水热法合成Zn1-xMnxO：Sn和Zn1-x-yMnxCoyO：Cu晶体的磁性

本文采用水热法,以ZnO为前驱物,添加适量的MnCl2·4H2O、SnCl2·2H2O和MnCl2·4H2O、CoCl2·6H2O、CuCl2·2H2O,3 mol/L KOH作矿化剂,430℃反应24 h,分别合成了Zn1-xMnxO:Sn晶体和Zn1-x-yMnxCoyO:Cu晶体.用扫描电镜(SEM)对合成物形貌进行分析,结果表明,Zn1-MnxO:Sn晶体为六棱柱状晶体,直径约为10 μm,较大面积显露正极面c{0001},同时也显露负极面-c{0001}、正锥面p{1011}、负锥面-p{1011}和柱面m{1010}.Zn1-x-yMnxCoyO:Cu晶体也显露负极面-c{0001}、正锥面p{1011}、负锥面-p{1011}和柱面m{1010},{0001}显露面小于{0001}.X射线能谱(EDS)分析表明晶体主要成分为ZnO,Mn2 、Co2 离子掺杂量超过2%;SQUID磁性测量显示所合成晶体在25 K具有反铁磁特征,高温为顺磁性.     

水热法合成氧化锌晶体

本文采用水热法,通过改变矿化剂浓度,合成了具有不同晶体形态的氧化锌晶体.在430℃,填充度为35;,矿化剂浓度为1M KOH时,只合成了氧化锌微晶.氧化锌晶体的长度为几百纳米到几微米,晶体形状为六棱锥体.当矿化剂为3M KOH或2M KOH、1M KBr时,合成了高质量的氧化锌晶体.反应 24h后,合成的最大晶体长度(c轴方向)超过1mm,晶体呈单锥六棱柱体,显露柱面m{1010}、锥面p{1011}、负极面o面{0001}.另外还生成多种不同形态的微晶体,最小几微米,中等的几十微米,为六棱锥体,显露锥面p{1011}、负极面o面{0001},没有显露柱面.     

In掺杂对水热法合成ZnO晶体形貌的影响

本文采用水热法,在ZnO中添加In2O3为前驱物,3mol/L KOH作矿化剂,温度430℃,填充度35;,反应24h,制备了掺In的ZnO晶体.未掺杂In2O3合成的纯ZnO晶体呈六棱锥状,显露负极面-c{0001}、六棱锥面+p{1011}和-p{1011},一般不显露{0001}面.前驱物中掺杂In2O3所合成的ZnO晶体呈六角片状,直径约为5～20 μm,大面积显露{0001}面,另外还显露正锥面+p{1011}、负锥面-p{1011}和负极面-c{0001}.由此可见In掺杂可以明显的改变晶体的形态,使c轴极性快速生长趋向得到明显改善,有利于降低晶体生长缺陷.当采用ZnO晶片为籽晶时,通过水热反应在晶片上生长了一层掺In的ZnO薄膜,通过Hall参数测量得到晶体膜层的电子迁移率约为22cm2/(V·s),载流子浓度约为2×1020 cm-3,具有良好的导电性,同时也说明In可以微量掺入氧化锌晶体.     

LiOH矿化剂对水热合成ZnO晶体形貌的影响

本文研究了在430℃,填充度为35用了3mol/L,5mol/L LiOH做矿化剂,所获得晶体均为10μm以下的微晶.当矿化剂为1mol/L LiOH和1mol/L KBr时,所获得晶体同样为几微米的微晶,显露完整的正极面{0001}、负极面{0001}、锥面{1011}和柱面{1010}.矿化剂为3M LiOH和3M KBr时,出现个体较大的晶体,直径超过100μm,显露正极面{0001}、正锥面{1011}和柱面{1010},负极面出现缺损现象.由此说明和K+相比溶液中的Li+不利于生成大尺寸ZnO晶体.     

水热法合成Mnx Zn1-xO微晶体

本文采用水热法合成了MnxZn1-xO晶体,水热反应条件为3mol·L-1KOH作为矿化剂,填充度为35;,温度为430℃,在Zn(OH)2中添加一定量的MnO2为前驱物,反应时间为24h.通过X射线能谱仪测量了晶体中的Mn含量,随着前驱物中MnO2含量的增加,晶体中Mn的原子百分比随着增加,Mn最大原子百分比含量超过了2;,晶体的形貌具有纯ZnO晶体的六角柱形特征.显露柱面m{1010}、锥面p{1011}、负极面O面{0001}和正极面{0001}.晶体直径为50～200μm,高度为20～100μm.     

