Solid-state NMR Lab
Institute for Planetary Materials, Okayama University
Misasa, Tottori 682-0193 Japan

Managed by: Dr. Xianyu Xue, Professor of Mineralogy & Magmalogy Ph.D. 1993, Stanford U. (USA) M.Sc. 1988, U. Alberta (Canada) B.Sc. 1984, Peking U. (China) E-mail: xianyu@misasa.okayama-u.ac.jp Speciaty: mineralogy, magmalogy, NMR spectroscopy researchmap (JST): Link Google Scholar: Link Web of Science: Link Pure (Elsevier): Link ORCID: Link

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Announcements

• Call for Joint-use/Joint-research in FY2025 (April 1 2025~March 31 2026)

  • The deadline (Jan 31) for applications for joint-use/joint research during FY2025 (April 1 2025~March 31 2026) is over. Nevertheless, for those who have a strong need to collaborate with us, but did not manage to apply before the deadline, it is still possible to apply. If you are interested in collaborative research with us using NMR, Raman, etc. in our lab, please feel free to discuss with Xue. The application deadline is January 31, 2025. For details of the joint-use/joint research program, please visit this site.
    

• New papers recently published:

  • Xue, X., Kanzaki, M. & Yin, R. Unravelling the incorporation mechanisms of water in aluminous orthoenstatite: II. comprehensive 1H, 29Si and 27Al NMR measurements. Contrib Mineral Petrol 179, 105 (2024). https://doi.org/10.1007/s00410-024-02182-5 (Published: November 11, 2024, Open access).[Link]
    
  • Xue, X., and Kanzaki, M. (2024) Unravelling the incorporation mechanisms of water in aluminous orthoenstatite: I. First-principles calculations. Contributions to Mineralogy and Petrology, 179, 104, https://doi.org/10.1007/s00410-024-02171-8 (Published: November 9, 2024, Open access).[Link]
    
  • Xue, X., and Kanzaki, M. (2024) Correlation between Si-Al disorder and hydrogen-bonding distance variation in ussingite (Na2AlSi3O8OH) revealed by one- and two-dimensional multi-nuclear NMR and first-principles calculation. American Mineralogist, 109(5), 858-871. (First online: May 1, 2024).[Link]
    
  • Xue, X., Kanzaki, M., Djirar, A.-E., and Gregson, C. (2024) Incorporation mechanisms and infrared absorption coefficients of water in MgSiO3 orthoenstatite clarified via comprehensive NMR and vibrational spectroscopic measurements, and first-principles calculations. Contributions to Mineralogy and Petrology, 179(4), 33 (Published: 25 March 2024, Open access) [Link]
    
    

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  Facilities

• NMR Instrumentation:

  • Bruker Avance NEO 400 MHz NMR Spectrometer (NB)(3 chanels (HXY) (installed in 2018)
  • Bruker 3.2 mm HX MAS probe (spinning rate up to 24 kHz)(installed in 2018)
  • Bruker 1.9 mm HX MAS probe (spinning rate up to 42 kHz)(installed in 2018)
  • Varian 2.5 mm T3 double-resonance MAS probe (spinning rate up to 30 kHz; frequency range: BB chanel: ³⁹K ~ ³¹P; DC chanel: ¹H & ¹⁹F)
  • Varian 1.6 mm T3 HXY triple-resonance MAS probe (spinning rate up to 40 kHz) (installed in 2008)
  • Agilent (Varian) 1.2 mm T3 HXY triple-resonance MAS probe (spinning rate up to 60 kHz) (installed in 2012)
  
  These facilities are open to joint use/joint researches. Please contact Xue for details.
  
  

• Other Instrumentation (micro-Raman, HP-HT experimental facilities, computers, etc.):

  We also have a self-assembled micro-Raman system that is capable of measurements in the low-frequency region (< 100 cm-1) using a 488 nm laser, and measurements using a near-infrared (785 nm) laser, various high-pressure and high-temperature experimental facilities (QuickPress piston-cylindar apparatus, internally heated gas pressure vessel, hydrothermal DAC, etc.) and computers for first principles calculations using Quantum Espresso, etc., which have been developed/managed by Prof. Masami Kanzaki, in our group. For details, please visit Masami Kanzaki's page.
  
