176

REFERÊNCIAS [1] E. Giannini, R.Passerini, P. Tde, E. Walker, M. Lomello-Tafin,D. Sheptyankov, R. Flukiger. “Bi, Pb (2223) equilibrium and decomposition in situ high-temperature neutron difraction study” . Physica C 372 – 376 (2002) 895-898. [2] M.A. Neves, M.F. da Silveira, V. Soares. “Relevence of cooling rates on formation from the melt of superconducting bismuth-based cuprate phases”. Physica C 354(2001) 391-395. [3] A. Polasek, P. Majewski, E. T. Serra, F. Rizzo. “Insights into the phase relationships involved in the bi-2223 melting and crystallization regions”. Physica C 408-410 (2004) 860-861. [4] F. Ostermann & P. Pureur . “Supercondutividade”. Editora Livraria da Física, primeira edição, ano de 2005. [5] Retirado do site www.dcbs.joinville.udesc.br/pearson/cap12.pdf, visita dia 12 de julho de 2007. [6] Retirado do site www.superconductores.org, visita dia 3 de janeiro de 2007. [7] Retirado do site www.nature.com/nmat/journal, visita dia 25 de maio de 2007. [8] Adir Moysés Luiz. “Aplicações da Supercondutividade”.Editora Edgard Blucher LTDA, 1ªedição, ano de 1992. [9] William D. Callister, Jr. “Ciência e Engenharia de Materiais: Uma Introdução”. Ed. LTC. 5ª edição, ano de 2002. [10] Marcelo Azevedo Neves. “Sobre a influencia de taxas de resfriamento na formação por “Melt Processing” e nas propriedades de fases supercondutoras no sistema Bi-Sr-Ca-Cu-O” . Tese de Doutorado. CCMN IF 2000- UFRJ. [11] Peter Majewski. “Materials aspects of the high-temperature superconductors in the system Bi2O3-SrO-CaO-CuO”. J. Mater. Res. Vol.15, Nº4, Apr 2000. [12] Gomes Junior, G. G. “Automação do Difratômetro de Raios X para Policristais Philips PW 1850/25: uma contribuição para a otimização da análise de amostras de interesse Geológico”. Tese de dissertação, Instituto de geociências (Geologia) UFRJ, 2006. [13] P. Majewski. “Phase diagram studies in the system Bi-Pb-Sr-Ca-Cu-O-Ag”. Suprecond. Sci. Technol. 10 (1997) 453-467. Printed in the UK. [14] Giancarlo Cordeiro da Costa, “Estudo da levitação magnética e determinação da corrente crítica de blocos supercondutores de alta Tc pelo método dos elementos finitos”. Tese de doutoramento, junho/2005, COPPE/UFRJ. [15] W.D. Kingery, H.K. Bowen, D.R. Uhlmann. “Introduction to Ceramics”. Editora Wiley Interscience, 2ª edição, ano de 1975. [16] D.A . Porter and K.E. Easterling. “Phase Transformations in Metals and Alloys”. Ed. Chapman & Hall, 2ªedição, ano de 1980.

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[17] Sebastião Lauro Nau, et al. “On the melt processing of Bi-2223 high – Tc superconductor”. [18] Dursino, Eliana. “Desenvolvimento e caracterização de fitas monofilamentares de Ag/Bi2212 texturizadas pelo método de fusão parcial”. Faculdade de engenharia química de Lorena-Faenquil. Tese de Doutoramento defendida em Agosto de 2004. [19] Robert A . Hein Thomas L. Francavilla and Donald H. Lindenberg. “Magnetic Suceptibility of Superconductors and Other Spin Systems” . Ed. Plenum Publishing Corporation. 1ªedição, ano de 1991. [20] S.X. Dou, Y.C.Guo, R.K. Wang, M. Ionescu, H.K. Liu. “Effect of silver on phase formation and superconducting properties of Bi-2223/Ag Tapes”. IEEE transactions on applied superconductivity, vol.5,nº2,june 1995, (1830-1833). [21] C.C. e Faria, A.J. A. de Oliveira e W. A. Ortiz. “Estudo de Materiais pela Técnica de suscetibilidade Magnética AC”. Revista Brasileira de Ensino da Física, vol.22, nº3, Setembro, 2000. [22] H. London. “Alternating Current Losses in Superconductors of the second kind”. Physics Letter, vol.06, nº2, september,1963, (162-168). [23] Bispo, E. R.; Polasek, A.; Neves, M. A.; Rizzo, F. “Investigação sobre a decomposição e recristalização do supercondutor de alta temperatura (Bi, Pb)-2223”. Revista Matéria (Rio J.) Vol. 13, n°1, Rio de Janeiro, Jan./Mar.2008. [24] Programa de refinamento BRASS 2.0 (2006). Autores: J. Birkenstock, R. X. Fischer, Th. Messner. Training manual for an exemplary Rietveld Refinement. University of Bremen. [25] M. A. Neves e M. F. da Silveira, comunicação pessoal, Julho de 2008. [26] E. Giannini, I. Savysyuk, V. Garnier, R. Passerini, P. Toulemonde and Flukiger. “Reversible melting and equilibrium phase formation of (Bi, Pb)2Sr2Ca2Cu3O10+δ” . 2002 Supercond. Sci. Technol. 15 1577-1586 doi:10.1088/0953-2048/15/11/316. [27] http://www.webelements.com/webelements/compounds/text/Ag/Ag2O1-20667123.html (data de consulta: 14/12/2007) [28] http://www.webelements.com/webelements/compounds/text/Ag/Ag1O1-1301968.html (data de consulta: 14/12/2007). [29] http://www.webelements.com/webelements/elements/text/Pb/heat.html (data de consulta: 14/12/2007). [30] http://www.webelements.com/webelements/elements/text/Ag/heat.html (data de consulta: 14/12/2007). [31] Alexander Polasek, Xia Sike, Luis Antônio Saléh, Bojan Marinkovic, Fernando Rizzo, Eduardo Torres Serra. “Estudo da Fusão de Precursores do Supercondutor de alta temperatura Bi-2223”(em processo de submissão).

