TEM characterization of dislocations and slip systems in stishovite deformed at 14 GPa, 1,300°C in the multianvil apparatus

Transmission electron microscopy (TEM) has been used to investigate deformation microstructures of synthetic stishovite specimens deformed at 14 GPa, 1,300°C. Geometrical characteristics of numerous dislocations have been characterized by dislocation contrast and stereographic analyses in order to identify the easy slip systems of stishovite. TEM data allowed us to characterize the following slip systems: 〈100〉{001}, 〈100〉{010}, 〈100〉{021}, [001]{100}, [001]{110}, [001]{210} and Observation of sub-grain boundaries and scalloped edge dislocations suggest that climb has been activated in the specimens.     

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 recrystallisation mechanisms in naturally deformed cordierite

Cordierite — (Mg,Fe)₂Al₄Si₅O₁₈ — occurs as porphyroclasts within metapelitic and metavolcanic rocks from the Kemiö-Orijärvi belt, SW Finland. After crystallisation the cordierites have been deformed at temperatures between 550–825° C and pressures of 3–5 kbar. Optical microscopy reveals the following deformation-induced microstructures: a bimodal size distribution between host, 0.3 to 4.0 mm, and recrystallised (new) grains, 0.1 to 0.5 mm; the intracrystalline defect-structures of host grains yield undulatory extinction, subgrains and some twinning. Recrystallised grains are optically strain free. Grain and subgrain boundaries are generally straight and parallel to crystallographic low-index planes. Orientation distribution diagrams for host and recrystallised grains yield similar fabric diagrams, i.e. [010] perpendicular to foliation -S-, [001] and [100] parallel to S and [001] parallel to lineation -L-. The fabric diagrams indicate that [001] (010) is the dominant slip system. Transmission electron microscopy reveals straight free dislocations, glide and climb loops, minor {130} and {110} microtwins, isolated nodal points and dislocation walls. Contrast analyses yield Burgers vector b = [001] being dominant and b = [100] subordinate. Climb loops consist of 〈c〉-dislocations that are dissociated in (001) planes, glide loops are defined by [100] [010] and [001] (100). The cordierite microstructures have been interpreted to be generated by dislocation creep. The dominant recrystallisation mechanism is thought to be subgrain rotation subsequently followed by minor grain or twin-band boundary migration.     

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.     

Transmission electron microscope study of experimentally deformed K-Feldspar single crystals

Single crystals of sanidine which were experimentally deformed so as to introduce the (010)[100] slip system were examined by transmission electron microscopy (tem). Dislocation glide is mainly manifested in the samples deformed at 700° C, with a strain rate \(\dot \varepsilon = 1 - 2 \times 10^{ - 6} s^{ - 1} \) . In addition to the expected slip system another more important one, (12 \(\bar 1\) )[101], was found. The dislocations lying in (010) present a glissile dissociation. These observations have been discussed in term of the feldspar structure. Models for glissile dissociation in (010) are proposed: [100]=1/2[100]+1/2[100] or 1/2[101]+1/2[10 \(\bar 1\) ] and [101]=1/2[101]+1/2[101].     

Quantitative characterization of plastic deformation of zircon and geological implications

The deformation-related microstructure of an Indian Ocean zircon hosted in a gabbro deformed at amphibolite grade has been quantified by electron backscatter diffraction. Orientation mapping reveals progressive variations in intragrain crystallographic orientations that accommodate 20° of misorientation in the zircon crystal. These variations are manifested by discrete low-angle (<4°) boundaries that separate domains recording no resolvable orientation variation. The progressive nature of orientation change is documented by crystallographic pole figures which show systematic small circle distributions, and disorientation axes associated with 0.5–4° disorientation angles, which lie parallel to rational low index crystallographic axes. In the most distorted part of the grain (area A), this is the [100] crystal direction. A quaternion analysis of orientation correlations confirms the [100] rotation axis inferred by stereographic inspection, and reveals subtle orientation variations related to the local boundary structure. Microstructural characteristics and orientation data are consistent with the low-angle boundaries having a tilt boundary geometry with dislocation line [100]. This tilt boundary is most likely to have formed by accumulation of edge dislocations associated with a 〈001〉{100} slip system. Analysis of the energy associated with these dislocations suggest they are energetically more favorable than TEM verified 〈010〉{100} slip. Analysis of minor boundaries in area A indicates deformation by either (001) edge, or [100](100) and [001](100) screw dislocations. In other parts of the grain, cross slip on (111), and (112) planes seems likely. These data provide the first detailed microstructural analysis of naturally deformed zircon and indicate ductile crystal-plastic deformation of zircon by the formation and migration of dislocations into low-angle boundaries. Minimum estimates of dislocation density in the low-angle boundaries are of the order of ∼3.10¹⁰ cm⁻². This value is sufficiently high to have a marked effect on the geochemical behavior of zircon, via enhanced bulk diffusion and increased dissolution rates. Therefore, crystal plasticity in zircon may have significant implications for the interpretation of radiometric ages, isotopic discordance and trace element mobility during high-grade metamorphism and melting of the crust.     

