Patent
(Bi, Pb).sub.2, Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x superconductor and method of making same utilizing sinter-forging
| العنوان: | (Bi, Pb).sub.2, Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x superconductor and method of making same utilizing sinter-forging |
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| Patent Number: | 5,821,201 |
| تاريخ النشر: | October 13, 1998 |
| Appl. No: | 08/748,259 |
| Application Filed: | November 13, 1996 |
| مستخلص: | A (BiPb).sub.2 Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x (Bi223) superconductor with high J.sub.c, phase purity, density and mechanical strength is formed from Bi2223 powder which is synthesized from a mixture of Bi.sub.2 O.sub.3, PbO, SrCO.sub.3, CaCo.sub.3 and CuO. The mixture is milled, then dried and calcined to synthesize the Bi2223 powder with the desired phase purity. The calcination is performed by heating the dried mixture for 50 hours at 840.degree. C. The partially synthesized powder is then milled for 1-4 hours before calcining further for another 50 hours at 855.degree. C. to complete the synthesis. After calcination, the Bi2223 powder is cold pressed to a predetermined density and sinter forged under controlled temperature and time to form a Bi2223 superconductor with the desired superconducting properties. |
| Inventors: | Chen, Nan (Downers Grove, IL); Goretta, Kenneth C. (Downers Grove, IL); Lanagan, Michael T. (Woodridge, IL) |
| Assignees: | The United States of America as represented by the United States Department of Energy (Washington, DC) |
| Claim: | The embodiments of this invention in which an exclusive property or privilege is claimed are defined as follows |
| Claim: | 1. A method of manufacturing a high temperature (Bi,Pb).sub.2 Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x (Bi2223) superconductor with high J.sub.c and mechanical strength, comprising the steps of |
| Claim: | preparing a mixture of Bi.sub.2 O.sub.3, PbO, SrCO.sub.3, CaCo.sub.3 and CuO; |
| Claim: | conducting a first milling of the mixture; |
| Claim: | conducting a first calcination of the milled mixture; |
| Claim: | conducting a second milling of the calcined mixture; |
| Claim: | conducting a second calcination of the twice milled, calcined mixture to synthesize Bi2223 powder containing between 1-10 atomic percent nonsuperconducting. non-Bi2223 phase, comprising Pb, Bi and Cu, which form a liquid phase during sinter forging; |
| Claim: | cold pressing the Bi2223 powder to a predetermined density; and |
| Claim: | sinter forging the cold pressed powder to form a Bi2223 superconductor. |
| Claim: | 2. The method of claim 1 including the step of placing a silver foil on the cold pressed powder to prevent unwanted chemical reaction during sintering and to form a low resistance electrical contact on the superconductor. |
| Claim: | 3. The method of claim 1 including the step of cooling the sinter forged superconductor at a rate between 60-300.degree. C./hour. |
| Claim: | 4. The method of claim 1 wherein the sinter forging is conducted at a temperature between 840-848.degree. C. |
| Claim: | 5. The method of claim 1 wherein the sinter forging is conducted for a duration between 2-10 hours. |
| Claim: | 6. The method of claim 1 wherein the sinter forging is conducted at a pressure between 1-6 MPa. |
| Claim: | 7. The method of claim 1 wherein the Bi2223 powder is cold pressed to a density between 60-90%. |
| Claim: | 8. The method of claim 1 wherein the cold pressing includes uniaxial pressing and isostatic pressing. |
| Claim: | 9. The method of claim 1 wherein the second milling is conducted for a duration between 14 hours. |
| Claim: | 10. The method of claim 1 wherein the second milling includes vibratory ball-milling. |
| Claim: | 11. The method of claim 1 wherein the first calcination is conducted for 50 hours at 840.degree. C. |
| Claim: | 12. The method of claim 1 wherein the second calcination is conducted for 50 hours at 855.degree. C. |
| Claim: | 13. The method of claim 1 wherein the first milling is conducted for 16 hours. |
