Transmission electron microscope study of dislocations in orthopyroxene (Mg,Fe)2Si2O6

The orthopyroxene crystal structure can be viewed as the stacking of alternating tetrahedral and octahedral layers parallel to the (100) plane. Easy glide occurs in the (100) plane at the level of the octahedral layer to prevent breakage of the strong Si-O bonds. Dislocations with c and b Burgers vectors have been activated in (100) by room temperature indentation in an orthoenstatite gem quality single crystal. Investigations in transmission electron microscopy show that the b dislocations (b?9 Å) are not dissociated while the c's (c=5.24 Å) are dissociated into four partials. This result is interpreted by considering the oxygen sublattice as a distorted FCC one. The four c partials are thus Shockley partials bounding three stacking faults. For the two outer ones, synchroshear of the cations is necessary to keep unchanged their sixfold coordination; the oxygen sublattice is locally transformed into a HCP lattice. This accounts for the observed low splitting (?100 Å) of these faults as compared to the median one (?500 Å) which does not affect the oxygen sublattice and does not require cation synchroshear. In a Fe rich orthopyroxene (eulite), semi coherent exsolution lamellae have been studied. Either only c edge dislocations or both b and c edge dislocations occur in the phase boundaries depending upon the thickness of the lamellae. Only the c dislocations are dissociated. From the observed spacing between these mismatch dislocations a crude estimate of the exsolution temperature is proposed T _ex ? 700° C.     

Formation mechanism of pigeonite lamellae in skaergaard augite

Fine textures of exsolution lamellae and interface boundaries between augite and pigeonite in augite crystals from Skaergaard ferrogabbro 4430 have been studied by high resolution electron microscopy and X-ray methods. Thick pigeonite lamellae have higher densities of (100) stacking faults than thin lamellae. The displacement vector of the faults has been determined as 5/6c from the measured density of faults and the relative rotation of the augite and pigeonite lattices. The augite and pigeonite lattices are apparently coherent, and no growth ledges were observed at the interfaces. The stacking faults are often combined with the antiphase boundary of pigeonite resulting in a total displacement vector of 1/2(a+b)+5/6c. The observation of thick and thin pigeonite lamellae indicated that the thickening of (001) pigeonite lamellae was controlled by coherency strains accumulated at the interfaces between augite and pigeonite.     

Coherent elastic energies of exsolution boundaries in peristerite and böggild intergrowths

Elastic energy calculations based upon the coherent model of Willaime and Brown [Acta Cryst. A30, 316–331 (1974)] have been carried out for some exsolution textures in peristerite and Böggild intergrowths. For peristerites it is demonstrated that substitution of K for Na moves the orientation of the exsolution lamellae from (08 \(\overline {\text{1}} \) ) to about ( \(\overline {\text{1}} \) , 21, \(\overline {\text{2}} \) ) in agreement with observations. An electron microscope study of exsolution textures in labradorite and andesine plagioclases has been carried out and information about small structural differences in these lamellar structures has been obtained from elastic energy calculations.     

Electron microscopical study of garnet exsolution in orthopyroxene

By means of electron-optical methods the structure and orientation of lamella-like garnet exsolutions in an orthopyroxene from the eclogite of Gilsberg, Saxony Granulite Complex, are investigated. It can be shown that besides the macroscopic and microscopic submicroscopic exsolution lamellae also exist; they have widths up to nearly 5 nm. The intergrowth conditions are such shat (100)_op is parallel to {100}_gr and [001]_op parallel to 〈110〉_gr. The lamellae are coherent, but sometimes extended dislocation arrangements are found in microscopic lamellae which are caused by a deformation. These investigations point to formation of the rock as a result of a solid state reaction under high pressure conditions with subsequent diffusive-dissociative exsolution of garnet from primary pyroxene.     

