the Creative Commons Attribution 4.0 License.
the Creative Commons Attribution 4.0 License.
Grain size dependent large rheology contrasts of halite at low deviatoric stress: evidence from microstructural study of naturally deformed gneissic Zechstein-2 rock salt (Kristallbrockensalz) from the Northern Netherlands
Abstract. Constitutive laws of rock salt are required for the prediction of long-term deformation of radioactive waste repositories and solution mined caverns, which are used for energy storage and play an important role in the energy transition. Much of this deformation is at differential stresses of a few MPa. The vast majority of laboratory measurements of salt creep are at much higher differential stress and require extrapolation over many orders of magnitude. This extrapolation can be made more reliable by including microphysical information on the deformation mechanisms in the laboratory samples, integrated with microstructural analysis of samples deformed in natural laboratories at low differential stress.
Rock salt can deform at widely different rates at the same temperature and deviatoric stress, depending on state variables such as grain size, solid solution- and second phase- impurities, crystallographic preferred orientation, water content and grain boundary structure. Both dislocation creep and dissolution-precipitation creep processes are common, but dissolution-precipitation creep (pressure solution) is not commonly included in current engineering predictions.
Here we show evidence for large grain size-dependent differences in halite rheology based on microstructural observations from Zechstein rock salt cores of the Northern Netherlands that experienced different degrees of tectonic deformation. We studied the relatively undeformed Z2 (Stassfurt Formation)‚ horizontal-layered salt from Barradeel, and compare it with much stronger deformed equivalent in diapiric salt form Winschoten, Zuidwending, and Pieterburen. We used optical microscopy of Gamma-irradiated thin sections for microtectonic analysis, recrystallized grain size measurements and subgrain size piezometry, SEM-EDX and XRD for second phase mineralogy. Subgrain size piezometry shows that this deformation took place at differential stress between 0.5 and 2 MPa, providing a natural laboratory.
In the undeformed, layered salt from Barradeel we find cm-thick layers of single crystalline halite (Kristalllagen) alternating with fine-grained halite and thin anhydrite layers. The domal salt samples are typical of the well-known "Kristallbrocken" salt, and consist of cm-size tectonically disrupted megacrystals surrounded by fine-grained halite with grain size of a few mm. We infer high strains in the fine-grained halite as shown by folding and boudinage of thin anhydrite layers, as compared to the megacrystals, which are internally much less deformed and develop subgrains during dislocation creep. Subgrain size shows comparable differential stresses in Kristallbrocken than in matrix salt. The fine-grained matrix salt is dynamically recrystallized, has few subgrains and microstructures indicating deformation by solution-precipitation processes. We infer that the finer grained halite deformed dominantly via pressure solution and the megacrystals dominantly by dislocation creep.
This provides evidence that the fine-grained matrix salt is much weaker than Kristallbrocken because of different dominant deformation mechanisms. This is in agreement with microphysical models of pressure solution creep in which grain size has a significant effect on strain rate at these low differential stress. Our results on the operation of pressure solution creep in rock salt at differential stress of a few MPa point to the importance of this mechanism at low differential stresses around engineered structures but also in most salt tectonic settings. We suggest that including results of microstructural analysis can strongly improve engineering models of rock salt deformation.
We recommend that this mechanism of grain size dependent rheology is included more consistently in the constitutive laws describing deformation of engineered structures in rock salt.
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Notice on discussion status
The requested preprint has a corresponding peer-reviewed final revised paper. You are encouraged to refer to the final revised version.
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Preprint
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The requested preprint has a corresponding peer-reviewed final revised paper. You are encouraged to refer to the final revised version.
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Interactive discussion
Status: closed
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RC1: 'Comment on egusphere-2022-655', Prokop Závada, 08 Sep 2022
This is a very nice microstructural study on the Zechstein salt sequence rocksalt samples that address the rheology of subsurface salt formations. The manuscript is concisely written, reads well, English is good and the imagery and diagrams are also well prepared. The microstructures of selected samples are also nicely illustrated in traced grain boundaries (Fig. 3). The outcomes are relevant for salt tectonics researchers and salt mine engineers.
