PROBLEMA 1: MATCH

1) Se abre el difractograma a con formato CSV (delimitado por comas), el cual puede ser
realizado con Excel. Obteniendo la siguiente pantalla.

2) Se observa que hay una alta posibilidad de que el material estudiado este compuesto de
Calcita, por lo que se marca un “Match” para seguir analizando que otros compuestos se
tienen. Teniendo en cuenta que la fase candidata sea un compuesto que sea probable.
3) Se sigue la misma metodología hasta que el porcentaje del posible compuesto sea muy
baja, menor que un 80-90%.
4) Se le aplica el método estadístico chi-square con el fin de obtener datos mas confiables
como por ejemplo la composición del material. Para ello se utiliza la función Rietveld
Parameter Turn-On, en donde se corre una prueba.

5) Se obtienen los datos modificados para que estadísticamente sean confiables.

6) Se imprimen los resultados en donde se podrán observar los datos acerca del
difractograma del material, así como datos de los compuestos acerca de su estructura
cristalina que forman parte del material.
 Match! Phase Analysis Report

Sample: quickstart
Sample Data
File name quickstart.rd
File path C:/Program Files/Match3/Tutorial
Data collected feb. 13, 2020 18:19:10
Data range 18.845º - 88.354º
Original data range 18.845º - 88.355º
Number of points 2318
Step size 0.030
Rietveld refinement converged Yes
Alpha2 subtracted No
Background subtr. No
Data smoothed No
2theta correction -0.00299º
Specimen displacement correction (Bragg-Brentano geometry)T = (-s/R) = -2.4977E-05
Radiation X-rays
Wavelength 1.540598 Å

Matched Phases
Index Amount (%) Name Formula sum
A 60.1 Corundum Al2 O3
B 23.1 Calcite C Ca O3
C 16.8 Quartz O2 Si
1.1 Unidentified peak area

A: Corundum (60.1 %)
Formula sum Al2 O3
Entry number 96-900-9679
Figure-of-Merit (FoM) 0.891567
Total number of peaks 30
Peaks in range 24
Peaks matched 21
Intensity scale factor 0.83
Space group R -3 c
Crystal system trigonal (hexagonal axes)
Unit cell a= 4.7607 Å c= 12.9947 Å
I/Ic 1.08
Calc. density 3.983 g/cm³
Reference Finger L. W., Hazen R. M., "Crystal structure and compression of ruby to 46 kbarP = 0.001 kbar", Journal of
Applied Physics 49, 5823-5826 (1978)

B: Calcite (23.1 %)
Formula sum C Ca O3
Entry number 96-900-9668
Figure-of-Merit (FoM) 0.928563
Total number of peaks 43
Peaks in range 33
Peaks matched 29
Intensity scale factor 1.09
Space group R -3 c
Crystal system trigonal (hexagonal axes)
Unit cell a= 4.9910 Å c= 17.0680 Å
I/Ic 3.72
Calc. density 2.708 g/cm³
Reference Sitepu H., O´Connor B H, Li D., "Comparative evaluation of the March and generalized spherical
harmonicpreferred orientation models using X-ray diffraction data for molybditeand calcite powdersNote: March
modelLocality: synthetic", Journal of Applied Crystallography 38, 158-167 (2005)

C: Quartz (16.8 %)
Formula sum O2 Si
Entry number 96-901-2601
Figure-of-Merit (FoM) 0.908734
Total number of peaks 35
Peaks in range 27
Peaks matched 26
Intensity scale factor 0.71
Space group P 31 2 1
Crystal system trigonal (hexagonal axes)
Unit cell a= 4.9140 Å c= 5.4060 Å
I/Ic 3.32
Calc. density 2.648 g/cm³
Reference Hazen R. M., Finger L. W., Hemley R. J., Mao H. K., "High-pressure crystal chemistry and amorphization of
alpha-quartzLocality: syntheticSample: P = 1 bar", Solid State Communications 72, 507-511 (1989)
 Candidates
Name Formula Entry No. FoM
(Fe0.9 Ni0.1) Fe0.9 Ni0.1 96-152-2985 0.6204

Search-Match
Settings
Reference database used COD-Inorg REV218120 2019.09.10
Automatic zeropoint adaptation Yes
Minimum figure-of-merit (FoM) 0.60
2theta window for peak corr. 0.30 deg.
Minimum rel. int. for peak corr. 1
Parameter/influence 2theta 0.50
Parameter/influence intensities 0.50
Parameter multiple/single phase(s) 0.50