碱土金属离子对ZnO极性生长的影响

本文采用水热法,以3mol/L KOH为矿化剂,填充度35%,温度430℃,通过添加适量比例的MgCl2.7H2O和CaO,合成了非极性生长的ZnO晶体。当Mg2 :Zn2 =2%和Ca2 :Zn2 =2~3%时,晶体c轴方向生长速度明显减弱,{0001}方向的极性生长得到控制,所合成的晶体大面积显露正极面 c{0001},同时显露负极面-c{1001-}、正锥面 p{101-1}、负锥面-p{101-1-}和柱面m{101-0}。X光能谱(EDS)没有检测到晶体中含有碱土金属离子。     

不同矿化剂对水热法生长的ZnO晶体发光的影响

采用水热法,以3 mol/L KOH为矿化剂,填充度35%,温度430℃,前驱物Zn(OH)2,比较研究了三种矿化剂条件下合成晶体的形貌和发光性能。三种矿化剂条件分别为样品1,3 mol/L KOH;样品2,3 mol/L KOH,1 mol/LLiOH;样品3,3 mol/L KOH,CaO∶Zn(OH)2=2%(物质的量百分比)。添加适量比例的LiOH或CaO,合成了非极性生长的ZnO晶体,晶体c轴方向生长速度明显减小,所合成的晶体大面积显露正极面c{0001},同时显露负极面-c{0001}、正锥面p{101}、负锥面-p{10}和柱面m{100}。只添加KOH或辅助添加LiOH时,合成晶体的发光光谱中只有可见光谱,无紫外线带边跃迁发光谱,说明晶体缺陷发光中心较多。添加CaO时合成晶体的发光光谱中有较强的紫外带边跃迁发光,说明晶体缺陷发光中心减少。     

石英晶体碱(KOH)腐蚀像及其与酸(HF)腐蚀像对比研究

本文用KOH溶液对石英晶体进行腐蚀实验.对石英晶体不同结晶学方向的5个品面(切面)的腐蚀像进行观察,建立了石英碱腐蚀形貌的立体模型,并与酸(HF)溶液所腐蚀的同样5个面的腐蚀像进行对比.研究发现碱腐蚀与酸腐蚀在柱面{1010}和菱面{1011}、{0111}上有很人不同,在柱切面{1120}、{2110}上有相同之处.但它们都反映各品面及晶体的对称特点.该研究对揭示矿物晶体在不同酸碱地质环境下腐蚀的特点具有指导意义.     

水热合成奇异形态的ZnO晶体

本文采用水热法,以3mol/L KOH为矿化剂,填充度35;,温度430℃,在Zn(OH)2中添加SnCl2·2H2O,添加量为Sn2+:Zn2+=2;条件下,合成出ZnO晶体.产物中除了大量短六棱柱形晶体外,还出现了部分冰激凌形晶体.六棱柱形晶体具有典型的ZnO特征,显露正极面c{0001}、负极面-c{000-1}、柱面m{10-10}、正锥面p{10-11}和负锥面-p{10-1-1}.而冰激凌形晶体有明显的六棱锥晶体外壳,X光能谱(EDS)检测证实晶体各部位的组分均为ZnO.     

Mn、Cu共掺ZnO磁性的研究

本文采用水热法,分别以ZnO、Zn(OH)2为前驱物,添加一定量的MnCl4.4H2O和CuSO4.2H2O, 3mol/LKOH作矿化剂,温度430℃,填充度35%,反应24h,制备了Mn、Cu共掺ZnO晶体。当前驱物为Zn(OH)2时,所得晶体大部分为短柱状晶体,显露正负极面{0001}、{0001-}、负锥面-p{101-1-}和柱面m{1-010},长度约为30 ～50μm。少部分晶体为单锥六棱柱状,显露正锥面p{101-1},柱面m{1-010},负极面-c{0001-},晶体的长度约为100μm,长径比为5:1。当ZnO用作前驱物时,短柱状晶体长度大约为10 ～30μm,晶体的六棱对称性都出现较大的偏差。X射线荧光能谱分析表明,前驱物为ZnO、Zn(OH)2时,Mn离子含量在分别为3.19%和1.62%原子分数,没有检测到Cu离子。虽然Mn、Cu离子的掺入会明显影响晶体形态,磁性测量显示掺杂Mn、Cu的ZnO仍为反铁磁。     

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.     

Kinetic Investigations within the Transition Region from Polyhedral to Skeletal Growth Mode (V). Growth Kinetics of the Pyramidal Face of Zinc Single Crystals under Diffusion Conditions

The growth kinetics of the pyramidal face of zinc single crystals is studied in the presence of argon. The curves size vs. time provide evidence that smaller crystals grow in a kinetic regime and after reaching a certain critical size their growth continues in a diffusion regime. The growth kinetics of faces {101 } and {0001} are compared. It is established that the growth of both faces simultaneously changes from a kinetic to a diffusion growth mode. During the transition between the two regimes, however, loss of the morphological stability only of the smooth {0001} face is observed, while the {101 } face with macro steps formed on the surface acquires a skeletal shape after prolonged growth. It is shown that the appearance of morphological instability depends on the surface structure of the crystal faces.     