Deformation of shock-loaded andalusite studied with X-ray diffraction techniques

The structural deformation of an andalusite single crystal, shockloaded up to 400 kb with shock wave direction approximately parallel to c, was investigated by means of X-ray powder (Guinier) and single crystal techniques (Weissenberg, precession). Exposure to the dynamic pressure revealed a fracturing of the crystal into lattice blocks, with a mean size >1,000 Å. No change of the lattice constants could be observed after pressure release. From the streaks of X-ray reflection spots measured within the hk0, h0l, 0kl, and hhl planes the shock-induced lattice deformation is interpreted in terms of rotational gliding and/or microfracturing. The distortion mode is highly structure controlled. It follows preferrably two different structural motion systems: (1) Gliding parallel to (001) occurs, which produces lamellae parallel to (001), mainly arranged in two sublattices with common c-axis. The stacking sequence of lamellae along c is irregular. The lamellae-type structure may also result from an orientated transformation into a high pressure phase of lower symmetry and subsequent inversion into the original phase after pressure release. (2) Gliding parallel to (100) occurs. In this case the deformation mode is asymmetrical with respect to the undistorted crystal. The common direction b of the (001) and (100) deformation planes is probably the main direction of the shock-induced lattice deformation.     

An electron microscopic study of amphibole lamellae in augite

Ion-thinned samples of augite from four plutonic igneous rocks have been examined in the electron microscope at 100 kV. Lamellae less than 0.08 m thick were observed parallel to (010) in all four samples. Electron diffraction shows that the lamellae consist of clino-amphibole, space group I2/m, with crystallographic axes parallel to those of the augite. Analytical electron microscopy of the lamellae in one specimen shows that they are a hornblende. The amphibole lamellae have nucleated at the interface between the augite host and exsolution lamellae of orthopyroxene parallel to (100) of the augite. The interface between the amphibole lamellae and the augite is coherent.It is thought that the amphibole lamellae have formed by exsolution from the augite, implying the existence of finite solid solution between members of the pyroxene and amphibole groups of minerals.     

Luna 20 pyroxenes: exsolution and phase transformation as indicators of petrologic history

Pyroxenes from our sample of Luna 20 soil are predominantly orthopyroxene with subordinate pigeonite. The orthopyroxenes are chromium-rich bronzites and contain submicroscopic lamellae of augite in a twinned orientation exsolved on (100). These lamellae have a composition close to the diopside-hedenbergite join. Asymmetric diffuse streaks parallel to $\text{a}{}^1$ indicate stacking faults parallel to (100) and possibly very thin (10–20 Å) lamellae of clinobronzite parallel to (100). Pigeonite crystals are very complex crystallographically and chemically, with optically visible (001) augite exsolution lamellae and two sets of chromite exsolution lamellae. In addition, there are submicroscopic (100) augite lamellae and a second generation of clinohypersthene lamellae which appear to have exsolved from the (001) augite lamellae. The clinohypersthene host, which has a large number of stacking faults parallel to (100), has partially inverted to hypersthene of the same composition. The hypersthene occurs as very fine lamellae (less than 1000 Å) parallel to the (100) plane of the clinohypersthene. X_D^Fe-Mg values for five host-lamellae pairs in pigeonite K-4 indicate a significant amount of subsolidus readjustment. We tentatively conclude that many of the bronzite and pigeonite crystals were derived from rocks crystallized from a high level magma chamber in the lunar highland crust.     

Garnet exsolution in pyroxene from clinopyroxenites in the Moldanubian zone: constraining the early pre-convergence history of ultramafic rocks in the Variscan orogen

