セメント試料のX線回折(XRD)測定 Bruker Japan Webinar 2 セメント試料のX線回折(XRD)測定～含まれる結晶相の特徴、各種の非晶質定量方法～ X線回折法

X(XRD)

2018315

X

X(XRD)

X

XRD

2018/3/15 Bruker Japan Webinar 2

X(XRD)

X

XRD


X(XRD)

X

2018/3/15 Bruker Japan Webinar 42q()

qX()

X

X

2q

q

5

X(XRD)

Bruker Japan Webinar2018/3/15

6Bruker Japan Webinar

X(XRD)SiO2

2018/3/15

1.

2.

3.

()

X

X(XRD)

2q()


X


X

X

2q

q

XS/N

Burker JapanXRD

X

D2 PHASER 100V

X

D8 ADVANCE

X

D8 DISCOVER 2XRD XRD/XRR


D8 ENDEVOR

Bruker Japan Webinar

D8 ADVANCE66

2018/3/15 10

2018/3/15 11Bruker Japan Webinar

>1,450C

XRD

XRF&XRD

12

XRD

XRFX

f51.5 mm

XRDXRF

XRFS8 TIGER

2018/3/15 Bruker Japan Webinar

13

2Th Degrees656055504540353025201510

Counts

34,000

32,000

30,000

28,000

26,000

24,000

22,000

20,000

18,000

16,000

14,000

12,000

10,000

8,000

6,000

4,000

2,000

0

Calcite 86.12 %

Dolomite 7.26 %

Quartz 4.03 %

Illite 1.64 %

Albite 0.42 %

Microcline 0.28 %

Kaolinite 0.26 %

XRD

0.1wt%

2018/3/15 Bruker Japan Webinar

X(XRD)

X

XRD



Ca3SiO5 C3S, Alite

Ca2SiO4 C2S, Belite

Ca3Al2O6C3A,

Calucium Alminate

Ca4(AlxFe1-x)4O10C4AF,

Brownmillerite , Fe

CaO Free Lime ,

Ca(OH)2 Calciumhydroxide ,

CaSO4xH2O Gypsum,

CaCO3 Calcite

MgO Periclase


Ca3SiO5 C3S, Alite

Ca2SiO4 C2S, Belite

Ca3Al2O6C3A,

Calucium Alminate

Ca4(AlxFe1-x)4O10C4AF,

Brownmillerite , Fe

CaO Free Lime ,

Ca(OH)2 Calciumhydroxide ,

CaSO4xH2O Gypsum,

CaCO3 Calcite

MgO Periclase

C3SC2SC3AC4AF

Ca, Si, Al, O

C3S, Alite - Ca3SiO5

M3C1m1 (8)

a=33.083, b=7.027, c=18.499

b=94.12, Z=36

Pm(7) (M1) : R3m (160), : P-1 (2)

CaSiO


3

C3S, Alite


CaSiO

M1

M1

CaSiO

M3

M2

M3

XRD

C3S, Alite


M1 M2 M3

M. Courtial et al., (2003) Powder Diffraction, 18(1), pp.7-15 https://doi.org/10.1154/1.1523079

https://doi.org/10.1154/1.1523079

C2S, Belite Ca2SiO4


(b-C2S)P121/n1 (14)

a=5.506, b=6.757, c=9.310 b=94.46, Z=4

a-C2S: , P63/mmc (194) g-C2S: , Pnma (62)

3

CaSiO

C3A - Ca3Al2O6

CubicPa-3 (205)a=15.263 , Z=24

: Pbca (61)

2


CaAlO

CaO, Free Lime

Ca(OH)2

CubicFm-3m (225)a=4.810 , Z=4


CaO

Lin

(C

ou

nts

)

