The role of impurity dispersion and hardness anisotropy studies in NaCl:Sm crystals

The effect of the distributed impurities and their state of dispersion on hardness of crystal is studied from microhardness measurements on NaCl crystals doped with different concentrations of samarium both in as-grown state as well as after quenching them from various elevated temperatures. It is found that the small additions of impurity decrease the hardness. This has been explained on the basis of formation and dissolution of precipitates     

Effect of lattice oxygen on optical absorption, radiation hardness and thermally stimulated luminescence of BaF2 crystal

The influence of the presence of BaO impurity on the optical absorption, radiation hardness and thermally stimulated luminescence of BaF₂ has been investigated. The presence of oxygen impurity gives rise to three absorption bands in the UV region, peaking around 220, 280 and 335 nm. Further, the impurity is found to be detrimental to crystal hardness against ionizing radiations. The thermally stimulated luminescence (TSL) has been studied from gamma-irradiated crystals containing different fractions of BaO impurity. Four prominent glow peaks around 100°C (peak I), 150°C (peak II), 220°C (peak III) and 290°C (peak IV) are observed for crystals containing BaO impurity concentrations lower than 0.5% (by wt). For crystals containing higher impurity concentrations, two additional peaks around 75°C and 260°C are also observed. The kinetics of TSL emission is observed to be of first order, implying that the absorption and the emission centers responsible for TSL are the same. The normalized TSL output for peak I is found to vary linearly with the concentration of oxide impurity. This fact can be utilized to detect the presence of minute amounts of oxygen in BaF₂ lattice, which is crucial to the growth of crystals exhibiting high radiation hardness.     

纳米金刚石的结构、光学性能和热稳定性研究

纳米金刚石兼具纳米材料和金刚石的双重特性,呈现出与微米金刚石、块体金刚石截然不同的特点。本文以不同尺寸金刚石样品为研究对象,采用扫描电镜、X射线衍射、光谱学、热重分析技术对其结构、光学性能和热稳定性进行研究。结果显示样品尺寸分别为300 μm、30 μm和100 nm,大尺寸样品结晶质量较好,富含孤氮杂质,为Ⅰb型金刚石。纳米金刚石样品结晶较差,含有少量石墨残留,并含有H₂O、N—H和C—H键,说明其表面存在诸多有机活性基团。大尺寸金刚石样品存在中性和带负电荷的氮空位缺陷,产生较强荧光,而纳米金刚石由于存在诸多的有机基团和表面缺陷,形成非辐射中心,导致荧光猝灭。大尺寸样品在300~525 nm具有较强吸收,而纳米金刚石样品在紫外-可见-近红外整个区域均呈现出较强吸收,透过率显著较低。随着颗粒尺寸的减小,金刚石的起始氧化温度逐渐下降,氧化速率降低,因此大颗粒尺寸金刚石样品具有更好的热稳定性。     

掺杂对GaN晶体力学性能影响的研究

对GaN单晶力学性能的研究有助于解决其在生长、加工和器件应用中的开裂问题。本文围绕掺杂对GaN单晶力学性能的影响,通过纳米压痕法测试了不同掺杂类型(非掺、Si掺和Fe掺)GaN单晶的弹性模量和硬度,测试结果表明掺杂对GaN单晶的硬度有重要影响。Si掺、Fe掺GaN较非掺样品硬度有所提升,用重掺杂的氨热GaN单晶作为对照,也证明了这一结论。通过高分辨X射线衍射分析和原子力显微镜表征实验发现,晶体结晶质量、接触面积等因素对GaN单晶硬度的影响较小。对GaN表面纳米压痕滑移带长度和晶体晶格常数进行测试,结果表明,掺杂影响GaN单晶硬度的主要原因是缺陷对GaN位错增殖、滑移的阻碍作用和掺杂引起的GaN晶格常数的变化。     

Vibrational,optical and microhardness studies of trimethoprim DL ‐malate

Trimethoprim malate, an organic crystal, has been synthesized using slow evaporation method from its aqueous solution. Structural, optical and the mechanical properties of the grown crystal have been investigated by various characterization techniques which include FTIR spectra, single crystal XRD, UV‐Vis spectra and Vickers microhardness testing. The structure of the compound predicted by analysing the recorded FTIR spectrum compliments the structure determined using single crystal X‐ray diffraction. Single crystal X‐ray diffraction study reveals that the crystals are monoclinic [P2₁/c, a=12.9850 Å, b=9.3038 Å, c=15.6815 Å and β=111.065°]. The UV‐Vis spectrum exhibits maximum transparency (98%) for a wide range suggesting the suitability of the title compound for optical applications. The optical constants have been calculated and illustrated graphically. Microhardness tests have been performed on the cystal under study and the Vicker hardness number has been calculated. The work hardening coefficient is found to be 2.85 which suggest that the crystal belongs to the family of soft materials. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Connection of the Thermocapillary Flow Characteristics and the Impurity Distribution Pattern in Floating Zone Molten Molybdenum Single Crystals