Cordierite microstructure and texture in a moldanubian gneiss

The microstructure and texture in cordierites of a moldanubian gneiss from the Bohemian Massif has been analysed by transmission electron microscopy (TEM) and universal stage in order to get information on the deformation mechanisms and textural development of this rock-forming mineral. Deformation may have taken place at temperatures between about 500° C and 630° C and pressures smaller than about 3 kb. The elongated cordierite xenoblasts show a typical dislocation creep microstructure consisting of subgrain boundaries and free dislocations. The dislocations have [001], [010] and 1/2<110> Burgers vectors. [001] dislocations often have pure screw and edge character the latter type being climb-dissociated on (001). Among the dislocations reactions are common. The main subgrain boundaries observed are (010)[001], {110}[001] and (001)[010] tilt boundaries. Burgers vectors and dislocation line directions reveal (100)[001], (010)[001], (100)[010], {110} 1/2<110> and (001)1/2<110> as activated slip systems. The crystallographic preferred orientation (here referred to as texture) consists of a [001] maximum in the foliation parallel to the mineral lineation. [100] and [010] maxima are perpendicular to it within and normal to the foliation, respectively, with a girdle tendency normal to the lineation. The texture may be explained by simple shear deformation on the {hkO}[001] slip systems with preference of (010)[001].     

Transmission electron microscopy of experimentally deformed chalcopyrite single crystals

Two crystals of natural chalcopyrite, CuFeS₂, experimentally deformed at 200° C have been studied by means of transmission electron microscopy (TEM). The activated glide planes are (001) and {112}. The dislocations in (001) have the Burgers vector [110] and a predominating edge character. They are split into two colinear partials b=1/2[110] and can cross split into {112}. The dislocations in {112} consist of straight segments along low index lattice lines. They are often arranged in dipoles generating trails of loops. Few dislocations with b=1/2[ \(\overline {11} \) 1] and [1 \(\bar 1\) 0] are present and dislocations with b=[0 \(\bar 2\) 1] occur in low angle subgrain boundaries. From weak beam contrasts it is presumed that most of the dislocations gliding in {112} have b=1/2〈3 \(\overline {11} \) 〉. They are dissociated into up to four partials. Microtwins and different types of stacking faults in {112} also occur. Models of the dissociation of dislocations are discussed.     

Analysis of dislocations in some naturally deformed plagioclase feldspars

Dislocations in intermediate plagioclase feldspars, which were deformed under granulite facies conditions, have been analysed. The study reveals extensive ductile deformation by intracrystalline slip and by twinning. Six out of the seven possible Burgers vectors were identified: \(b = \left[ {001} \right],\tfrac{1}{2}\left[ {110} \right],\tfrac{1}{2}\left[ {1\bar 10} \right],\left[ {101} \right],\tfrac{1}{2}\left[ {112} \right]and\tfrac{1}{2}\left[ {1\bar 12} \right]\) . Most, perhaps all, dislocations are dissociated by up to 200 Å. The microstructure is dominated by [001] screw dislocations, most of which appear to be dissociated in (010). The dominant slip system appears to be (010) [001]. Large grain-to-grain variations in the density of free dislocations indicate that the plastic strain in individual grains depended upon the Schmid factor for (010) [001]. The microstructure suggests that the rate-controlling step for high-temperature creep of plagioclase is cross-slip of extended [001] screw dislocations. The rheological contrast between feldspar and quartz is partly due to a difference in stacking fault energy.     

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.     

Characterization of the glide planes of the [001] screw dislocations in olivine using electron tomography

A San Carlos olivine polycrystal has been deformed under uppermost mantle conditions, by compression at 900 °C, at a strain rate of 1.1 × 10^?5 s^?1, under a confining pressure of 300 MPa, using the Paterson press. Transmission electron tomography of dislocations has been performed by scanning transmission electron microscopy, by conventional transmission electron microscopy using the weak-beam dark-field technique, associated with precession or not, in order to determine the glide planes of [001] screw dislocations. This recent technique is the most suitable one since most [001] dislocations exhibit straight screw segments due to the high lattice friction on this character at low temperature. We find that [001] dislocations glide in (100), (010) and {110} as already reported, but also more unexpectedly in {120} and {130}. We show that at 900 °C, [001] {110} glide is dominant in polycrystals. We have, however, noted and characterized numerous cross-slip events in the specimen.     

