Conclusion générale
Conclusion générale
Dans cette étude, l'objectif de notre travail
était consacré à la synthèse, la
caractérisation et l'étude de la stabilité
électrochimique , de quelques poudres ayant pour structure celle des
multicouches(Ruddlesden-Popper) de formule générale
La3-xCaxMn2O7 avec x=1.8, 1.6 et
2.
Pour la synthèse on a utilisé deux
méthodes de la voie Sol-gel (La méthode
Péchini et méthode citrate).
L'analyse des résultats obtenus a donnée lieu
aux conclusions suivantes :
La caractérisation des phases par DRX nous a
permis de conclure que les poudres préparées par les deux
méthodes sont polyphasiques. Les phases majoritaires représentent
nos phases qui se cristallisent dans le système orthorhombique (S.G
Pbcm), les phases minoritaires se cristallisent dans des différents
systèmes.
La caractérisation des phases par le MEB confirme
que les échantillons Ph1, Ph2, Ph3 et Cit1 sont conducteurs, par contre
Cit2 et Cit3 présentent un caractère isolant. La taille des
grains pour la méthode Péchini est plus grande que celle pour la
méthode citrate (ph1 et cit1).
Dans le future, pour essayer de trouver des phases pures,
plusieurs paramètres peuvent être étudiés à
savoir le temps de traitement thermique,la température, le pH de la
solution ainsi que l'agent complexant. D'autres méthodes peuvent
être étudiées (coprécipitation,
microémulsion..).
Les tests électrochimiques ont été
réalisés d'une manière succincte, ils nous ont
révélés que ce domaine et très vaste et peut ouvrir
beaucoup de perspectives et beaucoup d'études pourront être
réalisées pour essayer de trouver une débouché pour
l'application de ces matériaux surtout dans le domaine de
l'electrocatalyse.
ANNEXE
ANNEXE
CELREF Version 3. 14/06/2007 10:00:02
----------------------------------------------------------------------
P1
(La1.2Ca1.8Mn2O7)
Initial values : (Raffinement keys on 2nd line)
-------------- :
Zero Lambda a b c alpha
beta gamma volume
0.000 1.54060 5.7851 5.6766 19.3500 90.00 90.00 90.00
635.448
0 0 1 1 1
0 0 0
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
1 0 0 15.3740 15.3740 15.3036
0.0704
0 0 6 27.5930 27.5930 27.6377
-0.0447
0 2 1 31.8260 31.8260 31.8405
-0.0145
0 2 2 32.7840 32.7840 32.8586
-0.0746
1 1 6 35.5340 35.5340 35.5496
-0.0156
1 0 8 40.3820 40.3820 40.3862
-0.0042
2 1 6 45.0170 45.0170 44.9896
0.0274
0 2 7 45.8630 45.8630 45.7824
0.0806
2 2 3 47.0140 47.0140 46.9742
0.0398
2 3 1 58.4870 58.4870 58.4296
0.0574
1 1 12 61.9190 61.9190 61.8807
0.0383
0 4 2 66.4840 66.4840 66.5417
-0.0577
0 2 12 66.6260 66.6260 66.6539
-0.0279
3 0 10 68.6910 68.6910 68.6589
0.0321
4 2 0 73.4190 73.4190 73.4206
-0.0016
1 3 11 75.5340 75.5340 75.5470
-0.0130
4 0 8 76.7810 76.7810 76.7143
0.0667
4 2 5 78.1010 78.1010 78.1057
-0.0047
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0492
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0450
Final values : (Standard errors on 2nd line)
------------
Zero Lambda a b c
alpha beta gamma volume
0.000 1.54060 5.7817 5.6791 19.3467 90.00 90.00
90.00 635.244
0.0000 0.00000 0.0021 0.0024 0.0078 0.000 0.000
0.000 0.000
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
1 0 0 15.3740 15.3740 15.3127
0.0613
0 0 6 27.5930 27.5930 27.6425
-0.0495
