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.     

Ätzuntersuchungen an Alaunen mit nichtwäßrigen Lösungsmitteln. Will Kleber zum Gedenken

This paper presents investigations on etching of KAl-, NH₄Al-, KCr- and K(Al, Cr)-alum crystals. The etchant was a solution of tartaric acid in ethyl alcohol which produces well-defined etch pits on {111} faces. The correspondence of etch pits with dislocations was investigated by KAl-alum crystals. Between microscopic holes in the crystals and dislocations are not stated.     

Etching Studies on Potassium Dichromate (KBC) Crystals

An investigation of the revelation of dislocations in potassium dichromate (KBC) crystals by etching in water, alcohls, and in inorganic acids mixes with acetone and alcohols is carried out. It is observed that several solutions including water, alcohols and organic acids produce disslocation etch pits on various faces of KBC crystals. Observations of twining and dissolution anisotorpy of (001) faces are also presented. Etching of (001) cleavage faces of same crystals in an etchant composed from 1 part HNO₃ and 3 parts acetone indicates the possible growth of another phase at low temperatures.     

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.     

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.     

Structural Etching of {001} and {110} Faces of Various AIIIBV Compounds

The present paper discusses the use of selective photoetching with H₃PO₄:H₂O₂ for characterizing various A^IIIB^V compounds and detecting misfit dislocations in transition layers. For GaP, the results obtained are compared with those realized with the use of an AB etchant for which suitable conditions for the structural etching of {001} material and the characterization of cleavage faces are given. The direction of the dislocation line is inferred from the shape and orientation of etch pits. The etch figures of different types of misfit dislocations are discussed.     

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.     

Low-angle grain boundaries in synthetic calcite crystals

Single crystals of calcite grown in this laboratory by the solution method have been cleaved along (100) planes and have been chemically etched in 20% NH₄Cl and 5% citric acid solutions. Rows of equally spaced etch pits have been observed. By etching matched cleavage faces, correspondence has been established for low angle grain boundaries. Correspondence of grain boundaries has also been observed on the two sides of a thin plate 0.68 mm thick. It is observed that the density of pits in all the corresponding rows of matched cleavage faces and on the two sides of a thin plate is the same. Correspondence in the matching of four boundaries forming a node has also been observed on the matched faces and the relation n_a = n_b = n_c + n_d (where n is the pit density along the boundary line) has also been established. The implications are discussed.     

Selective etching of ZnTe in HF:H2O2:H2O solution: Interpretation of extended defect‐related etch figures

HF:H₂O₂:H₂O solution (40%wt.HF: 30wt.%H₂O₂: H₂O, 3:2:1 by volume) was used to reveal extended defects (line, face and volume defects) in bulk ZnTe crystals grown from Te solution. The etch patterns were analyzed based on their size, shape and distribution. The etch figures, both in the shape of pits and hillocks with high resolution, show forms controlled by the symmetries of the respective faces were produced. Two different sizes of pits were observed, the larger‐size pits correspond to dislocations penetrating the surface, however, the smaller‐size texture pits are produced on the defect‐free region, which serve as standard pits on respect faces. The face defects, such as grain boundaries, sub‐grain boundaries, dislocation walls, twins and stacking faults, can be all displayed clearly. Another essential feature of the etchant is that, it can effectively dissolve Te‐rich phase (Te inclusion/precipitates), which makes it promising to reveal the shape of this volume defect.     

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.     

Etching of CaF2 single crystals in silica gels

Etching of {111} cleavage faces of CaF₂ crystals in aqueous solution of 50% HCl is carried out in citric acid set silica gel, and the kinetics of growth of etch pits at the sites of dislocations is investigated as a function of temperature, time of etching and height of gel column above the crystal surface. It is observed that the transient period required to initiate etch pit at the sites of a dislocation decreases (1) at particular temperature, with a decrease in gel height, and (2) for a particular gel height, with an increase in the temperature of etching. It is also observed that the morphology of dislocation etch pits remains triangular irrespective of the gel height and the temperature of etching. The results are compared with those of solution etching and discussed.     

硫镓银晶体(112)面蚀坑形貌研究

本文报道了一种能在室温下对硫镓银晶体(112)面进行择优腐蚀的新腐蚀液配方,采用新腐蚀液对改进的Bridgman法生长的AgGaS2晶体进行腐蚀,用扫描电镜对蚀坑进行了观察,得到了清晰的(112)面蚀坑形貌,形状为三角锥形.初步解释了蚀坑的形成原因.AgGaS2晶体低指数的{100}面的腐蚀速度较慢,在腐蚀过程中逐渐显露出来,最终使晶体(112)面呈现出三角锥形蚀坑形貌.     

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.     

Etching studies of tungstenite (WS2) crystals in acids

Single crystals of tungstenite (WS₂) have been grown by direct vapour transport or sublimation method. An etchant capable of revealing the sites of dislocations has been developed. The effects of etching time, etchant concentration and temperature on the selective etch rate have been worked out. It is seen that the etch rate is independent on time, but is influenced by the temperature and concentration of the etchant. The values of activation energy determined from the etch rate against temperature plots established that the process of etching in chromic acid is chemical reaction rate controlled. The effect of addition of HF to the above etchant has led to some further interesting results.     

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.     

Etching and kinetics of dissolution of Mo1−x WxSe2 single crystals

The dislocation etchant has been established for single crystals of Mo_1−xW_xSe₂ system. Effect of concentration of an etchant on the etch rate has been discussed. The morphology of etch pits is also described. The etch activation energies for all the compositions of these crystals for a particular concentration (7 N) of an etchant has been found out. The etch activation energies for a particular composition (x = 0.4) of crystals with different concentrations of an etchant have been investigated and the results have been discussed.     

Studies on twin boundaries in calcite crystals

Natural single crystals of calcite have been cleaved along (100) planes and cleavage faces have been etched in 2% and 3% citric acid solutions. Etching produces twin boundaries oriented in 〈010〉 directions. The etch pits on the two sides of the twin boundary are oppositely oriented. It has been conjectured that the rows of pits might have been formed due to etching of dislocations on twin boundaries. One to one correspondence of twin boundaries has been established on matched cleavage faces. This is further confirmed by studying the induced twin regions produced on a (100) cleavage plane by indenting that plane itself. The implications are discussed.     

Chemical kinetics of dissolution of BaMoO4 crystals

An etchant capable of revealing the sites of dislocations in the flux-grown crystals of BaMoO₄ has been established. Using this etchant (HNO₃), effect of etching time, acid concentration and temperature on the selective etch rate is demonstrated. It is established that the process of dissolution in unstirred HNO₂ solutions is one of the diffusion rate controlled; an empirical equation governing the kinetics has been suggested.     

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.     

Dislocation Etch Studies on Diammonium Hydrogen Citrate Single Crystals

Diammonium Hydrogen Citrate single crystals have been grown from aqueous solution. The etch technique for defect studies is applied to these crystals. Propionic acid is shown to be a reliable etchant capable of bringing out dislocations intersecting the (001) face. Various other interesting features observed during etching are also presented and discussed.