Chemical etching of deformation sub-structures in quartz

Chemical etching of dislocations has been studied in natural and synthetic quartz single crystals, in deformed synthetic quartz and in naturally and experimentally deformed quartzites. The ability of different etchants to produce polished or preferentially etched surfaces on quartz is described. Dislocation etching was achieved on all crystal planes examined by using a saturated solution of ammonium bifluoride as the etchant. Appropriate etching times were determined for etching quartzites for grain size, subgrain boundaries, deformation lamellae, dislocations and twins. Growth and polished surfaces of synthetic single crystal quartz were similarly etched and dislocation etch pits, characteristic of various orientations were found. The use of ammonium bifluoride proved to be expecially advantageous for the basal plane, producing a polished surface with etch pits, suitable for dislocation etch pit counting. “Double” etch pits have been found on Dauphiné twin boundaries on the basal plane and the first order prism, using this etchant. Slip lines and deformation bands were suitably etched on deformed synthetic crystal surfaces for identification of the slip planes. Other acidic etchants have been explored and their application to the study of deformation structures in quartz crystals is discussed.     

藏南超基性岩的塑性流变

随着深部构造研究的不断深入,岩石流变作用日益受到人们重视,普遍认为塑性流变是地壳深部构造形成的主要机制。超基性岩的流变作用目前已成为研究上地幔流变、岩石圈板块动力学和热对流,甚至震源机制的重要内容。 本文拟通过对构成雅鲁藏布江蛇绿岩套底部的藏南超基性岩的研究,重点划分塑性流变的结构类型,探讨不同结构类型中橄榄石的组构特征及实际存在的滑动系,用不同方法计算超基性岩形成和侵位过程中的流动应力值,并认为由于橄榄石塑性流变而获得的晶格方位排列是造成地震波速度不连续性的主因,岩石的塑性流动有可能是深部能量释放和诱发     

Dislocation recovery in fine-grained polycrystalline olivine

The rate of static dislocation recovery in Fo₉₀ olivine has been studied under conditions of high temperature and controlled atmosphere in compressively deformed polycrystals hot-pressed from synthetic (sol–gel) and natural (San Carlos) precursor powders. The sol–gel olivine, containing a small fraction of orthopyroxene, was deformed to a final strain of 19% with a maximum differential stress of 266 MPa whereas the San Carlos specimen was deformed to 15% strain and 260 MPa differential stress. Small samples cut from these deformed materials were annealed under high-temperature, controlled atmosphere conditions, for different durations to allow partial recovery of the dislocation sub-structures. Oxidative-decoration of the microstructural features, followed by backscattered electron imaging at 5 kV and image analysis, was used to determine dislocation density. The variation of dislocation density ρ with time t at absolute temperature T was fitted to a second-order rate equation, in integral form, 1/ρ(t) − 1/ρ(0) = kt with k = k ₀ exp(−E _a/RT). The activation energy E _a of the recovery process is 240 ± 43 and 355 ± 81 kJ mol⁻¹ for sol–gel and San Carlos olivine polycrystals, respectively. The measured rates are one to two orders of magnitude lower than those reported in previous studies on natural single crystal olivine. The difference may be explained by several factors such as high dislocation densities measurable from large areas at high magnification for the SEM and the technique used to estimate dislocation densities. Comparison between fine-grained sol–gel olivine and the coarser-grained San Carlos olivine aggregate did not indicate that grain boundaries play an important role in dislocation recovery, but the absence of grain boundaries might also have contributed to the high dislocation recovery rates previously measured for single crystals.     

Growth and characterization of synthetic iron-bearing olivine

Single crystals of olivine were grown at 0.1 MPa total pressure in a floating-zone image furnace. Composition of crystals grown ranged from 67 mol% forsterite to 90 mol% forsterite. Improvements in the crystal growth technique allowed growth of large crystals (0.005 m diameter, 0.070 m length) with very low dislocation density, no visible bubbles, and no cracks. The most significant improvement was the addition of a platinum-wound resistance heater internal to the image furnace. This heater provided the dual improvements of better control over oxygen fugacity from a CO/CO₂ gas mix and alteration of the crystal growth interface resulting in a significant reduction in crystal defects. No subgrain boundaries have been observed in crystals growth here and dislocation densities on the order of 10⁸-10⁹ m^-2 have been achieved. Iron concentration is nearly uniform across the diameter (0.005 m) of crystals and varies approximately 5 mol% along the crystal length (0.040 to 0.050 m).     

