Conclusion générale
L'ensemble des travaux présentés dans ce
mémoire a été axé sur la synthèse de trois
phases à structure pérovskite dont la formule
générale est LaMO3 (M=Fe, Mn, Ti) par voie solide (méthode
céramique), les différents échantillons ont
été traités à température 900°C puis
à 1000°C afin d'obtenir les phases recherchées, vient en
suit l'étape de caractérisation de ces échantillons par la
diffraction des rayons X. Les différents spectres obtenus ont
été comparés avec la base de données.
Les résultats de ce travail sont rassemblés comme
suit:
L'échantillon E1 :
La caractérisation par diffraction des RX nous a permis de
conclure que la poudre E1 est monophasique et après l'affinement par le
logiciel CELREF on trouve :
T=900°C :
LaFeO3 : SG : Pnma du système orthorhombique :
a=5.5590 A°, b=5.5647 A°, c=7.8598 A°
T=1000°C :
LaFeO3 : SG : Pnma du système orthorhombique :
a=5.5580 A° b=5.5652 A° c=7.8627 A°
L'échantillon E2 :
De même que l'échantillon E1 :
T=900°C :
LaMnO3 : SG : Pbnm du système orthorhombique :
a=5.5198 A° , b=5.7517 A° , c=7.7377 A°
T=1000°C:
LaMnO3 : SG : Pbnm du système orthorhombique :
a=5.5226 A° , b=5.7527 A° , c=7.7541 A°
L'échantillon E3:
T=1000°C:
LaTiO3 : SG : Pm-3m du système cubique
a=b=c=3,9085 A°
TiO2 : SG : P42/mmm du système
tetragonal
a=b= 4,58 A° c= 2,95 A°
La2O3 : SG : P-3m1du système hexagonal
a= b= 3.9417 A° c=6.1372 A°
La2Ti2O7 : SG : P21/m du système
monoclinique
a=13.0031 A° b= 5.5410A° c= 7.7994 A°
â=98.46 °
La phase LaFeO3 d'après la base de
données
CELREF VERSION 3 P1:LaFeO3
(T=900°C)
Initial values : (Refinement keys on 2nd line)
Zero Lambda a b c alpha beta gamma volume
0.000 0
H
|
1.54060
0
K L
|
5.5582 5.5645
1 1
2Th (obs)
|
7.8614 90.00
1 0
2Th_obs-shift
|
90.00 90.00 243.142
0 0
2Th (Calc) diff.
|
0
|
0
|
2
|
22.6065
|
22.6065
|
22.6028
|
0.0037
|
1
|
1
|
1
|
25.3037
|
25.3037
|
25.3033
|
0.0004
|
2
|
0
|
0
|
32.1855
|
32.1855
|
32.1835
|
0.0020
|
2
|
0
|
1
|
34.1590
|
34.1590
|
34.1935
|
-0.0345
|
2
|
0
|
2
|
39.6834
|
39.6834
|
39.6876
|
-0.0042
|
0
|
0
|
4
|
46.1503
|
46.1503
|
46.1506
|
-0.0003
|
2
|
2
|
1
|
47.6397
|
47.6397
|
47.6359
|
0.0038
|
1
|
1
|
4
|
51.9892
|
51.9892
|
51.9735
|
0.0157
|
1
|
3
|
1
|
53.3070
|
53.3070
|
53.3127
|
-0.0057
|
2
|
0
|
4
|
57.3796
|
57.3796
|
57.3768
|
0.0028
|
4
|
0
|
0
|
67.3297
|
67.3297
|
67.3322
|
-0.0025
|
3
|
1
|
4
|
72.0183
|
72.0183
|
72.0179
|
0.0004
|
1
|
1
|
6
|
76.6079
|
76.6079
|
76.5862
|
0.0217
|
2
|
4
|
1
|
77.6419
|
77.6419
|
77.6476
|
-0.0057
|
Final values : (Standard errors on 2nd line)
Zero Lambda a b c alpha beta gamma volume
0.000
0.0000
H
|
1.54060
0.00000
K L
|
5.5590 5.5647
0.0006 0.0007
2Th (obs)
|
7.8598 90.00
0.0007 0.000
2Th_obs-shift
|
90.00 90.00
0.000 0.000
2Th (Calc)
|
243.13
0.000
diff.
