Materials Research Bulletin 42 (2007) 10511060

www.elsevier.com/locate/matresbu

Lead substitutions for promoted critical current

density Jc and mechanical properties of
Mg1xPbxB2 regime
Khaled M. Elsabawy *, Elsayed E. Kandyel
Chemistry Department, Faculty of Science, Tanta University,
Tanta 31725, Egypt
Received 5 May 2006; received in revised form 13 September 2006; accepted 20 September 2006
Available online 24 October 2006

Abstract
Lead was used as softener dopant element to replace on magnesium sites in Mg1xPbxB2 regime (where x = 0.0, 0.05, 0.1 and
0.2 mole). Samples were prepared via high temperature solid-state reaction technique depending upon diffusion mechanism of Mg/
Pb-vapour ions through boron-matrix. The maximum solubility limit of lead n was found to be 0.2 mole, which emphasises that
substitution on MgB2 system is stilling too limited and needs many precautions to be successful.
The crystalline lattice constants were evaluated and exhibit noticeable length elongation in case of c-axis as x increases while a,
b-axes were nearly constant. Furthermore, effect of Pb-doping was investigated carefully on microstructure and superconducting
properties of MgB2 system. SE-microscopic analysis indicated that lead ions diffuse regularly through surface and bulk in case of
(x = 0.05 and 0.1 mole) and grain size was estimated and found in between 0.43 and 1.6 mm. Critical current densities (Jcs values)
recorded an reasonable increase as Pb-content increase (from x = 0 to 0.1 mole) while recorded a slight decrease for sample with
maximum lead content (x = 0.2 mole). The mechanical tensile strength of the samples was clearly improved linearly as Pb-content
increase recording maximum tensile 31.7 MPa for sample with x = 0.2 mole.
# 2006 Elsevier Ltd. All rights reserved.
Keyword : A. Ceramics; B. Chemical synthesis; C. X-ray diffraction; D. Electrical properties; D. Mechanical properties

1. Introduction
The discovery of superconductivity in magnesium diboride 39 K superconductor regime [1,2], introduces a
huge progress in the material synthesis and processing as well as in understanding of its physical properties [38].
Many diborides crystallize in the same hexagonal-type of structure as MgB2 these compounds have been known
and investigated before carefully [9]. For magnesium site substitutions apparently only Al, Mn and Ir were
showing good substitutions to enter the structure unambiguously [1015] although it was successfully only for a
limited concentration range. For boron site substitutions a number of attempts with different elements were
made including (C, Zn, Na, K, Ag and Si). Carbon substitution was reported in several publications [1621].
Sekkina and Elsabawy [22] have been investigated effect of fluoride substitiution partially on B-site on the

* Corresponding author. Tel.: +20 40 2533200; fax: +20 40 3350804.

E-mail address: ksabawy@yahoo.com (K.M. Elsabawy).
0025-5408/$ see front matter # 2006 Elsevier Ltd. All rights reserved.
doi:10.1016/j.materresbull.2006.09.017

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K.M. Elsabawy, E.E. Kandyel / Materials Research Bulletin 42 (2007) 10511060