0 2 1 31.8260 31.8260 31.8266
-0.0006
0 2 2 32.7840 32.7840 32.8455
-0.0615
1 1 6 35.5340 35.5340 35.5544
-0.0204
1 0 8 40.3820 40.3820 40.3960
-0.0140
2 1 6 45.0170 45.0170 45.0037
0.0133
0 2 7 45.8630 45.8630 45.7763
0.0867
ANNEXE
2 2 3 47.0140 47.0140 46.9779 0.0361
2 3 1 58.4870 58.4870 58.4214 0.0656
1 1 12 61.9190 61.9190 61.8914 0.0276
0 4 2 66.4840 66.4840 66.5098 -0.0258
0 2 12 66.6260 66.6260 66.6555 -0.0295
3 0 10 68.6910 68.6910 68.6887 0.0023
4 2 0 73.4190 73.4190 73.4529 -0.0339
1 3 11 75.5340 75.5340 75.5400 -0.0060
4 0 8 76.7810 76.7810 76.7577 0.0233
4 2 5 78.1010 78.1010 78.1389 -0.0379
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0442
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0404
ANNEXE
CELREF Version 3. 14/06/2007 10:07:06
----------------------------------------------------------------------
Phase secondaire
Initial values : (Refinement keys on 2nd line)
-------------- :
Zero Lambda a b c alpha
beta gamma v
0.000 1.54060 8.4571 8.4571 9.6739 90.00 90.00 90.00
691.902
0 0 1 0 1 0 0
0
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
0 2 1 23.0020 23.0020 22.9346
0.0674
3 0 3 42.6020 42.6020 42.5623
0.0397
3 3 0 45.5460 45.5460 45.4655
0.0805
3 4 0 54.1410 54.1410 54.1834
-0.0424
2 2 5 56.6450 56.6450 56.6164
0.0286
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0712
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0551
Final values : (Standard errors on 2nd line)
------------
Zero Lambda a b c
alpha beta gamma volume
0.000 1.54060 8.4530 8.4530 9.6673 90.00 90.00
90.00 690.761
0.0000 0.00000 0.0141 0.0000 0.0039 0.000 0.000
0.000 0.000
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
0 2 1 23.0020 23.0020 22.9466
0.0554
3 0 3 42.6020 42.6020 42.5878
0.0142
3 3 0 45.5460 45.5460 45.4888
0.0572
3 4 0 54.1410 54.1410 54.2118
-0.0708
2 2 5 56.6450 56.6450 56.6550
-0.0100
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0623
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0483
ANNEXE
CELREF Version 3. 14/06/2007 10:16:47
----------------------------------------------------------------------
P2
(La1.4Ca1.6Mn2O7) à
1100°c
Initial values : (Refinement keys on 2nd line)
-------------- :
Zero Lambda a b c alpha
beta gamma volume
0.000 1.54060 5.7851 5.6766 19.3500 90.00 90.00
90.00 635.448
0 0 1 1 1
0 0 0
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
1 0 0 15.3600 15.3600 15.3036
0.0564
0 0 6 27.5810 27.5810 27.6377
-0.0567
0 2 1 31.8410 31.8410 31.8405
0.0005
0 2 2 32.7270 32.7270 32.8586
-0.1316
1 1 6 35.5380 35.5380 35.5496
-0.0116
1 1 7 39.5080 39.5080 39.4293
0.0787
1 0 8 40.3340 40.3340 40.3862
-0.0522
2 1 6 44.9910 44.9910 44.9896
0.0014
0 0 10 46.9260 46.9260 46.9174
0.0086
1 2 8 52.1240 52.1240 52.0928
0.0312
3 0 6 55.4470 55.4470 55.4749
-0.0279
1 2 9 55.9920 55.9920 55.9094
0.0826
2 3 1 58.3900 58.3900 58.4296
-0.0396
1 1 12 61.8330 61.8330 61.8807
-0.0477
2 1 12 68.5930 68.5930 68.5967
-0.0037
1 3 11 75.5270 75.5270 75.5470
-0.0200
0 4 8 78.0185 78.0185 78.0000
0.0185
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0573
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0520
Final values : (Standard errors on 2nd line)
------------
Zero Lambda a b c alpha
beta gamma volume