  Although Professor Kanzaki officially retired at the end of March 2024, he is currently continuing working with us, as a visiting researcher, in managing/developing these facilities and serving the needs of joint-use/research from both Japan and overseas.
  
  If you are interested in joint use/joint research using these facilities, please contact Xue.
  
  

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  Useful information

  • NMR periodic table (pdf) (by M. Kanzaki)
    
    

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  Research projects

  • Water in nominally anhydrous and hydrous mantle minerals

    Water is the most important volatile component that may significantly affect the thermodynamic and physical properties of minerals even at trace level, and thus knowledge about how and how much water is incorporated into mantle minerals is indispensable in order to understand the structure and dynamics of Earth and planetary interiors, and how they are related to the planetary habitability. Despite extensive studies, the current understanding on these issues are limited (and often wrong) due to difficulties of interpreting data of more commonly used spectroscopic techniques, such as infrared spectroscopy.
    
    We take a unique, comprehensive approach of combining multi-nuclear, multi-dimensional NMR, vibrational spectroscopy and first-principles calculation, which allows us to gain an unambiguous understanding of these issues. We have carried out extensive work over the years on diverse hydrous mantle minerals (and silicate glasses) synthesized using high P-T apparatus, which provided us with deep insights in the behavior of water in Earth materials and the expertise to study them even at trace levels (see publication list). Our recent work on the more challenging nominally anhydrous minerals, including the most abundant upper mantle minerals, olivine (Xue et al., 2017, Am Mineral) and pyroxene (Xue et al. 2024, Contrib Mineral Petrol; Xue et al., in prep), demonstrated the power of this approach. It allowed us to unambiguously clarify how water is incorporated in these mantle minerals, and also revealed that the commonly used infrared spectroscopic technique failed to detect part of the incorporated OH defects in orthoenstatite (pyroxene) that have strong hydrogen bonding, and thus underestimated the water solubility. This finding has implications well beyond pyroxene, and may change our common sense about how much water may be stored in the deep planetary interiors. The goal of our ongoing project is to extend the approach to all major mantle minerals, especially the most important lower mantle mineral, bridgmanite.
    
    It is expected that our understanding about how water is present in the deep Earth and other planets may be significantly advanced in the coming years with the progress of this exciting and ambitious ongoing project.
    
    

  • NMR crystallography of minerals and related inorganic compounds

    The rich variety of structural information that may be provided by multi-nuclear, multi-dimensional NMR can be combined with powder X-ray diffraction (NMR crystallography) for structural determination of minerals and related materials with complicated crystal structure that may be difficult to solve with other means. Together with Prof. Masami Kanzaki, we have used this approach and successfully determined the crystal structures of a number of high-pressure phases synthesized in the lab, that were either discovered by us (e.g. three AlPO4 phases: Kanzaki et al., 2011; Kanzaki and Xue, 2012), or reported by others long time ago, but with structures remaining unsolved (e.g. two Zn2SiO4 phases: Liu et al., 2013; two oxygen-deficient perovskite phases in the CaSiO3-CaAlO2.5 join: Kanzaki et al., 2017).
    