The results of the impurity distribution in W-doped Molybdenum single crystals grown by electron beam floating zone melting are related to the characteristics of computed steady thermocapillary flow and impurity distribution within the molten zone. Particularly the influence of the number and the strength of eddies in the molten zone on the impurity distribution pattern in the grown crystal for different aspect ratios is considered.     

On the incorporation mechanism and distribution mode of impurities in potassium acid phthalate crystals grown from aqueous solutions

Mechanism of impurity structure formation in crystals grown from aqueous solutions has been studied on the example of potassium acid phtalate (abbreviated hereafter as KAP) single crystals. Gold decoration technique at an electronmicroscopic scale has been applied to the study of the distribution of uncontrolled impurities on KAP cleavage face (010) after 10, 20 and 30 days of growth, taking into consideration different growth rates in 〈001〉 and 〈001 〈 directions. A technique for visualization of impurities in water, based on the adsorption of these impurities by the surface of amorphous film of nitrocellulose (parlodion) and the vacuum decoration with gold of these impurities, has been developed. Differences in the impurity structure of KAP regions located in 〈001〉 and 〈001〉 directions from the seed have been established. In 〈001〉 direction after 20 days of growth impurity assemblies 0.1—0.4 μm in size are revealed, and in 〈001〉 direction heterogeneous impurity structure is revealed only after 30 days of growth. The real (impurity) structure of KAP outside impurity assemblies is quite homogeneous and is the same throughout the whole crystal volume, the impurities incorporating mainly into complex active centres. From comparison of the changes in time of the impurity structure of water used for crystallization solutions and the impurity structure of KAP crystals a conclusion is made that the impurity structure of crystals is “programmed” in the impurity structure of crystallization solutions which regularly changes with time, i. e. impurities from different kinds of assemblies which are selectively adsorbed by the growing crystal faces. The role of the adjacent to the growing face interfacial layers which control the growth rate and have a complex impurity structure is stressed.     

Effect of Various Impurities on the Hardness of NaCl Crystals

The hardness of NaCl crystal in the presence of mono, divalent and polyvalent ions were measured. Measurements were made in the indentation load range from 5 x 10^‐3 to 20 x 10^‐3 N. The measured data showed that there is an indentation size effect. Classical Meyer's law was used for the characterization of crystal hardness f NaCl. The Meyer index was found to be smaller than 2 indicating brittle material characteristic. The PRS model was also used for the determination of the load‐independent microhardness value. It was found that the crystal hardness of NaCl is chancing depending on the type of impurity and the concentration.     

Preparation of (KBr‐KCl)(OH−):(F2+)H color center laser crystal series and their spectral characteristics

In order to adjust and broaden the absorption spectrum and emission spectrum of the (F₂⁺)H type color center so as to match up to the pumping and to fit in with the demand of application, a (KBr‐KCl)(OH⁻):(F₂⁺)H color center laser crystal series was prepared by the process of single crystal growth, additive coloration, anneal, and light aggregation at 290 K and 77 K. The spectral characteristics of (KBr‐KCl)(OH⁻) crystals are investigated. It is found that the absorption and emission band of the (F₂⁺)H color centers in KBr‐KCl complex host crystals has a considerable adjustment and extensions compared to the color centers in single KBr or KCl crystal. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

红外LED用GaAs单晶的垂直梯度凝固制备研究

GaAs单晶是当前光电子器件的主要衬底材料之一,在红外LED中有着重要应用。但杂质浓度高、迁移率低等缺点会严重影响红外LED器件性能。为生产出低杂质浓度、高迁移率、载流子分布均匀、高利用率的红外LED用掺硅垂直梯度凝固(VGF)法GaAs单晶,本文研究了热场分布、合成舟和炉膛材质、工艺参数对单晶的成晶质量、杂质浓度、迁移率、载流子分布的影响。利用CGSim软件对单晶生长热场系统进行数值模拟研究,温区一至温区六长度比例为8∶12∶9∶5∶5∶7时,恒温区达到最长,位错密度达到1 000 cm^-2以下,成晶率达到85%。采用打毛石英合成舟进行GaAs合成,用莫来石炉膛替代石英炉膛,可以获得迁移率整体高于3 000 cm²/(V·s)的GaAs单晶,满足红外LED使用要求。对单晶生长工艺参数展开研究,采用提高头部生长速度、降低尾部生长速度的方式提高单晶轴向载流子浓度均匀性,头尾部载流子浓度差降低33%,尾部迁移率从2 900 cm²/(V·s)提高到3 560 cm²/(V·s)。单晶有效利用长度提高33...     