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[45] C. Park, W. Wg-Ng, L.P Cook, R.L. Snyder, P.V.P.S.S. Sastry, A.R. West, “Melting investigation of Bi2Sr1,9Ca2,1Cu3O10+x by high temperature X-ray diffraction quenching”. Physica C 304 (1998) 265-276. [46] Susana Petrick Casagrande, Ronald Castilho Blanco. “Método de Rietveld para el estudio de estruturas cristalinas” . Universidad Nacional de Ingenieria. [47] Bigansolli, Antonio Renato. “Avaliação da influencia dos perfis de tratamento térmico na píntese, orientação cristalográfica e texturização de Bi2Sr2CaCu2O8+ δ”. Faculdade de engenharia química de Lorena-Faenquil. Tese de Doutoramento defendida em Março de 2005. [48] Robert J. Cava. “Oxide Superconductors”. Centennial Feature Journal. J. Am. Ceram. Soc, 83 [1] 5 28 (200). [49] A. P. Malozemoff (American Supercondutor) and J. Bock (Nexans). “Technical Trend of superconducting and Electrical insulating Materials for power applications”. Working group SC D1.15- Materials Section – Supercondustors. [50] Winnie Wong-Ng, Lawrence P. Cook, Anthony Kearsley, Andrew Roosen. ”Roles of Melting equilibria in the processing of high Tc superconductors in the BSCCO system”. Physic C 335 (2000) 120-123. [51] Joachim Bock, Frank Breuer, Heibert Walter, Steffen Elschner, Martin Kleimaier, Ronald Kreutz, Mathias Noe. “CURL 10: Developmenet and Field-Test of a 10KV/10MVA resistive current limiter based on bulk MCP-BSCCO 2212”. [52] Hansen. “Constitution of binary alloys”. Second edition - McGraw-Hill Book Company (ano de 1958). [53] Andreas Nilsson, Wolfgang Gruner, Jorg Acker, Klaus Wetzig. “Cristical aspects on preparation of Bi-2223 glassy precursor by melt-process”. ScienceDirect (Article in press)-Journal of non-crystaline solids. Received August 2007. [54] I. H. Gul, F. Amin, et al. “Effect of Ag2CO3 addition on the morphology and physical proprieties of Bi-based (2223) high – Tc superconductors”. Physica C 449 (2006) 139-147. [55] H. Maeda, et al. “Texture development in Bi-Based superconductors grown in high magnetic fields fields and its effect on transformation of Bi(Pb)2212 to Bi(Pb)2223’. Physica C 354 (2001) 338-341. [56] Y. T. Huang, et al. “Phase evolution of co-precipited Bi-Pb-Sr-Ca-Cu-O powder”. Physica C 294 (1998) 140-146. [57] W. E. Pickett. “The next breakthough in phonon-mediated superconductivity”. Physica C 468 (2008) 126-135. [58] Jie Yang, et al. “Superconductivity at 53.5K in GdFeAsO1-δ”. Supercond. Sci. Technol. 21 (2008) 082001 (3pp). [59] U. R. Oliveira , et al. “Influência dos reforços mecânicos sobre as características supercondutoras e microestruturas de fitas supercondutoras de Bi-222/Ag”. 17° CBECIMAT, 15 a 19 de Novembro de 2006, Foz do Iguaçu, PR, Brasil.

180

ANEXOS

A.1. DIFRATOGRAMA DA LÂMINA DE VIDRO

A figura 131 é uma análise de DRX do vidro do porta amostras, isso confirma o

problema da linha de base que aparece durante as análises, acredita-se que isso seja

devido a pouca quantidade de material usado para fazer DRX.

Position [°2Theta]

10 20 30 40 50

Counts

0

100

400

900

Teste Vidro Porta Amostra

Figura 130. DRX da lamina de vidro usada como base para as misturas analisadas.

181

A.2. CARTAS DE REFERÊNCIA, USADAS PARA ANÁLISE DE DRX

A) Ag (Prata) Name and formula Reference code: 00-004-0783 Mineral name: Silver-3C, syn PDF index name: Silver Empirical formula: Ag Chemical formula: Ag Crystallographic parameters Crystal system: Cubic Space group: Fm-3m Space group number: 225 a (Å): 4,0862 b (Å): 4,0862 c (Å): 4,0862 Alpha (°): 90,0000 Beta (°): 90,0000 Gamma (°): 90,0000 Calculated density (g/cm^3): 10,50 Measured density (g/cm^3): 10,50 Volume of cell (10^6 pm^3): 68,23 Z: 4,00 RIR: 5,20 Subfiles and Quality Subfiles: Inorganic Mineral Alloy, metal or intermetalic Common Phase Educational pattern

182

Forensic NBS pattern Quality: Indexed (I) Comments Color: Light gray metallic General comments: Purity >99.999%. Opaque mineral optical data on specimen from

Great Bear Lake, Canada: RR2Re=94.1, Disp.=16, VHN100=55-63, Color values .314, .321, 94.2, Ref.: IMA

Commission on Ore Microscopy QDF.

Sample source: Sample obtained from Johnson Matthey Company, Ltd.

Analysis: Spectrographic analysis indicated faint traces of Ca, Fe and Cu.

Optical data: B=0.181 Additional pattern: See ICSD 64706 (PDF 87-597). Melting point: 960.6° Temperature: Pattern taken at 27 C. References Primary reference: Swanson, Tatge., Natl. Bur. Stand. (U.S.), Circ.

539, I, 23, (1953) Optical data: Winchell., Elements of Optical Mineralogy, II, 17 Peak list No. h k l d [A] 2Theta[deg] I [%]

1 1 1 1 2,35900 38,117 100,0

2 2 0 0 2,04400 44,279 40,0

3 2 2 0 1,44500 64,428 25,0

4 3 1 1 1,23100 77,475 26,0

5 2 2 2 1,17960 81,539 12,0

6 4 0 0 1,02150 97,891 4,0

7 3 3 1 0,93750 110,501 15,0

8 4 2 0 0,91370 114,928 12,0

9 4 2 2 0,83410 134,890 13,0

Stick Pattern

183

B) Bi-2201 rico em Cálcio Name and formula Reference code: 01-078-2019 ICSD name: Bismuth Strontium Calcium Copper Oxide Empirical formula: Bi2Ca0.4CuO6Sr1.6 Chemical formula: Bi2 ( Sr1.6Ca0.4 ) CuO6 Crystallographic parameters Crystal system: Orthorhombic Space group: Bbmb Space group number: 66 a (Å): 5,3826 b (Å): 5,3761 c (Å): 24,3840 Alpha (°): 90,0000 Beta (°): 90,0000

184

Gamma (°): 90,0000 Calculated density (g/cm^3): 6,91 Volume of cell (10^6 pm^3): 705,61 Z: 4,00 RIR: 5,44 Subfiles and Quality Subfiles: Inorganic Corrosion Superconducting Material ICSD Pattern Quality: Calculated (C) Comments ICSD collection code: 063216 Test from ICSD: At least one TF missing. References Primary reference: Calculated from ICSD using POWD-12++, (1997) Structure: Imai, K., Nakai, I., Kawashima, T., Sueno, S.,

Ono, A., Jpn. J. Appl. Phys. Part 2, 27, L1661, (1988)

Peak list No. h k l d [A] 2Theta[deg] I [%]

