ᐇ㦂ሗ࿌᭩ᵝᘧ䠄୍⯡฼⏝ㄢ㢟䞉ᡂᯝබ㛤฼⏝䠅㻌䠄 䈜ᮏሗ࿌᭩䛿ⱥㄒ䛷グ㏙䛧䛶䛟䛰䛥䛔䚹䛯䛰䛧䚸⏘ᴗ฼⏝ㄢ㢟䛸䛧䛶᥇ᢥ䛥䜜䛶䛔䜛᪉䛿᪥ᮏㄒ䛷グ㏙䛧䛶䛔䛯䛰䛔䛶䜒⤖ᵓ䛷䛩䚹 䠅㻌Experimental
Report Report㻌MLFExperimental

承認日Dateof Approval
2015/6/3
ᥦฟ᪥ Dateof Report㻌
承認者Approver TakanoriH attori㻌 㻌 㻌 㻌 㻌 㻌 㻌 㻌 of
㻌 㻌report
㻌 2015.6.3
提出日Date2015/6/3

ㄢ㢟␒ྕ㻌 Project No.㻌 㻌 2014A0158㻌

⿦⨨㈐௵⪅ Name of responsible person㻌㻌

Takanori Hattori㻌ᐇ㦂ㄢ㢟ྡ㻌 Title of experiment㻌⿦⨨ྡ Name of Instrument/䠄BL No.䠅㻌

HydrogenpositionofAl-bearinghydrousphase

DandATSUHIME (BL11, PLANET)

superhydrous phase B㻌ᐇ᪋᪥ Date of Experiment㻌ᐇ㦂㈐௵⪅ྡ㻌 Name of principal investigator㻌