    

  • Cation disorder and hydrogen bonding in natural minerals

    Cation order/disorder (e.g. Al/Si) and hydrogen bonding are two important factors controlling the thermodynamic and physical properties of minerals. NMR has long been regarded as a powerful tool in providing such information, for which X-ray diffraction tends to be insensitive. Traditionally, the interpretation of NMR spectra relies on empirical knowledge about the correlation between NMR parameters and local structural parameters, which tend to be ambiguous. The approach we adopted in combining multi-nuclear, multi-dimensional NMR with first-principles calculation has revolutionized the situation, and allowed us to gain detailed, unambiguous picture. A good example is our recent work on the natural mineral, ussingite (Na2AlSi3O8OH) (Xue and Kanzaki, 2024). We were able to completely clarify the nature of Si-Al disorder and how it affects the next-nearest neighbor environments of Si/Al and H, with the experimental NMR data in complete agreement with first-principles calculation results, providing a 3D view of the disordered local structure. Our study also revealed an intriguing correlation between the Si-Al disorder and the hydrogen bonding distance variation, which may be a universal phenomenon applicable also to other hydrous minerals.
    
    

  • Structure of silicate melts (glasses)

    We also did extensive work over the years on the structure of silicate melts (glasses). In particular, our series of work on hydrous (alumino)silicate melts with different degrees of polymerization and cation types clarified how the water incorporation mechanisms change as a function of melt composition, and provided the basis for understanding the behavior of natural magma of different compositions.
    Xue and Kanzaki (2009, J Am Ceramic Soc, feature article) provided a good review of our work up to then.
    
    

  • Application of NMR spectroscopy to diverse Earth and planetary materials and related materials

    It is our goal that the power of NMR spectroscopic technique is fully utilized to help solve diverse structural issues on Earth and planetary materials and related materials. Toward that goal, we welcome collaboration with researchers both in Japan and worldwide (including students and young researchers). Some examples of past and ongoing collaborative projects include crystalline and amorphous carbonates (with Prof. Hiroyuki Kagi, Tokyo Univ), CaTiO3-CaAl2O5 defect perovskite (with Prof. Takuya Nagai, Hokaido Univ), natural zeolite, garnet and synthetic hydrogarnet minerals (with Prof. Charles Geiger, Austria), natural and synthetic prehnite minerals (with Prof. Jonathan Stebbins, Stanford Univ).
    
    If you have a project that may benefit from NMR measurements, do not hesitate to contact Xue for potential collaboration. Travel and accommodation fees may be provided via IPM's joint-use/joint research program. It is also possible to send the samples for us to do the analyses.
    
    

  • Application of Raman spectroscopy to diverse Earth and planetary materials and related materials

    Dr. Masami Kanzaki, now a visiting researcher in our lab, has developed a unique micro-Raman system that is capable of measurements in the low-frequency region (< 100 cm-1) using a 488 nm laser, and measurements using a near-infrared (785 nm) laser, among other self-developed facilities, which has led to a number of unique new insights into the structure and dynamics of diverse minerals, from high-pressure hydrous silicate phases to natural zeolite minerals. For details, please visit Masami Kanzaki's page. We welcome collaborations using this facility on diverse Earth and planetary materials and related materials with researchers in Japan and worldwide (including students and young researchers).
    
    If you have a project that may benefit from measurements using our facility, do not hesitate to contact Xue for potential collaboration. Travel and accommodation fees may be provided via IPM's joint-use/joint research program. It is also possible to send the samples for us to do the analyses.
    
    
  
  

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  Opportunities

  • Call for M.Sc. and Ph.D. students and collaborations

    We are looking for highly motivated students with a background in mineralogy or related fields (e.g. chemistry, physics, materials science) to join our M.Sc. or Ph.D. program in pursuing exciting projects on spectroscopic and experimental studies of minerals and melts (glasses) produced under high P-T. Financial supports may be available for successful applicants.
    
    We also welcome collaborations in utilizing NMR and/or Raman spectroscopic techniques to gain valuable structural information on diverse Earth and planetary materials and related materials. Students and young researchers are in particular encouraged to discuss with us. Educational support is also available. Travel and accommodation fees may be provided via IPM's joint-use/joint research program. It is also possible to send the samples for us to do the analyses.
    