1 0 0 2 12,19200 7,245 34,5

2 0 0 4 6,09600 14,519 1,1

3 1 0 1 5,25607 16,855 3,7

4 1 0 3 4,48776 19,767 0,9

5 0 0 6 4,06400 21,852 19,9

6 1 1 1 3,75832 23,654 9,5

7 1 0 5 3,61404 24,613 0,3

8 1 1 3 3,44517 25,840 96,6

9 0 0 8 3,04800 29,277 25,6

10 1 1 5 2,99932 29,763 100,0

11 1 0 7 2,92444 30,544 2,1

12 2 0 0 2,69130 33,263 66,1

13 2 0 2 2,62803 34,088 5,1

14 1 1 7 2,56895 34,897 10,9

185

15 2 0 4 2,46204 36,465 0,3

16 0 0 10 2,43840 36,831 4,0

17 1 0 9 2,42005 37,120 0,3

18 1 2 1 2,39323 37,552 0,3

19 2 1 2 2,36103 38,083 1,3

20 1 2 3 2,30603 39,028 0,3

21 2 0 6 2,24388 40,155 4,1

22 2 1 4 2,23847 40,256 5,4

23 1 1 9 2,20677 40,860 1,0

24 1 2 5 2,15686 41,849 0,2

25 2 1 6 2,07075 43,677 1,3

26 1 0 11 2,04971 44,149 0,1

27 0 0 12 2,03200 44,554 2,7

28 2 0 8 2,01742 44,893 23,3

29 1 2 7 1,97904 45,813 0,3

30 1 1 11 1,91523 47,431 22,6

31 2 2 0 1,90189 47,785 22,6

32 2 2 4 1,81558 50,209 0,3

33 2 0 10 1,80702 50,464 1,6

34 3 0 1 1,78936 50,997 1,2

35 1 0 13 1,77123 51,557 0,1

36 3 0 3 1,75202 52,165 0,4

37 0 0 14 1,74171 52,497 0,7

38 2 2 6 1,72259 53,125 1,6

39 2 1 10 1,71285 53,451 0,9

40 3 1 1 1,69779 53,964 0,3

41 3 0 5 1,68228 54,502 9,0

42 3 1 3 1,66580 55,087 7,3

43 2 0 12 1,62168 56,719 2,1

44 2 2 8 1,61354 57,031 6,0

45 3 1 5 1,60688 57,289 12,8

46 3 0 7 1,59505 57,754 1,2

47 1 0 15 1,55618 59,339 0,1

48 2 1 12 1,55258 59,490 0,4

49 3 1 7 1,52798 60,547 2,8

50 0 0 16 1,52400 60,722 3,2

51 2 2 10 1,49966 61,814 1,0

52 3 0 9 1,49592 61,986 1,2

53 3 2 1 1,48952 62,282 0,6

54 2 3 2 1,48058 62,701 0,1

55 3 2 3 1,46778 63,310 0,2

56 2 0 14 1,46222 63,579 0,9

57 2 3 4 1,44887 64,235 0,1

58 3 1 9 1,44117 64,620 0,2

59 3 2 5 1,42699 65,341 0,1

60 2 1 14 1,41096 66,178 0,1

61 2 3 6 1,40028 66,748 0,1

186

62 2 2 12 1,38856 67,387 1,3

63 1 0 17 1,38599 67,528 0,7

64 3 2 7 1,37173 68,327 0,6

65 3 1 11 1,34994 69,587 4,8

66 1 2 15 1,34565 69,841 5,0

67 1 1 17 1,34210 70,052 2,8

68 0 4 2 1,33593 70,424 0,3

69 2 0 16 1,32614 71,022 2,4

70 0 4 4 1,31250 71,874 0,1

71 3 2 9 1,30714 72,215 0,2

72 4 1 2 1,29796 72,807 0,6

73 2 1 16 1,28755 73,492 0,1

74 2 2 14 1,28448 73,697 0,1

75 4 1 4 1,27644 74,238 1,1

76 2 3 10 1,27242 74,513 0,6

77 3 1 13 1,26041 75,345 2,4

78 3 3 3 1,25277 75,886 0,4

79 4 1 6 1,24284 76,602 0,5

80 1 2 17 1,23102 77,473 1,5

81 3 3 5 1,22713 77,765 1,6

82 0 0 20 1,21920 78,367 0,2

83 1 1 19 1,21602 78,612 0,8

84 2 0 18 1,21002 79,078 0,1

85 4 2 0 1,20329 79,608 2,4

86 4 1 8 1,19996 79,873 1,3

87 2 4 2 1,19662 80,141 0,1

88 3 3 7 1,19145 80,560 0,7

89 2 2 16 1,18928 80,737 1,5

90 2 1 18 1,18049 81,465 0,1

91 4 0 10 1,17815 81,661 0,2

92 3 1 15 1,17553 81,882 0,3

93 3 2 13 1,16780 82,541 0,1

94 4 2 6 1,15378 83,769 0,1

95 4 1 10 1,15084 84,032 0,5

96 3 3 9 1,14839 84,252 0,3

97 1 0 21 1,13503 85,478 0,1

98 2 3 14 1,13293 85,675 0,1

99 4 0 12 1,12194 86,720 0,4

100 4 2 8 1,11923 86,982 1,6

101 1 1 21 1,11055 87,835 1,0

102 0 0 22 1,10836 88,053 0,6

103 3 3 11 1,10061 88,835 0,5

104 4 1 12 1,09828 89,074 0,5

105 3 1 17 1,09679 89,227 0,4

Stick Pattern

187

C) Bi-2201: Name and formula Reference code: 00-045-0214 PDF index name: Copper Strontium Bismuth Oxide Chemical formula: Bi2.125Sr1.875Cu1.031Oz Crystallographic parameters Crystal system: Tetragonal a (Å): 5,3850 b (Å): 5,3850 c (Å): 24,6300 Alpha (°): 90,0000 Beta (°): 90,0000 Gamma (°): 90,0000 Volume of cell (10^6 pm^3): 714,23

188

RIR: - Subfiles and Quality Subfiles: Inorganic Corrosion Superconducting Material Quality: Indexed (I) Comments General comments: The diffraction data showed a pseudotetragonal

cell and a 1-dimensional structural modulation. Zero resistance at ~8 K. Sample preparation: Prepared from a mixture of 99.5% pure Bi2O3 ,

SrCO3 and CuO fired in air from 700-1000 C for 48-150 hours with intermittent mixing, grinding and pelletizing.

