Physics and Chemistry of Minerals

, Volume 42, Issue 7, pp 541–558 | Cite as

High-pressure and high-temperature deformation experiments on polycrystalline wadsleyite using the rotational Drickamer apparatus

  • Robert Farla
  • George Amulele
  • Jennifer Girard
  • Nobuyoshi Miyajima
  • Shun-ichiro Karato
Original Paper


High-pressure, torsional deformation experiments on polycrystalline wadsleyite were carried out using the rotational Drickamer apparatus (RDA). The experimental conditions ranged between temperatures of ~2000–2200 K at pressures of ~20 ± 1 GPa. Prior to deformation, the fine-grained (1–5 µm) wadsleyite specimens were synthesized from San Carlos olivine in a Kawai-type multi-anvil apparatus. The samples were loaded in the RDA, pressurized and heated, and deformed at stepped strain rates of 5–60 × 10−6 s−1. The stress was determined through the analysis of the orientation dependence on changes in lattice spacing for the (141), (240) and (040) planes. The strain was determined from the orientation of a molybdenum strain marker. Most stepped strain-rate tests reveal the stress exponent n to be 4.7 ± 0.5, suggesting power-law dislocation creep operated. Various samples exhibit grain-size reduction (to 0.1–0.6 µm), possibly associated with dynamic recrystallization or with partial phase transformation to ringwoodite. Transmission electron microscopy and electron backscatter diffraction analyses provide information on the dominant slip system in wadsleyite as 1/2〈111〉 slip on {101} planes, as well as slip in the [100] direction. Dislocation density, even in recrystallized grains, is very high (likely >1014 m−2), reflecting the final high stresses in the samples during deformation. The results provide greater constraints on the regimes of various deformation mechanisms in wadsleyite at various experimental conditions.


Wadsleyite Deformation Rheology Transition zone Lattice-preferred orientation Dislocations 



We thank Michael Vaughan, Haiyan Chen and Matthew Whitaker for technical assistance at NSLS. We also thank Kanani Lee for assistance with EOS pressure calculations for TiC and alumina. The study was substantially improved by three anonymous reviewers. This work was supported by NSF and COMPRES.

Conflict of interest

We declare that this work is not subject to conflict of interest.

Supplementary material

269_2015_742_MOESM1_ESM.pdf (40 kb)
Fig. S1 A sketch showing the decrease in pressure with distance from the centre of the anvil experienced by the cell assembly materials and sample (the anvil culets have a total radius of 2 mm). The profile curves are constructed based on diffraction data from B069 and thermal equations of state for Al2O3 and TiC for a range of temperatures. The pressures in the sample range (d = 0.5 to 0.8 mm) are constrained by the wadsleyite–ringwoodite transition at different temperatures (PDF 40 kb)
269_2015_742_MOESM2_ESM.pdf (3.2 mb)
Fig. S2 Backscatter electrons images and temperature estimations on polished cross sections of enstatite–diopsite quarter rings (panels 1 through 5) that were positioned radially in the same locations as the wadsleyite samples. Pairs of enstatite and diopside neighbouring grains are analysed using the electron probe micro-analyser for Ca concentrations. Using the relations in Gasparik 1996, we calculate temperatures for each enstatite-diopside pair as indicated. The odd temperature estimations reported in brackets for B072 are not included in the final temperature estimation for this sample (PDF 3230 kb)
269_2015_742_MOESM3_ESM.pdf (89 kb)
Fig. S3 Complementary stress-strain data showing the independent evolution of both axial compressive stress and shear stress over time for each sample (panels a–d). The regions indicated by I, II, and III represent incrementally increasing rotation/strain rates (PDF 88 kb)
269_2015_742_MOESM4_ESM.pdf (190 kb)
Fig. S4 Grain size histograms determined from image analysis of the etched grains in each of the samples. The number of grains analysed per sample is given by ‘n’. Panel (a) shows a near-normal distribution in grain size of the annealed sample B068. Panel (b) shows a strong log-normal distribution in grain size, indicating grain size reduction in some regions. Panels (c–e) show a bimodal distribution in grain size where a new population of small grains developed during deformation (PDF 189 kb)
269_2015_742_MOESM5_ESM.pdf (12.2 mb)
Fig. S5 Backscatter electrons images of re-polished sample surfaces showing the distribution of ringwoodite in each sample as indicated by the lighter patches. The bottom row of panels shows the distribution and amount of ringwoodite in each sample with the background subtracted (PDF 12496 kb)
269_2015_742_MOESM6_ESM.pdf (5.3 mb)
Fig. S6 Panels (a) and (b) are typical WBDF-TEM images of transformed ringwoodite grains in B070, indicating in (a) substantial grain flattening and zigzag boundaries in the grain and (b) <101> dislocations on the {111} planes. The inset in (b) is a stereo plot of crystal axes in the nearest zone axis, by using the EDANA software (Kogure, 2003). Panel (c) shows a wadsleyite grain in bright-field TEM mode (B071). Panels (d-f) are typical WBDF-TEM images of wadsleyite in B071, indicating (d) a high density of 1/2〈111〉 dislocations on the {101} planes. (e) [100] and 1/2〈111〉 dislocations are visible. (f) The [100] dislocations on the (001) plane are invisible, but 1/2〈111〉 dislocations are still visible in the same grain of image (e). The inset in (f) is a stereo plot of crystal axes in the nearest zone axis (PDF 5407 kb)
269_2015_742_MOESM7_ESM.docx (15 kb)
Supplementary material 7 (DOCX 14 kb)
269_2015_742_MOESM8_ESM.docx (19 kb)
Supplementary material 8 (DOCX 19 kb)


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Copyright information

© Springer-Verlag Berlin Heidelberg 2015

Authors and Affiliations

  • Robert Farla
    • 1
    • 2
  • George Amulele
    • 1
  • Jennifer Girard
    • 1
  • Nobuyoshi Miyajima
    • 2
  • Shun-ichiro Karato
    • 1
  1. 1.Department of Geology and GeophysicsYale UniversityNew HavenUSA
  2. 2.Bayerisches GeoinstitutUniversität BayreuthBayreuthGermany

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