Exsolution lamellae of garnet in clinopyroxene and orthopyroxene porphyroclasts from garnet pyroxenites in the Moldanubian zone were studied to elucidate the pressure–temperature conditions of the exsolution process and to reconstruct the burial and exhumation path of ultramafic rocks in the Variscan orogen. The porphyroclasts occur in a fine-grained matrix with metamorphic fabrics, which consists of clinopyroxene and small amounts of garnet, orthopyroxene and amphibole. The clinopyroxene porphyroclasts contain garnet + orthopyroxene lamellae as well as ilmenite rods that have orientation parallel to (100) planes of the porphyroclasts. Orthopyroxene porphyroclasts host garnet and clinopyroxene lamellae, which show the same lattice preferred orientation. In both cases, lamellar orthopyroxene, clinopyroxene and garnet were partially replaced by secondary amphibole. Composition of exsolution phases and that of host pyroxene were reintegrated according to measured modal proportions and demonstrate that the primary pyroxene was enriched in Al and contained 8–11 mol.% Tschermak components. Conventional thermobarometry and thermodynamic modelling on the reintegrated pyroxene indicate that primary clinopyroxene and orthopyroxene megacrysts crystallized at 1300–1400 °C and 2.2–2.5 GPa. Unmixing and exsolution of garnet and a second pyroxene phase occurred in response to cooling and pressure increase before the peak pressure of 4.5–5.0 GPa was reached at ∼1100 °C. This scenario is consistent with a burial of hot upper-mantle ultramafics into a cold subcratonic environment and subsequent exhumation through 900 °C and 2.2–3.3 GPa, when the pyroxenites would have partially recrystallized during tectonic incorporation into eclogites and felsic granulites.     

Electron microscopy of clinoenstatite from a boninite and a chondrite

Clinoenstatite crystals from a boninite and the Yamato-74191 chondrite have been studied with an analytical electron microscope. (100) twins and cracks perpendicular and parallel to the c axis are characteristic of their submicroscopic textures. The frequency in appearance along the c axis and widths of the cracks have been explained by the dimensional change of the c axis in the direct transformation of protoenstatite to clinoenstatite and by the cooling rate around the transformation temperature. The cracks in the crystals from the boninite are filled with fibrous crystals of talc, while those from the chondrite are open or filled with glass in which fine crystals of plagioclase are common.     

Mechanical twinning in diopside Ca(Mg,Fe)Si2O6: Structural mechanism and associated crystal defects

Diopside twins mechanically on two planes, (100) and (001), and the associated macroscopic twinning strains are identical (Raleigh and Talbot, 1967). An analysis based on crystal structural arguments predicts that both twin mechanisms involve shearing of the (100) octahedral layers (containing Ca²⁺, Mg²⁺ and Fe²⁺ ions) by a magnitude of c/2. Small adjustments or shuffles occur in the adjacent layers containing the [SiO₄]^4? tetrahedral chains. While the (100) twins are conventional with shear parallel to the composition plane, this analysis predicts that (001) twins form by a mechanism closely related to kinking. A polycrystalline diopside specimen was compressed 8% at a temperature of 400° C, a pressure of 16 kilobars, and a compressive strain rate of about 10^?4/s. Transmission electron microscopy on this specimen has revealed four basic lamellar features:

1. (100) mechanical twin lamellae;
2. (100) glide bands containing unit dislocations;
3. (001) twin lamellae;
4. (101) lamellar features, not as yet identified.

The (001) twins often contain remnant (100) lamellae of untwinned host. Twinning dislocations occur in these (100) lamellae and in the (001) twin boundaries with very high densities. Diffraction contrast experiments indicate that the twinning dislocations associated with both twin laws glide on (100) with Burgers vector b=X [001] where X is probably equal to 1/2 on the basis of the structural analysis. Parallels are drawn between mechanical twinning in clinopyroxenes and clinoamphiboles. The exclusive natural occurrence of basal twins in shock-loaded clinopyroxenes and of analogous ( \(\bar 1\) 01) twins in clinoamphiboles is given a simple explanation in terms of the relative difficulty of the “kinking” mechanism as compared to direct glide parallel to the composition plane.     

