xrd20180622.pages
II
1
RIETAN-FP [1] VESTA [2]

-

y1, y2,!, yN{ } Y1,Y2,!,YN{ }
σ 1,σ 2,!,σ N{ }
−−
L2 L2
L2



exp − Yj − yj( )2 2σ j
2
= 1 2πσ 1
2
2
2
exp − j=1
2
3
0, 1, 2, ...

−−
ν < 2 ν < 2


L1
L1 L1

−−
ν → ∞
σ j = yj
N

L∞ L∞


(1)
(2) (3) (4) (5) (1)
g x, y, z B
(2)
a, b, c, α, β, γ(3), (4), (5)

L∞ = lim ν→∞
Yj − yj ν
σ j ν




bond valence
Brown Altermatt bond
valence sum

bond valence parameter b
0.37 Brown Altermatt 1985 141 bond valence
parameter [3]
b BVS

-
AtomWork AtomWork (MatNavi)
AtomWork
“AtomWork” “NIMS”
(2) “AtomWork” →
“”
−−

TeraPad Crrl
(1)ShiftShiftShiftShift
(2)CtrlC (3)CtrlV
(4)CtrlF
−− RIETAN-FP
RIETAN-FP
Web “RIETAN-FPVENUS ”
RIETAN-FPVENUS
(2) “RIETAN-FPVENUS ”
“documentation.zip” →
…
C: Z:

“Windows_versions_20170913.zip”
“Windows_versions_20170913.zip”
“RIETAN_VENUS” “RIETAN_VENUS_examples”

8
(7)→PC→ ID (Z:) “” “Program Files”
“Program Files”
(9) “RIETAN_VENUS_exapmles” “Z:”
−− RIETAN-FP
RIETAN-FP
(1) “RIETAN_VENUS_examples”
“FapatiteJ”
(2) “FapatiteJ” “*.ins”, “*.int”
Ctrl→
(3) Web “FapatiteJ.bat.txt”
“FapatiteJ” “FapatiteJ.bat”
(4) “FapatiteJ.bat”


VESTA
VESTA
“VESTA”

−−

(2) “RIETAN_VENUS” “RIETAN_VENUS_examples”
“BaSO4_LB” “BaSO4”
“BaSO4.int” “BaSO4”
(3) “BaSO4.int”
“BaSO4.int” →→
...→...→ “ TeraPad.exe ” →OK
TeraPad
(4) “GENERAL”
(5) “BaSO4.int”
−−
11
(4) “Search materials | Inorganic Material Database” “Find materials that have ...”
“Chemical system - e.g. Mg Al” “Ba S O” Search materials
Ba S O
(5) Ba[SO4]
Mineralogist” Am. Mineral. [M. Miyake, I. Minato, H. Morikawa
and S. Iwai, Am. Mineral. 63, 506–510 (1978)] Web
“Data type” “Structure”
(7) Space group
Space group: Pnma, No. 62
(8) “Crystal Structure (Standardized)” cell parameters “Crystal structure (Published)”
“...
(Standardized)”
Cell parameters: a = 0.8884 nm, b = 0.5457 nm, c = 0.7157 nm, α = 90º, β = 90º, γ = 90º
(9) “Crystal Structure (Standardized)” “Atom coordinates”
Ba,

“*.ins”
“FapatiteJ.ins” “BaSO4”
“BaSO4.ins” Web http://www.crl.nitech.ac.jp/~ida
BaSO4.bat
*.ins
−−−
(1)43
(2) NBEAM = 1: 48 BaSO4
(3) NMODE = 0: 53
(4) NPRINT = 1:64
(5) NTARG = 4: 82 CuKα
(6) R12: Kα2/Kα1 87 BaSO4 “BaSO4.int” Kα2
R12 = 0.5: ...
13
(9) NTRAN = 0: 99 - (10)146
‘O-’ ‘P’ ‘Ca2+’ ‘F-’ /
PHNAME1 = 'Fluorapatite': (68).
VNS1 = 'A-176': (Vol.No. of Int.Tables: A or I)-...

(13) HKLM1: 186
HKLM1 = 'P 63/m ': hklmHermann-Mauguin...
HKLM1 = 'P n m a ': hklmHermann-Mauguin...
(14) LPAIR1: Bijvoet 193 Barite

(15) INDIV1: 203
(16) IHA1, IKA1, ILA1: 206208
(17) IHP1, IKP1, ILP1: 218220
hkl h k l
IHP1 = 1
IKP1 = 0
ILP1 = 0
(18) IHP2, IKP2, ILP2, IHP3, IKP3, ILP3: 222228
(19) NPRFN: 246 NPRFN = 1
(20) NSHIFT: 261 NSHIFT = 4

(1) SHIFTN: 301
SHIFTN 7.11466E-2 2.42176E-2 3.77026E-3 0.0 1000

SHIFTN 0.0 0.0 0.0 0.0 0000
(2) ROUGH: 305 (3) BKGD: 312313
# , bj (j = 011).
BKGD 114.731 -1.26701E2 139.203 -1.01934E2 68.1125 -3.94252E1 23.2694 -7.40064 -2.04399 3.59303 0.0 0.0 111111111100
10 9