| Claim: | 14. A method of manufacturing a high temperature (Bi,Pb).sub.2 Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x (Bi2223) superconductor with high J.sub.c and mechanical strength, and having silver electrical contacts, comprising the steps of |
| Claim: | preparing a mixture of Bi.sub.2 O.sub.3 , PbO, SrCO.sub.3, CaCo.sub.3 and CuO; |
| Claim: | conducting a second milling of the calcinated mixture for 1-4 hours; |
| Claim: | cold pressing the Bi2223 powder to a density between 60-90%; |
| Claim: | placing a silver foil on the cold pressed powder to prevent unwanted chemical reaction during sinter forging and to form a low resistance electrical contact directly on the superconductor; |
| Claim: | sinter forging the cold pressed powder for 2-10 hours at 840.degree.-848.degree. C. to form a superconductor; and |
| Claim: | cooling said sinter forged superconductor at a rate between 60.degree.-300.degree. C./hour. |
| Claim: | 15. A method of manufacturing a high temperature (Bi,Pb).sub.2 Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x (Bi2223) superconductor with high J.sub.c and mechanical strength, comprising the steps of |
| Claim: | conducting a second calcination of the twice milled, conducting a second calcination of the twice milled, calcined mixture to synthesize Bi2223 powder containing between 1-10 atomic percent nonsuperconducting, non-Bi2223 phase, comprising Pb, Bi and Cu; |
| Claim: | sinter forging the cold pressed powder to liquify said nonsuperconducting, non-Bi2223 phase comprising Pb, Bi and Cu, and form a Bi2223 superconductor. |
| Claim: | 16. A method of manufacturing a high temperature (Bi,Pb).sub.2 Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x (Bi2223) superconductor with high J.sub.c and mechanical strength, comprising the steps of |
| Claim: | milling and calcining the mixture to synthesize Bi2223 powder containing between 1-10 atomic percent nonsuperconducting phase, comprising Pb, Bi and Cu; cold pressing the Bi2223 powder to a predetermined density; and |
| Claim: | 17. The method of claim 16 wherein said 1-10 atomic percent nonsuperconducting phase forms a liquid phase during sinter forging. |
| Current U.S. Class: | 505/432; 505/433; 505/450; 505/739 |
| Current International Class: | C04B 35626; C04B 35645 |
| Patent References Cited: | 5189011 February 1993 Itozaki et al. 5273956 December 1993 Johnson et al. |
| Other References: | Tampieri et al "Densification of Bi.sub.1.8 (Pb).sub..35 Sr.sub.1.9 Ca.sub.2.1 Cu.sub.3 O.sub.x . . . " JJAP, Part 1 (1993) 32(10) pp. 4490-4495, (No Month). Chen et al "Sinter-Forged (Bi, Pb).sub.2 Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x . . . " Supercond. Sci Technol. 6(1993) 674-677 (No Month). Yang et al "Alignment of grains in Bi.sub.1.6 Pb.sub.4 Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x . . . " Supercond. Sci. Technol. 6(1993) 269-275. ( No Month). Jin et al "The Specific Heat of the Single-Phase (Bi,Pb).sub.2 Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.10xy . . . " Physica C. vol. 158, 1989 pp. 255-257. Che et al "Composition & Superconductivity in Bi--Sr--Ca--Cu--O . . . " Journal of Materials Science, vol. 24, May 1989, pp. 1725-1728. Lusk et al "High Pressure Studies of the Superconducting Transition in (Bi,Pb).sub.2 Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.10 " Aust. J. Phys, vol. 42, #4, 1989 pp. 425-429. Robinson et al "Sinter-Forged YB.sub.2 Cu.sub.3 O.sub.7-8 " Ad. Cer. Materials, vol. 2, #3B, Special Issue Jul.,1987, pp. 380-388. Yamada et al "Pb Introduction to the High-Tc Superconductor . . . " J.J.A.P. vol. 27, No. 6, Jun. 1988 pp. 1996-1998. Jin et al "High-Tc Superconductors-composite wire fabrication" Appl. Phys. Lett. Vol. 51(3) Jul. 1987 pp. 203-204. |
| Primary Examiner: | Lieberman, Paul |
| Assistant Examiner: | Kopec, Mark |
| Attorney, Agent or Firm: | Park, Daniel D. Anderson, Thomas G. Moser, William R. |
| رقم الانضمام: | edspgr.05821201 |
| قاعدة البيانات: | USPTO Patent Grants |
| الوصف غير متاح. |