Deformation and transformation in experimentally shock-loaded quartz

Single crystals of quartz, shock-loaded along the a axis to pressures of 22 Gpa, 24 GPa, 26 GPa and 30 GPa were examined by high-voltage transmission electron microscopy (TEM), scanning electron microscopy (SEM) and X-ray diffraction. Asymmetric broadenings of X-ray lines indicate spatial inhomogeneity of shock effects. X-ray streaking angles in the reciprocal lattice planes h0 \(\bar h\) l, 0k \(\bar k\) l and hki0 indicate a slight tilting deformation by rotation about [00.1] in (0001). TEM reveals glass lamellae which are mostly in (01 \(\bar 1\) 2) orientation, and are correlated with optical planar elements and with surface steps seen in SEM. No dislocations are found. There are (0001) lamellar features, probably Brazil twins. The (01 \(\bar 1\) 2) glass lamellae develop directly from bands of quartz in which intense deformation has produced a fine-scale lamellar to blocky structure, possibly also originating by twinning. Relics of crystalline structure are found in almost completely vitrified lamellae. Stishovite occurs in heavily deformed parts of the 22 GPa and 24 GPa specimens, in patches of densified glass distinct from the sharply bounded lamellae. The nucleationless, pervasive transformation of lamellae to glass, with preservation of their sharp boundaries, is attributed to defect coalescence analogous to vitrification by radiation damage (metamictization). Some patchy glass may be due to melting.     

Exsolution in augite from the Skaergaard Intrusion

The exsolution phenomena of augite from Ferrogabbro 4430 of the Skaergaard Intrusion were examined in detail by single crystal X-ray diffraction and heating experiments to study the stepwise exsolution process. In the augite crystals, five different phases were detected: pigeonite (001), pigeonite (100), orthopyroxene (a), orthopyroxene (p) and a small amount of clinoamphibole. The two different pigeonites nearly share the corresponding (001) and (100) planes with the host. Orthopyroxene (a) and orthopyroxene (p) have (100) in common with the host and with exsolved pigeonite (001), respectively. Clinoamphibole was observed in the form of rather weak reflections in many crystals. It has (010) in common with the host.A large number of augite crystals exhibited a pigeonite (001) phase with curved, rotated reflections and diffuse streaks along the a* direction in (h0l) precession photographs. It appears that these streaks are related to orthopyroxene (p). Orthopyroxene (p) seems to be crystallized from pigeonite (001) by nucleation at (100) stacking fault planes (inverted pigeonite). Pigeonite (100) may be formed at growth ledges between augite host and exsolved orthopyroxene (a) at a later stage of exsolution to stabilize the boundaries.From the X-ray diffraction profiles and the results of the heating experiments, a possible exsolution sequence is suggested. Clinoamphibole appears to be a product of alteration at the latest stage of the exsolution process. It seems to be related to particular conditions of partial water pressure.     

Exsolution and coarsening in iron-free clinopyroxene during isothermal annealing

Exsolution and coarsening in Fe-free clinopyroxene of composition En_45.1Di_54.9 was studied at temperatures of 1300, 1200, and 1100°C, and annealing times between 10 min and 4320 h. Based on the wavelength of the exsolution lamellae, the exsolution process can be divided into exsolution sensu stricto and coarsening. During exsolution sensu stricto, the average wavelength of the “001” and “100” lamellae remains constant in contrast to the subsequent coarsening process. A progressive development of the microstructure is observed before coarsening which includes formation of island-like regions of dark contrast without phase separation, occurrence of pigeonite and diopside domains predominantly elongated along (100), formation of “100” exsolution lamellae, dissolution of the “100” lamellae, and predominant occurrence of “001” exsolution lamellae. All observations are in accordance with the exsolution mechanism of spinodal decomposition. After termination of the exsolution process, coarsening of the exsolution lamellae is observed. The “001” lamellae coarsen according to the rate law

     