I only have some minor comments and suggestions on how to improve the manuscript. These suggestions are provided as embedded „sticky notes“ within the annotated pdf that I attach to this review.
I would point out the two main remarks that should be addressed by the authors in the revised version.
- The rheology contrast between the coarse rectangular halite grains in the ‘Kristalllage/Kristallbrocken’ and the fine-grained ‘matrix halite’ is attributed to the different deformation mechanisms. I quite agree with this, but the reason for this difference is mainly the original grain size, explained on line 314. All other features are secondary. The Bromide impurity content discussion is redundant as no Br content data from this study or earlier studies is indicated. Can you offer the explanation for these enigmatic Kristalllage layers in the introduction, and how the large crystals of halite may have formed? Does it reflect a special sedimentary/diagenetic environment? Can we expect such very coarse-grained in other salt basins?
- The discussion does not completely reflect the datasets acquired in the manuscript. The quantitative datasets - grain sizes presented in Figure 7 are completely omitted in the description (Results section), although this is the only link between the salt samples from the 4 diapirs studied. Can you evaluate the meaning of the grain size distributions from the diapirs a bit more? Do you find any correlation in grain size, the degree of macroscopic deformation (e.g. intensity of folding, boudinage at sampling site), and the modal content of Kristallbrocken layers vs. matrix rocksalt between the studied diapirs? Do the samples show any difference? Instead, the discussion about the composite rheology of the mechanically anisotropic rock sequences containing the coarse-grained layers is inaccurate and not supported by the datasets.
I suggest dividing the Results and Discussion sections into subsections. For the results section, you can provide first the microstructural description (shapes of crystals, the relationship between layers, modal content of Kristalllagen/Kristallbrocken), second the quantitative microstructural analysis (grain sizes, subgrain sizes), and third the EBSD data.
Reference to figure 7 is completely missing!!! Dataset presented in Fig. 7 is not described or discussed, although this is one of the primary results of this whole quantitative microstructural study.
Keep the sequential referencing of the figures throughout the text. For example, Figure 8 is called before Figure 6 in the text.
Revise the micrographs, few of them would be more distinct when their contrast and brightness are enhanced (Fig. 5b, f, g, also 4b).
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AC2: 'Reply on RC1', Jessica Barabasch, 30 Nov 2022
We thank Prokop Závada and address the embedded comments and suggestions in the revised manuscript version.
As suggested, we omit the reference to Bromide content distribution and correlation to microstructure similarity. However, we keep the reference to the role of solid solution content on viscosity in the introduction and conclusion section. We agree that more information regarding the enigmatic Kristalllagen and their genesis would help to better asses the rheology of the sequence. We include further information on the Kristalllagen and Kristallbrocken crystallographic orientation, however we present no new hypothesis regarding their genesis or possible further deposits as this was not studied and would be somewhat speculative. As suggested, we add more evaluation regarding the quantitative grain size dataset in the results and discussion section. We slightly modify the discussion about the composite rheology of mechanically anisotropic rock sequence to be more accurate. However, we decide to keep the part of the discussion even though the suggested model is only supported by our data to some extent (subgrainsize analysis) as we think this adds insight into the rheological aspect of the sequence. We add one subsection (EBSD results) in the results part and modify one subheading to make the structure of the results section more clear. We add subsections in the discussion part of the manuscript as suggested. We agree and elaborate more on results shown in figure 7. Sequential referencing is corrected. Micrographs are contrast and brightness are enhanced as suggested to help making our observations more clear.
Citation: https://doi.org/10.5194/egusphere-2022-655-AC2
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RC2: 'Comment on egusphere-2022-655', Hans de Bresser, 16 Sep 2022
This is well written paper with a thorough, detailed, and very welcome description of salt microstructures. The main message, the role of grain size, comes across well. I have added comments and suggestions directly in the attached document.
There is one general point that requires clarification, to my opinion.