|
0
|
0
|
2
|
22.6065
|
22.6065
|
22.6075
|
-0.0010
|
1
|
1
|
1
|
25.3037
|
25.3037
|
25.3024
|
0.0013
|
2
|
0
|
0
|
32.1855
|
32.1855
|
32.1785
|
0.0070
|
2
|
0
|
1
|
34.1590
|
34.1590
|
34.1896
|
-0.0306
|
2
|
0
|
2
|
39.6834
|
39.6834
|
39.6863
|
-0.0029
|
0
|
0
|
4
|
46.1503
|
46.1503
|
46.1606
|
-0.0103
|
2
|
2
|
1
|
47.6397
|
47.6397
|
47.6322
|
0.0075
|
1
|
1
|
4
|
51.9892
|
51.9892
|
51.9817
|
0.0075
|
1
|
3
|
1
|
53.3070
|
53.3070
|
53.3107
|
-0.0037
|
2
|
0
|
4
|
57.3796
|
57.3796
|
57.3822
|
-0.0026
|
4
|
0
|
0
|
67.3297
|
67.3297
|
67.3208
|
0.0089
|
3
|
1
|
4
|
72.0183
|
72.0183
|
72.0192
|
-0.0009
|
1
|
1
|
6
|
76.6079
|
76.6079
|
76.6021
|
0.0058
|
2
|
4
|
1
|
77.6419
|
77.6419
|
77.6429
|
-0.0010
|
CELREF Version 3 P1:LaFeO3 (T=1000°C)
Initial values : (Refinement keys on 2nd line)
Zero 0.000 0
|
Lambda
1.54060
0
H K L
|
a b
5.5579 5.5646
1 1
2Th (obs)
|
c alpha
7.8646 90.00
1 0
2Th_obs-shift
|
beta gamma volume
90.00 90.00 243.232
0 0
2Th (Calc) diff.
|
1
|
1
|
0
|
22.5919
|
22.5919
|
22.5929
|
-0.0010
|
1
|
1
|
1
|
25.3011
|
25.3011
|
25.3015
|
-0.0004
|
2
|
0
|
0
|
32.1787
|
32.1787
|
32.1853
|
-0.0066
|
2
|
0
|
2
|
39.6856
|
39.6856
|
39.6834
|
0.0022
|
0
|
0
|
4
|
46.1435
|
46.1435
|
46.1307
|
0.0128
|
2
|
2
|
1
|
47.6358
|
47.6358
|
47.6356
|
0.0002
|
3
|
1
|
0
|
51.9775
|
51.9775
|
51.9813
|
-0.0038
|
1
|
3
|
1
|
53.3017
|
53.3017
|
53.3110
|
-0 .0093
|
3
|
1
|
2
|
57.3744
|
57.3744
|
57.3727
|
0.0017
|
1
|
3
|
3
|
63.6406
|
63.6406
|
63.6420
|
-0.0014
|
4
|
0
|
0
|
67.3254
|
67.3254
|
67.3363
|
-0.0109
|
4
|
0
|
2
|
72.0274
|
72.0274
|
72.0266
|
0.0008
|
4
|
2
|
0
|
76.5945
|
76.5945
|
76.5839
|
0.0106
|
Final values : (Standard errors on 2nd
line)
Zero Lambda a b c alpha beta gamma volume
0.000
0.0000
H
|
1.54060 0.00000
K L
|
5.5580 5.5652
0.0002 0.0005
2Th (obs)
|
7.8627 90.00
0.0009 0.000
2Th_obs-shift
|
90.00 0.000
2Th (Calc)
|
90.00 243.205
0.000 0.000
diff.
|
1
|
1
|
0
|
22.5919
|
22.5919
|
22.5915
|
0.0004
|
1
|
1
|
1
|
25.3011
|
25.3011
|
25.3015
|
-0.0004
|
2
|
0
|
0
|
32.1787
|
32.1787
|
32.1846
|
-0.0059
|
2
|
0
|
2
|
39.6856
|
39.6856
|
39.6862
|
-0.0006
|
0
|
0
|
4
|
46.1435
|
46.1435
|
46.1425
|
0.0010
|
2
|
2
|
1
|
47.6358
|
47.6358
|
47.6333
|
0.0025
|
3
|
1
|
0
|
51.9775
|
51.9775
|
51.9798
|
-0.0023
|
1
|
3
|
1
|
53.3017
|
53.3017
|
53.3062
|
-0.0045
|
3
|
1
|
2
|
57.3744
|
57.3744
|
57.3738
|
0.0006
|
1
|
3
|
3
|
63.6406
|
63.6406
|
63.6424
|
-0.0018
|
4
|
0
|
0
|
67.3254
|
67.3254
|
67.3349
|
-0.0095
|
4
|
0
|
2
|
72.0274
|
72.0274
|
72.0275
|
-0.0001
|
4
|
2
|
0
|
76.5945
|
76.5945
|
76.5806
|
0.0139
|
La phase LaMnO3 d'après la base de
données
CELREF version 3 P2:LaMnO3 (900°C)
Initial values : (Refinement keys on 2nd line) Zero Lambda
a b c alpha beta gamma volume
0.000 0
H
|
K
|
1.54060 0
L
|
5.5341 5.7438
1 1
2Th (obs)
|
7.7235 90.00
1 0
2Th_obs-shift
|
90.00 90.00
0 0
2Th (Calc)
|
245.505
diff.