Structure and chemical composition of LiB3O5 surfaces

The electronic and structural properties of LiB₃O₅ (LBO) surfaces have been studied by X‐ray photoemission spectroscopy (XPS) and reflectance high‐energy electron diffraction (RHEED). The as‐grown (110) crystal face and mechanically polished (001) surfaces have been investigated comparatively. Electronic structure of LBO has been determined on as‐grown (110) crystal face previously cleaned by chemical etching with RHEED control. The correlation of valence band structure and measured binding energies with earlier reported results has been discussed. Core‐level spectroscopy reveals strong enriching of mechanically polished LBO surface with carbon, when nanodiamond powder is used as an abrasive. So high carbon level as C:B = 0.7 has been observed at the surface while the ratio Li:B:O remains according to LBO chemical composition. The association of LBO Kikuchi‐lines with strong background has been shown by RHEED analysis of the surface. Thus, the polished LBO surface constitutes a high structure quality LBO with the inclusions of some amorphous carbon compound. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of mercurous chloride single crystals

Mercurous chloride was purified by repeated sublimation using multichamber distillation column. Single crystals were grown by Physical Vapour Transport technique. During the process of purification of the material, very interesting habit modifications like dendrites and needles were observed. Vickers hardness tests were carried out on the (110) plane of the crystal for different orientations of the indentor. The shape of the impressions for different orientations of the indentor reveals the non-cubic structure of the plane. No structural phase transition in mercurous chloride was observed in calorimetry and optical studies.     

Growth and characterization of Bis Thiourea Zinc Acetate (BTZA)

Single crystals of BTZA have been grown by low temperature solution growth method using slow cooling process at an optimized pH of 3.5. The grown crystals have been examined under an optical microscope to study its surface morphology. The morphological studies show that the growth takes place by spreading of growth layers. Formation of rectangular shaped etch pit on the as‐grown crystal has been explained in relation to the growth conditions. Single crystal X‐ray diffraction analysis has been carried out to confirm the monoclinic system. Transmission spectrum reveals that the crystal has a low UV cut off of 434.5 nm and has a transmittance of 100%. Dependence of micro hardness on load has been studied. Powder X‐ray Diffraction and FT‐IR have been carried out to characterize the grown crystals. BTZA forms metal – sulfur bond and has good optical transmission in the entire visible region, which is the essential requirement for a non‐linear crystal. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The role of hydration and complexing in the mechanism of impurity influence on crystal growth

The influence of impurities of chlorides and nitrates of divalent Ca²⁺ and Ba²⁺ cations on the kinetic growth of potassium dihydrophosphate KH₂PO₄ crystals at a saturation temperature of 323 K and relative supersaturation of 0.03 has been investigated experimentally. It is established that the impurity acts differently, depending on the face index, the impurity concentration, cation hydration, and the stability of the complexes formed in the solution by impurity salt ions. A model is proposed to explain the different influence of impurity ions on the growth of crystal faces. This influence is determined by the different hydration of cations and enhanced association of cations and anions of impurity salts in the surface layer with a lower dielectric constant.     

FT‐IR spectroscopic and thermal studies on pure and impurity added calcium tartrate tetrahydrate crystals

Pure and impurity (strontium) added calcium tartrate tetrahydrate single crystals were grown by the gel method. The FT‐IR spectra of these crystals were recorded in the wavenumber range 400–4000 cm^–1. The thermograms of the grown crystals were recorded in the temperature range 50–900 °C. FT‐IR spectra reveals the presence of water molecules, O‐H bond, C‐O and carbonyl C=O bonds. The thermograms show that these crystals are thermally unstable and decompose into its oxide through many stages. DTA curve of the pure crystal shows three endothermic and one exothermic peaks. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

氧化锌单晶的水热生长与结晶习性

本文应用水热生长法,采用双温区高压反应釜,黄金内衬(φ35mm ×2mm),碱性溶液矿化剂,生长出了毫米级的透明氧化锌单晶,最大单晶可达2mm ×3mm ×6mm.所生长氧化锌晶体为纤锌矿型的六方晶体,晶体呈上部锥形的六棱柱体,{10(1-)1}、{10(1-)0}和{000(1-)}面有较大的显露平面.本文中从温差和填充度方面研究了实验条件对ZnO晶体的生长及其形貌的影响,使用黄金内衬前后的结果表明,用贵金属内衬可以有效阻止釜内壁杂质的进入,使晶体完整透明.     