0.000 1.54060 5.7859 5.6780 19.3496 90.00 90.00
90.00 635.675
0.0000 0.00000 0.0061 0.0033 0.0098 0.000 0.000
0.000 0.000
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
1 0 0 15.3600 15.3600 15.3015
0.0585
0 0 6 27.5810 27.5810 27.6382
-0.0572
0 2 1 31.8410 31.8410 31.8329
0.0081
0 2 2 32.7270 32.7270 32.8513
-0.1243
1 1 6 35.5380 35.5380 35.5474
-0.0094
1 1 7 39.5080 39.5080 39.4274
0.0806
1 0 8 40.3340 40.3340 40.3860
-0.0520
ANNEXE
2 1 6 44.9910 44.9910 44.9854 0.0056
0 0 10 46.9260 46.9260 46.9183 0.0077
1 2 8 52.1240 52.1240 52.0876 0.0364
3 0 6 55.4470 55.4470 55.4691 -0.0221
1 2 9 55.9920 55.9920 55.9046 0.0874
2 3 1 58.3900 58.3900 58.4164 -0.0264
1 1 12 61.8330 61.8330 61.8801 -0.0471
2 1 12 68.5930 68.5930 68.5943 -0.0013
1 3 11 75.5270 75.5270 75.5380 -0.0110
0 4 8 78.0185 78.0185 77.9840 0.0345
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0569
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0516
ANNEXE
CELREF Version 3. 14/06/2007 10:11:32
----------------------------------------------------------------------
Phase secondaire
Initial values : (Refinement keys on 2nd line)
-------------- :
Zero Lambda a b c
alpha beta gamma volume
0.000 1.54060 8.0381 3.8679 7.4100 90.00 105.43
90.00 222.078
0 0 1 1 1
0 1 0
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
1 0 1 18.9550 18.9550 18.9917
-0.0367
-2 0 1 22.9990 22.9990 23.0017
-0.0027
0 1 1 26.1810 26.1810 26.1793
0.0017
-2 0 2 29.1010 29.1010 29.1281
-0.0271
1 1 1 30.0110 30.0110 29.9751
0.0359
2 1 1 37.3220 37.3220 37.2942
0.0278
1 0 3 42.6050 42.6050 42.5511
0.0539
-2 1 3 45.5400 45.5400 45.5142
0.0258
-3 0 4 54.1460 54.1460 54.0653
0.0807
0 1 4 56.6966 56.6966 56.7338
-0.0372
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0510
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0395
Final values : (Standard errors on 2nd line)
------------
Zero Lambda a b c alpha
beta gamma volume
0.000 1.54060 8.0324 3.8665 7.4073 90.00 105.40
90.00 221.791
0.0000 0.00000 0.0206 0.0057 0.0120 0.000 0.192
0.000 0.748
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
1 0 1 18.9550 18.9550 18.9958
-0.0408
-2 0 1 22.9990 22.9990 23.0196
-0.0206
0 1 1 26.1810 26.1810 26.1881
-0.0071
-2 0 2 29.1010 29.1010 29.1487
-0.0477
1 1 1 30.0110 30.0110 29.9843
0.0267
2 1 1 37.3220 37.3220 37.3072
0.0148
1 0 3 42.6050 42.6050 42.5587
0.0463
-2 1 3 45.5400 45.5400 45.5389
0.0011
-3 0 4 54.1460 54.1460 54.1008
0.0452
0 1 4 56.6966 56.6966 56.7496
-0.0530
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0454
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0351
ANNEXE
CELREF Version 3. 14/06/2007 10:22:24
----------------------------------------------------------------------
P3 (LaCa2Mn2o7) à
1100°c
Initial values : (Refinement keys on 2nd line)
-------------- :
Zero Lambda a b c
alpha beta gamma volume
0.000 1.54060 5.7851 5.6766 19.3500 90.00 90.00
90.00 635.448
0 0 1 1 1
0 0 0
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
1 0 0 15.3390 15.3390 15.3036
0.0354
0 0 6 27.5640 27.5640 27.6377
-0.0737
0 2 1 31.7940 31.7940 31.8405
-0.0465
0 2 2 32.7410 32.7410 32.8586
-0.1176
1 2 1 35.5090 35.5090 35.5054
0.0036
1 0 8 40.3670 40.3670 40.3862
-0.0192
2 1 6 44.9730 44.9730 44.9896
-0.0166
0 2 7 45.8440 45.8440 45.7824