|
1
|
1
|
0
|
22.7367
|
22.7367
|
22.2893
|
0.4474
|
2
|
0
|
0
|
32.5073
|
32.5073
|
32.3275
|
0.1798
|
2
|
1
|
0
|
35.8669
|
35.8669
|
35.9983
|
-0.1314
|
2
|
0
|
2
|
40.2804
|
40.2804
|
40.0548
|
0.2256
|
0
|
0
|
4
|
46.5880
|
46.5880
|
47.0236
|
-0.4356
|
1
|
1
|
4
|
52.5428
|
52.5428
|
52.6288
|
-0.0860
|
3
|
1
|
2
|
57.8179
|
57.8179
|
57.6075
|
0.2104
|
2
|
0
|
4
|
57.9733
|
57.9733
|
58.2171
|
-0.2438
|
2
|
0
|
4
|
58.3252
|
58.3252
|
58.2171
|
0.1081
|
2
|
3
|
2
|
63.8060
|
63.8060
|
63.7881
|
0.0179
|
3
|
1
|
3
|
64.0299
|
64.0299
|
64.1354
|
-0.1055
|
1
|
1
|
5
|
64.7707
|
64.7707
|
64.6637
|
0.1070
|
4
|
0
|
0
|
67.8068
|
67.8068
|
67.6649
|
0.1419
|
1
|
4
|
1
|
68.3478
|
68.3478
|
68.5417
|
-0.1939
|
0
|
4
|
2
|
69.5210
|
69.5210
|
69.8249
|
-0.3039
|
2
|
3
|
3
|
69.9709
|
69.9709
|
69.9877
|
-0.0168
|
3
|
1
|
4
|
72.8807
|
72.8807
|
72.7232
|
0.1575
|
0
|
4
|
3
|
75.8770
|
75.8770
|
75.7933
|
0.0837
|
4
|
2
|
0
|
76.6573
|
76.6573
|
76.3412
|
0.3161
|
4
|
2
|
1
|
77.4414
|
77.4414
|
77.5114
|
-0.0700
|
Final values : (Standard errors on 2nd line)
Zero Lambda a b c alpha beta gamma volume
0.000 0.0000
H
|
K
|
1.54060
0.00000
L
|
5.5198
0.0074
2Th (obs)
|
5.7517 7.7377 90.00 90.00
0.0092 0.0139 0.000 0.000
2Th_obs-shift 2Th (Calc)
|
90.00 245.660
0.000 0.000
diff.
|
1
|
1
|
0
|
22.7367
|
22.7367
|
22.3047
|
0.4320
|
2
|
0
|
0
|
32.5073
|
32.5073
|
32.4134
|
0.0939
|
2
|
1
|
0
|
35.8669
|
35.8669
|
36.0668
|
-0.1999
|
2
|
0
|
2
|
40.2804
|
40.2804
|
40.1002
|
0.1802
|
0
|
0
|
4
|
46.5880
|
46.5880
|
46.9320
|
-0.3440
|
1
|
1
|
4
|
52.5428
|
52.5428
|
52.5518
|
-0.0090
|
3
|
1
|
2
|
57.8179
|
57.8179
|
57.7035
|
0.1144
|
2
|
0
|
4
|
57.9733
|
57.9733
|
58.1924
|
-0.2191
|
2
|
0
|
4
|
58.3252
|
58.3252
|
58.1924
|
0.1328
|
2
|
3
|
2
|
63.8060
|
63.8060
|
63.7640
|
0.0420
|
3
|
1
|
3
|
64.0299
|
64.0299
|
64.2022
|
-0.1723
|
1
|
1
|
5
|
64.7707
|
64.7707
|
64.5542
|
0.2165
|
4
|
0
|
0
|
67.8068
|
67.8068
|
67.8637
|
-0.0569
|
1
|
4
|
1
|
68.3478
|
68.3478
|
68.4524
|
-0.1046
|
0 4 2 69.5210 69.5210 69.7107 -0.1897
2 3 3 69.9709 69.9709 69.9424 0.0285
3 1 4 72.8807 72.8807 72.7555 0.1252
0 4 3 75.8770 75.8770 75.6611 0.2159
4 2 0 76.6573 76.6573 76.5072 0.1501
4 2 1 77.4414 77.4414 77.6723 -0.2309
CELREF version 3
P2: LaMnO3 (1000°C)
Initial values : (Refinement keys on 2nd line)
Zero Lambda a b c alpha beta gamma volume
0.000 1.54060 5.5308 5.7583 7.7447 90.00 90.00 90.00 246.653
0 0 1 1 1 0 0 0
H K L 2Th (obs) 2Th_obs-shift 2Th (Calc) diff.