Additional pattern: To replace 42-241. References Primary reference: Ikeda, Y., Ito, H., Shimomura, S., Oue, Y., Inaba,

K., Hiroi, Z., Takano, M., Physica C: Superconductivity, 159, 93, (1989)

Peak list No. h k l d [A] 2Theta[deg] I [%]

1 0 0 2 12,41000 7,117 15,0

2 0 0 4 6,17000 14,344 3,0

3 1 0 1 5,28000 16,778 6,0

4 1 0 3 4,50200 19,704 3,0

5 0 0 6 4,11000 21,605 58,0

6 1 1 1 3,76600 23,605 5,0

7 1 1 3 3,45500 25,765 58,0

8 0 0 8 3,08000 28,967 100,0

9 1 1 5 3,01300 29,625 92,0

10 2 0 0 2,69300 33,242 42,0

11 2 0 2 2,63000 34,062 5,0

12 1 1 7 2,58400 34,687 9,0

13 0 0 10 2,46300 36,450 19,0

14 1 0 9 2,44100 36,790 6,0

15 2 0 6 2,24800 40,078 5,0

16 1 0 11 2,06700 43,760 6,0

189

17 0 0 12 2,05200 44,097 10,0

18 2 0 8 2,02700 44,670 26,0

19 1 1 11 1,93000 47,046 22,0

20 2 2 0 1,90300 47,755 16,0

Stick Pattern

D) (Bi, Pb)-2223 Name and formula Reference code: 00-049-0616 PDF index name: Copper Calcium Lead Strontium Bismuth Oxide Empirical formula: Bi1.24Ca1.91Cu3O8.68Pb0.52Sr1.83 Chemical formula: Bi1.24Pb0.52Sr1.83Ca1.91Cu3O8.68 Crystallographic parameters

190

Crystal system: Orthorhombic Space group: A2aa Space group number: 37 a (Å): 5,4084 b (Å): 5,4209 c (Å): 37,0750 Alpha (°): 90,0000 Beta (°): 90,0000 Gamma (°): 90,0000 Volume of cell (10^6 pm^3): 1086,98 RIR: - Subfiles and Quality Subfiles: Inorganic Corrosion Superconducting Material Quality: Indexed (I) Comments General comments: These reflections are from a modulated structure. Sample preparation: Prepared by a mixture of Bi2O3 , Pb3O4 , SrCO3 ,

CaCO3 and CuO (molar composition Bi:Pb:Sr:Ca:Cu = 1.7:0.3:2.0:2.0:3.0) was calcined at 838 C for 45 hours, pelletized and sintered at 856 C for 50 hours, ground, pressed and again sintered at 858 C for 120 hours.

References Primary reference: Li, D., MacKinnon, C., Powder Diffraction, 12,

141, (1997) Peak list No. h k l d [A] 2Theta[deg] I [%]

1 0 0 2 18,60000 4,747 27,0

2 0 0 4 9,29000 9,513 2,0

3 0 1 1 5,37000 16,494 2,0

4 0 1 3 4,95400 17,890 3,0

191

5 0 0 8 4,64200 19,104 6,0

6 1 1 1 3,80700 23,347 7,0

7 0 0 10 3,71300 23,947 65,0

8 1 1 3 3,65700 24,319 15,0

9 1 1 5 3,40200 26,173 51,0

10 0 1 9 3,27600 27,199 10,0

11 3,20600 27,805 9,0

12 1 1 7 3,09900 28,785 100,0

13 3,04000 29,356 3,0

14 1 1 9 2,80400 31,890 48,0

15 2 0 0 2,70500 33,090 77,0

16 0 0 14 2,64800 33,824 52,0

17 1 1 11 2,53000 35,452 38,0

18 0 0 16 2,31700 38,836 4,0

19 1 1 13 2,28600 39,384 5,0

20 2,21200 40,759 8,0

21 2 0 10 2,18200 41,345 5,0

22 2,11100 42,803 1,0

23 0 0 18 2,05900 43,939 4,0

24 2 0 12 2,03500 44,485 31,0

25 2,01200 45,021 3,0

26 2 2 0 1,91200 47,516 39,0

27 2 0 14 1,89300 48,023 30,0

28 0 0 20 1,85600 49,043 6,0

29 0 3 1 1,80700 50,464 1,0

30 1 1 19 1,73800 52,618 16,0

31 1 3 3 1,69700 53,991 4,0

32 3 1 5 1,66600 55,080 7,0

33 2 0 18 1,63900 56,066 3,0

34 3 1 7 1,62700 56,517 16,0

35 1 1 21 1,60300 57,441 5,0

36 3 1 9 1,58000 58,357 8,0

37 0 0 24 1,54500 59,812 9,0

38 1 3 11 1,52600 60,634 11,0

39 2 1 19 1,52000 60,899 3,0

40 0 0 26 1,42400 65,495 2,0

41 1,40000 66,763 1,0

42 0 4 2 1,35100 69,524 7,0

43 0 2 24 1,34100 70,118 10,0

44 2 2 20 1,33200 70,663 2,0

45 1,25600 75,656 3,0

46 4 0 12 1,23900 76,882 3,0

47 1,21700 78,536 2,0

48 2 2 24 1,20200 79,710 6,0

49 4 1 13 1,19200 80,515 2,0

50 1 1 33 1,07800 91,215 4,0

51 0 2 32 1,06600 92,540 2,0

192

52 2 4 18 1,04400 95,095 1,0

53 4 2 20 1,01300 99,002 2,0

54 0,93800 110,413 2,0

Stick Pattern

A) (Bi, Pb)-2223

Name and formula Reference code: 00-041-0374 PDF index name: Calcium Copper Strontium Bismuth Lead Oxide Empirical formula: Bi1.9Ca1.98Cu3O10Pb0.13Sr1.98

Chemical formula: Bi1.9Pb0.13Sr1.98Ca1.98Cu3O10

Crystallographic parameters Crystal system: Orthorhombic Space group: Bbmb Space group number: 66 a (Å): 5,4101

193

b (Å): 5,4101 c (Å): 37,1293 Alpha (°): 90,0000 Beta (°): 90,0000 Gamma (°): 90,0000 Volume of cell (10^6 pm^3): 1086,74 RIR: - Subfiles and Quality Subfiles: Inorganic Corrosion Superconducting Material Quality: Star (S) Comments Color: Black General comments: Reflections calculated from cell parameters given in

reference. Pattern is from highly oriented sample, plane parallel to

001. References Primary reference: Nakahigashi, K., Sasakura, H., University of Osaka

Prefecture, Osaka, Japan., Private Communication, (1990) Contributed: Nakahigashi, K., Japan., Private Communication Sample preparation: Sasakura, H., Minamigawa, S., Nakahigashi, K., Kogachi,

M., Nakanishi, S., Fukuoka, N., Yoshikawa, M., Noguchi, S., Okuda, K., Yanase, A., Jpn. J. Appl. Phys. Part 2, 28, L1163, (1989)

Peak list No. h k l d [A] 2Theta[deg] I [%]

