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.     

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.     

Mechanism of chemical dissolution of calcite in lactic acid

Effect of etching time and temperature on morphology of etch pits and etch rates in controlled dissolution of calcite by lactic acid it optically investigated in detail. Arrhenius equation is used to determine activation energy which is observed to change with the morphology of etch pits. Further, an attempt is made to understand the mechanism of dissolution by considering Laidler's theory of heterogeneous catalytic reactions.     

Surface structures of fluorite crystals

Optical studies have been made of the microstructures on the natural {100} and {111} faces of natural fluorite crystals. The protrudance of triangular elevations, growth pyramids, and natural etch pits have been observed on a large number of crystals. It is suggested that fluorite crystals grown by two-dimensional spreading and piling of growth layers parallel to {100} faces. The natural etch pits on {100} and {111} faces suggest that they have been produced as a result of a dissolution process in nature. The natural faces have been etched in the laboratory and it is established that the pits indicate the existence of linear defects in the crystals. The implications are discussed.     

Microtopographical studies of ‘a’-faces of natural analcite crystals

Vertical striation, isolated elliptical natural etch pits, natural etch grooves, flat-bottomed natural etch pits on ‘a’-(prism) faces of natural analcite crystals are illustrated and described. Freshly exposed surfaces due to general dissolution of these faces are reported. Isolated, well defined eccentric rhombus shaped natural etch pits are illustrated and, it is established that they are nucleated at sites of emergence of inclined dislocations on the face. Rows of tiny rhombus shaped etch pits along horizontal lines perpendicular to c-axis are illustrated and explained.     

Investigations on Flux Grown Cadmium Sulphide Crystals

Observations on surface microtopography of flux grown CdS crystals are reported. Crystals resulting with cooling rate above 30 °C/hr are reported to be dendritic crystals, while those with cooling rate below 30 °C/hr are reported to be normal crystals like mineral greenockite as reported in standard books on mineralogy. Reasoning for dendritic growth is briefly discussed. Growth patterns and etch pits formation on them are interpreted. It is established that these crystals grow by two-dimensional nucleation mechanism and by spreading and piling of growth layers.     

Etch pits of precipitates in CdZnTe crystals on (1 1 1) B surface

The etch pits of Te-rich and Cd-rich precipitates of the Cd_0.94Zn_0.04Te crystals situated on (1 1 1) B surface were distinguished from the dislocation etch pits and evaluated by using Everson Etching for the first time. By using an IR transmission microscope and a scanning electron microscope (SEM) with an energy-dispersive x-ray spectroscopy (EDX) analytical system, the characteristics of the precipitate etch pits were studied. The etch pit of the Te-rich precipitate which would influence the etch rate of its ambient materials shows the shape of triangle or hexagon with a rough surface different from the cone-shaped triangle etch pit as the dislocation etch pit. The etch pit of the Cd-rich precipitate is always enwrapped by large quantities of dislocation etch pits, which indicates the existence of the damaged layers around the Cd-rich precipitate. Base on the characteristics of the precipitate etch pits, the areal densities of the precipitates with the size larger than 5 μm on the substrate surfaces can be measured by the optical microscope with a magnification of 50 and under Nomarski mode. Compared with the conventional measurement method based on the IR transmission microscope (IRTM), the method of the etch pit observation (EPO) is more practical for measuring the areal densities of the precipitates of CdZnTe substrates.     

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.     

硫镓银晶体的化学腐蚀研究

采用改进的垂直布里奇曼(Bridgman)法自发成核生长AgGaS2晶体,在生长初期对生长安瓿籽晶袋进行上提回熔,生长出外观完整、无裂纹的大尺寸AgCaS2单晶体.采用XRD对晶体进行分析,获得了(112)、(001)和(101)面的高强度尖锐衍射峰.采用不同配比的腐蚀剂对晶体(101)、(112)及(001)晶面进行化学腐蚀,然后采用金相显微镜和扫描电镜观察,结果显示,(101)晶面蚀坑为清晰的近似三角形的四边形蚀坑,(112)晶面蚀坑为清晰的近似三角锥形,(001)晶面则呈现互相垂直的腐蚀线.初步分析了不同蚀坑的形成原因,计算出(101)和(112)面蚀坑密度约为105/cm2数量级.结果表明,改进方法生长出的大尺寸AgGaS2单晶体结构完整、位错密度低,质量较好.     