0 0 2 22.7478 22.7478 22.9480 -0.2002
2 0 0 32.2843 32.2843 32.3473 -0.0630
1 0 3 38.2504 38.2504 38.4512 -0.2008
2 0 2 40.4070 40.4070 40.0325 0.3745
0 0 4 46.5658 46.5658 46.8872 -0.3214
3 1 0 52.2885 52.2885 52.0440 0.2445
1 1 4 52.6792 52.6792 52.4935 0.1857
3 1 2 57.6304 57.6304 57.5940 0.0364
2 2 3 58.4506 58.4506 58.4264 0.0242
4 0 0 67.6516 67.6516 67.7107 -0.0591
1 4 1 68.3997 68.3997 68.3596 0.0401
1 1 6 77.6943 77.6943 77.6931 0.0012
Final values : (Standard errors on 2nd line)
Zero Lambda a b c alpha beta gamma volume
0.000 1.54060 5.5226 5.7527 7.7541 90.00 90.00 90.00 246.342
0.0000 0.00000 0.0101 0.0163 0.0138 0.000 0.000
0.000 0.000
H K L 2Th (obs) 2Th_obs-shift 2Th (Calc) diff.
0 0 2 22.7478 22.7478 22.9199 -0.1721
2 0 0 32.2843 32.2843 32.3969 -0.1126
1 0 3 38.2504 38.2504 38.4223 -0.1719
2 0 2 40.4070 40.4070 40.0568 0.3502
0 0 4 46.5658 46.5658 46.8273 -0.2615
3 1 0 52.2885 52.2885 52.1248 0.1637
1 1 4 52.6792 52.6792 52.4518 0.2274
3 1 2 57.6304 57.6304 57.6566 -0.0262
2 2 3 58.4506 58.4506 58.4475 0.0031
4 0 0 67.6516 67.6516 67.8256 -0.1740
1 4 1 68.3997 68.3997 68.4329 -0.0332
1 1 6 77.6943 77.6943 77.6033 0.0910
CELREF Version 3
P3:LaTiO3 (1000°C)
Initial values : (Refinement keys on 2nd line)
Zero Lambda a b c alpha beta gamma volume
0.000
0
H
|
1.54060 0
K L
|
3.9111 3.9111
1 0 2Th (obs)
|
3.9111 90.00 90.00 90.00 59.827
0 0 0 0
2Th_obs-shift 2Th (Calc) diff.
|
0
|
1 1
|
32.5320
|
|
32.5320
|
32.3453
|
0.1867
|
1
|
1 1
|
39.8120
|
|
39.8120
|
39.8916
|
-0.0796
|
0
|
0 2
|
46.3754
|
|
46.3754
|
46.3953
|
-0.0199
|
2
|
0 1
|
52.4121
|
|
52.4121
|
52.2586
|
0.1535
|
2
|
1 1
|
57.9244
|
|
57.9244
|
57.6888
|
0.2356
|
2
|
0 2
|
67.6657
|
|
67.6657
|
67.7061
|
-0.0404
|
1
|
2 2
|
72.3127
|
|
72.3127
|
72.4357
|
-0.1230
|
|
|
Final values
|
: (Standard errors on 2nd line)
|
|
Zero
|
Lambda
|
a
|
b
|
c alpha
|
beta gamma
|
volume
|
0.000
|
1.54060
|
3.9085
|
3.9085
|
3.9085 90.00
|
90.00
|
90.00 59.706
|
0.0000
|
0.00000
|
0.0078
|
0.0000
|
0.0000 0.000
|
0.000
|
0.000 0.000
|
H
|
K L
|
2Th (obs)
|
2Th_obs-shift
|
2Th (Calc) diff.
|
0
|
1
|
1
|
32.5320
|
32.5320
|
32.3677
|
0.1643
|
1
|
1
|
1
|
39.8120
|
39.8120
|
39.9197
|
-0.1077
|
0
|
0
|
2
|
46.3754
|
46.3754
|
46.4285
|
-0.0531
|
2
|
0
|
1
|
52.4121
|
52.4121
|
52.2966
|
0.1155
|
2
|
1
|
1
|
57.9244
|
57.9244
|
57.7314
|
0.1930
|
2
|
0
|
2
|
67.6657
|
67.6657
|
67.7581
|
-0.0924
|
1
|
2
|
2
|
72.3127
|
72.3127
|
72.4924
|
-0.179
|
CELREF Version 3
P4:TiO2
Initial values : (Refinement keys on 2nd line)
Zero Lambda a b c alpha beta gamma volume
0.000 1.54060 4.5793 4.5793 2.9560 90.00 90.00 90.00 61.987
0 0 1 0 1 0 0 0
H K L 2Th (obs) 2Th_obs-shift 2Th (Calc) diff.