−−−
(1) SCALE: 331 (2)369384

15
# , Ue and Pe.
ANISOBR12 0.0 0.0 00
# 16.
DUMMY12 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0000000000000000

# , Ue and Pe.
ANISOBR12 0.0 0.0 00
# 16.
DUMMY12 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0000000000000000
(3) PREF: 416
PREF 1.0 0.998462 0.0 0.0 0.0 0.0 010000

16
(4) CELLQ: 421 BaSO4 AtomWork
CELLQ 9.36903 9.36903 6.88384 90.0 90.0 120.0 0.0 1010000

(5)431
BaSO4 AtomWork
O1/O- 1.0 0.324174 0.485349 0.25 0.744733 01101
O2/O- 1.0 0.591772 0.469808 0.25 0.743478 01101
O3/O- 1.0 0.339147 0.257266 6.98124E-2 0.835736 01111
P/P 1.0 0.397305 0.367871 0.25 0.552323 01101
Ca1/Ca2+ 1.0 0.333333 0.666667 1.33243E-3 0.648404 00011
Ca2/Ca2+ 1.0 0.241797 -7.95224E-3 0.25 0.531459 01101
F/F- 1.0 0.0 0.0 0.25 1.42612 00001


(1) NVOXA,NVOXB,NVOXC: 482484
NVOXA = 132: a.
NVOXB = 132: b.
(2) NCUT: 544
(3) NEXC: 527 (4) NINT: 539 1
(5) NRANGE: 554
(6) PC: 603 7.00

(7) NLESQ: 663 (NLESQ = 0)
(8) NESU: 666
(9) NAUTO: 676
(10)NCYCL: 679 100
(11) CONV: (1)680 0.0001
(12) NCONV: (2)681 6
(13) NC: 683 0
(14) TK, FINC: 686687 (15) NUPDT: 787788

NUPDT = 1: ...
(16) NPAT: 796798 “Igor Pro”
“*.itx” “RIETVIEW.EXE”
NPAT = 1: ... *.plt*.gpd
NPAT = 2! ... Igor*.itx

(17) IWIDTH, IHEIGHT, IYMIN, IYMAX, LBG, LDEL, IOFFSETD, IPSIZE,
IFSIZE, ILSIZE: 847864
(18) INDREF: 866
(19) IOFFSET1: 869 (20) NDA: 933
NDA = 1
(22) NMEM: 979
NMEM = 1

19
(23) LANOM, LGR, LFOFC, EPSD, TSCAT1, TSCAT2: 982993
“*.ins” “*.ins”
VESTA (1) VESTA
(2) “File” → “Open ...” “BaSO4.ins”
(3) [Edit] → [Bonds...] “Bonds - BaSO4.ins”
(4) Ba–O [Delete]
(5) [Apply] S O
(6) [Ok] “Bonds - BaSO4.ins”
(7) [Style] “Style” Polyhedral
(8)
−−
−−

(3) 6,000
R
(7)R Rwp Rwp 20 %
“Structure parameters”

- - ...
- - ...
- - ...
- - ...
- - ...
O3 8d 4c
“x, 1/4, z”
Ba, S, O1, O2 y 0.25
22
O B
0.5 1.0
−−−
(1) “BaSO4.ins” 301
SHIFTN 0.0 0.0 0.0 0.0 0000

IYMAX = 20000: y ().
(5) PDF Viewer
(1) “BaSO4.ins”
# : pseudo-Voigt, ...

“BaSO4.ins” U W
V
(3) “BaSO4.bat”
(1) “BaSO4.ins” (2) (a0, a1, a2)
# : pseudo-Voigt, ...
FWHM12
ASYM12 1.04564 0.14424 -4.14686E-2 0.0 1110
24
(1) “BaSO4.ins” (2) (eta_L0, eta_L1, eta_H0, eta_H1)

FWHM12 ASYM12
ETA12 0.6106 0.13955 0.502513 0.177147 1111
(3) “BaSO4.bat”
(4) PDF Viewer
(1) “BaSO4.ins”
(2)Ba x z Ba y
0.25

25
(3) “BaSO4.bat”
(1) “BaSO4.ins”
(2)Ba BS, O1, O2, O3 x,
y, z Ba, S, O1, O2 y 0.25
Ba/Ba 1.0 0.1845 0.25 0.6585 0.5 01010
S/S 1.0 0.0625 0.25 0.1911 1.0 00000
O1/O 1.0 0.4122 0.25 0.394 1.0 00000
O2/O 1.0 0.1823 0.25 0.0494 1.0 00000
O3/O 1.0 0.0801 0.0298 0.3114 1.0 00000
Ba x, z
Ba/Ba 1.0 0.1845 0.25 0.6585 0.5 01011
S/S 1.0 0.0625 0.25 0.1911 1.0 01010
O1/O 1.0 0.4122 0.25 0.394 1.0 01010
O2/O 1.0 0.1823 0.25 0.0494 1.0 01010
O3/O 1.0 0.0801 0.0298 0.3114 1.0 01110
(3) “BaSO4.bat”
(4) PDF Viewer
(1) “BaSO4.ins”
Ba/Ba 1.0 0.1845 0.25 0.6585 0.5 01011
26
S/S 1.0 0.0625 0.25 0.1911 1.0 01010
O1/O 1.0 0.4122 0.25 0.394 1.0 01010
O2/O 1.0 0.1823 0.25 0.0494 1.0 01010
O3/O 1.0 0.0801 0.0298 0.3114 1.0 01110
Ba B S, O1, O2, O3 x, y, z