Electron microscope study of peridotite xenoliths in kimberlites

Dislocation structures in naturally deformed olivine from garnet peridotite xenoliths from South African kimberlites have been studied by electron microscopy. The substructure consists mainly of straight subboundaries of dislocations with Burgers vectors [001]. Most of the dislocations have both edge and screw components, and the slip planes are mainly (100). The dislocation density between the subboundaries is low.The slip planes in olivine are discussed in relation to the olivine structure. The observed dislocation structures seem to indicate that the large difference in strain rate between natural and experimental deformation will produce a difference in the slip mechanisms.The nature of the deformation lamellae visible in optical microscope is discussed.     

Experimental deformation of a synthetic dunite at high temperature and pressure. II. Transmission electron microscopy

We have performed detailed transmission electron microscope on most of the deformed synthetic dunite specimens prepared in the study by Zeuch and Green (1984). We have identified three basic types of sub-boundaries, simple tilt walls in (100) and (001). composed by b = [100] and b = [001] edge dislocations, respectively, and twist boundaries in (010) composed of b = [100] and b = [001] screws. We have also observed more complex, asymmetric lilt boundaries in (100) and (001). Like the (010) twist boundaries, these asymmetric tilt walls are common only at the highest temperatures and lowest strain rates. Subgrain development is extensive at the higher temperatures and lower strain rates, and subgrains are composed of the above-mentioned three types of sub-boundaries; edge components in (100) and (001) ire “knitted” to screw components in (010) as described by Kirby and Wegner (1978) for naturally deformed olivine. In many areas of the samples which we studied, subgrain development is not observed, but parallel arrays of tilt boundaries of one type or the other are present. At higher temperatures and lower strain rates. “(100) organization” (Durham et al., 1977) is common; this structure consists of parallel arrays of (100) tilt boundaries with b = [100] screws connecting the sub-boundaries. At lower temperatures we have observed an analogous arrangement of (001) sub-boundaries and b = [001] screws, which we refer to as “(001) organization”. Under all experimental conditions, dislocations with b = [100] and b = [001] are present in approximately equal numbers. However, the two types of dislocations also have distinctly different geometries under all test conditions. We suggest that the transition from slip parallel to [001] to slip parallel to [100] with increasing temperature, which has been reported in earlier studies may also depend upon water content. The substructures which we observe are virtually identical to those seen in many naturally deformed peridolites. and we conclude that the mechanisms involved in both natural and laboratory deformation of olivine polycrystals are similar. On the other hand, the substructures reported here are very different from those observed in experimentally deformed olivine single crystals. It seems likely that these substructural differences reflect fundamental differences in the behavior oh single crystals and polycrystals. which are in turn reflected in different measured creep strengths.     

Deformation microstructures of olivine in peridotite from Spitsbergen, Svalbard and implications for seismic anisotropy

To understand the deformation mechanism and seismic anisotropy in the uppermost mantle beneath Spitsbergen, Svalbard, in the Arctic, the deformation microstructures of olivine in the peridotite of Spitsbergen were studied. Seismic anisotropy in the upper mantle can be explained mainly by the lattice-preferred orientation (LPO) of olivine. The LPOs of the olivine in the peridotites were determined using electron backscattered diffraction patterns. Eight specimens out of 10 showed that the [100] axis of the olivine was aligned subparallel to the lineation and that the (010) plane was subparallel to the foliation, showing a type A LPO. In the other two specimens the [100] axis of olivine was aligned subparallel to the lineation and both the [010] and [001] axes were distributed in a girdle nearly perpendicular to the lineation, showing a type D LPO. The dislocation density of the olivine in the samples showing a type D LPO was higher than that in the samples showing a type A LPO. The result of an Fourier transformation infrared study showed that both the types A and D samples were dry. These observations were in good agreement with a previous experimental study ( Tectonophysics , 421 , 2006, 1 ): samples showing a type D LPO for olivine were observed at a high stress condition and samples showing both types A and D LPO were deformed under dry condition. Observations of both strong LPOs and dislocations of olivine indicate that the peridotites studied were deformed by dislocation creep. The seismic anisotropy calculated from the LPOs of the olivine could be used to explain the seismic anisotropy of P - and S -waves in the lithospheric mantle beneath Spitsbergen, Svalbard.     

