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High Pressure Synthesis in Crystalline Materials

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A special issue of Crystals (ISSN 2073-4352). This special issue belongs to the section "Inorganic Crystalline Materials".

Deadline for manuscript submissions: closed (31 January 2020) | Viewed by 25429

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Special Issue Editors

Prof. Dr. Przemyslaw Dera

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Guest Editor

Hawai'i Institute of Geophysics and Planetology, University of Hawaii at Manoa School of Ocean and Earth Science and Technology, Honolulu, HI 96822, USA
Interests: high-pressure materials; non-quenchable phases; new chemical compounds

Dr. Dongzhou Zhang

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Guest Editor

PX^2 Beamline Scientist 9700 S Cass Ave, Bldg 434A Argonne, IL 60439, USA
Interests: optical spectroscopy, condensed matter physics, high pressure experiment, and planetary interiors

Special Issue Information

Dear colleagues,

Pressure is a principal thermodynamic parameter able to control the state, structure, physical properties and chemical behavior of matter. One of most unique properties of high pressure is the ability to change the pathways of chemical reactions and enable the synthesis of materials that cannot be obtained under ambient pressure conditions. New chemical compounds with unusual and unexpected stoichiometries, new types of bonding, and properties that may be of significant future technological applications have been synthesized in high-pressure experiments. This Special Issue will focus on reports of such results, from experiments, as well as based on computational predictions. Our understanding of the exact mechanisms of high-pressure solid state reactions and the factors controlling their progress and direction is still very preliminary, and improving this knowledge is key to harnessing the power of high pressure for practical applications.

Prof. Przemyslaw Dera
Dr. Dongzhou Zhang
Guest Editors

Manuscript Submission Information

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Keywords

High-pressure materials
non-quenchable phases
new chemical compounds

Published Papers (7 papers)

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Research

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18 pages, 2867 KiB

Open AccessArticle

Crystal-Chemical Properties of Synthetic Almandine-Pyrope Solid Solution by X-Ray Single-Crystal Diffraction and Raman Spectroscopy

by Yunqian Kuang, Jingui Xu, Bo Li, Zhilin Ye, Shijie Huang, Wei Chen, Dongzhou Zhang, Wenge Zhou and Maining Ma

Crystals 2019, 9(10), 541; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst9100541 - 19 Oct 2019

Cited by 3 | Viewed by 3869

Abstract

Crystal-chemical properties of synthetic Almandine-Pyrope (Alm-Pyr) solid solutions were investigated by X-ray single-crystal diffraction and Raman spectroscopy. Garnet solid solution with different compositions were synthesized from powder at 4.0 GPa and annealed at 1200 °C for 48 h by a multi-anvil pressure apparatus. Garnet crystals with different sizes (about 60–1000 μm) were obtained from synthesis. The results of X-ray single-crystal diffraction show that the unit cell constants decrease with increasing Pyr contents in the synthetic Alm-Pyr crystals due to the smaller ionic radius of Mg²⁺ in eightfold coordination than that of Fe²⁺. The data exhibit obviously positive deviations from ideal mixing volumes across the Alm-Pyr join which may be caused by the distortion of the SiO₄ tetrahedron. Moreover, the significant decrease in the average M-O bond length and volume of the [MgO₈]/[FeO₈] dodecahedron with increasing Pyr contents are the most important factors to the decrease in the Alm-Pyr crystal unit cell constant and volume. On the other hand, selected bond distances (average <M-O>, <Al-O>, and <D-O> distances) have a linear correlation with the unit-cell parameter, but the <Si-O> distance has nonlinear correlation. With increasing the unit-cell parameter, the average <M-O> distance increases significantly, followed by the average <D-O> and <Al-O> distances. While the <Si-O> distance changes negligibly further confirming the conclusion that the significant decrease of the average M-O bond length of the [MgO₈]/[FeO₈] dodecahedron with increasing Pyr contents are the most important factors to the decrease in the Alm-Pyr crystal unit cell volume. In the Raman spectra collected for the Alm-Pyr solid solutions, Raman vibration mode assignments indicate that the Raman vibrational spectra change along the Alm-Pyr binary solution. The mode frequencies of Si-O stretching, Si-O bending, and the rotation of the SiO₄-tetrahedron (R(SiO₄)) decrease linearly, while the translational modes of the SiO₄-tetrahedron (T(SiO₄)) increase with increasing Alm contents. Full article

(This article belongs to the Special Issue High Pressure Synthesis in Crystalline Materials)