0

100

200

300

400

500

600

700

800

900

1000

1100

1200

1300

1400

1500

1600

1700

1800

1900

2000

2100

2200

2300

2400

2500

2600

2700

2800

2900

3000

3100

3200

2-Theta - Scale

10 20 30 40 50

PDF No.85-1378 Ca3SiO5, C3S, Alite, Monoclinic

PDF No.33-0302 CaSiO4, C2S, Belite

PDF No.38-1429 Ca3Al2O6, C3A, Cubic

PDF No.30-0226 Ca4(Alx, Fe1-x)4O10, C4AF, Brownmillerite

PDF No.37-1497 CaO, Free lime



2theta64626058565452504846444240383634323028262422201816141210

Counts

11,500

11,000

10,500

10,000

9,500

9,000

8,500

8,000

7,500

7,000

6,500

6,000

5,500

5,000

4,500

4,000

3,500

3,000

2,500

2,000

1,500

1,000

500

0

-500

-1,000

-1,500

-2,000

-2,500

-3,000

-3,500

-4,000

-4,500

C3S monoclinic (NISHI) 61.67 %

C2S beta (MUMME) 17.78 %

C3A cubic 1.55 %

C3A Na orthorhombic 3.76 %

C4AF (Colville) 10.54 %

Lime 0.51 %

Gypsum 1.56 %

Bassanite 1.12 %

Periclase 1.45 %

Anhydrite 0.06 %

10

Wt% - Rietveld


C2S beta (MUMME) 17.78 % C3A cubic 1.55 %C3A Na orthorhombic 3.76 %


Lime 0.51 %Gypsum 1.56 %Bassanite 1.12 %Anhydrite 0.06 %Periclase 1.45 %

2theta64626058565452504846444240383634323028262422201816141210

Counts

11,500

11,000

10,500

10,000

9,500

9,000

8,500

8,000

7,500

7,000

6,500

6,000

5,500

5,000

4,500

4,000

3,500

3,000

2,500

2,000

1,500

1,000

500

0

-500

-1,000

-1,500

-2,000

-2,500

-3,000

-3,500

-4,000

-4,500



C3A cubic 1.55 %



Lime 0.51 %

Gypsum 1.56 %

Bassanite 1.12 %

Periclase 1.45 %

Anhydrite 0.06 %


C3SC2SC3AC4AF

X(XRD)

X

XRD



BG BG

2q

A.


(S/N)

2q

D8 ADVANCE

A.


(2q)

(2q)

X

X

A.


1 2 3 5 7 10 15 20 25 30 40 2q()0.05 14.0 7.0 4.7 2.8 2.0 1.4 0.9 0.7 0.6 0.5 0.4

0.1 28.1 14.0 9.3 5.6 4.0 2.8 1.9 1.4 1.1 0.9 0.7

0.2 56.6 28.1 18.7 11.2 8.0 5.6 3.7 2.8 2.3 1.9 1.4

0.4 117 56.6 37.5 22.4 16.0 11.2 7.5 5.6 4.5 3.8 2.9

0.6 185 85.9 56.6 33.7 24.1 16.8 11.2 8.4 6.8 5.7 4.3

1.0 373 149 96.0 56.6 40.2 28.1 18.7 14.1 11.3 9.4 7.1

2.0 373 210 117 81.7 56.6 37.6 28.2 22.6 18.9 14.3

(mm)

D8 ADVANCE X (mm)

X (W) = [1/sin(a+b/2)+ 1/sin(a-b/2)]Rsin(b/2)(a; (rad)b; DS (rad)R; (mm))

S/N

B.


2q

2q

X

2018/3/15


BG

BG

X

X


1


192

LYNXEYE

150

LYNXEYE XE-T

< 380eV

Kb

LYNXEYE


5,000counts

100counts

16,700counts

6,500counts

vs. BKG 3.3 : 65

X

LYNXEYE XE-T


XE-T Edition

BG

BG


X(XRD)

X

XRD



33.50 35.50 37.50 39.50 41.50 43.50

qq

CeO2 (ILL D1A)

12.70 12.75 12.80 12.85 12.90 12.95 13.00

qq

CeO2 (NSLS X3B1)

1.89 1.90 1.91 1.92 1.93d []

CeO2 (ISIS HRPD)

Size-Strain Round Robin, Balzar (2004);

28.00 28.20 28.40 28.60 28.80 29.00

qq

CeO2 (D8 ADVANCE)

DIFFRAC.TOPAS=

DIFFRAC.TOPAS

402018/3/15

NaAlSi3O8

SiO2

CaCO3


(wt%)


DIFFRAC.TOPAS

1. 2. 3.

3

Windows

TOPAS BBQ

D2 PHASER() & TOPAS


2theta64626058565452504846444240383634323028262422201816141210

Counts

10,000

9,500

9,000

8,500

8,000

7,500

7,000

6,500

6,000

5,500

5,000

4,500

4,000

3,500

3,000

2,500

2,000

1,500

1,000

500

0

-500

-1,000

-1,500

Wt% - Rietveld


C2S beta (MUMME) 20.72 % C3A cubic 5.8 %



Lime 0.11 %Gypsum 0.51 %

Bassanite 2.84 %Portlandite 1.18 %Periclase 0.94 %

--

GOF:1.92

Rwp: 6.12%

Rexp:3.19%

: 10

: 5

90.1wt%

2018/3/15


2Th Degrees64626058565452504846444240383634323028262422201816141210

Sqrt

(Counts

)

62

60

58

56

54

52

50

48

46

44

42

40

38

36

34

32

30

28

26

24

22

20

18

16

14

12

10

8

6

4

2

0

-2

-4

-6

-8

hkl_Slug 31.19 %



C3A cubic 1.24 %



Lime 0.27 %

Gypsum 0.95 %

Bassanite 0.70 %

Anhydrite 0.84 %

Periclase 0.77 %

Akermanite 0.26 %

?