Chemical Etching of Calcite Cleavages by Diluted Solutions

Very low concentration of mineral acids and monocarboxylic acid (less then 0.001%) produces triangular etch pits on calcite cleavages at dislocations intersecting the surface. The orienation of triangular etch pits is opposite with respect to percussion mark on calcite cleavages. This may be due to opposite process of percussion and reaction at very low concentrations. When percentage of water is slightly decreased in both above acids, rhombic etch pits were formed. The non-coincidence of depth points and geometerical centres of rhombic etch pits are explained. The similarity of shape cycle will not hold at higher concentrations.     

Growth of Li2CO3 Single Crystals by Zone Melting Technique

Li₂CO₃ single crystals have been grown by zone melting technique in carbondioxide atmosphere. The diameter of the grown crystal depends on the growth rate. The quality of the crystal depends on the growth rate, temperature of the molten zone, choice of the seed and the temperature of the auxiliary furnace. The crystal shows cleavage plane. The etch studies on cleavage planes show that the etch pits are always triangular in character.     

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.     

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.     

Imaging crystal growth features using scanning force microscopy (SFM)

Crystal growth features on stearic acid, potassium nitrate, and potash alum have been determined by means of scanning force microscopy (SFM). Structures like growth spirals, etch pits, 2D-nuclei, and growth hillocks could be observed. The analysis of the face specific surface topographies leads to structures which correspond to those expected from kinetic measurements.     

Zum Nachweis von Versetzungen in β-Kupferphthalocyanin-Einkristallen

An etching technique was developed to investigate dislocations in β-copper phthalocyanine single crystals. Considering the expected content of dislocations and the etch pit symmetry the symmetric etch pits are correlated to [010]-edge dislocations on {201 }- and {001}-lattice planes with (001)- and (201 )-slip planes. Asymmetric etch pits on {001}- and {201 }-planes are connected with [010]-edge dislocations related to (100)- and (101 )-slip planes. The dislocation density on growth planes and cleavage planes is commonly lower than 100 cm⁻². [010]-screw dislocations are not observed, but their existence could not be excluded.     

Die Anwendung des Quantimet zur Ätzgrubendichtebestimmung an Silizium-Einkristallen

A quantitative estimation of the structure of etched silicon crystals is possible with the microscope Quantimet by a fast counting the number of particles, i.e. etch pits on {111}-planes. Boundary conditions of the measuring technique are the requisite size of the etch pits of from > 3 … 5 μm, a plane specimen surface, the correct optical magnification, threshold and acceptance width. Sources of errors due to the structure result from the overlap of etch pits at dislocation densities > 10⁴ cm⁻² which leads to an underestimation of the number of etch pits because of the reduced signal output. An overestimation is most caused by an unwished contrast in the surface which yields additional signal outputs. The errors will be eliminated by using a calibration curved. Due to the short time which is necessary for counting, the Quantimet is well suitable for routine testings and for quantitative evaluation of the structure defects (etch pit density) in silicon, including consideration of possible errors.     

Chiral Etch Pits on Sodium Chlorate Crystals

Microtopography of {100}, {110}, {111}, and {210} surfaces of sodium chlorate crystals etched in various solvents has been studied by optical microscopy. It has been established that etch pits formed on left- and right-handed crystals are chiral, and directions of dissolution steps reveal bond chains of the structure.     

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.     

Studies on Surface Structures and Etch Patterns on Habit Faces of Gel-grown Crystals of Iodates of Barium,Strontium, and Calcium

Microtopographical studies on habit faces of gel grown crystals (of different habits) of iodates of Ba, Sr, and Ca are illustrated and described. Etch patterns on these faces are illustrated and correlated to the observed growth patterns on the respective faces. Growth mechanism of the crystals is explained in light of the observed surface structures and etch pits suitably produced.     

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.