Peak List
No. 2theta [º] d [Å] I/I0 FWHM Matched
1 20.86 4.2557 166.97 0.1800 C
2 23.05 3.8551 84.30 0.1800 B
3 25.57 3.4812 412.44 0.1800 A
4 26.64 3.3439 907.02 0.1800 C
5 29.40 3.0357 1000.00 0.1800 B
6 29.76 2.9992 7.59 0.1800
7 31.43 2.8437 19.12 0.1800 B
8 35.14 2.5518 687.87 0.1800 A
9 35.97 2.4950 134.76 0.1800 B
10 36.54 2.4570 62.23 0.1800 C
11 37.76 2.3803 306.18 0.1800 A
12 39.42 2.2841 249.53 0.1800 B,C
13 40.29 2.2369 28.24 0.1800 C
14 42.45 2.1278 51.82 0.1800 C
15 43.33 2.0864 718.45 0.2400 A,B
16 45.79 1.9800 27.41 0.1800 C
17 46.17 1.9647 9.80 0.1800 A
18 47.11 1.9275 64.68 0.1800 B
19 47.50 1.9125 200.19 0.1800 B
20 48.50 1.8754 216.45 0.1800 B
21 50.13 1.8181 118.15 0.1800 C
22 52.53 1.7406 341.43 0.1800 A
23 54.87 1.6719 36.94 0.1800 C
24 55.32 1.6594 16.47 0.1800 C
25 56.56 1.6259 37.47 0.1800 B
26 57.47 1.6022 781.10 0.1800 A,B,C
27 58.07 1.5872 14.44 0.3000 B
28 59.95 1.5417 89.75 0.1800 A,C
29 60.66 1.5254 60.84 0.2400 B
30 61.06 1.5164 44.37 0.3000 A,B
31 61.31 1.5108 77.27 0.3000 A,B
32 63.05 1.4733 22.07 0.1800 B
33 64.03 1.4531 17.41 0.2400 C
34 64.65 1.4405 73.59 0.1800 B
35 65.61 1.4217 41.82 0.2400 B,C
36 66.49 1.4050 262.91 0.1800 A
37 67.74 1.3822 56.97 0.1800 C
38 68.18 1.3743 491.59 0.1800 A,C
39 69.18 1.3569 16.34 0.1800 B
40 70.25 1.3388 27.75 0.1800 A,B
41 72.89 1.2967 31.17 0.1800 B
42 73.46 1.2880 23.35 0.1800 B,C
43 74.27 1.2759 9.65 0.1800 A
44 75.65 1.2561 28.78 0.1800 C
45 76.27 1.2475 14.03 0.2400 B
46 76.85 1.2395 113.10 0.1800 A
47 77.20 1.2348 81.90 0.2400 A,B
48 77.66 1.2285 16.13 0.1800 C
49 79.89 1.1998 32.16 0.1800 C
50 80.67 1.1901 44.66 0.1800 A
51 81.15 1.1842 28.19 0.2400 B,C
52 81.50 1.1801 57.99 0.1800 B,C
53 83.78 1.1537 71.38 0.1800 B,C
54 84.32 1.1476 36.92 0.1800 A
55 84.80 1.1424 29.25 0.1800 B,C
56 86.39 1.1254 36.19 0.3000 A,B

Rietveld Refinement using FullProf

Automatic refinement Yes
Final weighted average Bragg R- 4.0
factor
Final reduced chi2 1.3
FullProf comment Your refinement seems to be very good! => Your refinement seems to be very good!