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  Recent publications (2016-present)

  • Xue, X., Kanzaki, M. & Yin, R. Unravelling the incorporation mechanisms of water in aluminous orthoenstatite: II. comprehensive 1H, 29Si and 27Al NMR measurements. Contrib Mineral Petrol 179, 105 (2024). https://doi.org/10.1007/s00410-024-02182-5 (Published: November 11, 2024, Open access).[Link]
    
    
  • Xue, X., and Kanzaki, M. (2024) Unravelling the incorporation mechanisms of water in aluminous orthoenstatite: I. First-principles calculations. Contributions to Mineralogy and Petrology, 179, 104, https://doi.org/10.1007/s00410-024-02171-8 (Published: November 9, 2024, Open access).[Link]
    
    
  • Xue, X., and Kanzaki, M. (2024) Correlation between Si-Al disorder and hydrogen-bonding distance variation in ussingite (Na2AlSi3O8OH) revealed by one- and two-dimensional multi-nuclear NMR and first-principles calculation. American Mineralogist, 109(5), 858-871. (First online: May 1, 2024).[Link]
    
    
  • Xue, X., Kanzaki, M., Djirar, A.-E., and Gregson, C. (2024) Incorporation mechanisms and infrared absorption coefficients of water in MgSiO3 orthoenstatite clarified via comprehensive NMR and vibrational spectroscopic measurements, and first-principles calculations. Contributions to Mineralogy and Petrology, 179(4), 33 (Published: 25 March 2024, Open access) [Link]
    
    
  • Marugata, S., Kagi, H., Ijichi, Y., Komatsu, K., Xue, X., and Sugiyama, K. (2022) Experimental evidence of static disorder of carbonate ions in Ba-doped calcite. Journal of Solid State Chemistry, 312, 123258.[Link]
    
    
  • Xue, X. (2020) Comment on "Towards the reconciliation of viscosity change and CO2-induced polymerization in silicate melts" by Yann Morizeta, Michael Paris, David Sifre, Ida Di Carlo, Sandra Ory, and Fabrice Gaillard [Chemical Geology 458 (2017) 38-47]. Chemical Geology, 550, 119675.[Link]
    
    
  • Xianyu Xue, Masami Kanzaki, Paul Floury, Tsubasa Tobase, James Eguchi, Carbonate speciation in depolymerized and polymerized (alumino)silicate glasses: Constraints from 13C MAS and static NMR measurements and ab initio calculations, (2018) Chemical Geology,479, 151-165, ISSN 0009-2541,[Link]
    
    
  • Kanzaki, M. and Xue, X. (2017) Protoenstatite in MgSiO3 samples prepared by conventional solid state reaction, J. Mineral. Petrol. Sci., 112 (Adv. Publication online). doi:10.2465/jmps.170616[Link]
    
    
  • Kanzaki, M., Xue, X., Wu, Y., and Nie, S.F. (2017) Crystal structures of two oxygen-deficient perovskite phases in the CaSiO3-CaAlO2.5 join. Physics and Chemistry of Minerals, 44, 717-733.[Link]
    
    
  • Xue, X., Kanzaki, M., Turner, D., and Loroch, D. (2017) Hydrogen incorporation mechanisms in forsterite: New insights from 1H and 29Si NMR spectroscopy and first-principles calculation. American Mineralogist, 102,519-536.[Link]
    
    
  • Kanzaki, M., & Xue, X. (2016). Cation distribution in Mg-Zn olivine solid solution: a 29Si MAS NMR and first-principles calculation study. Journal of Mineralogical and Petrological Sciences, 111, 292-296.[Link]
    
    

  [Link to complete publication list (1989-present)]

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  Recent meeting presentations (2016-present)

  • Xianyu Xue (2025) Unravelling the structures of Earth materials using solid-state NMR and first-principles calculations: Recent progress, Solid-state NMR for Materials Forum June 6, 2025 at Tohoku University, Sendai (Invited)(planned)
  
  
  • Xianyu Xue and Masami Kanzaki (2025) Water in nominally anhydrous mantle minerals: Insights from comprehensive spectroscopic measurements and first-principles calculations, The American Ceramic Society Glass and Optical Materials Division Meeting (GOMD 2025) in Vancouver, Canada (May 6, 2025) (Invited)
  