0.0616
2 2 3 46.9750 46.9750 46.9742
0.0008
2 3 1 58.4320 58.4320 58.4296
0.0024
1 1 12 61.8920 61.8920 61.8807
0.0113
0 4 2 66.4730 66.4730 66.5417
-0.0687
0 2 12 66.6290 66.6290 66.6539
-0.0249
2 1 12 68.6270 68.6270 68.5967
0.0303
2 1 13 73.3760 73.3760 73.3997
-0.0237
1 2 13 73.6820 73.6820 73.6450
0.0370
1 3 11 75.4910 75.4910 75.5470
-0.0560
4 0 8 76.7420 76.7420 76.7143
0.0277
4 2 5 78.1309 78.1309 78.1057
0.0252
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0500
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0459
Final values : (Standard errors on 2nd line)
------------
Zero Lambda a b c
alpha beta gamma volume
0.000 1.54060 5.7817 5.6815 19.3500 90.00 90.00
90.00 635.626
0.0000 0.00000 0.0025 0.0022 0.0059 0.000 0.000
0.000 0.000
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
1 0 0 15.3390 15.3390 15.3126
0.0264
0 0 6 27.5640 27.5640 27.6376
-0.0736
0 2 1 31.7940 31.7940 31.8128
-0.0188
0 2 2 32.7410 32.7410 32.8318
-0.0908
1 2 1 35.5090 35.5090 35.4844
0.0246
1 0 8 40.3670 40.3670 40.3898
-0.0228
2 1 6 44.9730 44.9730 44.9979
-0.0249
ANNEXE
0 2 7 45.8440 45.8440 45.7620 0.0820
2 2 3 46.9750 46.9750 46.9673 0.0077
2 3 1 58.4320 58.4320 58.4023 0.0297
1 1 12 61.8920 61.8920 61.8792 0.0128
0 4 2 66.4730 66.4730 66.4782 -0.0052
0 2 12 66.6290 66.6290 66.6379 -0.0089
2 1 12 68.6270 68.6270 68.6029 0.0241
2 1 13 73.3760 73.3760 73.4057 -0.0297
1 2 13 73.6820 73.6820 73.6321 0.0499
1 3 11 75.4910 75.4910 75.5155 -0.0245
4 0 8 76.7420 76.7420 76.7534 -0.0114
4 2 5 78.1309 78.1309 78.1298 0.0011
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0426
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0391
ANNEXE
CELREF Version 3. 14/06/2007 10:27:15
----------------------------------------------------------------------
Phase secondaire
Initial values : (Refinement keys on 2nd line)
-------------- :
Zero Lambda a b c alpha
beta gamma volume
0.000 1.54060 11.5565 11.5565 9.3992 90.00 90.00 90.00
1255.288
0 0 1 0 1
0 0 0
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
0 0 2 18.9250 18.9250 18.8676
0.0574
0 3 0 23.0110 23.0110 23.0699
-0.0589
1 4 2 37.2940 37.2940 37.3249
-0.0309
4 0 3 42.5750 42.5750 42.5293
0.0457
2 4 3 45.5110 45.5110 45.4615
0.0495
3 6 1 54.1030 54.1030 54.0764
0.0266
1 6 3 56.6223 56.6223 56.6104
0.0119
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0512
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0433
Final values : (Standard errors on 2nd line)
------------
Zero Lambda a b c alpha
beta gamma volume
0.000 1.54060 11.5485 11.5485 9.3920 90.00 90.00 90.00
1252.598
0.0000 0.00000 0.0269 0.0000 0.0060 0.000 0.000
0.000 0.000
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
0 0 2 18.9250 18.9250 18.8821
0.0429
0 3 0 23.0110 23.0110 23.0861
-0.0751
1 4 2 37.2940 37.2940 37.3524
-0.0584
4 0 3 42.5750 42.5750 42.5616
0.0134
2 4 3 45.5110 45.5110 45.4961
0.0149
3 6 1 54.1030 54.1030 54.1170
-0.0140
1 6 3 56.6223 56.6223 56.6543
-0.0320
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0500
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0423
ANNEXE
CELREF Version 3. 14/06/2007 08:56:22
----------------------------------------------------------------------
C1 (
La1.2Ca1.8Mn2O7) à
1100°C