()

Slag


PONKCS 100%

100%

DIFFRAC.TOPAS


1.

2. 15wt%

3.

4. Rietveld

5. wt% of spiked

6.


45.1%wt

30.8%wt

48

1.

2. K 1.P.3

3. 1.

4. X (MAC) XRF

5. K MAC

K

=


49

Al2O3corundum

TiO2 (rutile)

ZnO (zincite)

Cr2O3 (eskolaite)

Fe2O3 (hematite)

CeO2 (cerianite)

CaF2 (fluorite)

C (diamond)

1.

2Th Degrees120110100908070605040302010

Sqrt

(Counts

)

750

700

650

600

550

500

450

400

350

300

250

200

150

100

50

0

Corundum99.raw_1 Corundum 100.00 %

Round Robin example: Al2O3, 99% crystalline


50

K = ()

Scor = Scale factor (TOPAS)

cor = / g cm-3 (TOPAS)

Vcor = / 3 (TOPAS)

cor = X/ cm2 g-1 ()

Ccor = / % (, e.g. 100%)

2. K

=

2


51

3.XMAC

=

2

= fraction O MAC O + fraction Al MAC Al

= 0.47077 11.2 + 0.52923 49.2 = 31.281 (cm2

g)

TOPAS XMAC C:TOPAS5Mac MAC8.0keV


fraction: Al2O3

O: 16.003=48.00, Al: 26.982=53.96

fraction(O)= 48.00(48.00+53.96) = 0.47077, fraction(Al)= 53.96(48.00+53.96) = 0.52923

2018/3/15


5.

KMAC

2018/3/15

PONKCS


100%

=

(PONKCS)

MZ

wi:is: M: 1Z: V:

n

j

jjjj

iiii

i

ZMVs

ZMVsw

1

?

PONKCS


-1

-2Cell Mass

100% .inp

Cell Mass.inp

PONKCS

2018/3/15 55Bruker Japan Webinar55

-1

100%

WPPD

nm

TOPAS User's Mtg. 2014

PONKCS


2Th Degrees64626058565452504846444240383634323028262422201816141210

Sqrt

(Counts

)

58

56

54

52

50

48

46

44

42

40

38

36

34

32

30

28

26

24

22

20

18

16

14

12

10

8

6

4

2

0

-2

-4

-6

-8

-10

hkl_Slug 45.01 %



C3A cubic 0.47 %



Lime 0.32 %

Gypsum 0.68 %

Bassanite 0.56 %

Anhydrite 0.79 %

Periclase 0.64 %

Akermanite 0.73 %

2Th Degrees64626058565452504846444240383634323028262422201816141210

Sqrt

(Counts

)

58

56

54

52

50

48

46

44

42

40

38

36

34

32

30

28

26

24

22

20

18

16

14

12

10

8

6

4

2

0

-2

-4

-6

-8

-10

hkl_Slug 45.01 %



C3A cubic 0.47 %



Lime 0.32 %

Gypsum 0.68 %

Bassanite 0.56 %

Anhydrite 0.79 %

Periclase 0.64 %

Akermanite 0.73 %

-2

1

MZ


10

PONKCS

TOPAS BBQ

X(XRD)

X

XRD


Q&A



TOPAS Users meeting (: )

516~18

PONKCS

XRD WEBINARS:

531() 16:00~

1213() 16:00~

XRD WEBINARS:


https://www.bruker.com/jp/service/education-training/webinars/xrd.html

Documents

セメント試料のX線回折(XRD)測定 Bruker Japan Webinar 2 セメント試料のX線回折(XRD)測定 ～含まれる結晶相の特徴、各種の非晶質定量方法～ X線回折法

セメント試料のX線回折(XRD)測定 Bruker Japan Webinar 2 セメント試料のX線回折(XRD)測定～含まれる結晶相の特徴、各種の非晶質定量方法～ X線回折法