1
|
1
|
0
|
27.5243
|
27.5243
|
27.5241
|
0.0002
|
1
|
0
|
1
|
36.1531
|
36.1531
|
36.1383
|
0.0148
|
0
|
0
|
2
|
62.8203
|
62.8203
|
62.8225
|
-0.0022
|
3
|
0
|
1
|
69.2146
|
69.2146
|
69.2149
|
-0.0003
|
1
|
3
|
1
|
72.6278
|
72.6278
|
72.6462
|
-0.0184
|
Final values : (Standard errors on 2nd
line)
Zero
|
Lambda
|
a
|
b c
|
alpha beta gamma
|
volume
|
0.000
|
1.54060
|
4.5793
|
4.5793 2.9560
|
90.00 90.00
|
90.00
|
61.987
|
0.0000
|
0.00000
|
0.0010
|
0.0000 0.0003
|
0.000 0.000
|
0.000
|
0.000
|
H K
|
L
|
2Th (obs)
|
2Th_obs-shift
|
2Th (Calc)
|
diff.
|
|
1
|
1
|
0
|
27.5243
|
27.5243
|
27.5243
|
0.0000
|
1
|
0
|
1
|
36.1531
|
36.1531
|
36.1380
|
0.0151
|
0
|
0
|
2
|
62.8203
|
62.8203
|
62.8215
|
-0.0012
|
3
|
0
|
1
|
69.2146
|
69.2146
|
69.2152
|
-0.0006
|
1
|
3
|
1
|
72.6278
|
72.6278
|
72.6465
|
-0.0187
|
CELREF Version 3
P 5:La2O3
Initial values : (Refinement keys on 2nd
line)
Zero Lambda a b c alpha beta gamma volume
0.000 1.54060 3.9415 3.9415 6.1373 90.00 90.00 120.00 82.572
0 0 1 0 1 0 0 0
H K L 2Th (obs) 2Th_obs-shift 2Th (Calc) diff.
0 1 1 29.9259 29.9259 29.9292 -0.0033
1 1 3 65.7766 65.7766 65.7391 0.0375
1 2 0 73.3067 73.3067 73.3190 -0.0123
1 1 4 79.0052 79.0052 79.0269 -0.0217
Final values : (Standard errors on 2nd line)
Zero Lambda a b c alpha beta gamma volume
0.000 1.54060 3.9417 3.9417 6.1372 90.00 90.00 120.00 82.577
0.0000 0.00000 0.0049 0.0000 0.0015
0.000 0.000 0.000 0.001
H K L 2Th (obs) 2Th_obs-shift 2Th (Calc) diff.
0 1 1 29.9259 29.9259 29.9283 -0.0024
1 1 3 65.7766 65.7766 65.7380 0.0386
1 2 0 73.3067 73.3067 73.3157 -0.0090
1 1 4 79.0052 79.0052 79.0261 -0.0209
CELREF Version 3
P6:La2Ti2O7
Initial values : (Refinement keys on 2nd line)
Zero Lambda a b c alpha beta gamma volume
0.000 1.54060 13.0031 5.5410 7.7994 90.00 98.46 90.00 555.833
0 0 1 1 1 0 1 0
H K L 2Th (obs) 2Th_obs-shift 2Th (Calc) diff.
2
|
0
|
0
|
13.8275
|
13.8275
|
13.7591
|
0.0684
|
1
|
1
|
0
|
17.4933
|
17.4933
|
17.4127
|
0.0806
|
2
|
1
|
0
|
21.2188
|
21.2188
|
21.1479
|
0.0709
|
-2
|
1
|
1
|
23.1136
|
23.1136
|
23.1104
|
0.0032
|
2
|
1
|
1
|
25.0670
|
25.0670
|
25.0859
|
-0.0189
|
3
|
1
|
0
|
26.2020
|
26.2020
|
26.2617
|
-0.0597
|
-3
|
1
|
1
|
27.5340
|
27.5340
|
27.4517
|
0.0823
|
-1
|
1
|
2
|
28.1952
|
28.1952
|
28.1821
|
0.0131
|
-3
|
0
|
2
|
28.7170
|
28.7170
|
28.7426
|
-0.0256
|
3
|
1
|
1
|
29.9809
|
29.9809
|
29.9703
|
0.0106
|
0
|
2
|
0
|
32.2966
|
32.2966
|
32.2861
|
0.0105
|
-4
|
1
|
1
|
32.7942
|
32.7942
|
32.7858
|
0.0084
|
-3
|
1
|
2
|
33.0580
|
33.0580
|
33.0562
|
0.0018
|
-4
|
0
|
2
|
33.5228
|
33.5228
|
33.5287
|
-0.0059
|
0
