1. NMR measurement using diamond anvil cell 7/6 Shimizu-Lab M1 Masuda Akiyoshi 1

2. History 2 H 3 S (150 GPa)

3. Introduction-sulfur hydride 3

4. The structure in high-T c phase H 3 S-R3mH 3 S-Im-3m M. Einaga et al., arXiv:1509.03156v1 (2015) D. Duan et al., PRB. 91 (2015)180502. From electrical measurements From XRD and calculation 4

5. Motivation I want to see the position of hydrogen. → Try NMR measurements Why sulfur hydride has such high T c ? Today’s paper 「 NMR in a diamond anvil cell 」 Sam‐Hyeon Lee, K. Luszczynski, R. E. Norberg, and Mark S. Conradi Rev. Sci. Instrum. 58, 415 (1987). 5

6. Diamond anvil cell The goal of pressure in my experiment … Over 100 GPa Sample size …very small Main experiments ①X-ray diffraction (XRD) ②Electrical resistance measurements ③Magnetic susceptibility measurements gasket diamond anvil sample room 6

7. How to measure NMR spectra ① ③ ② Apply static magnetic field Apply RF magnetic field 7

8. How to measure NMR spectra Static magnetic field 8

9. Difficulty in NMR using DAC Reasons ①Very small sample ②Metal gaskets shield RF magnetic fields. ③Inhomogeneity of static magnetic field Purpose… Verify the practicability of NMR with DAC ( 不均一性 ) Metal gasket 9 Sample room

10. 1mm Ruby (for pressure measurement) diamond Metal gasket Sample RF coil Setting Sample …methanol : ethanol (4 : 1) Gasket …Be-Cu ( 3 GPa) Culet size (diameter) …1.0mm Sample room (diameter) …0.5mm Gasket RF magnetic field 10

11. Measurements 1.Measure T 2 *. 2.Measure the pressure dependence of T 1 and T 2. T 1 : 縦緩和時間 useful for analyzing molecular motion, etc. T 2 : 横緩和時間 T 2 * : ( 不均一磁場を含む ) 横緩和時間 Certain being able to obtain the right signals clearly. 11

12. 1, Measure T 2 * the susceptibility of materials (samples, metal gasket and diamonds) Be-Cu is better than Re as for resolving power. → However Hardness : Re > Be-Cu susceptibility: 磁化率 resolving power: 分解能 ダイヤモンドアンビルセル NMR 奥地 拓生 高圧力の科学と技術 Vol. 15, No. 4 (2005) Materialsusceptibility Diamond-21.7 Methanol-6.7 Ethanol-7.3 Rhenium95 Be-Cu (HSBC)42 Be-Cu (HSBC)-5 Metal gasket 12

13. liquid solid 2, Measure the pressure dependence of T 1 and T 2 The values of T 1 and T 2 are changing with pressurization. The state of sample < 5.2 GPa …liquid ○ > 5.2 GPa …solid × 1 kbar = 0.1 GPa 13

14. Conclusion Good points Succeeded observing signals in this setting. Bad points Couldn’t measure signals in solid state Gasket Resolving power: Be-Cu > Re Hardness: Be-Cu < Re resolving power: 分解能 14

15. My work Gasket: Re (for high pressure) Sample size: much smaller 30-50 μm (diameter) × 30 μm (thickness ) Solid state → bad resolving power 15