  
  • Xianyu Xue, Masami Kanzaki and Rongzhang Yin (2024) The incorporation mechanisms of water in aluminous orthoenstatite clarified via comprehensive NMR measurements and first-principles calculations, Japan Association of Mineralogical Sciences Annual Meeting 2024 (Sept 14)
  
  
  • Xianyu Xue and Masami Kanzaki (2024) Water in nominally anhydrous mantle minerals: Are you seeing them all? JpGU SIT15-05, 10:00 - 10:15, May 30, 2024 (Invited)
  
  
  • Xianyu Xue (2023) Water Incorporation Mechanisms in Nominally Anhydrous Minerals, Bjorn Mysen’s Retirement Symposium, 2023 (Nov 3) (Invited)
  
  
  • Xianyu Xue and Masami Kanzaki (2023) H and Al incorporation mechanisms in stishovite: New insights from multi-nuclear NMR and first-principles calculation, Japan Association of Mineralogical Sciences Annual Meeting 2023 (Sept 16)
  
  
  • Xianyu Xue (2023) Relationship between Si-Al distribution & hydrogen bonding distance: Insight from ussingite (Na2AlSi3O8OH) JpGU 2023 (May 25)
  
  
  • Xianyu Xue (2022) Revealing cation disorder and hydrogen bonding in minerals via multi-nuclear NMR and first-principles calculation The 61st Annual Meeting of the NMR Society of Japan (Nov 9)
  
  
  • Xianyu Xue (2022) Si-Al distribution & hydrogen bonding in ussingite (Na2AlSi3O8OH): Unraveled by multi-nuclear NMR and first-principles calculation Japan Association of Mineralogical Sciences Annual Meeting 2022 (Sept 19)
  
  
  • Xianyu Xue, Masami Kanzaki, Jianjun Jiang (2020) Synthesis and structural characterization of a new zinc silicate phase A (Zn7Si2O8(OH)6) by 1H and 29Si NMR and powder X-ray diffraction, JpGU2020
  
  
  • Xianyu XUE, Masami KANZAKI (2019) Dissolution mechanisms of H2O and CO2 in silicate melts (glasses): Insight from NMR spectroscopy, The 36th Japan-Korea International Seminar on Ceramics (2019.11.22.) Torigin Bunka Kaikan, Tottori(Invited)
  
  
  • Xianyu Xue and Masami Kanzaki (2019) Hydrogen defects in high-pressure crystalline silicates: Insights from NMR spectroscopy, 14th International Conference on the Structure of Non-Crystalline Materials 3-8 November 2019, Kobe, Japan (Invited)
  
  
  • Xianyu Xue, Masami Kanzaki and Jianjun Jiang (2018) Hydrogen incorporation mechanisms in enstatite JpGU2018.
    
    
  • Goldschmidt 2017 (August 13 -August 18, 2017, Paris, France):
  • Xue X., Kanzaki M. & Geiger, C.A. (2016) Hydrogen incorporation mechanism in synthetic katoite-grossular and natural grossular: 1H static and MAS NMR and first-principles calculation, August 16 (session 07l), oral
  
  
  • The 2016 Annual Meeting of Japan Association of Mineralogical Sciences (JAMS) , Sept. 23-25, 2016, Kanazawa Univ.
  
  
  • Xianyu Xue and Masami Kanzaki (2016) 4H=1Si substitution in grossular and forsterite: Information from 1H NMR and first-principles calculation. Sept. 25, oral (R2-03)
  
  
  • Goldschmidt 2016 (June 26-July 1, 2016, Yokohama, Japan):
  • Xue X., Kanzaki M., Turner D. & Loroch D. (2016) Hydrogen incorporation mechanisms in forsterite: 1H NMR measurement and first-principles calculation, June 29 (session 04c), oral
  
  

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Copyright: Xianyu Xue