橄榄石位错构造的扫描电子显微镜研究

利用扫描电镜的背散射电子图象(BEI)对玄武岩及金伯利岩所含幔源包体中橄榄石的缀饰位错进行了研究。实验结果表明,位错类型和颗粒边界图象清晰,又便于观察。这种观察位错的方法其分辨率比光学显微镜观察结果约高一个数量级。背散射电子图象位错方法特别适用于研究天然的和实验变形橄榄石的高位错密度和密集型边界,对于确定显微构造的定量参数也十分有利。     

Evaluation of the non-hydrostatic stress produced in a multi-anvil high pressure apparatus

Olivine single crystals have been deformed under high confining pressure (P=5?GPa) and temperature (T=1400?°C) conditions in a multi-anvil high pressure apparatus. NaCl, diamond and NaCl+diamond (2:1 by volume) powders were encapsulated along with the olivine single crystals in order to produce a range of stress states. The change of the non-hydrostatic stress transmitted to the olivine samples, enclosed within these three different media, during heating has been evaluated by observation of dislocation microstructure and density. A higher differential stress can be generated with diamond powder (0.1?GPa) than with NaCl powder (0.02?GPa). Although an intermediate differential stress between 0.1?GPa and 0.02?GPa had been expected to be generated using NaCl+diamond powder, the generation of non-hydrostatic stress in the olivine sample was unsuccessful. This may be caused by the fact that compaction (or sintering) proceeded in the capsule throughout the experiments. The most important finding of these experiments is that a constant non-hydrostatic stress can be applied to a sample under very high pressure and temperature conditions within the multi-anvil high pressure apparatus for the duration of the experiment. This approach is therefore suitable for investigating the steady-state rheological properties of mantle minerals at near-mantle conditions.     

橄榄石腐蚀像立体模型构建及其岩石组构研究之启示

利用20% 浓度的氢氟酸（HF）对橄榄石晶体不同方向之切面进行了腐蚀实验,以期建立三维立体构型。在晶体上选 取垂直任一结晶轴的单形,如（100）,（010）,（001）等平行双面,（110）,（011）,（101）等菱方柱和（111）菱方双锥进 行了腐蚀实验,由原子力显微镜记录各个切面腐蚀像。结果显示,相同切面上的腐蚀像具有固定的几何形状及角度,且在 晶面上的结晶学方向固定。各腐蚀像形状具有共性,即长轴为[010] 方向,短轴为[100] 方向。由不同切面腐蚀像的变化规律, 建立了橄榄石腐蚀像三维立体模型。相同腐蚀剂对不同晶面腐蚀的容易程度差异巨大,以蚀坑在DIC200× 下能清晰观察到 腐蚀像形态为标准,橄榄石各切面的腐蚀速率为v（010）>v（110）>v（100）>v（111）>v（101）>v（001）>v（011）。由橄榄石晶体腐蚀像的唯一 性及其结晶学定向,在橄榄岩切片中将橄榄石颗粒切面指数化,并获得其结晶学定向及结晶优选方向。由此,在大别山碧 溪岭石榴子石二辉橄榄岩中推断橄榄石[100] 主极密垂直面理面,[010] 主极密平行于线理面。腐蚀像所确定的晶体结晶优选 性为当地构造动力提供了一定有价值资料,开拓了腐蚀像的地质应用意义。     

下扬子地区若干上地幔橄榄岩的显微构造研究

本文对下扬子区内２个玄武岩产地（江苏六合瓜埠山、安徽当涂釜山）的幔源包体进行研究,结果表明本区上地幔尖晶石二辉橄榄岩具原生粒状结构、碎斑结构、板状镶嵌等粒结构及部分熔融结构四种类型。在光学岩组图上显示出从原生粒状结构→碎斑结构→板状镶嵌等粒结构,其橄榄石光性方位优选性逐渐增强。变形橄榄石滑移轴为［１００］,滑移面以｛０ｋ１｝为主,（０１０）次之。高温高压人工变形实验证实,这种滑移系形成于高温低应变速率条件下。橄榄石位错类型多样,（１００）、（００１）位错壁分布广泛,位错壁间距显示对数正态分布特征．估算的本区上地幔高温蠕交流动差异应力为（１０．９～１１．５ＭＰａ）。上地幔流变速率、流动应力、等效粘滞度与深度关系指示本区新生代大地构造性质为大陆拉张带或大陆裂谷带。     

Olivine intergranular plasticity at mantle pressures and temperatures

The ductile behavior of olivine-rich rocks is critical to constrain thermal convection in the Earth's upper mantle. Classical olivine flow laws for dislocation or diffusion creep fail to explain the fast post-seismic surface displacements observed by GPS, which requires a much weaker lithosphere than predicted by classical laws. Here we compare the plasticity of olivine aggregates deformed experimentally at mantle pressures and temperatures to that of single crystals and demonstrate that, depending on conditions of stress and temperature, strain accommodated through grain-to-grain interactions – here called intergranular strain – can be orders of magnitude larger than intracrystalline strain, which significantly weakens olivine strength. This result, extrapolated along mantle geotherms, suggests that intergranular plasticity could be dominant in most of the upper mantle. Consequently, the strength of olivine-rich aggregates in the upper mantle may be significantly lower than predicted by flow laws based on intracrystalline plasticity models.     