Initial values : (Refinement keys on 2nd line)
-------------- :
Zero Lambda a b c
alpha beta gamma volume
0.000 1.54060 5.7851 5.6766 19.3500 90.00 90.00
90.00 635.448
0 0 1 1 1 0 0
0
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
1 0 0 15.3350 15.3350 15.3036
0.0314
0 0 6 27.5660 27.5660 27.6377
-0.0717
1 0 6 31.7000 31.7000 31.7405
-0.0405
0 2 1 31.8680 31.8680 31.8405
0.0275
0 2 2 32.7200 32.7200 32.8586
-0.1386
1 1 6 35.5330 35.5330 35.5496
-0.0166
1 0 8 40.3540 40.3540 40.3862
-0.0322
2 1 6 44.9930 44.9930 44.9896
0.0034
0 0 10 46.9140 46.9140 46.9174
-0.0034
1 2 8 52.1170 52.1170 52.0928
0.0242
1 3 3 52.8120 52.8120 52.8023
0.0097
2 3 1 58.3430 58.3430 58.4296
-0.0866
2 3 2 59.1220 59.1220 59.0669
0.0551
1 1 12 61.8190 61.8190 61.8807
-0.0617
0 4 2 66.5810 66.5810 66.5417
0.0393
2 1 12 68.5360 68.5360 68.5967
-0.0607
4 2 0 73.4280 73.4280 73.4206
0.0074
4 2 1 73.6210 73.6210 73.6100
0.0110
4 0 8 76.7530 76.7530 76.7143
0.0387
0 4 8 77.9901 77.9901 78.0000
-0.0099
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0548
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0505
Final values : (Standard errors on 2nd line)
------------
Zero Lambda a b c
alpha beta gamma volume
0.000 1.54060 5.7831 5.6768 19.3655 90.00 90.00
90.00 635.762
0.0000 0.00000 0.0024 0.0021 0.0083 0.000 0.000
0.000 0.000
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
1 0 0 15.3350 15.3350 15.3089
0.0261
0 0 6 27.5660 27.5660 27.6151
-0.0491
1 0 6 31.7000 31.7000 31.7232
-0.0232
0 2 1 31.8680 31.8680 31.8387
0.0293
ANNEXE
0 2 2 32.7200 32.7200 32.8553
-0.1353
1 1 6 35.5330 35.5330 35.5338
-0.0008
1 0 8 40.3540 40.3540 40.3596
-0.0056
2 1 6 44.9930 44.9930 44.9826
0.0104
0 0 10 46.9140 46.9140 46.8775
0.0365
1 2 8 52.1170 52.1170 52.0702
0.0468
1 3 3 52.8120 52.8120 52.7989
0.0131
2 3 1 58.3430 58.3430 58.4341
-0.0911
2 3 2 59.1220 59.1220 59.0704
0.0516
1 1 12 61.8190 61.8190 61.8346
-0.0156
0 4 2 66.5810 66.5810 66.5376
0.0434
2 1 12 68.5360 68.5360 68.5575
-0.0215
4 2 0 73.4280 73.4280 73.4435
-0.0155
4 2 1 73.6210 73.6210 73.6326
-0.0116
4 0 8 76.7530 76.7530 76.7184
0.0346
0 4 8 77.9901 77.9901 77.9782
0.0119
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0496
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0458
ANNEXE
CELREF Version 3. 14/06/2007 08:36:50
----------------------------------------------------------------------
Phase secondaire
Initial values : (Refinement keys on 2nd line)
-------------- :
Zero Lambda a b c
alpha beta gamma volume
0.000 1.54060 11.9138 9.4875 6.0626 90.00 90.00
90.00 685.269
0 0 1 1 1 0 0
0
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
1 1 1 18.9750 18.9750 18.8854
0.0896
2 1 1 22.9740 22.9740 22.9147
0.0593
4 0 0 29.9810 29.9810 29.9769
0.0041
3 0 2 37.3450 37.3450 37.2877
0.0573
0 4 1 40.8500 40.8500 40.8198
0.0302
4 0 2 42.6020 42.6020 42.5169
0.0851
1 0 3 45.5280 45.5280 45.4884
0.0396
3 4 2 54.1420 54.1420 54.2210
-0.0790
6 1 2 56.1740 56.1740 56.1737
0.0003
2 4 3 62.2720 62.2720 62.2880
-0.0160
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0666
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0557
Final values : (Standard errors on 2nd line)
------------
Zero Lambda a b c
alpha beta gamma volume
0.000 1.54060 11.9102 9.4979 6.0558 90.00 90.00