Room temperature microplasticity of a spodumene LiAlSi2O6

As uniaxial compression tests of α spodumene LiAlSi₂O₆ at various temperatures and strain rates systematically led to brittle fracture, room-temperature microindentations have been performed with a view to characterizing the glide systems. Transmission electron microscopy (TEM) investigations show that only the [010] (100) glide system is activated. The resulting dislocations are widely dissociated (up to 3,000 Å) following the reaction [010]→[0 1/2 1/6]+[0 1/2 \(\bar 1\) /6]. In contrast, in naturally deformed spodumene the activated glide systems found in TEM studies are [001] {110} and 1/2〈110〉{1 \(\bar 1\) 0} and the corresponding dislocations are not dissociated. Such a difference in mechanical behaviour is interpreted in considering the necessary impingement of the oxygen atoms during dislocation glide. It is shown that only the dissociated b dislocations can glide with a moderate lattice friction at room temperature. The proposed model is supported by the first exploratory deformation runs performed under confining pressure.     

Plastic deformation of wadsleyite: I. High-pressure deformation in compression

 We have studied the plastic deformation of Mg₂SiO₄ wadsleyite polycrystals. Wadsleyite was synthesized from a forsterite powder in a multianvil apparatus. It was then recovered and placed in a second multianvil assembly designed to induce plastic deformation by compression between two hard alumina pistons. After the deformation experiment, the microstructures are characterized by transmission electron microscopy (TEM) and large-angle convergent beam electron diffraction (LACBED). Deformation experiments have been carried out at 15–19 GPa and at temperatures ranging from room temperature to 1800–2000 °C. Five different dislocation types have been identified by LACBED: [100], 1/2〈111〉, [010], 〈101〉 and [001]. The [001] dislocations result from dislocation reactions and not from activation of a slip system. The [010] dislocations are activated under high stresses at the beginning of the experiments and further relax by decomposition into 1/2〈111〉 dislocations or by dissociation into four 1/4[010] partial dislocations. The following slip systems have been identified: 1/2〈111〉{101}, [100](010), [100](001), [100]{011}, [100]{021}, [010](001), [010]{101} and 〈101〉(010). Received: 15 July 2002 / Accepted: 14 February 2003 Acknowledgements High-pressure experiments were performed at the Bayerisches Geoinstitut under the EU IHP – Access to Research Infrastructures Programme (Contract no. HPRI-1999-CT-00004 to D.C. Rubie). P.C. has benefited from a Congé thématique pour recherche from the University of Lille, and would like to thank warmly all the people in Bayreuth who contributed to this work by daily assistance and discussions: Nathalie Bolfan-Casanova, Daniel Frost, Jed L. Mosenfelder and Brent Poe. The quality of the preparation of the TEM specimens by H. Schultze is greatly appreciated.     

Deformation of dolomite single crystals from 20–800° C

Dolomite single crystals of six different crystallographic orientations were tested in compression under confining pressure at temperatures of 20 to 800° C. The chosen orientations favoured slip or twinning on particular systems. The deformed crystals were analysed by optical and high voltage transmission electron microscopy to determine activated deformation systems, dislocation behaviour, etc., and to assist in interpreting stress-strain data. It is shown that slip on c≡(0001) and on \(f \equiv (\bar 1012)\) ), and twinning on f between 300 and 600° C, are the principal modes of deformation. At low temperatures there is considerable cataclasis, and shear-fracturing must be counted as a significant deformation mechanism. The effects of climb become apparent at temperatures ?600° C. A pronounced increase in strength with testing temperature shown by some orientations of the crystals is largely associated with c slip, but f twinning also shows similar although weaker tendencies. The yield stress for f slip decreases markedly with temperature. Values of critical resolved shear stress are obtained for c and f slip, and for f twinning. Major and minor slip systems, dislocation and twin configurations generated by deformation under different regimes are documented and illustrated. Some of the characteristics of the deformation systems are attributed to the details of atomic displacements. In particular, the increase in strength with temperature for c slip is explained by friction of CO ₃ ^2? groups during dislocation movement, which is unique for c slip. This friction increases with thermal vibration, expansion and rotation of the CO ₃ ^2? groups.     

High-pressure transformations in CaSiO3

Wollastonite transforms to a triclinic high-pressure polymorph, wollastonite II, at pressures > 25 kb. The equilibrium boundary [P(bars)=-4.7×T°C+32.810] has a rather flat negative P-T slope. The rapid reactivity of the transition over at least a 1000° C range, its insensitivity to T and its location around 30 kb are indicative of its potential for a pressure calibration curve at high T.     