The behavior of protons during wet olivine deformation under the conditions of the kimberlite process

This paper reports the results of optical and electron microscopic investigations of mantle olivine samples with H₂O contents of tens-hundreds ppm weight. Samples were obtained from the xenoliths and xenocrysts of the Udachnaya pipe. At the scale of optical microscope magnification, a peculiar banded microstructure was observed in thin sections prepared parallel to the olivine (010) plane. It is formed by cross-hatched bands parallel to four crystallographic directions of the olivine structure: [100], [001], [101], and [−101]. At the scale of electron optical magnifications, the banded microstructure is observed as nanometer-sized heterogeneities of various types which are related to olivine deformation: (a) planar defects parallel to (100) and (001) corresponding to the (100)[010] and (001)[100] dislocation glide systems, respectively; they are occasionally transformed into lamellae or decorated by nanoinclusions; and (b) nanometer-sized heterogeneities formed by nanoinclusion arrays not related to planar defects and oriented along the same directions of the olivine structure as the optically visible bands. The deformation structures are decorated by coupled point OH-bearing defects, which were initially present in the olivine. The crystallographically oriented arrays of nanoinclusions of high-pressure hydrous silicates are considered as a result of olivine deprotonization (elimination of OH-bearing defects from the olivine structure) in the zones of previous deformation compression in the crystal. Light refraction effects on the nanoinclusions make these zones optically visible and produce the banded microstructure, which is a consequence of previous deformation.     

晶面腐蚀像与晶面对称及晶面结构的关系

综合分析了石英、石榴子石、橄榄石、锆石、红柱石的各不同结晶学意义的晶面腐蚀像特点,总结了晶面腐蚀像与晶面对称性及晶面结构特点之间的关系.腐蚀像不仅可以揭示晶面及晶体的对称性,还可以揭示晶面的结晶学意义,即同一晶体上的不同结晶学意义的晶面,尽管对称性相同,也具有不同的腐蚀像;不同晶体之间的具有相同对称性的晶面可能会有相同的腐蚀像;腐蚀像类似于一种宏观晶体形态,主要与晶面的对称性有关,与晶面上原子、离子排列的结构细节关系不大;同一晶体的同一晶面在不同的腐蚀剂中所得的腐蚀像也可能完全不同;有些晶面的腐蚀像可以用晶体生长形态的常见晶面与被腐蚀面的交棱来解释.该研究在揭示晶体溶解形态机理、将溶解形态与晶体生长形态对比、用溶解形态来反映晶体曾经经历的酸-碱环境等方面具有理论与实际意义.      

Flow behavior and microstructures of hydrous olivine aggregates at upper mantle pressures and temperatures

Deformation experiments on olivine aggregates were performed under hydrous conditions using a deformation-DIA apparatus combined with synchrotron in situ X-ray observations at pressures of 1.5–9.8 GPa, temperatures of 1223–1800 K, and strain rates ranging from 0.8 × 10^?5 to 7.5 × 10^?5 s^?1. The pressure and strain rate dependencies of the plasticity of hydrous olivine may be described by an activation volume of 17 ± 6 cm³ mol^?1 and a stress exponent of 3.2 ± 0.6 at temperatures of 1323–1423 K. A comparison between previous data sets and our results at a normalized temperature and a strain rate showed that the creep strength of hydrous olivine deformed at 1323–1423 K is much weaker than that for the dislocation creep of water-saturated olivine and is similar to that for diffusional creep and dislocation-accommodated grain boundary sliding, while dislocation microstructures showing the [001] slip or the [001](100) slip system were developed. At temperatures of 1633–1800 K, a much stronger pressure effect on creep strength was observed for olivine with an activation volume of 27 ± 7 cm³ mol^?1 assuming a stress exponent of 3.5, water fugacity exponent of 1.2, and activation energy of 520 kJ mol^?1 (i.e., power-law dislocation creep of hydrous olivine). Because of the weak pressure dependence of the rheology of hydrous olivine at lower temperatures, water weakening of olivine could be effective in the deeper and colder part of Earth’s upper mantle.     