|
2
|
1
|
34.4367
|
34.4367
|
34.3657
|
0.0710
|
-4
|
1
|
2
|
37.3570
|
37.3570
|
37.3488
|
0.0082
|
0
|
1
|
3
|
38.6073
|
38.6073
|
38.5664
|
0.0409
|
2
|
0
|
3
|
39.5815
|
39.5815
|
39.5808
|
0.0007
|
-1
|
2
|
2
|
40.0583
|
40.0583
|
40.0490
|
0.0093
|
1
|
2
|
2
|
41.2840
|
41.2840
|
41.2866
|
-0.0026
|
-6
|
0
|
0
|
42.1893
|
42.1893
|
42.1204
|
0.0689
|
-5
|
1
|
2
|
42.4538
|
42.4538
|
42.4871
|
-0.0333
|
4
|
2
|
0
|
43.1249
|
43.1249
|
43.0626
|
0.0623
|
-3
|
2
|
2
|
43.7581
|
43.7581
|
43.7652
|
-0.0071
|
6
|
1
|
0
|
45.3428
|
45.3428
|
45.3249
|
0.0179
|
-5
|
0
|
3
|
46.1500
|
46.1500
|
46.0543
|
0.0957
|
-1
|
0
|
4
|
46.5320
|
46.5320
|
46.5391
|
-0.0071
|
-4
|
2
|
2
|
47.2043
|
47.2043
|
47.2344
|
-0.0301
|
-6
|
1
|
2
|
48.2796
|
48.2796
|
48.2751
|
0.0045
|
1
|
0
|
4
|
48.6583
|
48.6583
|
48.7226
|
-0.0643
|
-2
|
2
|
3
|
48.8658
|
48.8658
|
48.8260
|
0.0398
|
-2
|
1
|
4
|
50.0812
|
50.0812
|
50.0767
|
0.0045
|
1
|
1
|
4
|
51.6388
|
51.6388
|
51.6069
|
0.0319
|
7
|
0
|
1
|
52.8950
|
52.8950
|
52.8502
|
0.0448
|
6
|
1
|
2
|
54.3891
|
54.3891
|
54.4725
|
-0.0834
|
0
|
3
|
2
|
55.0687
|
55.0687
|
55.0844
|
-0.0157
|
7
|
1
|
1
|
55.4909
|
55.4909
|
55.5804
|
-0.0895
|
|
|
|
|
|
|
Annexe
|
1
|
3
|
2
|
56.0488
|
56.0488
|
56.0715
|
-0.0227
|
-6
|
2
|
2
|
56.6660
|
56.6660
|
56.6605
|
0.0055
|
-7
|
0
|
3
|
57.1486
|
57.1486
|
57.1176
|
0.0310
|
-5
|
1
|
4
|
57.7098
|
57.7098
|
57.7687
|
-0.0589
|
-3
|
3
|
2
|
58.0559
|
58.0559
|
58.0675
|
-0.0116
|
-8
|
0
|
2
|
58.8393
|
58.8393
|
58.8411
|
-0.0018
|
8
|
1
|
0
|
59.8705
|
59.8705
|
59.8534
|
0.0171
|
7
|
2
|
0
|
60.4161
|
60.4161
|
60.4049
|
0.0112
|
-8
|
1
|
2
|
61.3564
|
61.3564
|
61.3955
|
-0.0391
|
-2
|
3
|
3
|
62.3364
|
62.3364
|
62.2841
|
0.0523
|
-4
|
0
|
5
|
62.8288
|
62.8288
|
62.8002
|
0.0286
|
2
|
0
|
5
|
64.1094
|
64.1094
|
64.0488
|
0.0606
|
-7
|
0
|
4
|
64.6749
|
64.6749
|
64.6612
|
0.0137
|
-9
|
0
|
0
|
65.2306
|
65.2306
|
65.2343
|
-0.0037
|
-5
|
0
|
5
|
65.8244
|
65.8244
|
65.7873
|
0.0371
|
-9
|
1
|
1
|
66.9879
|
66.9879
|
66.9217
|
0.0662
|
3
|
0
|
5
|
67.4620
|
67.4620
|
67.4096
|
0.0524
|
1
|
4
|
0
|
67.9852
|
67.9852
|
68.0133
|
-0.0281
|
-5
|
1
|
5
|
68.1219
|
68.1219
|
68.1935
|
-0.0716
|
-9
|
1
|
2
|
68.6949
|
68.6949
|
68.6637
|
0.0312
|
-1
|
2
|
5
|
69.0624
|
69.0624
|
69.0651
|
-0.0027
|
4
|
2
|
4
|
69.2228
|
69.2228
|
69.1908
|
0.0320
|
6
|
2
|
3
|
69.8576
|
69.8576
|
69.8596
|
-0.0020
|
8
|
2
|
1
|
70.2700
|
70.2700
|
70.2349
|
0.0351
|
-9
|
0
|
3
|
70.4508
|
70.4508
|
70.4600
|
-0.0092
|
9
|
1
|
1
|
70.8575
|
70.8575
|
70.8135
|
0.0440
|
1
|
3
|
4
|
71.7877
|