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8 pages, 2824 KiB

Open AccessArticle

Effect of Pressure Treatment on the Specific Surface Area in Kaolin Group Minerals

by Soyeon Kwon, Huijeong Hwang and Yongjae Lee

Crystals 2019, 9(10), 528; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst9100528 - 14 Oct 2019

Cited by 14 | Viewed by 3327

Abstract

Pressure can tailor the properties of a material by changing its atomistic arrangements and/or crystal morphology. We have investigated the changes in the adsorption properties of kaolin group minerals as a function of pressure treatment in the gigapascal range. External pressures have been applied using a large volume press (LVP) to kaolinite (Al₂Si₂O₅(OH)₄) and halloysite (H₄Al₂O₉Si₂·2H₂O), which represent natural 2D layered and 1D nanowire structures, respectively. Powdered samples have been compressed up to 3 GPa in 1 GPa steps at room temperature and recovered by up to ca. 0.35 g from each pressure step. Brunauer–Emmett–Teller (BET) measurements were conducted using N₂ gas to measure the specific surface area, pore size distribution, and pore volume of the pressure-treated samples. As the treatment pressure increased, kaolinite showed an increase in the adsorption behavior from nonpores to mesopores, whereas halloysite responded in an opposite manner to show a decrease in its adsorption capability. We discuss the contrasting effects of pressure-treatment on the two morphologically distinct kaolin group minerals based on field-emission scanning electron microscope (FE-SEM) images measured on each recovered material. We observed that the layers in kaolinite separate into smaller units upon increasing pressure treatment, whereas the tubes in halloysite become flattened, which led to the contrasting changes in surface area. Further study is in progress to compare this effect to when water is used as the pressure-transmitting medium. Full article

(This article belongs to the Special Issue High Pressure Synthesis in Crystalline Materials)

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10 pages, 1776 KiB

Open AccessArticle

New Tetragonal ReGa₅(M) (M = Sn, Pb, Bi) Single Crystals Grown from Delicate Electrons Changing

by Madalynn Marshall, Karolina Górnicka, Ranuri S. Dissanayaka Mudiyanselage, Tomasz Klimczuk and Weiwei Xie

Crystals 2019, 9(10), 527; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst9100527 - 14 Oct 2019

Cited by 1 | Viewed by 3357

Abstract

Single crystals of the new Ga-rich phases ReGa_~5(Sn), ReGa_~5(Pb) and ReGa_~5(Bi) were successfully obtained from the flux method. The new tetragonal phases crystallize in the space group P4/mnc (No. 128) with vertex-sharing capped Re₂@Ga₁₄ oblong chains. Vacancies were discovered on the Ga4 and Ga5 sites, which can be understood as the direct inclusion of elemental Sn, Pb and Bi into the structure. Heat capacity measurements were performed on all three compounds resulting in a small anomaly which resembles the superconductivity transition temperature from the impurity ReGa₅ phase. The three compounds were not superconducting above 1.85 K. Subsequently, electronic structure calculations revealed a high density of states around the Fermi level, as well as non-bonding interactions that likely indicate the stability of these new phases. Full article

(This article belongs to the Special Issue High Pressure Synthesis in Crystalline Materials)

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15 pages, 3133 KiB

Open AccessArticle

A New High-Pressure Phase Transition in Natural Gedrite

by Tommy Yong, Craig R. Bina, Gregory J. Finkelstein, Dongzhou Zhang and Przemyslaw Dera

Crystals 2019, 9(10), 521; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst9100521 - 11 Oct 2019

Cited by 4 | Viewed by 4238

Abstract

High-pressure diamond-anvil cell synchrotron X-ray diffraction experiments were conducted on single-crystal samples of natural orthoamphibole; gedrite; with composition; (K_0.002Na_0.394)(Mg₂)(Mg_1.637Fe_2.245Mn_0.004Ca_0.022Cr_0.003Na_0.037Al_1.052)(Si_6.517Al_1.483)O₂₂(OH)₂. The samples were compressed at 298 K up to a maximum pressure of 27(1) GPa. In this pressure regime, we observed a displacive phase transition between 15.1(7) and 21(1) GPa from the orthorhombic Pnma phase to a new structure with space group P2₁/m; which is different from the familiar P2₁/m structure of cummingtonite and retains the (+, +, −, −) I-beam stacking sequence of the orthorhombic structure. The unit cell parameters for the new phase at 21(1) GPa are a = 17.514(3), b = 17.077(1), c = 4.9907(2) Å and β = 92.882(6)°. The high-pressure P2₁/m phase is the first amphibole structure to show the existence of four crystallographically distinct silicate double chains. The orthorhombic to monoclinic phase transition is characterized by an increase in the degree of kinking of the double silicate chains and is analogous to displacive phase changes recently reported in orthopyroxenes, highlighting the parallel structural relations and phase transformation behavior of orthorhombic single- and double-chain silicates. Full article