2014/11/13 21:00- 11/199:00㻌

Toru Inoueᡤᒓ㻌 Affiliation㻌
Ehime University㻌㻌ヨᩱ䚸ᐇ㦂᪉ἲ䚸฼⏝䛾⤖ᯝᚓ䜙䜜䛯୺䛺䝕䞊䝍䚸⪃ᐹ䚸⤖ㄽ➼䜢䚸グ㏙䛧䛶ୗ䛥䛔䚹䠄㐺ᐅ䚸ᅗ⾲ῧ௜䛾䛣䛸䠅㻌
Please report your samples, experimental method and results, discussion and conclusions. Please add figures andtables for better explanation.
㻝㻚㻌 ヨᩱ Name of sample(s) and chemical formula, or compositions including physical form.㻌
We synthesized various Al-bearing hydrous phases in advance in Ehime University at 28 GPa and 1400䉝, and10 GPa and 900䉝. In our 2014A0158 experiments, we performed the neutron diffraction experiments using
these samples, which had the sintered forms with the dimension of φ ~2 and ~2 mm length and the weight of~30 mg, and the big sintered forms with φ ~6.5 and ~3 mm length and the weight of ~200 mg.
W2b & WH2a: Al-bearing deuterated & hydrous Mg-perovskite, ~MgSi0.9Al0.1O3D0.1 & ~MgSi0.9Al0.1O3H0.1
DO1a & DO2a: Al-bearing Mg-perovskites, ~MgSi0.95Al0.05O2.975 & ~MgSi0.9Al0.1O2.95
New phase D & H (Na, Nb, Nc, NHa, NHb, NHc): Al-bearing silicates, ~Mg5.5AlSi2O8(OD)6 &~Mg5.5AlSi2O8(OH)6㻌㻞㻚㻌 ᐇ㦂᪉ἲཬ䜃⤖ᯝ㻌 䠄ᐇ㦂䛜䛖䜎䛟䛔䛛䛺䛛䛳䛯ሙྜ䚸䛭䛾⌮⏤䜢グ㏙䛧䛶䛟䛰䛥䛔䚹䠅㻌
Experimental method and results. If you failed to conduct experiment as planned, please describe reasons.
The Al-bearing deuterated & hydrous Mg-perovskites and Al-bearing anhydrous Mg-perovskites weresynthesized at ~28 GPa and ~1600䉝, and Al-bearing deuterated & hydrous new phases were synthesized at ~10GPa and 900䉝 by Kawai-type high pressure apparatus in Ehime University. The recovered samples werecharacterized by X-ray powder diffraction, and confirmed that the Al-bearing deuterated & hydrous
Mg-perovskite, Al-bearing anhydrous Mg-perovskites, and Al-bearing deuterated & hydrous new phases were
the dominant phases in each run product.
We conducted the neutron diffraction experiments in MLF on 2014/11/13 21:00 - 11/19 9:00. Before theexperiments, we heard that the condition of ATSUHIME press was not so good because of terrible oil releasefrom the plunger pump. Because we are worried about the further damage of the piston scratch in the plunger
pump system, we decided to collect the clear neutron diffraction pattern of high pressure Al-bearing hydrous
phases at ambient condition which we have already synthesized by high pressure apparatus in Ehime University.
1㻞㻚㻌 ᐇ㦂᪉ἲཬ䜃⤖ᯝ䠄䛴䛵䛝䠅㻌 Experimental method and results (continued)
Al-bearing deuterated & hydrous Mg-perovskites, Al-bearing anhydrous Mg-perovskites, and Al-bearing
deuterated & hydrous new phases were successfully synthesized. The samples and the experimental details ofeach neutron diffraction experiments were summarized in Table.1. We measured 10 samples in this period. The Vrod, V tube and air (empty) were also measured for the data correction.
Figure 1 shows the representative pictures of synthesized Al-bearing㻌 hydrous Mg-perovskite (hy-Pv, D:deuterated, H: hydrous), oxygen-vacancy Mg-perovskite (O-Pv), and Al-bearing new hydrous phase (new phase,
D: deuterated, H: hydrous). We designed and developed larger cell assembly to synthesize large Mg-perovskite
sample at ~28 GPa and Al-bearing new hydrous phase at 10 GPa. The sample was sealed by Au capsule. As theresults, we succeeded to synthesize the samples which have the dimension of φ ~2.2 and ~2.5 mm length andthe weight of ~30 mg for various perovskite, and the dimension of φ ~6.5 and ~3 mm length and the weight of~200 mg for Al-bearing new hydrous phase. These dimensions were large enough to collect the neutron
diffraction data in less than ten hours.
Figure 2 shows the obtained neutron diffractions of Al-bearing Mg-perovskite of deuterated, hydrous andoxygen vacancy forms, and those of Al-bearing new hydrous phase at BL11 in MLF, J-PARC. Now we areconducting Rietveld analysis to determine the hydrogen position.
㻌㻌(Attached table and figure)Table 1. The sample and experimental details of each neutron diffraction experiments in 2014A.
Figure 1: The representative pictures of synthesized Al-bearing hydrous phases and the related phases used forour neutron diffraction experiments. The ruler graduation is 1 mm.
Figure 2. The obtained neutron diffractions of Al-bearing Mg-perovskite and Al-bearing new hydrous phase at
BL11 in MLF, J-PARC.
W2b: hy-Pv (aluminous deuterated Mg-perovskite), ~MgSi0.9Al0.1O3D0.1
WH2a: hy-Pv (aluminous hydrous Mg-perovskite), ~MgSi0.9Al0.1O3H0.1
DO1a: O-Pv (Oxygen vacancy Mg-perovskite), ~MgSi0.95Al0.05O2.975
DO2a: O-Pv (Oxygen vacancy Mg-perovskite), ~MgSi0.9Al0.1O2.95
Na: New phase_D (Al-bearing new deuterated phase), ~Mg5.5Si2AlO8(OD)6
NHa: New phase_H (Al-bearing new hydrous phase), ~Mg5.5Si2AlO8(OH)6
㻌2