J Supercond Nov Magn (2011) 24: 12411244 DOI 10.

1007/s10948-011-1149-x

LETTER

Preparation of the Silver-Superconductor Composite by Deposition of the Silver Nanoparticles in the Bismuth Cuprate Superconductor
V. Bartun k O. Smr kov e c

Received: 2 February 2011 / Accepted: 11 February 2011 / Published online: 2 March 2011 Springer Science+Business Media, LLC 2011

Abstract BiSCCO (BiSrCaCuO) is high temperature superconductor with a lot of possible applications. Interfaces between superconductors and metal conductors are one of the technological problems. In this work, silver-superconductor composite was prepared by using ow of silver nanoparticles suspension in DMF (N,Ndimethylformamide) through superconductors pore system. Silver nanoparticles were prepared by reaction of silver nitrate with DMF. Properties of prepared composite were measured by SEM charting, XRD and critical current measurements. SEM chart showed uniform distribution of silver across sample. XRD and critical current measurements validated superconducting properties of prepared composite. In the future, materials based on this method could be used as an interface between superconductors and metals or as a base for superconducting composite with much better mechanical properties. Keywords BiSCCO Silver Composite Nanoparticles Superconductors

1 Introduction Nitrogen-cooled high temperature superconductors are largely used in various types of devices [1, 2], like motors, generators, magnets, levitation devices, etc. Most common used high-superconducting materials are BiSCCO (BiSr CaCuO) and YBCO (YBaCuO), or derived materials obtained by substitution of some element [3]. Though,

V. Bart n k ( ) O. Smr kov u e c Institute of Chemical Technology, Technick 5, 166 28 Prague 6, Czech Republic e-mail: vilem.bartunek@vscht.cz

use of superconducting tapes and wires markedly outweighing bulk superconductors has some potential in industry, research and other applications [46]. BiSCCO superconductor contains two high-temperature superconducting phases: 2212 phase with lower critical temperature (90 K) and 2223 with critical temperature 110 K. Properties of interfaces between metal contacts and ceramic superconductors are crucial for most superconducting devices. In the case of thin tapes coated in silver with very good temperature and electric conductivity, the problem is nearly solved regarding good cohesion of silver layer on superconducting material. Silver shell is added on superconducting core before temperature processing and tape is usually multiply pressed. In the case of bulk material, the situation is different and interfaces between thick mass of bulk material and metal conductor may be problematic [710]. If resistance of interface is high, it may cause rapid heating and subsequently collapsing of superconducting state. It may lead to damaging of device by melting or evaporating of material. Therefore metal-superconductive composite materials [11] could be useful for many applications, for example for larger thermal and electrical conductivity in nonsuperconducting state. Preparation of composites by mixing of components before heat treatment is problematic. The most suitable and chemically stable with BiSCCO metal is silver. Silver has low melting temperature. So only relatively large pieces of silver could be used, or melting and owing of metal could appear. Large pieces of non-superconducting metal create barriers for supercurrent and so decrease critical current density. Moreover, they can also decrease mechanical characteristic of material. In this work another approach has been used. Instead of attempt to insert silver into material before the material an-

1242 Fig. 1 Typical distribution of pores in bulk BiSCCO superconductors

J Supercond Nov Magn (2011) 24: 12411244

Fig. 2 SEM image of the silver nanoparticles

nealing, we inserted silver nanoparticles into the material after its preparation.

Fig. 3 SEM chart of silver distribution (white) in the sample after experiment

2 Experimental Superconducting samples were prepared by standard solid state reaction with Bi2 O3 , PbO, SrCO3 , CaCO3 and CuO as starting compounds. Mixed powder was twice calcined at 800 C for 24 hours and then pulverized. Final powder was pressed into pellets with diameter of about 1.3 cm and weight of about 1.0 g. Pellets were sintered in tube furnace at 840 C for 168 hours and cooled in air. For the purpose of experiment, samples were shaped to the blocks with rectangular cross section. Superconductor prepared by this method usually contains both 2212 and 2223 phases. Typical pore distribution of samples, investigated by mercury pressing method in [12], is given in Fig. 1. Pore superconducting sample was used as a frit to capture silver nanoparticles.

Silver nanoparticles were prepared by reaction of silver nitrate with DMF (N,N-dimethylformamide) [13]. The molar concentration of silver nitrate in DMF was 5104 mol l1 . Temperature of solution was kept at 100 C using water bath. The reaction duration was three hours. Superconducting sample was sealed in the capillary from PE tube and then put into glass tube. The frit was merged into reacting solution inside balloon which was then tightened. Vacuum was created by suction pump and connected to the glass top. Every experiment was performed simultaneously with two samples to get control and standardization of experiment. Suction pumps were pushed in at the beginning of the experiment and continued working all the time. Subsequently the samples were cut out of the PE case and were boiled in isopropyl alcohol to ease off the DMF from the pore system. At last, the samples were dried in the dry kiln at 100 C.

J Supercond Nov Magn (2011) 24: 12411244 Fig. 4 Diffraction patterns of samples before and after experiment

1243

X-ray powder diffraction data were collected at room temperature with XPert PRO powder diffractometer with parafocusing BraggBrentano geometry using CuK radiation ( = 1.5418 , U = 40 kV, I = 30 mA). SEM elements chart was made using electron microscope Hitachi S-450 with EDS analyzer Kevex Delta 5. SEM picture of silver nanoparticles was made by electron microscope Hitachi S-4700. Distribution of the pores of samples was measured using mercury-pressing method by porosimeter Poresizer 9320. Critical current densities were measured by standard four-contact method in boiling nitrogen (77 K).

ferent orientation of grains before and after the experiment. This did not negatively affect superconducting properties of the sample. Orientation of grains is rather positive for superconductor.

4 Conclusion Silver-superconductor composite was successfully prepared by using Bi(Pb)SrCaCuO superconducting matrix as a frit. Solution of DMF with silver nanoparticles ows through superconductors pore system and silver deposits were created in the material. The process has no negative effect on superconducting properties of Bi(Pb)Sr CaCuO superconducting matrix. In the future, materials based on this method could be used as an interface between superconductors and metals or as a base for superconducting composite with much better mechanical properties.
Acknowledgements This work was supported by Ministry of Education Youth and Sports of the Czech Republic (MSM 6046137302). The authors wish to thank to Pavel Novk for the SEM measurements.

3 Results and Discussion Bi(Pb)SrCaCuO powder was boiled in DMF for 3 hours and no difference was detected in diffraction patterns before and after the experiment. Therefore Bi(Pb)SrCa CuO superconductor is inert to boiling DMF. Typical size of nanoparticles prepared by reduction of silver nitrate by DMF is about 50 nm as can be seen in Fig. 2. Deposition of silver was successful as can be found in SEM chart (Fig. 3). Distribution of small deposits of silver is well uniform in entire mass of sample. A picture was taken approximately from a middle of the sample. Critical current densities were nearly the same before and after the experiment, around 100 A cm2 as is usual for bulk, non-textured Bi(Pb)SrCaCuO superconductors. It shows that experimental conditions have no signicant effect on superconducting properties and so prepared composites could be still used as superconductors. XRD patterns before and after the experiment showed no difference in peak positions but showed difference in intensity of some peaks (Fig. 4). It is probably caused by dif-

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