Rietveld Parameter List

Parameter Final value Refined
Bck_0_pat1 0.992296 +
Scale_ph1_pat1 0.0069225 +
Bover_ph1_pat1 0.386092 +
U-Cagl_ph1_pat1 -0.000580471 +
Cell_A_ph1_pat1 4.76053 +
Cell_C_ph1_pat1 12.9955 +
Scale_ph2_pat1 0.00187804 +
Bover_ph2_pat1 -1.10873 +
U-Cagl_ph2_pat1 0.00344908 +
Cell_A_ph2_pat1 4.99005 +
Cell_C_ph2_pat1 17.0616 +
Scale_ph3_pat1 0.0148069 +
Bover_ph3_pat1 -0.242353 +
U-Cagl_ph3_pat1 -0.0013895 +
Cell_A_ph3_pat1 4.91401 +
Cell_C_ph3_pat1 5.40623 +
Zero_pat1 -0.00299162
SyCos_pat1 -0.00286216
SySin_pat1 0
Lambda_pat1 1.5406
P0_mabs_pat1 0
Cp_mabs_pat1 0
Tau_mabs_pat1 0.1
Bck_1_pat1 0
Bck_2_pat1 0
Bck_3_pat1 0
Strain1_ph1_pat1 0
Strain2_ph1_pat1 0
Strain3_ph1_pat1 0
G-Size_ph1_pat1 0
L-Size_ph1_pat1 0
Y-cos_ph1_pat1 0
EtaRght0_ph1_pat1 0
X-tan_ph1_pat1 0
V-Cagl_ph1_pat1 0
W-Cagl_ph1_pat1 0.0324
EtaPV_ph1_pat1 0.205251
Cell_B_ph1_pat1 4.76054
Cell_D_ph1_pat1 90
Cell_E_ph1_pat1 90
Cell_F_ph1_pat1 120
Or1_ph1_pat1 0
Or2_ph1_pat1 0
Asym1_ph1_pat1 0
Asym2_ph1_pat1 0
Asym3_ph1_pat1 0
Asym4_ph1_pat1 0
X_Al1_ph1 0
Y_Al1_ph1 0
Z_Al1_ph1 0.35216
Biso_Al1_ph1 0.31
Occ_Al1_ph1 1
X_O2_ph1 0.3061
Y_O2_ph1 0
Z_O2_ph1 0.25
Biso_O2_ph1 0.33
Occ_O2_ph1 1
Strain1_ph2_pat1 0
Strain2_ph2_pat1 0
Strain3_ph2_pat1 0
G-Size_ph2_pat1 0
L-Size_ph2_pat1 0
Y-cos_ph2_pat1 0
EtaRght0_ph2_pat1 0
X-tan_ph2_pat1 0
V-Cagl_ph2_pat1 0
W-Cagl_ph2_pat1 0.0324
EtaPV_ph2_pat1 0.182826
Cell_B_ph2_pat1 4.99011
Cell_D_ph2_pat1 90
Cell_E_ph2_pat1 90
Cell_F_ph2_pat1 120
Or1_ph2_pat1 0
 Or2_ph2_pat1 0
Asym1_ph2_pat1 0
Asym2_ph2_pat1 0
Asym3_ph2_pat1 0
Asym4_ph2_pat1 0
X_Ca1_ph2 0
Y_Ca1_ph2 0
Z_Ca1_ph2 0
Biso_Ca1_ph2 1.223
Occ_Ca1_ph2 1
X_C2_ph2 0
Y_C2_ph2 0
Z_C2_ph2 0.25
Biso_C2_ph2 1.398
Occ_C2_ph2 1
X_O3_ph2 0.245
Y_O3_ph2 0
Z_O3_ph2 0.25
Biso_O3_ph2 1.398
Occ_O3_ph2 1
Strain1_ph3_pat1 0
Strain2_ph3_pat1 0
Strain3_ph3_pat1 0
G-Size_ph3_pat1 0
L-Size_ph3_pat1 0
Y-cos_ph3_pat1 0
EtaRght0_ph3_pat1 0
X-tan_ph3_pat1 0
V-Cagl_ph3_pat1 0
W-Cagl_ph3_pat1 0.0324
EtaPV_ph3_pat1 0.151269
Cell_B_ph3_pat1 4.91401
Cell_D_ph3_pat1 90
Cell_E_ph3_pat1 90
Cell_F_ph3_pat1 120
Or1_ph3_pat1 0
Or2_ph3_pat1 0
Asym1_ph3_pat1 0
Asym2_ph3_pat1 0
Asym3_ph3_pat1 0
Asym4_ph3_pat1 0
X_Si1_ph3 0.4699
Y_Si1_ph3 0
Z_Si1_ph3 0.333333
Biso_Si1_ph3 0.51
Occ_Si1_ph3 1
X_O2_ph3 0.413
Y_O2_ph3 0.2668
Z_O2_ph3 0.214
Biso_O2_ph3 0.859
Occ_O2_ph3 1

Integrated Profile Areas

Based on Rietveld refinement

Profile area Counts Amount

Overall diffraction profile 2615033 100.00%
Background radiation 1521857 58.20%
Diffraction peaks 1093176 41.80%
Peak area belonging to selected phases 1064599 40.71%
Peak area of phase A (Corundum) 478309 18.29%
Peak area of phase B (Calcite) 317807 12.15%
Peak area of phase C (Quartz) 268482 10.27%
Unidentified peak area 28578 1.09%

Peak Residuals
Peak data Counts Amount
Overall peak intensity 35068 100.00%
Peak intensity belonging to selected phases 34931 99.61%
Unidentified peak intensity 137 0.39%

Diffraction Pattern Graphics

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