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  1. Pressure-induced phase transformations (PTs) in Si, the most important electronic material, have been broadly studied. However, strain-induced PTs in Si were never studied in situ. Here, we revealed in situ various important plastic strain-induced PT phenomena. A correlation between the particle size's direct and inverse Hall-Petch effect on yield strength and pressure for strain-induced PT is found. For 100 nm particles, strain-induced PT Si-I³Si-II initiates at 0.3 GPa versus 16.2 GPa under hydrostatic conditions; Si-I³Si-III PT starts at 0.6 GPa and does not occur under hydrostatic pressure. Pressure in small Si-II and Si-III regions is ~5-7 GPa higher than in Si-I. Retaining Si-II and single-phase Si-III at ambient pressure and obtaining reverse Si-II³Si-I PT demonstrates the possibilities of manipulating different synthetic paths. The obtained results corroborate the elaborated dislocation pileup-based mechanism and have numerous applications for developing economic defect-induced synthesis of nanostructured materials, surface treatment (polishing, turning, etc.), and friction. 
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    Free, publicly-accessible full text available March 6, 2025
  2. High-pressure synchrotron X-ray diffraction (XRD) studies have been conducted on three types of Si particles (micron, 100 nm, and 30 nm). The pressure for initiation of Si-I→Si-II phase transformation (PT) essentially increases with a reduction in particle size. For 30 nm Si particles, Si-I directly transforms to Si-XI by skipping the intermediate Si-II phase, which appears during the pressure release. The evolution of phase fractions of Si particles under hydrostatic compression is studied. The equation of state (EOS) of Si-I, Si-II, Si-V, and Si-XI for all three particle sizes is determined, and the results are compared with other studies. A simple iterative procedure is suggested to extract the EOS of Si-XI and Si-II from the data for a mixture of two and three phases with different pressures in each phase. Using previous atomistic simulations, EOS for Si-II is extended to ambient pressure, which is important for plastic strain-induced phase transformations. Surprisingly, the EOS of micron and 30 nm Si are identical, but different from 100 nm particles. In particular, the Si-I phase of 100 nm Si is less compressible than that of micron and 30 nm Si. The reverse Si-V→Si-I PT is observed for the first time after complete pressure release to the ambient for 100 nm particles. 
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    Free, publicly-accessible full text available February 23, 2025
  3. Severe plastic deformations under high pressure are used to produce nanostructured materials but were studied ex-situ. Rough diamond anvils are introduced to reach maximum friction equal to yield strength in shear and the first in-situ study of the evolution of the pressure-dependent yield strength and radial distribution of nano structural parameters are performed for severely pre-deformed Zr.ω-Zr behaves like perfectly plastic, isotropic, and strain-path-independent and reaches steady values of the crystallite size and dislocation density, which are pressure-, strain- and strain-path-independent. However, steady states forα-Zr obtained with smooth and rough anvils are different, causing major challenge in plasticity theory. 
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    Free, publicly-accessible full text available September 2, 2024
  4. Severe plastic deformations under high pressure are used to produce nanostructured materials but were studied ex-situ. We introduce rough diamond anvils to reach maximum friction equal to yield strength in shear and perform the first in-situ study of the evolution of the pressure-dependent yield strength and nanostructural parameters for severely pre-deformed Zr. ω-Zr behaves like perfectly plastic, isotropic, and strain-path-independent. This is related to reaching steady values of the crystallite size and dislocation density, which are pressure-, strain- and strain-path-independent. However, steady states for α-Zr obtained with smooth and rough anvils are different, which causes major challenge in plasticity theory. 
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  5. Pressure-induced phase transformations (PTs) between numerous phases of Si, the most important electronic material, have been studied for decades. This is not the case for plastic strain-induced PTs. Here, we revealed in-situ various unexpected plastic strain-induced PT phenomena. Thus, for 100 nm Si, strain-induced PT Si-I to Si-II (and Si-I to Si-III) initiates at 0.4 GPa (0.6 GPa) versus 16.2 GPa (∞, since it does not occur) under hydrostatic conditions; for 30 nm Si, it is 6.1 GPa versus ∞. The predicted theoretical correlation between the direct and inverse Hall-Petch effect of the grain size on the yield strength and the minimum pressure for strain-induced PT is confirmed for the appearance of Si-II. Retaining Si-II at ambient pressure and obtaining reverse Si-II to Si-I PT are achieved, demonstrating the possibilities of manipulating different synthetic paths. 
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  6. Study of the plastic flow, strain-induced phase transformations (PTs), and nanostructure evolution under high pressure is important for producing new nanostructured phases and understanding physical processes. However, these processes depend on an unlimited combination of five plastic strain components and an entire strain path with no hope of fully comprehending. Here, we introduce the rough diamond anvils (rough-DA) to reach maximum friction equal to the yield strength in shear, which allows determination of pressure-dependent yield strength. We apply rough-DA to compression of severely pre-deformed Zr. We found in situ that after severe straining, crystallite size and dislocation density of α and ω-Zr are getting pressure-, strain- and strain-path-independent, reach steady values before and after PT, and depend solely on the volume fraction of ω-Zr during PT. Immediately after completing PT, ω-Zr behaves like perfectly plastic, isotropic, and strain-path-independent. Rough-DA produces a steady nanostructure in α-Zr with lower crystallite size and larger dislocation density than smooth diamonds. This leads to a record minimum pressure (0.67 GPa) for α-ω PT. Kinetics of strain-induced PT, in addition to plastic strain, unexpectedly depends on time. The obtained results significantly enrich the fundamental understanding of plasticity, PTs, and nanostructure, and create new opportunities in material design, synthesis, and processing of nanostructured materials by coupling severe plastic deformations and PT at low pressure. 
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  7. Study of the plastic flow and strain-induced phase transformations (PTs) under high pressure with diamond anvils is important for material and geophysics. We introduce rough diamond anvils and apply them to Zr, which drastically change the plastic flow, microstructure, and PTs. Multiple steady microstructures independent of pressure, plastic strain, and strain path are reached. Maximum friction equal to the yield strength in shear is achieved. This allows determination of the pressure-dependence of the yield strength and proves that omega-Zr behaves like perfectly plastic, isotropic, and strain path-independent immediately after PT. Record minimum pressure for alpha-omega PT was identified. Kinetics of strain-induced PT depends on plastic strain and time. Crystallite size and dislocation density in omega-Zr during PT depend solely on the volume fraction of omega-Zr. 
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  8. Study of the plastic flow and strain-induced phase transformations (PTs) under high pressure with diamond anvils is important for material and geophysics. We introduce rough diamond anvils and apply them to Zr, which drastically change the plastic flow, microstructure, and PTs. Multiple steady microstructures independent of pressure, plastic strain, and strain path are reached. Maximum friction equal to the yield strength in shear is achieved. This allows determination of the pressure-dependence of the yield strength and proves that ω-Zr behaves like perfectly plastic, isotropic, and strain path-independent immediately after PT. Record minimum pressure for α-ω PT was identified. Kinetics of strain-induced PT depends on plastic strain and time. Crystallite size and dislocation density in ω-Zr during PT depend solely on the volume fraction of ω-Zr. 
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  9. null (Ed.)