1 0 0 2 18,56470 4,756 75,0

2 0 0 4 9,28230 9,520 4,0

3 0 0 6 6,18820 14,301 1,0

4 0 0 8 4,64120 19,107 12,0

5 1 1 1 3,80540 23,357 3,0

6 0 0 10 3,71290 23,948 100,0

7 1 1 3 3,65490 24,334 4,0

8 1 1 5 3,40080 26,183 35,0

9 1 1 7 3,10270 28,750 61,0

10 0 0 12 3,09410 28,832 46,0

11 1 1 9 2,80510 31,877 38,0

12 2 0 0 2,70500 33,090 23,0

13 2 0 2 2,67680 33,449 4,0

14 0 0 14 2,65210 33,770 65,0

15 1 1 11 2,53100 35,438 33,0

16 2 0 8 2,33710 38,489 1,0

194

17 1 1 13 2,28860 39,337 4,0

18 1 1 15 2,07820 43,512 2,0

19 0 0 18 2,06270 43,856 6,0

20 2 0 12 2,03650 44,450 10,0

21 2 2 0 1,91280 47,495 31,0

22 2 2 2 1,90270 47,763 1,0

23 1 1 17 1,89670 47,923 12,0

24 2 0 14 1,89380 48,001 5,0

25 0 0 20 1,85650 49,029 11,0

26 2 2 8 1,76850 51,643 2,0

27 1 1 19 1,74030 52,543 22,0

28 2 2 10 1,70040 53,874 7,0

29 1 3 3 1,69470 54,070 1,0

30 1 3 5 1,66720 55,037 3,0

31 2 0 18 1,64030 56,018 1,0

32 3 1 7 1,62820 56,471 8,0

33 2 2 12 1,62700 56,517 4,0

34 1 1 21 1,60490 57,367 2,0

35 1 3 9 1,58030 58,345 5,0

36 2 2 14 1,55140 59,540 9,0

37 0 0 24 1,54710 59,722 28,0

38 2 0 20 1,53070 60,428 1,0

39 3 1 11 1,52600 60,634 4,0

40 0 0 26 1,42810 65,284 4,0

41 1 3 15 1,40740 66,367 1,0

42 2 2 18 1,40260 66,624 1,0

43 1 1 25 1,38450 67,611 1,0

44 4 0 0 1,35250 69,436 5,0

Stick Pattern

195

F) Bi-2212 Name and formula Reference code: 00-046-0431 Common name: Bi-2212 phase PDF index name: Calcium Copper Strontium Bismuth Oxide Empirical formula: Bi2.1CaCu2O8.21Sr1.9 Chemical formula: Bi2.1Sr1.9CaCu2O8.21 Crystallographic parameters Crystal system: Orthorhombic Space group: A2aa Space group number: 37 a (Å): 5,4032 b (Å): 5,4032 c (Å): 30,7670 Alpha (°): 90,0000

196

Beta (°): 90,0000 Gamma (°): 90,0000 Calculated density (g/cm^3): 6,68 Volume of cell (10^6 pm^3): 898,23 Z: 4,00 RIR: - Subfiles and Quality Subfiles: Inorganic Corrosion Quality: Star (S) Comments Color: Black General comments: The phase has incommensurately modulated

structure. Cell parameters were refined in the pseudotetragonal symmetry with satellites included in the refinement.

The phase exhibits superconducting transition at 81 K.

Sample source: The sample was provided by Fomitchev, A., Moscow State Univ., Russia.

Sample preparation: The sample was prepared by solid state reaction of stoichiometric mixture of Bi2O3 , SrCO3 , CaCO3 and CuO by annealing in air at 830 C for 50 hours.

Temperature: Pattern taken at 20 C. References Primary reference: Mironov, A., Antipov, E., Moscow State Univ.,

Russia., ICDD Grant-in-Aid, (1994) Peak list No. h k l d [A] 2Theta[deg] I [%]