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.     

Dislocation dissociation in CaGeO3 perovskite

Dissociated dislocations have been observed for the first time by transmission electron microscopy in the perovskite-structure compound CaGeO₃. Dislocations with Burgers vectors \(\left[ {1\bar 10} \right]\) and [001] (in pseudo-cubic index) are dissociated into collinear partials on the (110) plane: $$\left[ {1\bar 10} \right] = {1 \mathord{\left/ {\vphantom {1 2}} \right. \kern-\nulldelimiterspace} 2}\left[ {1\bar 10} \right] + {1 \mathord{\left/ {\vphantom {1 2}} \right. \kern-\nulldelimiterspace} 2}\left[ {1\bar 10} \right]$$ and [001] = 1/2[001] + 1/2[001]. The partials react to form octagonal extended nodes. The stacking fault ribbons with displacement vector \(\left[ {1\bar 10} \right]\) have a width of 350 A, which corresponds to a stacking fault energy of 35 erg/cm² (or mJ/m²).     

Mica-feldspar equilibria in supercritical alkali chloride solutions

The equilibrium position of the reaction $$\begin{gathered} 1.5 KAlSi_3 O_8 + HCl = 0.5 KAl_3 Si_3 O_{10} (OH)_2 \hfill \\ + 3SiO_2 + KCl \hfill \\ \end{gathered} $$ has been located at 1 and 2 kb pressure and temperatures between 600° and 670° C using the Ag-AgCl buffer. These data can be combined with information on the dissociation of KC1, HC1 and H₂O to determine species abundances in supercritical aqueous fluids in equilibrium with muscovite — K-feldspar — quartz assemblages. Chloride species become increasingly associated with increasingT, increasing total molality, (m _tot or \(m_{Cl_{tot} } \) ), and decreasing \(P_{H_2 O} \) . Master variable diagrams indicate that the pH of the solutions may vary from near neutral to quite acid. Published data on the paragonite-albite-quartz reaction and exchange reactions involving feldspars and micas were included to calculate speciation in mica-feldspar-NaCl-KCl-HCl-H₂O fluids at 2kb pressure and temperatures between 300° and 600° C. The data are not accurate enough to distinguish different feldspar structural states. Concentration gradients were calculated for individual species between K-feldspar+quartz, muscovite+quartz and andalusite+quartz assemblages at 500° C, 2 kb. Assuming that the proton diffuses most rapidly and that there are no [H⁺] gradients, the molality of the solution must vary 30-fold, with feldspar+quartz at the more concentrated side. The data on mica-feldspar-chloride equilibria are used to interpret the spacial distribution of micas, feldspar and quartz in microfolds. This distribution can be accounted for by pressure solution, due to the fact that non-hydrostatic pressure affects congruently dissolving minerals, auch as quartz, differently from minerals which dissolve incongruently, such as micas and feldspars. We postulate, that during folding at constant \(P_{H_2 O} \) ,T and \(m_{Cl - } \) , gradients in KC1 and SiO₂ are created by stress differences between hinge and limb of a microfold, such that both migrate to the hinge area where quartz precipitates and muscovite is converted to K-felspar, thus accounting for the observed mineral distribution.     

Raman scattering and lattice vibrations of Ni2SiO4 spinel at elevated temperature

Raman spectra of Ni₂SiO₄ spinel (O _h ⁷ Z=8) have been measured in the temperature range from 20 to 600 °C and the Raman active vibrations (A _1g +E _g +3F _2g ) have been assigned. A calculation of the optically active lattice vibrations of this spinel has been made, assuming a potential function which combines general valence and short range force constants. The values of the force constants at 20 and 500 °C have been calculated from the vibrational frequencies of the observed Raman spectra and infrared (IR) spectral data. The Ni spinel at 20 °C has a prominently small Si-O bond stretching force constant of K(SiO)=2.356 ～ 2.680 md/Å and a large Ni-O bond stretching constant of K(NiO)=0.843 ～ 1.062 md/Å and these force constants at 500 °C decrease to K(SiO)=2.327 ～ 2.494 md/Å and K(NiO)=0.861 ～ 0.990 md/Å. The Si-O bond is noticeably weakened at high temperatures, despite the small thermal expantion from 1.657 Å (20 °C) to 1.660 Å (500 °C). These changes of the interatomic force constants of the spinel at high temperatures are in accord with the thermal structure changes observed by X-ray diffraction study. The weakened Si-O bond is consistent with the fact that Si atoms in the spinel lattice can diffuse at significant rates at elevated temperature.