doi:10.1016/S0921-4534(02)01840-3
Copyright © 2002 Elsevier Science B.V. All rights reserved.
Effects of stoichiometry, purity, etching and distilling on resistance of MgB2 pellets and wire segments
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R. A. Ribeiro
,
, S. L. Bud’ko, C. Petrovic and P. C. Canfield
Ames Laboratory and Department of Physics and Astronomy, Iowa State University, Ames, IA 50011, USA
Received 23 April 2002;
revised 18 June 2002;
accepted 19 June 2002.
Available online 12 October 2002.
Abstract
We present a study of the effects of non-stoichiometry, boron purity, wire diameter and post-synthesis treatment (etching and Mg distilling) on the temperature dependent resistance and resistivity of sintered MgB2 pellets and wire segments. Whereas the residual resistivity ratio (RRR) varies between RRR≈4 to RRR
20 for different boron purity, it is only moderately affected by non-stoichiometry (from 20% Mg deficiency to 20% Mg excess) and is apparently independent of wire diameter and presence of Mg metal traces on the wire surface. The obtained set of data indicates that RRR values in excess of 20 and residual resistivities as low as ρ0≈0.4 μΩ cm are intrinsic material properties of high purity MgB2.
Author Keywords: MgB2; Stoichiometry; Transport properties
PACS classification codes: 74.70.Ad; 74.25.Fy
Fig. 1. Powder X-ray (Cu Kα radiation) diffraction spectra of MgB2 (with h,k,l) for three different qualities (a) 90% pure natural boron; (b) 99.99% pure natural boron and (c) 99.95% pure isotopic enriched 11B. Samples (a) and (b) were synthesized for 3 h/950 °C, and sample (c) for 4 h/950 °C from [11]. The data gaps are due to the removal of the Si peaks.
Fig. 2. Variation of the zero-field resistivity in the 5–300 K range for MgB2 pellets with different boron purities. Inset: expanded scale near Tc.
Fig. 3. Resistivity curves normalized by their temperature derivative at room temperature, for different boron purities. Inset: expanded scale near Tc.
Fig. 4. X-ray spectra for three different nominal compositions of Mgx11B2 for x=0.8,1.0,1.2.
Fig. 5. Temperature dependence of the normalized resistivity for representative samples with nominal composition Mgx11B2 (0.8<x<1.2). Inset: expanded scale near Tc.
Fig. 6. Residual resistance ratio of Mgx11B2 (0.8<x<1.2). The open symbols represent different pieces selected from the same batch. The solid symbols are the average. The dotted box delimits the smaller variation (x=1±0.1).
Fig. 7. Resistivity curves normalized by temperature derivative at room temperature, for Mgx11B2 (x=0.8,0.9,1.0,1.1 and 1.2). x=1.2 data shown as dashed curve as discussed in the text. Inset: expanded scale near Tc.
Fig. 8. Resistivity curves of MgB2 filaments with four boron fiber initial diameters (100, 140, 190 and 300 μm): (a) for as-grown wires and (b) after etched in ethyl alcohol with 5% of HCl. Inset: expanded scale near Tc.
Fig. 9. Resistivity curves before and after distillation process in MgB2 wire with 300 μm boron fiber initial diameter.
Table 1. Boron form and purity (as provided by the seller)

Table 2. Main properties of MgB2 wires and resistivity at 300 K and RRR for as-grown, etched and distilled MgB2 filaments with different diameters

Note: samples designated by the diameter of initial boron filaments used.
Corresponding author. Tel.: +1-515-294-6270; fax: +1-515-294-0689; email: ribeiro@ameslab.gov