90.00 685.044
0.0000 0.00000 0.0131 0.0113 0.0060 0.000 0.000
0.000 0.000
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
1 1 1 18.9750 18.9750 18.8940
0.0810
2 1 1 22.9740 22.9740 22.9241
0.0499
4 0 0 29.9810 29.9810 29.9862
-0.0052
3 0 2 37.3450 37.3450 37.3195
0.0255
0 4 1 40.8500 40.8500 40.7856
0.0644
4 0 2 42.6020 42.6020 42.5484
0.0536
1 0 3 45.5280 45.5280 45.5414
-0.0134
3 4 2 54.1420 54.1420 54.2121
-0.0701
6 1 2 56.1740 56.1740 56.2043
-0.0303
2 4 3 62.2720 62.2720 62.3017
-0.0297
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0581
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0486
ANNEXE
CELREF Version 3. 14/06/2007 09:51:17
----------------------------------------------------------------------
C2
(La1.4Ca1.6Mn2O7) à
1100°c
Initial values : (Raffinement keys on 2nd line)
-------------- :
Zero Lambda a b c
alpha beta gamma volume
0.000 1.54060 5.7851 5.6766 19.3500 90.00 90.00
90.00 635.448
0 0 1 1 1 0 0
0
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
1 0 0 15.3060 15.3060 15.3036
0.0024
0 0 6 27.5370 27.5370 27.6377
-0.1007
0 2 1 31.8440 31.8440 31.8405
0.0035
0 2 2 32.6880 32.6880 32.8586
-0.1706
1 2 1 35.5090 35.5090 35.5054
0.0036
1 1 7 39.5070 39.5070 39.4293
0.0777
1 0 8 40.3280 40.3280 40.3862
-0.0582
2 2 1 44.9560 44.9560 44.9532
0.0028
0 0 10 46.8820 46.8820 46.9174
-0.0354
1 2 8 52.1230 52.1230 52.0928
0.0302
3 0 6 55.4340 55.4340 55.4749
-0.0409
1 2 9 55.9400 55.9400 55.9094
0.0306
2 3 1 58.3260 58.3260 58.4296
-0.1036
1 1 12 61.8200 61.8200 61.8807
-0.0607
0 4 2 66.5370 66.5370 66.5417
-0.0047
4 1 3 68.4710 68.4710 68.4507
0.0203
1 1 14 72.0550 72.0550 72.1518
-0.0968
4 2 0 73.4500 73.4500 73.4206
0.0294
1 3 11 75.4880 75.4880 75.5470
-0.0590
0 4 8 77.9790 77.9790 78.0000
-0.0210
0 0 16 79.0975 79.0975 79.1281
-0.0306
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0681
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0630
Final values : (Standard errors on 2nd line)
------------
Zero Lambda a b c alpha
beta gamma volume
0.000 1.54060 5.7839 5.6794 19.3624 90.00 90.00
90.00 636.039
0.0000 0.00000 0.0032 0.0027 0.0071 0.000 0.000
0.000 0.000
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
1 0 0 15.3060 15.3060 15.3067
-0.0007
0 0 6 27.5370 27.5370 27.6197
-0.0827
0 2 1 31.8440 31.8440 31.8243
0.0197
0 2 2 32.6880 32.6880 32.8416
-0.1536
ANNEXE
1 2 1 35.5090 35.5090 35.4921
0.0169
1 1 7 39.5070 39.5070 39.4094
0.0976
1 0 8 40.3280 40.3280 40.3646
-0.0366
2 2 1 44.9560 44.9560 44.9458
0.0102
0 0 10 46.8820 46.8820 46.8857
-0.0037
1 2 8 52.1230 52.1230 52.0645
0.0585
3 0 6 55.4340 55.4340 55.4738
-0.0398
1 2 9 55.9400 55.9400 55.8777
0.0623
2 3 1 58.3260 58.3260 58.4112
-0.0852
1 1 12 61.8200 61.8200 61.8415
-0.0215
0 4 2 66.5370 66.5370 66.5045
0.0325
4 1 3 68.4710 68.4710 68.4604
0.0106
1 1 14 72.0550 72.0550 72.1028
-0.0478
4 2 0 73.4500 73.4500 73.4256
0.0244
1 3 11 75.4880 75.4880 75.4996
-0.0116
0 4 8 77.9790 77.9790 77.9508
0.0282
0 0 16 79.0975 79.0975 79.0677
0.0298
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0599
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0554
ANNEXE
CELREF Version 3. 14/06/2007 09:03:17
----------------------------------------------------------------------