海南文昌二辉橄榄岩中辉石出溶结构的结晶学取向分析

本文用电子背散射衍射技术(electron backscatter diffraction,EBSD)测试了海南文昌玄武岩中二辉橄榄岩包体中的辉石主晶与其出溶片晶的结晶学取向关系。结合电子探针成分测试,得出:单斜辉石(透辉石)主晶中出溶了两组不同方向的片晶,一组为斜方辉石(顽火辉石-易变辉石)片晶,另一组为单斜辉石(普通辉石)片晶。由于出溶片晶在EBSD测试切面上体现为以线状体,因此需要找到一种方法将线状体所代表的片晶的晶面符号推算出来。本文介绍了一种利用吴氏网进行坐标系旋转的"晶带相交法",该方法可以作图推算出溶片晶的晶面符号。根据"晶带相交法"得出,斜方辉石(顽火辉石-易变辉石)出溶片晶为(100),单斜辉石(普通辉石)出溶片晶为~(401)。根据前人的研究资料,出溶片晶~(401)可能指示最小出溶压力为9.5~12.5GPa。出溶片晶的结晶学取向涉及到主晶与出溶体的晶体结构匹配关系,并且与出溶温度-压力有关,因此出溶片晶的结晶学取向分析具有晶体化学理论意义和反映地质温压过程的实际意义。这种"晶带相交法"可以推广应用于其他矿物出溶结构的结晶学取向研究中。     

Analysis of high-voltage,high-resolution images of lattice defects in experimentally-deformed dolomite

Deformation-induced stacking defects in dolomite have been characterised following examination at the cation sublattice level using high-resolution electron microscopy at 500kV. Slip on c (≡{0001}) is observed to produce stacking faults, often de-localised laterally, which are terminated by partial dislocations with Burgers vectors of the form 1/3 [1 \(\overline 1 \) 00]: a model for the faulted dolomite lattice has been constructed which agrees with the image appearance. Slip on f (≡{10 \(\overline 1 \) 2}) produces long planar faults which are established as not being stacking faults, in the normal sense, since there appear to be no offsets of the cation sublattice across the faults, nor any general indication of any terminating partial dislocations: it is proposed that the contrast arises from rotational disorder in CO₃ groups which has resulted from the prior passage of partial dislocations during deformation.     

Sigmoidal exsolution by internal shear stress in pyroxenes from chondritic meteorites

Pyroxenes of pigeonitic and augitic bulk compositions in H3–4 chondritic meteorites commonly exhibit sigmoidal precipitates, rather than the elsewhere common lamellar associations. Most often, submicrometric sigmoids with calcic clinopyroxene composition occur within clinoenstatite; more rarely, clinoenstatite sigmoids occur within calcic clinopyroxene. The sigmoids appear as 001 terminated lamellae, with terminations rotated in opposite directions towards the 100 orientation. Pre-exsolution pigeonite and augite formed at temperatures higher than 980 °C, whereas sigmoidal exsolution occurred between 990 and 830 °C. Local anomalous lattice parameters determined by electron diffraction suggest that lattice parameters are most strained where the exsolution texture is most poorly defined. Shear strain occurs during exsolution due to mismatching lattice parameters and variable angles. In response to shear stress, the lamellae relax and assume sigmoidal strained morphologies. Sigmoidal exsolution is strongly controlled by (100) orthoenstatite stacking faults that possibly trigger exsolution.     

Lamellar exsolution systems in clinopyroxene

Exsolution systems in synthetic pyroxenes were studied by transmission electron microscopy. An iron free sample En₈₀Wo₂₀ was prepared by devitrifying glass at 1300°C. Samples with bulk composition En₅₀Fs₃₀Wo₂₀ and En₃₅Fs₃₈Wo₂₇ were given various but well-defined heat treatments. The exsolution systems observed cannot unambiguously be related to the heat treatment. Periodic lamellar exsolution was observed parallel to (001) and (100) with sharp satellite reflections in the diffraction diagram. In more complex exsolution systems coarse (100) lamellae were found together with fine lamellae parallel to (001) and (100). An unusual phenomenon occurs at a (100) twin boundary where both individuals display exsolution lamellae parallel to (001). Pigeonite lamellae in one twin meet augite lamellae of the other individual at the twin boundary and vice-versa. The precise matching is achieved by a change in width near the boundary. Smoothly curved phase boundaries are developed in the obtuse angle of crosshatched (100) and (001) pigeonite lamellae in augite, whereas the boundaries in the acute angle are straight with sharp edges. This is consistent with elastic energy constraints.     