On the one hand, it is indicated that the matrix is dynamically recrystallized (e.g. lines 35, 129, 396), what I interpret as driven by differences in strain energy related to dislocations (there are subgrains in the matrix), on the other hand, the fraction of rex grains is interpreted to be low (line 359) and the fine grains are thought to have been present already before deformation (line 323). So the conclusion is that the matrix deformed by grain size dependent pressure solution creep, and not by disloc mechanisms. I propose that the authors are more clear on the observations regarding rex in the matrix and better underpin their interpretation that the small grain size in the matrix is pre-deformation.
Related to this point: data on the grain size of the matrix are presented in Fig. 7, but these data seem hardly been used (and there is no reference to the Figure in the text). Importantly, if one would assume that the matrix grains are recrystallized grains, and then apply the rex grain size piezometer from Ter Heege et al. (2005), one would get unrealistically high stresses. This supports the interpretation of the paper that the matrix did not deform by dislocation creep.
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AC1: 'Reply on RC2', Jessica Barabasch, 30 Nov 2022
We appreciate Hans de Bressers comments and individual ones are addressed in the revised manuscript version.
We clarify our observations and interpretation on the role of dynamic recrystallization also adding considerations (i.e. that after the Ter Heege et al. (2005) recrystallized grain size piezometer one would get unrealistically high stresses if the fine grained halite had been deformed dominantly via dynamic recrystallization). However, due to overprinting and complexity of the polyphase samples we cannot present more clear observations regarding quantitative contribution of dynamic recrystallization in the fine grained matrix halite. Similarly, we offer the interpretation that small grain size in the matrix is mostly pre-deformational by presenting an undeformed equivalent of the Barradeel samples with both fine-grained halite and Kristalllagen.
Citation: https://doi.org/10.5194/egusphere-2022-655-AC1
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AC1: 'Reply on RC2', Jessica Barabasch, 30 Nov 2022
Interactive discussion
Status: closed
-
RC1: 'Comment on egusphere-2022-655', Prokop Závada, 08 Sep 2022
This is a very nice microstructural study on the Zechstein salt sequence rocksalt samples that address the rheology of subsurface salt formations. The manuscript is concisely written, reads well, English is good and the imagery and diagrams are also well prepared. The microstructures of selected samples are also nicely illustrated in traced grain boundaries (Fig. 3). The outcomes are relevant for salt tectonics researchers and salt mine engineers.
I only have some minor comments and suggestions on how to improve the manuscript. These suggestions are provided as embedded „sticky notes“ within the annotated pdf that I attach to this review.
I would point out the two main remarks that should be addressed by the authors in the revised version.
- The rheology contrast between the coarse rectangular halite grains in the ‘Kristalllage/Kristallbrocken’ and the fine-grained ‘matrix halite’ is attributed to the different deformation mechanisms. I quite agree with this, but the reason for this difference is mainly the original grain size, explained on line 314. All other features are secondary. The Bromide impurity content discussion is redundant as no Br content data from this study or earlier studies is indicated. Can you offer the explanation for these enigmatic Kristalllage layers in the introduction, and how the large crystals of halite may have formed? Does it reflect a special sedimentary/diagenetic environment? Can we expect such very coarse-grained in other salt basins?
- The discussion does not completely reflect the datasets acquired in the manuscript. The quantitative datasets - grain sizes presented in Figure 7 are completely omitted in the description (Results section), although this is the only link between the salt samples from the 4 diapirs studied. Can you evaluate the meaning of the grain size distributions from the diapirs a bit more? Do you find any correlation in grain size, the degree of macroscopic deformation (e.g. intensity of folding, boudinage at sampling site), and the modal content of Kristallbrocken layers vs. matrix rocksalt between the studied diapirs? Do the samples show any difference? Instead, the discussion about the composite rheology of the mechanically anisotropic rock sequences containing the coarse-grained layers is inaccurate and not supported by the datasets.
I suggest dividing the Results and Discussion sections into subsections. For the results section, you can provide first the microstructural description (shapes of crystals, the relationship between layers, modal content of Kristalllagen/Kristallbrocken), second the quantitative microstructural analysis (grain sizes, subgrain sizes), and third the EBSD data.
Reference to figure 7 is completely missing!!! Dataset presented in Fig. 7 is not described or discussed, although this is one of the primary results of this whole quantitative microstructural study.