杂质和缺陷对SiC单晶导热性能的影响

目前关于SiC单晶室温的导热性能,以及导热特性随温度的变化方面的研究报道还存在较大的差异,有关SiC单晶热导率的研究主要是沿c轴<0001>晶向或者垂直于c轴的某一晶向进行的,无法有效地解释热导率的各向异性。本文研究了4H-SiC和6H-SiC单晶目前关于SiC单晶室温的导热性能,以及导热特性随温度的变化方面的研究报道还存在较大的差异,有关SiC单晶热导率的研究主要是沿c轴0001晶向或者垂直于c轴的某一晶向进行的,无法有效地解释热导率的各向异性。本文研究了4H-SiC和6H-SiC单晶■,■,0001三个不同晶向上热导率以及其随温度的变化。对SiC单晶切割分别得到沿■,■,0001晶向的样品,尺寸为■12.7 mm×3 mm,利用闪光法对样品测试得到热扩散系数,通过计算获得了SiC单晶不同晶向的热导率数值,采用辉光放电质谱仪(GDMS)和扫描电子显微镜(SEM)进行了杂质和缺陷表征。实验结果表明,SiC晶体■,■,0001三个晶向的热导率随温度升高而下降,沿0001晶向的SiC样品热导率最小;含有较高杂质离子浓度的6H-SiC样品热导率高于4H-SiC样品;缺陷相比杂质对SiC晶体导热性能影响更大,缺陷是SiC热导率具有各向异性的主要原因。     

Effect of zinc doping on pentaerythritol tetranitrate single crystals

In this study, the effect of zinc impurity on the organic high explosive pentaerythritol tetranitrate (PETN) single crystal has been investigated with optical microscopy and ex situ atomic force microscopy (AFM). The optical images show that the crystal shape has a transition with a predictable trend from long crystal to compact one as the zinc concentration is increased. Also, the 2‐dimentional (2‐D) growth hillocks are observed clearly on (110) face with contact AFM. The crystal growth occurs on monomolecular steps generated by 2‐D nucleation and followed by layer‐by‐layer expansion, and the macro‐steps formed onto the surface before spreading laterally as step bunches. The zinc ions are incorporated in growth steps as the zinc concentration is increased. The mechanism of inorganic impurity on molecular crystallization growth is still unclear. However, the incorporation of impurities may significantly affect growth kinetics of defect structure, and the bulk properties of molecular crystals. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

KDP晶体中包裹体形成机制的探讨

本文介绍了包裹体对KDP晶体质量的影响,并从两个方面探讨了KDP晶体生长过程中包裹体的形成机制.通过分析KDP晶体表面原子结构研究了不同杂质的吸附情况以及杂质对生长台阶的阻碍作用,通过分析晶体生长过程中流体动力学和质量输运条件的变化研究了旋转晶体的流体切应力和表面过饱和度,结果表明吸附杂质对生长台阶的阻碍和表面过饱和度的不均匀造成了生长台阶的弯曲和宏观台阶的形成,导致生长台阶形貌的不稳定是包裹体形成的重要原因.     

Investigation on the Aqueous Solution for Growth of Bimetallic Thiocyanate Complex Crystal Materials

The stability of cadmium mercury thiocyanate (CMTC) crystal growth solution was mainly discussed. The effects of temperature, pH value, time and KCl concentration on CMTC crystal growth were investigated. The effects of pH value and KCl concentration on crystallization habit of CMTC were also studied. The results show that when pH value ranges from 2.5 to 3.8, the solution is relatively stable, under the condition of pH ≤ 2.0 or pH ≥ 4.0, the solution has poor stability and some powder appears. The solution becomes unstable at high temperatures. When the concentration of KCl is more than 27% there has not generated CMTC crystal in the solution, a new kind of material produced from solution. The pH value and KCl concentration affect crystalline morphology of CMTC crystal.