Optical imaging of the growth kinetics and polar morphology of zinc tris(thiourea) sulphate single crystals

Growth kinetics of zinc tris(thiourea) sulphate (ZTS) single crystals was imaged in two different growth geometries using laser shadowgraphy technique. Growth rates of the {010} and {001} faces were computed as a function of supersaturation. The time evolution of polar morphology of ZTS crystal based on the growth rates is presented. Except (00 ) face, all the other three faces are found to have a dead zone resulting in large induction period of growth. The anisotropy in the growth rates of the (001) and (00 ) faces was very high, resulting in polar morphology. Different chemical environments on two sides of the (001) slice are suggested as the possible cause for the polar morphology of the crystals. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Yb∶YAl3(BO3)4晶体形貌与生长速度的关系

观察测量了不同生长速度(相应于不同降温速度)自发成核生长的Yb∶YAl3(BO3)4晶体形貌。粒度较大(>2mm)的晶体不管降温速度快慢形态都很简单,只发育六方柱｛1120｝和菱面体｛1011｝;粒度较小(<2mm)的晶体形态随降温速度增快而变复杂,发育一些罕见的高指数晶面。说明在生长速度较快的条件下,在晶体生长早期,一些高能面发育,在晶体生长后期已尖灭了,晶体生长的大部分时间是在低能面｛1120｝和｛1011｝上进行的。对比了不同生长条件下晶面的粗糙度,随着降温速度的增快,六方柱面｛1120｝和菱面体面｛1011｝由光滑变粗糙,顶面｛0001｝永远是粗糙的。从晶体结构上定性地探讨了3种晶面的杰克逊因子α及生长机理     

In situ Observed Twin Formation on ZnSe Crystals Growing by Sublimation

ZnSe crystals were grown by sublimation in closed ampoules between 1335 K and 1365 K. The growth was observed in situ with a video camera after an abrupt change of the supersaturation. The crystals developed preferably {110} faces. Repeatedly a nucleus was formed in ortho-twin position on a small {111} face which truncated the corner of three adjacent {110} faces. The repeated twin formation led to a preferred growth into the relevant 〈111〉 direction. The twinning already occurred at a low supercooling of less than 1 K and accelerated the growth distinctly.     

Growth‐Sector Boundaries and Growth‐Rate Dispersion in Potassium Alum Crystals

Crystals of potassium alum, pure and slightly doped with Cr³⁺, were grown from aqueous solution by slow temperature lowering. In addition, short re‐dissolution periods were introduced in order to provoke growth defects and changes of growth rates. Crystal slices of about 1 mm thickness were studied by conventional LANG X‐ray diffraction topography using MoKα radiation. For Cr‐doped crystals, boundaries between {100}, {100} and {111} growth sectors appear by pronounced dynamical X‐ray topographic contrast similar to that of stacking faults. Re‐dissolution experiments provoke the formation of inclusions on {100} faces, followed by an increase of the {100} growth rate by the factor of about six, relative to the neighboured {111} faces. X‐ray topographs show that this increase is correlated with the formation of dislocations, which interestingly have pure‐edge character. During further growth these dislocations penetrate the {100}‐{111} growth sector boundary and vanish from the {100} face, which slows down and finally adopts its former growth rate before re‐dissolution.     

水热法BSO晶体腐蚀像及与晶体对称的关系

对水热法生长的两种不同结晶习性的 BSO晶体进行了腐蚀像的观察研究,得到了{100}、{110}、{211}、{111}晶面的腐蚀形貌特征,建立了BSO晶体腐蚀像在三维空间分布的立体模型。研究发现不同单形晶面的蚀坑形态不同,但都体现了晶体的对称性。不同晶面腐蚀难易程度与晶体结构有关。     

Surface Smoothing of Copper Single Crystals Using POM (Potential Oscillating Method)

The deposition of metals is a process to get metallic coatings on metals. The potential oscillating method (POM) allows dissolution and deposition processes in parallel. Using this method the crystal's habit becomes more perfect, and the equilibrium form can be obtained. It is mostly dominated by the {111}- and the {100}-face, as usual for cubic face centered crystals. The crystallographic faces develop more clearly and become smoother. This paper deals with the determination of the ideal conditions for the electrochemical experiment using copper single crystals, and the analysis of the surface topography using light microscopy, and scanning force microscopy.