Dislocation etching of tin iodide single crystals

Single crystals of tin-iodide (SnI₂) have been grown using the controlled reaction between SnCl₂ and KI by diffusion process in gel medium. As grown (010) surfaces of the crystals have been optically studied. Characteristic etch pits have been observed on them. This suggests that SnI₂ crystals might go into dissolution in the acid-set gel. By successively etching (010) surfaces in a mixture of ammonia, acetic acid, and CdCl₂ solution, it is established that the pits indicate the site of dislocations in the crystals. This is further confirmed by comparing the etch patterns before and after chemically polishing (010) surfaces. The average dislocation density in the crystals have been evaluated and found to be 3.2 × 10³ cm⁻² and the implications are discussed.     

Dislocation studies by chemical etching on solution-grown NaSbF4 and Na3Sb4F15 single crystals

An attempt has been made to study the etch pit dislocations of isolated as well as matched pairs of cleavage planes of solution grown NaSbF₄ and Na₃Sb₄F₁₅ single crystals when etched with analar grade methyl alcohol and ethyl alcohol. On etching of cleavage faces the pits nucleate at the intersection sites of dislocations with the cleavage face. On successive etching of a cleavage face, arrays of triangular shape etch pits are observed. After prolonged etching some of the etch pits disappear. These pits are curved and terminated indicating that they are crystallographically non-oriented. One-to-one correspondence with respect to number, shape, position and structure of the pits has been established by etching of a matched cleavage face. The etch pit densities of both NaSbF₄ and Na₃Sb₄F₁₅ crystals are found to be 10³ per cm².     

Growth and dissolution of BaFCl crystals

Single crystals of BaFCl have been growth by flux technique using BaF₂ and BaCl₂. Etching with formic acid revealed dislocation etch pits on (001) cleavage faces of the crystals, at room temperature. The influence of etching parameters such as undersaturation, temperature and concentration of poison in the etchant is studied. Decreasing the undersaturation of formic acid by reducing the percentage of water and increasing the temperature of the etchant were found not to have any effect on the morphology of etch pits. However, as the CdCl₂ poison concentration is gradually increased, the orientation of the pits change from 〈100〉 to 〈110〉 at high concentration.     

Chemical dissolution of calcite cleavages in aqueous solutions of sodium hydroxide

Optical study of isotropic and anisotropic etch rates by controlled chemical dissolution of calcite cleavage surfaces employing aqueous solution of sodium hydroxide at various etching temperatures is presented. The etch rates are found to be independent of etching time. The isotropic etch rates are found to be smaller than anisotropic etch rates, whereas Arrhenius plots yield activation energy for anisotropic dissolution greater than that for isotropic etching. It is also shown from a comparative study of chemical effect of various etchants on calctie cleavages that for a given plane shape of dislocation etch pits the activation energy is constant and independent of etching temperature and etchant concentration and that it is a characteristic of the etchant and not of the crystal.     

pH值对KDP晶体位错结构的影响

在一定的过饱和度下,分别用点状和片状籽晶在不同pH值溶液中生长出了KDP晶体.利用化学腐蚀法对KDP晶体的不同晶面进行了腐蚀,得到了清晰的位错蚀坑.应用光学显微镜对位错蚀坑的分布特点和密度做了观察分析,发现很多位错蚀坑成线状排布.pH值对KDP晶体位错密度有较大影响,低pH值条件下生长出的晶体位错密度较大.测试了KDP晶体样本的透过率,结果表明位错密度对KDP晶体的透过率没有明显的影响.     

Thermal etch pits on calcite cleavages

Thermal etch pits are observed on calcite cleavages when the latter are kept at 520°C to 560°C in atmosphere for some hours. Boundaries of the above etch pits are circular, hexagonal and rhombic and they are dependent upon the temperature of etching. Different etch pit morphology is observed in chemical etching on calcite cleavages. It is conjectured that origin of thermal etch pits are different from that of chemical etch pits.     