(3) “BaSO4.bat”
(4)
PDF Viewer

−−− R
(1) PDF Viewer 20º 50º
(2) RIETAN “BaSO4.lst”
(3)“Reliability indices, ...”
Rwp 12 %
%
Re 10 % Re Rwp Re
Re

(4) “BaSO4.lst” “*** Summary of possible reflections
(based on the refined ...”
(5) PDF Viewer “BaSO4.lst”
hkl 2-theta Iobs Ical
28
100000 Ical
(6) h0l Iobs > Ical0k0 Iobs <
Ical b
b
−−−
(1) “BaSO4.ins”
(2)IHP1, IKP1, ILP1:


(4) “BaSO4.bat”
(5) PDF Viewer
(6) “BaSO4.lst”
29
March-Dollase [4] (0 1 0)
BaSO4 b
b
(8) “Reliability factors, ...”
Rwp 9 % Re 10 % Rwp Re
(9) “*** Summary of possible reflections (based on the refined ...” “POF” (preferred orientation correction)
hkl 2-theta Iobs Ical POF
011 20.468 25230 27636 0.865
111 22.810 41763 44912 0.911
002 24.879 32048 32047 1.156
210 25.869 92955 95074 0.957
102 26.858 76871 77113 1.156
020 32.831 36265 35715 0.748
30
(1)
(2) 1 2
1 2
(3)
(4)

CuKα1 X 2Θ: 20º – 130º 0.02º BaSO4
RIETAN-FP [1]
10 Miyake [2] Pnma
(#62) Rwp = ?.?? %
Z = ?dcalc = ?.?? Mg/m3
[1] F. Izumi and K. Momma, Solid State Phenom., 130, 15–20 (2007). [2] M. Miyake, I. Minato, H. Morikawa and S. Iwai, Am. Mineral., 63, 506–510 (1978).
−−−
Atom site g x y z B (2)
Ba 4c 1 0.18443(9) 1/4 0.65894(9) 0.739(18)
S ......
O1 ......
O2 ......
O3 ......
33
−−
BVS; Bond Valence Sum
−−−
SO42– (1) VESTA [File] → [Open...] “BaSO4.ins”
(2) [Edit] → [Bonds...] “Bonds - BaSO4.ins”
(3) “Bonds - …”
[Delete]
(4) [New] “Search mode” “Search A2 bonded to A1”
“Boundary mode” “Search additional atoms if A1 is included in the
boundary” “A1: ” “S”
“A2” “O” “Max. length: ” “3”
(5) [Apply] S O
(6) [Ok] “Bonds - BaSO4.ins”
(7) [Style] “Style” Polyhedral
(8) “Select”
“Select”
(10) “bond angle”
“bond angle” (11) “O1–S–O2” O1
→ S → O2
Ba BVSBond Valence Sum
(1) Web
“documents” VESTA
“bvparm2016.cif”
(2) “bvparm2016.cif”
Ba 2 O -2 ...
Ba +2 O –2 “bond valence parameter”
b 0.37 VESTA BVS b 0.37

(3) VESTA [Edit] → [Bonds...] “Bonds - BaSO4.ins”
(4) “Ba – O” [New]
“Search mode” “Search A2 bonded to A1” “Boundary
mode” “Search additional atoms if A1 is included in the boundary” “A1” “Ba” “A2” “O” “Max “S –
Bond type length ()
(5) VESTA
[Ctrl] Ba (6) Bond valence parameter “bvparm2016.cif”
”2.223” oxidation number “2”
(7) VESTA “bond valence sum” BVS
0.2
−−−
[5]
M. Miyake, I. Minato, H. Morikawa and S. Iwai, Am. Mineral., 63, 506–510 (1978).
URL:
EPMA
(4)
(5) [5] VESTA
37
-
507–0071
10–6–29
−−
Introduction
−−−

39
−−−
results discussion results and discussion
x

−−−
discussion Acta
Crystallographica discussion
discussion

40
conclusion
[1] F. Izumi and K. Momma, Solid State Phenom., 130, 15–20 (2007). [2] K. Momma and F. Izumi, J. Appl. Crystallogr., 44, 1272-1276 (2011). [3] I. D. Brown and D. Altermatt, Acta Cryst. B 41, 244–247 (1985). [4] W. A. Dollase, J. Appl. Crystallogr., 19, 267–272 (1986). [5] M. Miyake, I. Minato, H. Morikawa and S. Iwai, Am. Mineral., 63, 506–510 (1978).
41