Phase secondaire
Initial values : (Refinement keys on 2nd line)
-------------- :
Zero Lambda a b c alpha
beta gamma volume
0.000 1.54060 19.8391 6.8888 6.7696 90.00 90.00
90.00 925.185
0 0 1 1 1 0 0
0
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
1 1 1 18.9350 18.9350 18.9005
0.0345
1 2 0 26.1410 26.1410 26.2391
-0.0981
5 1 1 29.1290 29.1290 29.1062
0.0228
6 1 0 29.9830 29.9830 29.9515
0.0315
5 1 2 37.3120 37.3120 37.2471
0.0649
8 1 1 40.8510 40.8510 40.8759
-0.0249
2 3 1 42.5750 42.5750 42.5252
0.0498
4 3 1 45.5050 45.5050 45.5089
-0.0039
4 1 3 46.0820 46.0820 46.0769
0.0051
0 0 4 54.1360 54.1360 54.1495
-0.0135
8 1 3 56.6860 56.6860 56.7039
-0.0179
12 2 0 62.2395 62.2395 62.2384
0.0011
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0474
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0410
Final values : (Standard errors on 2nd line
------------
Zero Lambda a b c alpha
beta gamma volume
0.000 1.54060 19.8361 6.8894 6.7691 90.00 90.00
90.00 925.054
0.0000 0.00000 0.0130 0.0056 0.0042 0.000 0.000
0.000 0.000
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
1 1 1 18.9350 18.9350 18.9006
0.0344
1 2 0 26.1410 26.1410 26.2372
-0.0962
5 1 1 29.1290 29.1290 29.1089
0.0201
6 1 0 29.9830 29.9830 29.9548
0.0282
5 1 2 37.3120 37.3120 37.2502
0.0618
8 1 1 40.8510 40.8510 40.8809
-0.0299
2 3 1 42.5750 42.5750 42.5227
0.0523
4 3 1 45.5050 45.5050 45.5074
-0.0024
4 1 3 46.0820 46.0820 46.0804
0.0016
0 0 4 54.1360 54.1360 54.1536
-0.0176
8 1 3 56.6860 56.6860 56.7099
-0.0239
12 2 0 62.2395 62.2395 62.2459
-0.0064
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0471
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0408
ANNEXE
CELREF Version 3. 14/06/2007 09:39:23
----------------------------------------------------------------------
C3 (LaCa2Mn2O7) à
1100°C
Initial values : (Refinement keys on 2nd line)
-------------- :
Zero Lambda a b c alpha
beta gamma volume
0.000 1.54060 5.7851 5.6766 19.3500 90.00 90.00
90.00 635.448
0 0 1 1 1 0 0
0
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
1 0 0 15.3700 15.3700 15.3036
0.0664
1 1 0 21.8940 21.8940 21.9189
-0.0249
0 0 6 27.5950 27.5950 27.6377
-0.0427
0 2 1 31.8380 31.8380 31.8405
-0.0025
0 2 2 32.7540 32.7540 32.8586
-0.1046
1 1 6 35.5430 35.5430 35.5496
-0.0066
1 0 8 40.3770 40.3770 40.3862
-0.0092
2 1 6 45.0360 45.0360 44.9896
0.0464
0 2 7 45.8530 45.8530 45.7824
0.0706
2 2 3 46.9690 46.9690 46.9742
-0.0052
1 3 3 52.7730 52.7730 52.8023
-0.0293
2 3 1 58.4220 58.4220 58.4296
-0.0076
2 3 2 59.1190 59.1190 59.0669
0.0521
1 1 12 61.9210 61.9210 61.8807
0.0403
0 2 12 66.6470 66.6470 66.6539
-0.0069
2 1 12 68.6170 68.6170 68.5967
0.0203
4 2 0 73.4184 73.4184 73.4206
-0.0022
1 2 13 73.6700 73.6700 73.6450
0.0250
1 3 11 75.5320 75.5320 75.5470
-0.0150
4 0 8 76.7990 76.7990 76.7143
0.0847
4 2 5 78.1180 78.1180 78.1057
0.0123
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0465
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0431
Final values : (Standard errors on 2nd line)
------------
Zero Lambda a b c
alpha beta gamma volume
0.000 1.54060 5.7813 5.6797 19.3435 90.00 90.00
90.00 635.163
0.0000 0.00000 0.0020 0.0024 0.0061 0.000 0.000
0.000 0.000
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