Effect of Impurities on the Etching of Sodium Chloride Crystals

The results of a study of the effect of HgCl₂, ZnCl₂, PbCl₂ and CaCl₂ on the surface micro-morphology and kinetics of etching of {100} planes of NaCl crystals in methanol and ethanol are described and discussed. It was found that addition of an impurity to the solvent leads to the formation of contrasting dislocation etch pits, and that the overall dissolution rate in a solvent decreases with an increase in additive concentration. In the case of HgCl₂ impurity added to methanol terraced etch pits are observed, but their terracing behaviour diminishes with the increasing impurity concentration.     

Sub-boundaries on (002) cleavages of Li2CO3 single crystals

Linear arrays of dislocations (straight, terminating and curved) are observed on etching with 2% citric acid (002) cleavages of lithium carbonate (Li₂CO₃) single crystals, grown by zone melting technique. As the dislocations are non-uniformly spaced and disappear on successive etching, they may not be revealing low-angle grain boundary, nor slip traces as they are terminating and curved meaning crystallographically non-oriented. On the observation of experiments on successive etching and etching of matched pairs, it is concluded that the arrays of etch pits reveal dislocation walls (dislocation density 1.1 × 10⁶ — 1.5 × 10⁷ pits cm⁻²) probably created due to the localized thermal stresses released as a result of high temperature annealing of the crystal during growth. The implications are discussed.     

Etching behaviour of calcium fluoride crystals in hydrochloric acid vapour

Etching of octahedral cleavage faces of calcium fluoride crystals in hydrochloric acid vapour has been investigated. It is observed that dislocation etch pits and non-dislocation elevations are formed. The morphology of etch pits obtained by vapour etching is observed to be different from that obtained by weak acid solutions. The results are discussed in terms of the prevailing etching conditions.     

Etch pit morphology and calcium sulphate growth on {111} faces of calcium fluoride crystals etched in sulphuric acid

An investigation of the etching behaviour of cleaved octahedral faces of calcium fluoride crystals in sulphuric acid of different concentrations and at various temperatures is carried out. It is observed that the morphology of dislocation etch pits depends on the temperature and concentration of the acid. With an increase in the acid concentration, growth of whiskers, elongated platelets, hexagonal and dice-shaped elevations, spherulites and sheaves is observed. Temperature of the etchant also has an effect on their formation. By X-ray diffraction techniques, the compounds forming the whiskers and elongated platelets, and hexagonal and dice-shaped features are identified as CaSO₄ · 2 H₂O and CaSO₄, respectively. The mechanism of the growth of CaSO₄ · 2 H₂O and CaSO₄ and the change in the morphology of selective etch pit are discussed.     

化学腐蚀法研究Nd:YAG晶体位错

采用化学腐蚀法研究Nd∶YAG晶体位错.研究发现,腐蚀剂、腐蚀温度以及腐蚀时间对位错的显示都有影响.浓磷酸腐蚀剂在220 ℃下腐蚀20 min时,显示的位错最为清晰.蚀坑形状为菱形,经过计算,位错密度大约为10~3 cm~(-2).同一种腐蚀剂在不同的腐蚀时间所形成的位错蚀坑大小和形貌是不同的.同时发现在样品的边缘有位错塞积群.     

Etch- and Transmission Electron Microscope Investigations of Microdefects in (001) LEC-GaP Substrates

The etch pattern of (001) and (110) LEC-GaP doped with sulphur (N_DN_A in the range from 3–7 × 10¹⁷ cm⁻³) do not only show dislocation etch pits but fine pits, so-called “saucer pits” (S-pits). The distribution of S-pits, their etching behaviour and transmission electron microscope observations of etched samples indicated a clear correlation between S-pits and microdefects (fauted-, prismatic dislocation loops and precipitates).     

Dislocation activity in single crystals of stannic iodide

Single crystals of stannic iodide (SnI₄) have been grown employing the controlled-reaction between SnCl₂ and KI solutions by diffusion process in silica gels. As-grown (111) surfaces of the crystals have been optically studied. Characteristic growth spirals and hopper growth patterns have been observed on them. By successively etching (111) surfaces in a 0.2 N HCl solution, it is established that the pits indicate the sites of dislocations in the crystals. This is further confirmed by comparing the etch patterns before and after chemically polishing (111) surfaces. The average dislocation in the SnI₄ crystals have been determined and found to be 7.3 × 10² cm⁻². Observations of polygonisations are described and the implications are discussed.     

