Cu-Fe), grown by different slow solidification techniques (Czochralski, Bridgman, flux and annealing) was performed using high-resolution diffraction, including recording rocking curves combined with X-ray topography and phase contrast radiography, at a third-generation synchrotron radiation source (European Synchrotron Radiation Facility, Grenoble, France). For Al-Pd-Mn, additional coherent diffraction and diffuse scattering measurements were also carried out. After evaluating the potentialities of the techniques used, in the light of the criteria defined for crystals, it is shown that the structural perfection of icosahedral quasicrystals is quite comparable with that of metallic crystals but is considerably influenced by either uniform phason strains which can destroy the quasiperiodic long-range order, or by long-wavelength phason fluctuations leading to diffuse scattering. The structural perfection was also found to be extremely variable across the as-grown quasicrystalline grains and to be dependent on the presence and characteristics of inhomogeneities (pores and precipitates) often included in the quasicrystalline matrix. Regarding the grains that we used, it has been impossible to distinguish a clear influence of either the type of alloy or the growth method. It has, however, been noticed that Al-Pd-Mn and Al-Cu-Fe grains appeared less defective than Zn-Mg-RE grains and that the microstructure of these latter grains looks like that of crystals grown by the same technique. Annealing and mechanical polishing effects have also been analysed in the case of Al-Pd-Mn grains. It appeared that annealing improves the quasicrystalline lattice perfection by lowering phason strains insofar as no precipitates are nucleated. Mechanical polishing can introduce defects, located at the external surfaces, having the shape of bands.