1 0 0 8 3,84589 23,108 100,0

2 1 1 1 3,79296 23,435 3,0

3 1 1 3 3,57854 24,861 29,0

4 3,35795 26,523 1,0

5 1 1 5 3,24488 27,465 81,0

197

6 3,13938 28,407 3,0

7 0 0 10 3,07548 29,010 92,0

8 3,00459 29,710 4,0

9 1 1 7 2,88353 30,988 89,0

10 2,85079 31,353 7,0

11 0 2 0 2,70096 33,141 57,0

12 0 2 2 2,65949 33,673 4,0

13 0 0 12 2,56235 34,990 56,0

14 0 2 4 2,54810 35,192 27,0

15 2,43640 36,862 8,0

16 2 1 1 2,40854 37,304 1,0

17 0 2 6 2,38965 37,610 1,0

18 2,35878 38,121 2,0

19 1 2 4 2,30331 39,076 1,0

20 1 1 11 2,25724 39,907 1,0

21 0 2 8 2,21101 40,778 4,0

22 0 0 14 2,19837 41,023 1,0

23 1 2 6 2,18614 41,263 1,0

24 2,13684 42,260 1,0

25 2,11329 42,754 1,0

26 2,05749 43,973 3,0

27 0 2 10 2,02975 44,606 45,0

28 1 1 13 2,01056 45,055 18,0

29 1,98870 45,578 3,0

30 0 0 16 1,92342 47,217 10,0

31 2 2 0 1,91053 47,555 29,0

32 0 2 12 1,85855 48,971 18,0

33 1,83939 49,515 3,0

34 1 1 15 1,80731 50,455 43,0

35 0 3 1 1,79703 50,764 3,0

36 1,77544 51,426 3,0

37 1,71908 53,242 1,0

38 2 2 8 1,71131 53,503 6,0

39 1 3 3 1,68439 54,428 4,0

40 1,67434 54,782 1,0

41 1 3 5 1,64602 55,806 18,0

42 1 1 17 1,63493 56,218 15,0

43 2 2 10 1,62317 56,662 10,0

44 1,60177 57,489 4,0

45 1 3 7 1,59241 57,859 19,0

46 1,58441 58,179 5,0

47 1,57331 58,629 7,0

48 0 2 16 1,56636 58,915 7,0

49 0 0 20 1,53774 60,123 20,0

50 1,53080 60,424 12,0

51 1 3 9 1,52755 60,566 5,0

52 2 3 1 1,49729 61,923 1,0

198

53 1 3 11 1,45865 63,753 1,0

54 0 2 18 1,44443 64,456 2,0

55 1,42453 65,468 1,0

56 1,40487 66,502 1,0

57 0 0 22 1,39865 66,836 3,0

58 1 3 13 1,38518 67,573 5,0

59 1 1 21 1,36738 68,574 4,0

60 1,35638 69,209 3,0

61 0 4 0 1,35068 69,543 9,0

62 0 2 20 1,33631 70,401 11,0

63 1,31857 71,492 1,0

64 1 3 15 1,31267 71,863 6,0

65 1 2 20 1,29765 72,827 2,0

66 1 4 4 1,29234 73,175 1,0

67 0 4 8 1,27436 74,380 2,0

68 1 1 23 1,26198 75,235 4,0

69 3 3 5 1,24715 76,289 2,0

70 0 2 22 1,24193 76,668 6,0

71 0 4 10 1,23627 77,083 2,0

72 1,23250 77,363 2,0

73 1,22726 77,755 1,0

74 3 3 7 1,22300 78,077 4,0

75 1,21488 78,700 2,0

76 2 4 0 1,20790 79,244 10,0

77 2 2 20 1,19807 80,024 8,0

78 0 4 12 1,19476 80,291 6,0

79 0 0 26 1,18323 81,236 3,0

80 2 4 6 1,17623 81,822 1,0

81 1 1 25 1,17140 82,233 3,0

82 1,16764 82,555 1,0

83 3 3 11 1,15864 83,339 3,0

84 2 4 10 1,12494 86,432 5,0

85 1,11778 87,123 3,0

86 1 3 21 1,11222 87,669 6,0

87 0 0 28 1,09910 88,990 3,0

88 1 1 27 1,09185 89,740 7,0

Stick Pattern

199

G) Ca2PbO4 Name and formula Reference code: 00-046-0334 PDF index name: Calcium Lead Oxide Empirical formula: Ca2O4Pb

Chemical formula: Ca2PbO4

Crystallographic parameters Crystal system: Orthorhombic Space group: Pbam Space group number: 55 a (Å): 5,8407 b (Å): 9,7534 c (Å): 3,3820 Alpha (°): 90,0000 Beta (°): 90,0000 Gamma (°): 90,0000 Calculated density (g/cm^3): 6,06

200

Volume of cell (10^6 pm^3): 192,66 Z: 2,00 RIR: - Subfiles and Quality Subfiles: Inorganic Corrosion Superconducting Material Quality: Star (S) Comments Color: Yellow General comments: Average relative standard deviation in intensity of the ten

strongest reflections for three specimen mounts = 2.2%. Unit cell refined on 54 of 69 reflections. Trace lime (CaO) present in sample. Validated by a calculated pattern, with structure data from

Tromel, M., Z. Anorg. Allg. Chem., 371 237 (1969). Sample preparation: Sample prepared by firing CaCO3 and PbO in a 2:1 molar

ratio, with a slight excess of PbO, for 48 hours at 800 C. Additional pattern: To replace 24-207. References Primary reference: Scheer, M., Grier, D., McCarthy, G., North Dakota State

Univ., Fargo, ND, USA., ICDD Grant-in-Aid, (1994) Peak list No. h k l d [A] 2Theta[deg] I [%]

1 1 1 0 5,01100 17,685 100,0

2 0 2 0 4,87800 18,172 28,0

3 1 2 0 3,74400 23,746 1,0

4 0 0 1 3,38200 26,331 7,0

5 2 0 0 2,92000 30,591 19,0

6 1 3 0 2,84100 31,464 50,0

7 1 1 1 2,80300 31,902 77,0

8 0 2 1 2,77900 32,185 30,0

9 2 2 0 2,50500 35,818 10,0

10 0 4 0 2,43800 36,837 10,0

11 1 4 0 2,25000 40,041 3,0

12 2 0 1 2,21100 40,778 9,0

13 1 3 1 2,17500 41,484 7,0

14 2 1 1 2,15600 41,867 5,0

15 2 2 1 2,01300 44,997 30,0

16 0 4 1 1,97800 45,839 9,0

17 3 1 0 1,90930 47,588 6,0

18 2 4 0 1,87200 48,596 7,0

19 1 5 0 1,85040 49,201 4,0

20 2 3 1 1,82830 49,836 1,0

21 3 2 0 1,80820 50,428 1,0

201

22 0 0 2 1,69110 54,195 7,0

23 3 3 0 1,67020 54,929 7,0

24 3 1 1 1,66270 55,198 10,0

25 2 4 1 1,63760 56,118 10,0

26 1 5 1 1,62370 56,642 18,0

27 1 1 2 1,60230 57,468 7,0

28 0 2 2 1,59790 57,641 6,0

29 3 4 0 1,52180 60,819 1,0

30 3 3 1 1,49770 61,904 6,0

31 0 6 1 1,46490 63,449 4,0

32 2 0 2 1,46330 63,527 5,0

33 4 0 0 1,46020 63,678 4,0

34 1 3 2 1,45300 64,030 9,0

35 2 1 2 1,44730 64,313 2,0

36 4 1 0 1,44400 64,478 1,0

37 2 6 0 1,42050 65,677 4,0

38 2 2 2 1,40150 66,683 4,0

39 4 2 0 1,39870 66,834 5,0

40 0 4 2 1,38950 67,335 3,0

41 3 5 0 1,37800 67,973 1,0

42 1 7 0 1,35530 69,272 2,0

43 1 4 2 1,35210 69,460 2,0

44 4 0 1 1,34040 70,154 1,0

45 4 1 1 1,32780 70,920 1,0

46 2 6 1 1,30960 72,058 2,0

47 4 2 1 1,29260 73,158 2,0

48 3 5 1 1,27620 74,255 3,0

49 3 1 2 1,26590 74,962 2,0

50 1 7 1 1,25800 75,515 3,0

51 2 4 2 1,25460 75,756 4,0

52 4 4 0 1,25320 75,855 3,0

53 1 5 2 1,24820 76,214 3,0

54 3 2 2 1,23500 77,177 1,0

55 0 8 0 1,21880 78,398 1,0

56 3 3 2 1,18820 80,826 3,0

57 4 4 1 1,17450 81,969 2,0

58 0 6 2 1,17180 82,198 3,0

59 5 1 0 1,15980 83,237 1,0

60 0 8 1 1,14700 84,378 2,0

61 3 7 0 1,13310 85,659 1,0

62 2 8 0 1,12490 86,435 1,0

63 4 0 2 1,10510 88,380 1,0

64 1 1 3 1,09970 88,928 3,0

65 0 2 3 1,09860 89,041 3,0

66 5 1 1 1,09730 89,175 3,0

Stick Pattern

202

A.3. CARTAS COM AS ORIENTAÇÕES CRISTALOGRÁFICAS USADAS PARA ANÁLISE DE RIETVELD

A) FASE 2223 data_91970-ICSD #©2007 by Fachinformationszentrum Karlsruhe, and the U.S. Secretary of #Commerce on behalf of the United States. All rights reserved. _database_code_ICSD 91970 _audit_creation_date 2002/10/01 _chemical_name_systematic ; Bismuth Lead Strontium Calcium Copper Oxide (2/0.3/2/1.7/3/10) ; _chemical_formula_structural ; (Bi1.7 Pb0.3) Sr2 (Ca1.7 Bi0.3) Cu3 O10 ; _cell_length_a 5.402(1) _cell_length_b 5.419(1) _cell_length_c 36.9570(80) _cell_angle_alpha 90. _cell_angle_beta 90. _cell_angle_gamma 90. _cell_volume 1081.86 _cell_formula_units_Z 4 _symmetry_space_group_name_H-M 'A 2 a a' _symmetry_Int_Tables_number 37