Shape of thermal etch pits and crystal structure in tellurium crystals

During the systematic study of thermal etching of tellurium crystals, various shaped thermal etch pits were observed on the {101 0} cleavage faces of this crystal. An attempt has been made to explain the shape of non-dislocation and dislocation etch pits. A simple model based on crystal structure and bonding of atoms has been suggested to explain the shape of etch pits.     

Inclined Dislocations in Synthetic Calcite Crystals

A large number of perfect (100) cleavages were obtained by cleaving the laboratory grown synthetic calcite crystals. By etching such cleavages in 20% ammonium chloride solution, it is established that the pits indicate the sites of dislocations in the crystals. This is further confirmed by comparing the etch patterns on matched cleavage surfaces. Eccentricity of the pits has been attributed to the inclined nature of dislocations. Existence of parallel dislocations seems to be due to the purity of the crystal. These observations are verified by comparing etch patterns produced on opposite faces of a thin flake (0.048 mm thick) and also by successive etching and polishing a cleavage surface. It is conjectured that curl-bottomed pits nucleate at the sites of screw dislocations in the crystal. The implications are discussed.     

Etching studies on {100} faces of MgO crystals in H3PO4 acids

The effect of temperature (20–100°C) and concentration of H₃PO₄ etching solutions on the etching behaviour of {100} faces of MgO crystals in investigated. It is observed that the formation of etch pits and pyramids and the values of dissolution rate depend on the etching conditions. The density of the pyramids in 33.08 N H₃PO₄ solution was found to be maximum at 20°C. From the plots of logarithm of dissolution rate versus inverse of absolute temperature, the values of activation energy and pre-exponential factor for the dissolution process are computed. It is found that for H₃PO₄ concentrations upto 22.05 N the value of the activation energy remains constant but that of pre-exponential factor increases with acid concentration. At higher concentrations, the activation energy decreases. The results are systematically described and discussed.     

Dissolution Kinetics and Etch Pit Morphology of CaF2 Single Crystals

The effect of temperature and concentration of HCl aqeous solutions on the etching behaviour on the face {111} of CaF₂ single crystals is investigated. It has been observed that the shape and the evolution of etch pits and the values of dissolution rate depend on the etching conditions. From the plots of logarithm of dissolution rate versus inverse of absolute temperature the values of activation energy and the pre-exponential factor for the dissolution process are computed. It has been found that the value of the activation energy and of the pre-exponential factor do not remain constant with acid concentration, but exhibit a minimum for the concentration of 6 N.     

Change in morphology and dislocation Etch Pits on the (010) Surface of Magnesium Orthosilicate Crystals

Investigations made on the etching behaviour of magnesium orthosilicate crystals in hydrochloric acid and melts of potassium and sodium hydroxides are described. It is shown that the morphology and orientation of the etch pits depend upon the concentration, composition and temperature of the etchant used. At low concentrations of HCl acid solution, the boat shaped pits produced are oriented along [100] direction while in concentrated acid, the hexagonal pits produced are oriented along [001] direction. At intermediate concentrations of about 5 N HCl acid the pits are square. KOH melt at 400 °C is found to produce rectangular pits with their longer sides parallel to [100] direction. The effect of a mixture of KOH and NaOH in different proportions in the melt is investigated. It is observed that square pits are obtained in melt of the mixture of KOH and NaOH in the proportion of 6:4 respectively. The mechanism responsible for the change in orientation of etch pits have been explained. The implications are discussed.     

Thermal Etching on Calcite Cleavages

Thermal etch pits are observed on calcite cleavages at very small range of temperatures in atmosphere. Different characteristics such as nonmovement of cleavage lines and dislocations, thermal percussion by gas molecules, are observed in thermal etching. It is found that chemical and thermal etching are not the same process for calcite cleavage etching. The origin of thermal etch pits is not at dislocations intersecting the cleavage surfaces.     

Causes of the formation of etch pits of different size and morphology on {100} faces of CsI crystals

Causes of the formation of dislocation etch pits of different shape and size on {100} faces of cesium iodide crystals by an etchant composed from 25–35 mg/1 CuCl₂ · 2 H₂O in 96% ethanol are studied. It is shown that one of the reasons of the change in the morphology of etch pits is the segregation of excessive iodine at dislocations.