• Title/Summary/Keyword: $^{27}Al$ MAS & 3QMAS NMR

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A Solid-state 27Al MAS and 3QMAS NMR Study of Basaltic and Phonolitic Silicate Glasses (현무암과 포놀라이트 비정질 규산염의 원자구조 차이에 대한 고상핵자기 공명 분광분석 연구)

  • Park, Sun Young;Lee, Sung Keun
    • Journal of the Mineralogical Society of Korea
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    • v.28 no.1
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    • pp.61-69
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    • 2015
  • While the macroscopic properties and eruption style of basaltic and phonolitic melts are different, the microscopic origins including atomic structures are not well understood. Here we report the atomic structure differences of glass in diopside-anorthite eutectic composition (basaltic glass) and phonolitic glass using high-resolution 1D and 2D solid-state Nuclear Magnetic Resonance (NMR). The $^{27}Al$ MAS NMR spectra for basaltic glass and phonolitic glass show that the full width at half maximum (FWHM) of Al for basaltic glass is about twice than phonolitic glass, suggesting the topological disorder of basaltic magma is larger than that of phonolitic magma. The $^{27}Al$ 3QMAS NMR spectra for basaltic glass and phonolite glass show much improved resolution than the 1D MAS NMR, resolving Al and Al. Approximately 3.3% of Al is observed for basaltic glass, demonstrating the configurational disorder of basaltic magma is larger than phonolitic magma. This result confirms that the topological disorder of Al in basaltic glass is larger than that of phonolitic glass. The observed structural differences between basaltic glass and phonolitic glass can provide an atomistic origin for change of the macroscopic properties with composition including viscosity.

Probing Atomic Structure of Quarternary Aluminosilicate Glasses using Solid-state NMR (다성분계 현무암질 비정질 규산염의 원자 구조에 대한 고상핵자기 공명 분광분석연구)

  • Park, Sun-Young;Lee, Sung-Keun
    • Journal of the Mineralogical Society of Korea
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    • v.22 no.4
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    • pp.343-352
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    • 2009
  • High-resolution Solid-state NMR provides element specific and quantitative information and also resolves, otherwise overlapping atomic configurations in multi-component non-crystalline silicates. Here we report the preliminary results on the effect of composition on the structure of CMAS (CaO-MgO-$Al_2O_3-SiO_2$) silicate glasses, as a model system for basaltic magmas, using the high-resolution 1D and 2D solid-state NMR. The $^{27}Al$ MAS NMR spectra for the CMAS silicate glasses show that four-coordinated Al is predominant, demonstrating that $Al^{3+}$ is network forming cation. The peak position moves toward lower frequency about 4.7 ppm with increasing $X_{MgO}$ due to an increase in $Q^4$(4Si) fraction with increasing Si content, indicating that Al are surrounded only by bridging oxygen. $^{17}O$ MAS NMR spectra for $CaAl_2SiO_6$ and $CaMgSi_2O_6$ glasses qualitatively suggest that NBO fraction in the former is smaller than that in $CaMgSi_2O_6$ glasses. As $^{17}O$ 3QMAS NMR spectrum of model quaternary aluminosilicate glass resolved distinct bridging and non-bridging oxygen environments, atomic structure for natural magmas can also be potentially probed using high-resolution 3QMAS NMR.

27Al Solid-state NMR Structural Studies of Hydrotalcite Compounds Calcined at Different Temperatures

  • Park, Tae-Joon;Choi, Sung-Sub;Kim, Yong-Ae
    • Bulletin of the Korean Chemical Society
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    • v.30 no.1
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    • pp.149-152
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    • 2009
  • Hydrotalcites are anionic clays that are quite prevalent in nature and their importance is growing more and more because of their very wide range of potential applications and uses. Understanding the structural and compositional changes that occur on the molecular scale during the thermal decomposition of hydrotalcite compounds is essential for the basic prediction and comprehensive understanding of the behavior and technical application of these materials. In this study, several hydrotalcite compounds calcined at different temperatures for applications in a chlorine resistant textile were prepared and 27-Aluminm solid-state nuclear magnetic resonance (NMR) spectroscopy was used as a tool to study their local structure and behavior. The changes in the Al coordination of the hydrotalcite compounds were investigated with one dimensional (1D) solid-state magic angle spinning (MAS) NMR spectroscopy. The two broad resonances arising from the structurally different Al coordinations of these compounds were clearly resolved by two dimensional (2D) triple quantum magic angle spinning (3QMAS) NMR spectroscopy.

Pressure-load Calibration of Multi-anvil Press at Ambient Temperature through Structural Change in Cold Compressed Amorphous Pyrope (비정질 파이로프의 저온 압축에 따른 구조 변화를 이용한 멀티 앤빌 프레스의 상온 압력-부하 보정)

  • Lhee, Juho;Kim, Yong-Hyun;Lee, A Chim;Kim, Eun Jeong;Lee, Seoyoung;Lee, Sung Keun
    • Korean Journal of Mineralogy and Petrology
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    • v.35 no.1
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    • pp.65-73
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    • 2022
  • The proper estimation of physical and chemical properties of Earth materials and their structures at high pressure and high temperature conditions is key to the full understanding of diverse geological processes in Earth and planetary interiors. Multi-anvil press - high-pressure generating device - provides unique information of Earth materials under compression, mainly relevant to Earth's upper mantle. The quantitative estimation of the relationship between the oil load within press and the actual pressure conditions within the sample needs to be established to infer the planetary processes. Such pressure-load calibration has often been based on the phase transitions of crystalline earth materials with known pressure conditions; however, unlike at high temperature conditions, phase transitions at low (or room) temperatures can be sluggish, making the calibration at such conditions challenging. In this study, we explored the changes in Al coordination environments of permanently densified pyrope glasses upon the cold compression using the high-resolution 27Al MAS and 3QMAS NMR. The fractions of highly coordinated Al in the cold compressed pyrope glasses increase with increasing oil load and thus, the peak pressure condition. Based on known relationship between the peak pressure and the Al coordination environment in the compressed pyrope glasses at room temperature, we established a room temperature pressure-load calibration of the 14/8 HT assembly in 1,100-ton multi-anvil press. The current results highlight the first pressure-load calibration of any high pressure device using high-resolution NMR. Irreversible structural densification upon cold compression observed for the pyrope glasses provides insights into the deformation and densification mechanisms of amorphous earth materials at low temperature and high pressure conditions within the subducting slabs.