203

_symmetry_cell_setting orthorhombic Bi1 Bi3+ 8 d 0.044(7) 0.209(7) 0.0428(6) 0.85 0 1.9 Pb1 Pb2+ 8 d 0.044(7) 0.209(7) 0.0428(6) 0.15 0 1.9 Sr1 Sr2+ 8 d 0.5 0.25 0.1156(6) 1. 0 0.9 Cu1 Cu2+ 8 d 0 0.25 0.1604(3) 1. 0 0.9 Ca1 Ca2+ 8 d 0.5 0.25 0.2078(8) 0.85 0 0.9 Bi2 Bi3+ 8 d 0.5 0.25 0.2078(8) 0.15 0 0.9 Cu2 Cu2+ 4 c 0 0.25 0.25 1. 0 0.9 O1 O2- 8 d 0.25 0 0.2598(10) 1. 0 0.9 O2 O2- 8 d 0.25 0 0.1610(5) 1. 0 0.9 O3 O2- 8 d 0.25 0.5 0.1620(5) 1. 0 0.9 O4 O2- 8 d 0 0.25 0.0949(7) 1. 0 0.9 O5 O2- 8 d 0.488(15) 0.176(7) 0.0422(12) 1. 0 1.9

B) FASE 2212 data_65862-ICSD #©2007 by Fachinformationszentrum Karlsruhe, and the U.S. Secretary of #Commerce on behalf of the United States. All rights reserved. _database_code_ICSD 65862 _audit_creation_date 1990/12/27 _chemical_name_systematic ; Bismuth Calcium Strontium Copper Oxide (2/1/2/2/9.1) ; _chemical_formula_structural 'Bi2 Ca Sr2 Cu2 O9.07' _chemical_formula_sum 'Bi2 Ca1 Cu2 O9.07 Sr2' _publ_section_title ; On the coordination of bismuth in Bi2 Ca Sr2 Cu2 O8 - A2aa/Amaa structures revisited _cell_length_a 5.423(5) _cell_length_b 5.376(5) _cell_length_c 30.72(1) _cell_angle_alpha 90. _cell_angle_beta 90. _cell_angle_gamma 90. _cell_volume 895.61 _cell_formula_units_Z 4 _symmetry_space_group_name_H-M 'A m a a' _symmetry_Int_Tables_number 66 _refine_ls_R_factor_all 0.0322 Bi1 Bi3+ 8 l 0 0.238(4) 0.4463(5) 1. 0 5.2(3) Sr1 Sr2+ 8 l 0 0.750(5) 0.3578(8) 1. 0 2.9(4) Ca1 Ca2+ 4 f 0 0.75 0.25 1. 0 0.3(3) Cu1 Cu3+ 8 l 0 0.250(5) 0.3017(4) 1. 0 4.1(4) O1 O2- 8 h 0.25 0 0.3199(7) 1. 0 2.0(3) O2 O2- 8 h 0.25 0.5 0.2915(7) 1. 0 2.0(3) O3 O2- 8 l 0 0.59 0.451 1. 0 24.90(14)

204

O4 O2- 16 m 0.146 0.832 0.428 0.344 0 24.90(14) O5 O2- 8 l 0 0.367(6) 0.380(6) 0.85 0 4.5(9) #End of data_65862-ICSD

C) FASE 2201 SEM Pb data_67426-ICSD #©2007 by Fachinformationszentrum Karlsruhe, and the U.S. Secretary of #Commerce on behalf of the United States. All rights reserved. _database_code_ICSD 67426 _audit_creation_date 1991/07/10 _chemical_name_systematic ; Dibismuth Distrontium Copper Hexaoxide ; _chemical_formula_structural 'Bi2 Sr2 Cu O6' _chemical_formula_sum 'Bi2 Cu1 O6 Sr2' _publ_section_title ; Structures of the superconducting oxides Tl2Ba2CuO6 and Bi2Sr2CuO6 _cell_length_a 5.362(3) _cell_length_b 5.374(1) _cell_length_c 24.622(6) _cell_angle_alpha 90. _cell_angle_beta 90. _cell_angle_gamma 90. _cell_volume 709.49 _cell_formula_units_Z 4 _symmetry_space_group_name_H-M 'A m a a' _symmetry_Int_Tables_number 66 _refine_ls_R_factor_all 0.13 Bi1 Bi3+ 8 l 0 0.2758(5) 0.0660(2) 1. 0 0 Sr1 Sr2+ 8 l 0.5 0.2479(9) 0.1790(4) 1. 0 0 Cu1 Cu2+ 4 e 0.5 0.75 0.25 1. 0 0 O1 O2- 8 h 0.75 0.5 0.246(2) 1. 0 0.5(6) O2 O2- 8 l 0 0.226(12) 0.145(4) 1. 0 8.60(26) O3 O2- 8 l 0.5 0.334(15) 0.064(5) 1. 0 9.30(25) loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_B_11 _atom_site_aniso_B_22 _atom_site_aniso_B_33 _atom_site_aniso_B_12 _atom_site_aniso_B_13 _atom_site_aniso_B_23

205

Bi1 Bi3+ 10.1(3) 1.5(1) 6.1(3) 0.4(1) -5.1(1) -.5(1) Sr1 Sr2+ 0.7(2) 0.5(2) 7.2(6) 0 0 -.2(3) Cu1 Cu2+ 1.7(5) 0.3(4) 11.00(15) 0 0 0.1(5)