Interdiffusion of NaSi—CaAl in peristerite

The ‘average’ interdiffusion coefficient ( \(\bar D\) ) for NaSi—CaAl exchange in plagioclase for the interval from An₀ to An₂₆ was estimated from experimentally determined homogenization times for peristerite exsolution lamellae. The average spacing between adjacent (unlike) lamellae is 554±77 Å. Dry heating in air at 1,100°C for 98 days produced no change in the exsolution microstructure; thus \(\bar D\) (dry)<10^?17 cm²/s. This limit is consistent with the recently reported ‘average’ \(\bar D\) (dry) values for the Huttenlocher interval (An_70–90) at this temperature. At 1.5 GPa with about 0.2 weight percent water added the ‘average’ diffusion coefficient from 1,100°C to 900°C is given by: \(\bar D\) (wet)=18 _?15 ⁺¹⁰⁸ (cm²/s) exp (?97±5 (kcal/mol)/RT), where R is the gas constant, and T is °K. This \(\bar D\) (wet) at 1,100°C is more than three orders of magnitude greater than \(\bar D\) (dry) for Na- and Ca-rich plagioclases.     

Temperature History of Sheared Mantle Xenoliths from the West Eifel, West Germany: Evidence for Mantle Diapirism Beneath the Rhenish Massif

Mantle xenoliths from the West Eifel, West Germany revealingdistinct disequilibrium textures were formed by strong sheardeformation from coarse grained, high temperature spinel peridotites.Foliated structures are caused by the roughly parallel alignmentof elongated orthopyToxenc porphyroclasts up to 8 ? 2 mm insize and streched patches of clinopyroxene and spinel in a matrixof recrystallized olivine, orthopyroxene, clinopyroxene, andspinel. Bulk chemical disequilibrium finds its expression in a highdegree of chemical heterogeneity which is most evident in orthopyroxene.In orthopyroxene porphyroclasts, unmixed lamellae of clinopyroxeneand chromium-aluminium spinel are confined to the grain cores,because concentration gradients of Al, Cr, and Ca existed atthe time of their exsolution. Orthopyroxene neoblasts also revealdiffusion controlled concentration gradients of Al, Cr, andCa, which decrease from core to rim. The temperature historydetermining the orthopyroxene chemistries was derived from Al-solubilitiesin orthopyroxene using an empirical geothermometer. From thetextural relationships, in conjunction with the temperaturehistory, it is inferred that the shear process causing the deformationof the porphyroclastic xenoliths was associated with a temperaturedecrease from at least 1100 to about 800?C. The observed linkage of deformation and cooling in the xenolithsis related to the diapiric uplift of hot mantle material intoa cooler uppermost mantle beneath the West Eifel. It rules outa deformation due to secular mantle flow or movements along‘cold’ shear zones.     

A transmission electron microscope study of naturally deformed orthopyroxene

A model is proposed for the production of clinopyroxene lamellae in orthopyroxene by a dislocation mechanism based on simple shear. Four possible shears are described. Two shears apply to each subcell of orthopyroxene, one with =13.3° in one sense, the other with =18.3° in the opposite sense.The senses of shears of the same magnitude in adjacent cells are also opposite. All shears produce the same structure, but in two discrete orientations which can be distinguished from electron diffraction patterns. However, the operative shear cannot be uniquely determined from the diffraction patterns alone. The characteristics of the diffraction contrast fringes and associated partial dislocations observed by transmission electron microscopy in a naturally deformed orthopyroxene are shown to be consistent with the proposed model.