Keep the sequential referencing of the figures throughout the text. For example, Figure 8 is called before Figure 6 in the text.
Revise the micrographs, few of them would be more distinct when their contrast and brightness are enhanced (Fig. 5b, f, g, also 4b).
-
AC2: 'Reply on RC1', Jessica Barabasch, 30 Nov 2022
We thank Prokop Závada and address the embedded comments and suggestions in the revised manuscript version.
As suggested, we omit the reference to Bromide content distribution and correlation to microstructure similarity. However, we keep the reference to the role of solid solution content on viscosity in the introduction and conclusion section. We agree that more information regarding the enigmatic Kristalllagen and their genesis would help to better asses the rheology of the sequence. We include further information on the Kristalllagen and Kristallbrocken crystallographic orientation, however we present no new hypothesis regarding their genesis or possible further deposits as this was not studied and would be somewhat speculative. As suggested, we add more evaluation regarding the quantitative grain size dataset in the results and discussion section. We slightly modify the discussion about the composite rheology of mechanically anisotropic rock sequence to be more accurate. However, we decide to keep the part of the discussion even though the suggested model is only supported by our data to some extent (subgrainsize analysis) as we think this adds insight into the rheological aspect of the sequence. We add one subsection (EBSD results) in the results part and modify one subheading to make the structure of the results section more clear. We add subsections in the discussion part of the manuscript as suggested. We agree and elaborate more on results shown in figure 7. Sequential referencing is corrected. Micrographs are contrast and brightness are enhanced as suggested to help making our observations more clear.
Citation: https://doi.org/10.5194/egusphere-2022-655-AC2
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RC2: 'Comment on egusphere-2022-655', Hans de Bresser, 16 Sep 2022
This is well written paper with a thorough, detailed, and very welcome description of salt microstructures. The main message, the role of grain size, comes across well. I have added comments and suggestions directly in the attached document.
There is one general point that requires clarification, to my opinion.
On the one hand, it is indicated that the matrix is dynamically recrystallized (e.g. lines 35, 129, 396), what I interpret as driven by differences in strain energy related to dislocations (there are subgrains in the matrix), on the other hand, the fraction of rex grains is interpreted to be low (line 359) and the fine grains are thought to have been present already before deformation (line 323). So the conclusion is that the matrix deformed by grain size dependent pressure solution creep, and not by disloc mechanisms. I propose that the authors are more clear on the observations regarding rex in the matrix and better underpin their interpretation that the small grain size in the matrix is pre-deformation.
Related to this point: data on the grain size of the matrix are presented in Fig. 7, but these data seem hardly been used (and there is no reference to the Figure in the text). Importantly, if one would assume that the matrix grains are recrystallized grains, and then apply the rex grain size piezometer from Ter Heege et al. (2005), one would get unrealistically high stresses. This supports the interpretation of the paper that the matrix did not deform by dislocation creep.
-
AC1: 'Reply on RC2', Jessica Barabasch, 30 Nov 2022
We appreciate Hans de Bressers comments and individual ones are addressed in the revised manuscript version.
We clarify our observations and interpretation on the role of dynamic recrystallization also adding considerations (i.e. that after the Ter Heege et al. (2005) recrystallized grain size piezometer one would get unrealistically high stresses if the fine grained halite had been deformed dominantly via dynamic recrystallization). However, due to overprinting and complexity of the polyphase samples we cannot present more clear observations regarding quantitative contribution of dynamic recrystallization in the fine grained matrix halite. Similarly, we offer the interpretation that small grain size in the matrix is mostly pre-deformational by presenting an undeformed equivalent of the Barradeel samples with both fine-grained halite and Kristalllagen.
Citation: https://doi.org/10.5194/egusphere-2022-655-AC1
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AC1: 'Reply on RC2', Jessica Barabasch, 30 Nov 2022
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Jessica Barabasch
Joyce Schmatz
Jop Klaver
Alexander Schwedt
Janos L. Urai
The requested preprint has a corresponding peer-reviewed final revised paper. You are encouraged to refer to the final revised version.
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