1 0 0 15.3700 15.3700 15.3136
0.0564
1 1 0 21.8940 21.8940 21.9199
-0.0259
0 0 6 27.5950 27.5950 27.6471
-0.0521
0 2 1 31.8380 31.8380 31.8235
0.0145
0 2 2 32.7540 32.7540 32.8428
-0.0888
ANNEXE
1 1 6 35.5430 35.5430 35.5579
-0.0149
1 0 8 40.3770 40.3770 40.4024
-0.0254
2 1 6 45.0360 45.0360 45.0076
0.0284
0 2 7 45.8530 45.8530 45.7781
0.0749
2 2 3 46.9690 46.9690 46.9778
-0.0088
1 3 3 52.7730 52.7730 52.7813
-0.0083
2 3 1 58.4220 58.4220 58.4182
0.0038
2 3 2 59.1190 59.1190 59.0560
0.0630
1 1 12 61.9210 61.9210 61.9011
0.0199
0 2 12 66.6470 66.6470 66.6631
-0.0161
2 1 12 68.6170 68.6170 68.6245
-0.0075
4 2 0 73.4184 73.4184 73.4554
-0.0370
1 2 13 73.6700 73.6700 73.6597
0.0103
1 3 11 75.5320 75.5320 75.5438
-0.0118
4 0 8 76.7990 76.7990 76.7659
0.0331
4 2 5 78.1180 78.1180 78.1429
-0.0249
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0409
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0379
ANNEXE
CELREF Version 3. 14/06/2007 09:27:53
----------------------------------------------------------------------
Phase secondaire
Initial values : (Refinement keys on 2nd line)
-------------- :
Zero Lambda a b c
alpha beta gamma volume
0.000 1.54060 11.6185 11.6185 7.3838 90.00 90.00
90.00 996.736
0 0 1 0 1 0 0
0
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
0 3 0 22.9940 22.9940 22.9451
0.0489
0 1 3 37.3490 37.3490 37.3155
0.0335
2 2 3 42.6200 42.6200 42.7965
-0.1765
3 5 0 45.5520 45.5520 45.4848
0.0672
0 5 3 54.1430 54.1430 54.2450
-0.1020
2 5 3 56.6740 56.6740 56.6909
-0.0169
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.1117
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0912
Final values : (Standard errors on 2nd line)
------------
Zero Lambda a b c
alpha beta gamma volume
0.000 1.54060 11.6117 11.6117 7.4009 90.00 90.00
90.00 997.883
0.0000 0.00000 0.0746 0.0000 0.0030 0.000 0.000
0.000 0.000
H K L 2Th(obs) 2Th_obs-shift 2Th(Calc)
diff.
0 3 0 22.9940 22.9940 22.9586
0.0354
0 1 3 37.3490 37.3490 37.2309
0.1181
2 2 3 42.6200 42.6200 42.7271
-0.1071
3 5 0 45.5520 45.5520 45.5128
0.0392
0 5 3 54.1430 54.1430 54.1992
-0.0562
2 5 3 56.6740 56.6740 56.6493
0.0247
Sqrt(Sum(2Th O-C)**2)/(Nref-Npar)) : 0.0894
Sqrt(Sum(2Th O-C)**2)/Nref ) : 0.0730
Références bibliographiques:
[1] : J.O.M bockris et A.K.M.S .huq,
proc.R soc .london ser .A, 237(1956)277.
[2] : Mona bahout [order cationique et
propriétés magnétiques dans les oxydes à structure
Ruddlesden-popper], Sujet de thèse de
doctorat.
[3] : L.Smart, E.Moore [introduction
à la chimie du solide]. Edition masson Paris, 1997.
[4] : S.Coste [Evolutions structurale et
microstructurale de précurseurs d'oxyde de tellure
élaborés par voie sol-gel], Suget de
thèse de doctorat (2003)
[5] :
[6] : D.Pletcher et F.C.Walsh
[industrial electrochemistry,Chapman and Hall, London, 1990].
[7] : N.Heller-ling, et coll
[Electrochim. Acta.42 (1997) 197].
[8] : M.tarasevich et coll
[Oxygéne electrochemistry, in comprehensive].
[9]: R.Guinebretiére [Diffraction des
rayons X sur échantillons polycristallins].
[10]: K.Boubendira et B.Rahel
[Caractérisation des materiaux par microscopie électronique et
microanalyse EDAX], mémoire de fin d'étude, université de
Jijel (2005).
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