71.7877
|
71.8301
|
-0.0424
|
-3
|
4
|
1
|
72.1147
|
72.1147
|
72.0843
|
0.0304
|
-10
|
0
|
1
|
72.6359
|
72.6359
|
72.6712
|
-0.0353
|
3
|
4
|
1
|
73.3525
|
73.3525
|
73.3513
|
0.0012
|
2
|
2
|
5
|
73.5542
|
73.5542
|
73.5608
|
-0.0066
|
9
|
0
|
2
|
73.9923
|
73.9923
|
73.9901
|
0.0022
|
6
|
3
|
2
|
74.2391
|
74.2391
|
74.2240
|
0.0151
|
-3
|
4
|
2
|
75.0117
|
75.0117
|
75.0276
|
-0.0159
|
-4
|
0
|
6
|
75.3557
|
75.3557
|
75.4143
|
-0.0586
|
10
|
1
|
0
|
75.8212
|
75.8212
|
75.8801
|
-0.0589
|
3
|
4
|
2
|
77.5072
|
77.5072
|
77.5185
|
-0.0113
|
9
|
2
|
1
|
77.7216
|
77.7216
|
77.7201
|
0.0015
|
5
|
4
|
0
|
78.2756
|
78.2756
|
78.3334
|
-0.0578
|
5
|
1
|
5
|
78.6794
|
78.6794
|
78.7253
|
-0.0459
|
10
|
1
|
1
|
79.0492
|
79.0492
|
79.1161
|
-0.0669
|
Final values : (Standard errors on 2nd line)
Zero Lambda a b c alpha beta gamma volume
0.000
|
1.54060
|
13.0031
|
5.5410
|
7.7994
|
90.00
|
98.46
|
90.00
|
555.842
|
0.0000
|
0.00000
|
0.0023
|
0.0011
|
0.0017
|
0.000
|
0.013
|
0.000
|
0.126
|
H K L 2Th (obs) 2Th_obs-shift 2Th (Calc) diff.
2
|
0
|
0
|
13.8275
|
13.8275
|
13.7590
|
0.0685
|
1
|
1
|
0
|
17.4933
|
17.4933
|
17.4127
|
0.0806
|
2
|
1
|
0
|
21.2188
|
21.2188
|
21.1479
|
0.0709
|
-2
|
1
|
1
|
23.1136
|
23.1136
|
23.1109
|
0.0027
|
2
|
1
|
1
|
25.0670
|
25.0670
|
25.0851
|
-0.0181
|
3
|
1
|
0
|
26.2020
|
26.2020
|
26.2615
|
-0.0595
|
-3
|
1
|
1
|
27.5340
|
27.5340
|
27.4522
|
0.0818
|
-1
|
1
|
2
|
28.1952
|
28.1952
|
28.1822
|
0.0130
|
-3
|
0
|
2
|
28.7170
|
28.7170
|
28.7436
|
-0.0266
|
3
|
1
|
1
|
29.9809
|
29.9809
|
29.9693
|
0.0116
|
0
|
2
|
0
|
32.2966
|
32.2966
|
32.2862
|
0.0104
|
-4
|
1
|
1
|
32.7942
|
32.7942
|
32.7863
|
0.0079
|
-3
|
1
|
2
|
33.0580
|
33.0580
|
33.0570
|
0.0010
|
-4
|
0
|
2
|
33.5228
|
33.5228
|
33.5298
|
-0.0070
|
0
|
2
|
1
|
34.4367
|
34.4367
|
34.3658
|
0.0709
|
-4
|
1
|
2
|
37.3570
|
37.3570
|
37.3498
|
0.0072
|
0
|
1
|
3
|
38.6073
|
38.6073
|
38.5659
|
0.0414
|
2
|
0
|
3
|
39.5815
|
39.5815
|
39.5790
|
0.0025
|
-1
|
2
|
2
|
40.0583
|
40.0583
|
40.0492
|
0.0091
|
1
|
2
|
2
|
41.2840
|
41.2840
|
41.2861
|
-0.0021
|
-6
|
0
|
0
|
42.1893
|
42.1893
|
42.1198
|
0.0695
|
-5
|
1
|
2
|
42.4538
|
42.4538
|
42.4882
|
-0.0344
|
4
|
2
|
0
|
43.1249
|
43.1249
|
43.0624
|
0.0625
|
-3
|
2
|
2
|
43.7581
|
43.7581
|
43.7660
|
-0.0079
|
6
|
1
|
0
|
45.3428
|
45.3428
|
45.3244
|
0.0184
|
-5
|
0
|
3
|
46.1500
|
46.1500
|
46.0559
|
0.0941
|
-1
|
0
|
4
|
46.5320
|
46.5320
|
46.5389
|
-0.0069
|
-4
|
2
|
2
|
47.2043
|
47.2043
|
47.2353
|
-0.0310
|
-6
|
1
|
2
|
48.2796
|
48.2796
|
48.2763
|
0.0033
|
1
|
0
|
4
|
48.6583
|
48.6583
|
48.7210