D) 2201 com Pb data_50340-ICSD #©2007 by Fachinformationszentrum Karlsruhe, and the U.S. Secretary of #Commerce on behalf of the United States. All rights reserved. _database_code_ICSD 50340 _audit_creation_date 1999/11/30 _audit_update_record 2006/04/01 _chemical_name_systematic ; Bismuth Strontium Lead Copper Oxide (1.82/1.84/0.3/0.34/1/6) ; _chemical_formula_structural ; (Bi1.86 Pb0.14) (Sr1.84 Pb0.16) Cu O6 ; _chemical_formula_sum 'Bi1.86 Cu1 O6 Pb0.3 Sr1.84' _publ_section_title _cell_length_a 5.392(3) _cell_length_b 24.603(5) _cell_length_c 5.300(3) _cell_angle_alpha 90. _cell_angle_beta 90. _cell_angle_gamma 90. _cell_volume 703.09 _cell_formula_units_Z 4 _symmetry_space_group_name_H-M 'C c c m' _symmetry_Int_Tables_number 66 _refine_ls_R_factor_all 0.048 Bi1 Bi3+ 8 l 0.2682(1) 0.06340(4) 0 0.93 0 Pb1 Pb2+ 8 l 0.2682(1) 0.06340(4) 0 0.07 0 Sr1 Sr2+ 8 l 0.2473(3) 0.1776(1) 0.5 0.92(2) 0 Pb2 Pb2+ 8 l 0.2473(3) 0.1776(1) 0.5 0.08(2) 0 Cu1 Cu2.14+ 4 e 0.75 0.25 0.5 1. 0 O1 O2- 8 h 0.5 0.2512(6) 0.75 1. 0 O2 O2- 8 l 0.227(3) 0.144(1) 0 1. 0 O3 O2- 16 m 0.347(5) 0.070(1) 0.394(5) 0.5 0 loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12

206

_atom_site_aniso_U_13 _atom_site_aniso_U_23 Bi1 Bi3+ 0.0145(4) 0.0187(5) 0.0390(5) -.0008(4) 0 0 Pb1 Pb2+ 0.0145(4) 0.0187(5) 0.0390(5) -.0008(4) 0 0 Sr1 Sr2+ 0.0088(8) 0.033(1) 0.0064(2) -.0017(7) 0 0 Pb2 Pb2+ 0.0088(8) 0.033(1) 0.0064(2) -.0017(7) 0 0 Cu1 Cu2.14+ 0.003(2) 0.022(2) 0.0522(3) 0.000(1) 0 0 O1 O2- 0.008(8) 0.0038(10) 0.06(1) 0 -.004(8) 0 O2 O2- 0.018(9) 0.03(1) 0.11(2) -.003(7) 0 0 O3 O2- 0.02(1) 0.07(2) 0.05(1) -.02(1) -.004(10) 0.02(1) #End of data_50340-ICSD

E) FASE Ca2PbO4 data_36629-ICSD #©2007 by Fachinformationszentrum Karlsruhe, and the U.S. Secretary of #Commerce on behalf of the United States. All rights reserved. _database_code_ICSD 36629 _audit_creation_date 1993/01/06 _audit_update_record 2000/07/15 _chemical_name_systematic 'Dicalcium Lead(IV) Oxide' _chemical_formula_structural 'Ca2 Pb O4' _chemical_formula_sum 'Ca2 O4 Pb1' _cell_length_a 5.832(1) _cell_length_b 9.766(11) _cell_length_c 3.375(1) _cell_angle_alpha 90. _cell_angle_beta 90. _cell_angle_gamma 90. _cell_volume 192.22 _cell_formula_units_Z 2 _symmetry_space_group_name_H-M 'P b a m' _symmetry_Int_Tables_number 55 _refine_ls_R_factor_all 0.044 Pb1 Pb4+ 2 a 0 0 0 1. 0 0.45(2) Ca1 Ca2+ 4 h 0.0730(7) 0.3175(4) 0.5 1. 0 0.53(5) O1 O2- 4 h 0.2379(30) 0.0492(16) 0.5 1. 0 0.77(20) O2 O2- 4 g 0.3611(24) 0.3009(15) 0 1. 0 0.46(18) #End of data_36629-ICSD

F) FASE (Sr,Ca)2CuO2 data_63498-ICSD

207

#©2007 by Fachinformationszentrum Karlsruhe, and the U.S. Secretary of #Commerce on behalf of the United States. All rights reserved. _database_code_ICSD 63498 _audit_creation_date 1992/08/20 _chemical_name_systematic ; Calcium Strontium Copper Oxide (1.7/0.3/1/3) ; _chemical_formula_structural '(Ca1.66 Sr0.34) Cu O3' _chemical_formula_sum 'Ca1.66 Cu1 O3 Sr0.34' _publ_section_title ; X-Ray investigation of orthorhombic Ca1.66 Sr0.34 Cu O3 _cell_length_a 3.2825(6) _cell_length_b 3.792(1) _cell_length_c 12.288(1) _cell_angle_alpha 90. _cell_angle_beta 90. _cell_angle_gamma 90. _cell_volume 152.95 _cell_formula_units_Z 2 _symmetry_space_group_name_H-M 'I m m m' _symmetry_Int_Tables_number 71 _refine_ls_R_factor_all 0.034 Cu1 Cu2+ 0.0036(3) 0.0011(2) 0.0023(2) 0 0 0 Ca1 Ca2+ 0.0035(3) 0.0054(4) 0.0044(3) 0 0 0 Sr1 Sr2+ 0.0035(3) 0.0054(4) 0.0044(3) 0 0 0 O1 O2- 0.004(1) 0.007(1) 0.003(1) 0 0 0 O2 O2- 0.010(2) 0.003(1) 0.005(1) 0 0 0 #End of data_63498-ICSD

G) PRATA data_64706-ICSD #©2007 by Fachinformationszentrum Karlsruhe, and the U.S. Secretary of #Commerce on behalf of the United States. All rights reserved. _database_code_ICSD 64706 _audit_creation_date 1998/06/26 _audit_update_record 2006/04/01 _chemical_formula_structural Ag _publ_section_title _cell_length_a 4.0862 _cell_length_b 4.0862 _cell_length_c 4.0862 _cell_angle_alpha 90. _cell_angle_beta 90. _cell_angle_gamma 90. _cell_volume 68.23 _cell_formula_units_Z 4

208

_symmetry_space_group_name_H-M 'F m -3 m' _symmetry_Int_Tables_number 225 _symmetry_cell_setting cubic Ag1 Ag0+ 4 a 0 0 0 1. 0

H) FASE PbO data_15402-ICSD #©2007 by Fachinformationszentrum Karlsruhe, and the U.S. Secretary of #Commerce on behalf of the United States. All rights reserved. _database_code_ICSD 15402 _audit_creation_date 1980/01/01 _audit_update_record 2007/08/01 _chemical_name_systematic 'Lead Oxide - Ht' _chemical_formula_structural 'Pb O' _chemical_formula_sum 'O1 Pb1' _chemical_name_mineral Massicot _publ_section_title _cell_length_a 5.876 _cell_length_b 5.476 _cell_length_c 4.743 _cell_angle_alpha 90. _cell_angle_beta 90. _cell_angle_gamma 90. _cell_volume 152.62 _cell_formula_units_Z 4 _symmetry_space_group_name_H-M 'P b c m' _symmetry_Int_Tables_number 57 _refine_ls_R_factor_all 0.07 Pb1 Pb2+ 4 d 0.231 0.014 0.25 1. 0 O1 O2- 4 d -.132 0.082 0.25 1. 0