(This article belongs to the Special Issue High Pressure Synthesis in Crystalline Materials)

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8 pages, 2851 KiB

Open AccessArticle

Synthesis of Manganese Mononitride with Tetragonal Structure under Pressure

by Dajian Huang, Caoping Niu, Bingmin Yan, Bo Gao, Lailei Wu, Dongzhou Zhang, Xianlong Wang and Huiyang Gou

Crystals 2019, 9(10), 511; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst9100511 - 30 Sep 2019

Cited by 3 | Viewed by 2738

Abstract

The exploration of the vast phase space of transition metal nitrides is critical for discovering novel materials and potential technological applications. Manganese mononitride with a tetragonal structure (space group I4/mmm) was synthesized in a laser-heating diamond anvil cell, which could be quenched to ambient pressure. The bulk modulus of 173 GPa was measured using in situ high-pressure diffraction, and the axial compressibility shows that, under pressure, the a direction is much more compressible than the c direction in tetragonal MnN. DFT results with correction of the on-site repulsion (GGA + U) confirm that tetragonal MnN is energetically stable and antiferromagnetic. This study highlights the need to include on-site repulsion to understand 3d metal nitrides. Full article

(This article belongs to the Special Issue High Pressure Synthesis in Crystalline Materials)

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9 pages, 2104 KiB

Open AccessArticle

Experimental Evidence for Partially Dehydrogenated ε-FeOOH

by Yukai Zhuang, Zhongxun Cui, Dongzhou Zhang, Jin Liu, Renbiao Tao and Qingyang Hu

Crystals 2019, 9(7), 356; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst9070356 - 13 Jul 2019

Cited by 3 | Viewed by 2976

Abstract

Hydrogen in hydrous minerals becomes highly mobile as it approaches the geotherm of the lower mantle. Its diffusion and transportation behaviors under high pressure are important in order to understand the crystallographic properties of hydrous minerals. However, they are difficult to characterize due to the limit of weak X-ray signals from hydrogen. In this study, we measured the volume changes of hydrous ε-FeOOH under quasi-hydrostatic and non-hydrostatic conditions. Its equation of states was set as the cap line to compare with ε-FeOOH reheated and decompression from the higher pressure pyrite-FeO₂Hx phase with 0 < x < 1. We found the volumes of those re-crystallized ε-FeOOH were generally 2.2% to 2.7% lower than fully hydrogenated ε-FeOOH. Our observations indicated that ε-FeOOH transformed from pyrite-FeO₂Hx may inherit the hydrogen loss that occurred at the pyrite-phase. Hydrous minerals with partial dehydrogenation like ε-FeOOHx may bring it to a shallower depth (e.g., < 1700 km) of the lower mantle. Full article

(This article belongs to the Special Issue High Pressure Synthesis in Crystalline Materials)

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Review

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22 pages, 5747 KiB

Open AccessEditor’s ChoiceReview

From Molecules to Carbon Materials—High Pressure Induced Polymerization and Bonding Mechanisms of Unsaturated Compounds

by Xin Yang, Xuan Wang, Yida Wang, Kuo Li and Haiyan Zheng

Crystals 2019, 9(10), 490; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst9100490 - 24 Sep 2019

Cited by 17 | Viewed by 4407

Abstract

With the development of high-pressure apparatus, in situ characterization methods and theoretical calculations, high-pressure technology becomes a more and more important method to synthesize new compounds with unusual structures and properties. By compressing compounds containing unsaturated carbon atoms, novel poly-ionic polymers, graphanes and carbon nanothreads were obtained. Their compositions and structures were carefully studied by combining multiple cutting-edge technologies, like the in situ high-pressure X-ray and neutron diffraction, transmission electron microscopy, pair distribution function, solid-state nuclear magnetic resonance and gas chromatography-mass spectroscopy. The reaction mechanisms were investigated based on the crystal structure at the reaction threshold pressure (the pressure just before the reaction taking place), the long-range and short-range structure of the product, molecular structure of the intermediates, as well as the theoretical calculation. In this review, we will summarize the synthesis of carbon materials by compressing the unsaturated compounds and its reaction characteristics under extreme conditions. The topochemical reaction mechanism and related characterization methods of the molecular system will be highlighted. This review will provide a reference for designing chemical reaction and exploring novel carbon materials under high-pressure condition. Full article

(This article belongs to the Special Issue High Pressure Synthesis in Crystalline Materials)

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