|
-0.0627
|
-2
|
2
|
3
|
48.8658
|
48.8658
|
48.8264
|
0.0394
|
-2
|
1
|
4
|
50.0812
|
50.0812
|
50.0770
|
0.0042
|
1
|
1
|
4
|
51.6388
|
51.6388
|
51.6054
|
0.0334
|
7
|
0
|
1
|
52.8950
|
52.8950
|
52.8484
|
0.0466
|
6
|
1
|
2
|
54.3891
|
54.3891
|
54.4700
|
-0.0809
|
0
|
3
|
2
|
55.0687
|
55.0687
|
55.0843
|
-0.0156
|
7
|
1
|
1
|
55.4909
|
55.4909
|
55.5787
|
-0.0878
|
1
|
3
|
2
|
56.0488
|
56.0488
|
56.0712
|
-0.0224
|
-6
|
2
|
2
|
56.6660
|
56.6660
|
56.6617
|
0.0043
|
-7
|
0
|
3
|
57.1486
|
57.1486
|
57.1195
|
0.0291
|
-5
|
1
|
4
|
57.7098
|
57.7098
|
57.7704
|
-0.0606
|
-3
|
3
|
2
|
58.0559
|
58.0559
|
58.0682
|
-0.0123
|
-8
|
0
|
2
|
58.8393
|
58.8393
|
58.8424
|
-0.0031
|
8
|
1
|
0
|
59.8705
|
59.8705
|
59.8526
|
0.0179
|
7
|
2
|
0
|
60.4161
|
60.4161
|
60.4044
|
0.0117
|
-8
|
1
|
2
|
61.3564
|
61.3564
|
61.3967
|
-0.0403
|
-2
|
3
|
3
|
62.3364
|
62.3364
|
62.2846
|
0.0518
|
-4
|
0
|
5
|
62.8288
|
62.8288
|
62.8015
|
0.0273
|
2
|
0
|
5
|
64.1094
|
64.1094
|
64.0462
|
0.0632
|
-7
|
0
|
4
|
64.6749
|
64.6749
|
64.6636
|
0.0113
|
-9
|
0
|
0
|
65.2306
|
65.2306
|
65.2333
|
-0.0027
|
-5
|
0
|
5
|
65.8244
|
65.8244
|
65.7892
|
0.0352
|
-9
|
1
|
1
|
66.9879
|
66.9879
|
66.9218
|
0.0661
|
3
|
0
|
5
|
67.4620
|
67.4620
|
67.4064
|
0.0556
|
1
|
4
|
0
|
67.9852
|
67.9852
|
68.0135
|
-0.0283
|
-5
|
1
|
5
|
68.1219
|
68.1219
|
68.1954
|
-0.0735
|
-9
|
1
|
2
|
68.6949
|
68.6949
|
68.6649
|
0.0300
|
-1
|
2
|
5
|
69.0624
|
69.0624
|
69.0646
|
-0.0022
|
4
|
2
|
4
|
69.2228
|
69.2228
|
69.1879
|
0.0349
|
6
|
2
|
3
|
69.8576
|
69.8576
|
69.8566
|
0.0010
|
8
|
2
|
1
|
70.2700
|
70.2700
|
70.2332
|
0.0368
|
-9
|
0
|
3
|
70.4508
|
70.4508
|
70.4621
|
-0.0113
|
9
|
1
|
1
|
70.8575
|
70.8575
|
70.8114
|
0.0461
|
1
|
3
|
4
|
71.7877
|
71.7877
|
71.8290
|
-0.0413
|
-3
|
4
|
1
|
72.1147
|
72.1147
|
72.0848
|
0.0299
|
-10
|
0
|
1
|
72.6359
|
72.6359
|
72.6712
|
-0.0353
|
3
|
4
|
1
|
73.3525
|
73.3525
|
73.3511
|
0.0014
|
2
|
2
|
5
|
73.5542
|
73.5542
|
73.5585
|
-0.0043
|
9
|
0
|
2
|
73.9923
|
73.9923
|
73.9868
|
0.0055
|
6
|
3
|
2
|
74.2391
|
74.2391
|
74.2221
|
0.0170
|
-3
|
4
|
2
|
75.0117
|
75.0117
|
75.0283
|
-0.0166
|
-4
|
0
|
6
|
75.3557
|
75.3557
|
75.4155
|
-0.0598
|
10
|
1
|
0
|
75.8212
|
75.8212
|
75.8790
|
-0.0578
|
3
|
4
|
2
|
77.5072
|
77.5072
|
77.5178
|
-0.0106
|
9
|
2
|
1
|
77.7216
|
77.7216
|
77.7181
|
0.0035
|
5
|
4
|
0
|
78.2756
|
78.2756
|
78.3334
|
-0.0578
|
5
|
1
|
5
|
78.6794
|
78.6794
|
78.7209
|
-0.0415
|
10
|
1
|
1
|
79.0492
|
79.0492
|
79.1137
|
-0.0645
|
Références bibliographiques
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