Olivine xenocrysts in picritic magmas

Experimental partial melting of plagioclase lherzolite at 0.7 MPa confining pressure has produced euhedral olivine crystals by corrosion and overgrowth during cooling. The particular conditions of this experiment allow observation of both processes recorded in the crystal shape: corrosion boundaries are rounded, or straight when parallel to [001] intersection of {110} planes; (010) and {110} facets are developed by fast overgrowth during quenching. These observations support the contention that phenocrysts in basaltic or picritic magmas are, in part, xenocrysts. The possible mantle origin of olivine crystals in two natural occurrences of ultramafic magmas; the picritic pillow lavas of the Troodos, and a wehrlitic intrusion of the oman ophiolite, is investigated. In both cases discriminant characteristics are deduced from detailed microstructural study. The mantle origin of olivine megacrysts in the investigated picrites raises the question about the existence of picritic magmas in the mantle.     

大别山双河地区超高压变质岩矿物超微构造的HRTEM研究

报道了大别山双河地区超高压榴辉岩和硬玉石英岩矿物超微构造及缺陷结构的高分辨透射电镜研究结果。在天然变形绿辉石晶内的自由位错、位错倾斜壁、位错环、位错网、亚晶界、堆垛层错等亚构造中 ,发现了纳米级水分子团 ,这种球形状水分子团包体的存在是导致绿辉石晶体水解弱化和塑性变形的重要因素。在榴辉岩矿物中广泛发育的层错、(10 0 )变形双晶、晶畴结构、界面与晶面的交叉滑移、晶格畸变等变形构造及缺陷结构 ,指示超高压岩石经历了快速折返。在硬玉单晶大约 5 0 0nm的微晶畴内 ,发现了C2 /c和P2 1/n两种结构 ,C2 /c结构的晶体学参数对应于硬玉 ,而P2 1/n结构的晶体学参数对应于绿辉石 ,纳米级P2 1/n出溶结构的存在 ,表明在退变质过程中 ,硬玉在纳米尺度上部分转变为绿辉石 ,并且未能达到平衡。也说明在主体岩石的抬升过程中 ,硬玉晶体伴随有复杂的非平衡退变质作用。对于大别山超高压变质岩的p T轨迹描述及其构造解释具有重要意义。     

Dislocations associated with optical features in naturally-deformed olivine

Transmission electron microscopy has been used for the direct observation of dislocations in naturally-deformed olivine. The dislocations are arranged in arrays forming low-angle sub-boundaries which have been identified with features observed in the optical microscope. Comparison of this dislocation substructure with that observed in olivine, and in metals, experimentally deformed under various conditions, suggests that the deformation in nature has occurred by creep. Possible mechanisms of creep, involving the cooperative glide and climb of dislocations, are discussed.     

The effect of aluminum and water on the development of deformation fabrics of orthopyroxene

The effect of alumina and water solubility on the development of fabric in orthopyroxene in response to simple shear deformation has been investigated at a pressure of 1.5 GPa and a temperature of 1,100 °C using the D-DIA apparatus. The microstructure observations at these conditions indicate that dislocation glide is the dominant deformation mechanism. In MgSiO₃ enstatite and hydrous aluminous enstatite, partial dislocations bounding the stacking faults in [001] glide parallel to the (100) (or) the (100) [001] slip system. Electron backscattered diffraction analysis of anhydrous aluminous enstatite, however, indicates operation of the (010) [001] slip system, and microstructure analysis indicates dislocation movement involving [001] on both (100) and {210} planes. The strong covalent bonding induced by the occupation of M1 and T2 sites by Al could have restricted the glide on (100), activating slip on {210}. The resulting seismic anisotropies (~2 %) in orthopyroxene are weaker compared to olivine (~9.5 %), and reduced anisotropy can be expected if orthopyroxene coexists with olivine. Weak anisotropy observed in stable cratonic regions can be explained by the relatively high abundance of orthopyroxene in these rocks.     

Transmission electron microscopic study of experimentally deformed k-feldspar single crystals

A set of sanidine single crystals were previously deformed at 700° C in a Griggs triaxial press with different crystallographic orientations of the core so as to induce dislocation glide of different slip systems respectively. Deformed crystals have been studied by transmission electron microscopy (TEM) and the activated slip systems have been characterized for two orientations. (010)[001] and (001)1/2[ \(\overline 1 \) 10] systems expected for one orientation (main stress nearly parallel to [012]) are observed, whereas the (001)[100] system expected for the other orientation (main stress nearly parallel to [101]) is never observed. In the latter specimen the deformation is rather difficult and occurs through unexpected systems characterized as (110)1/2[1 \(\overline 1 \) 2] and (1 \(\overline 1 \) 1)1/2[110]. In all the samples studied the deformation is heterogeneous, exhibiting dislocation configurations related to temperature variations.