superconducting, structural and microstructural properties of MgB2. Cava et al. [23] have been proposed
the minimal criteria for judging a successful chemical doping/or substitution in MgB2 superconducting
system.
One of the surprising characteristics of superconducting MgB2 [1] is the simplicity of both its chemistry
and crystal structure. The structure consists of honeycomb layers of boron interleaved with simple triangular
layers of Mg, and the non-transition metal chemistry appears relatively straightforward. The very limited
substitutional chemistry possible [2427], however, suggests that the structure and chemistry are more complex
than they first appear. The substitution of Mg by Al in Mg1xAlxB2 further illustrates the complexity. The
substitution first leads to a decrease in superconducting transition temperature for small x (x < 0.1), and then
the disappearance of superconductivity in a manner consistent with expectations from electronic structure
calculations. However, the loss of superconductivity is accompanied by the partial collapse of the lattice in the
direction perpendicular to the boron planes at a chemical miscibility gap 0.1 < x < 0.2. The compounds with
compositions x > 0.2 show no bulk superconducting transition down to 4.2 K, and observations of
superconductivity in that composition range [28] are associated with the difficulty of preparing homogeneous
samples.
2. Experiments
2.1. Samples preparation
Mg1xPbxB2 (where x = 0.0, 0.05, 0.1, and 0.2 mole) was prepared through high temperature solid-state reaction
technique for stoichiometric amounts of the nominal compositions of starting materials (Mg, B and Pb). The average
particle size of boron and Pb metal powder used was <100 mm.
All powders are with purity grade 99.9%. The stoichiometric amounts mixed and ground together and were
pressed into pellets under pressure 4 tonnes/cm2 and were placed into Ta-ampule under argon pressure, the Ta-tube
carefully sealed in goodly way and forwarded to tubular quartz furnace at 950 8C sintering temperature. The thermal
cycle of preparation pure MgB2 and Pb-doped MgB2 included intermediate fixation step at 650 8C for 3 h, then gradual
increasing till 1000 8C by rate 50 8C/h and finally samples were sintered at 1000 8C for 10 h then the temperature
cooled down till R.T. by rate 25 C8/h.
It is well known that, both of Mg and Pb has very low melting point which are 648.6 and 327.5 8C, respectively, and
converted into vapour at temperature over 648.6 8C while, boron has very high melting point 2180 8C, so MgB2 and its
variant Pb-doped samples are produced through diffusion reaction mechanism of Mg and Pb ions vapour into boron
matrix.
2.2. Structural measurements
2.2.1. X-ray diffraction (XRD)
The X-ray diffraction measurements were carried out at room temperature on the ground samples using Cu Ka
radiation source and a computerized Shimadzu (Japan) diffractometer with 2u scan technique.
2.2.2. Scanning electron microscopy (SEM)
Scanning electron microscopy measurements were carried out along ab-plane using small pieces (cut into very thin
layer by diamond cutter) of the prepared samples by using a computerized SEM with elemental analyzer unit. The
morophological features and bulk grain size calculations were carried out through different sectors in the investigated
samples using high resolution SEM (Philips, USA).
2.3. Superconducting measurements
2.3.1. The DC electrical resistivity measurements
DC-electrical resistivity of the prepared materials were undertaken as a function of temperature using the modified
four-probe technique and the temperature was recorded in the cryogenic temperature zone down to 30 K using liquid
helium refrigerator.

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1053

2.3.2. Determination of Jc
For determining values of Jc for the prepared samples the magnetization was measured as a function of magnetic
field strength H at different temperatures to construct a MH hysteresis loops. The magnetic critical current density
(Jc) values for investigated samples were calculated using the relationship
20DM
Jc
(1)
a  a2 =3b
where Jc is in A/cm2, DM in emu/cm3 and a,b are the lateral dimension of pellet in cm.
2.4. Mechanical measurements
Samples were cut from the bulk by certain dimensions 4 mm  4 mm  4 mm, to make as possible the longitudinal
loading direction of the specimens parallel to a- or b-direction and perpendicular to the c-direction of the bulk. Tensile
tests were carried out at room temperature 295 K and details of loading was described by Tomita and Murakami [29],
the displacement speed of the actuator of testing machine was in between 0.10 and 0.15 mm/min. and observation of
fracture morphology of the samples was carried out using digital camera. Crushing pressure was obtained by applying
pressure by using hydraulic compressor on the cubic samples with dimensions 0.6  0.6  0.6 at room temperature.
The pressure and mold temperature were recorded at crush point.
3. Results and discussion
3.1. Structural measurements
Fig. 1ad shows X-ray diffraction patterns for investigated samples; Mg1xPbxB2 where (x = 0.0, 0.05, 0.1 and
0.2 mole, respectively) which were found mainly belong to single hexagonal phase with P6/mmm symmetry
corresponding to Mg1xPbxB2 superconductors in major phase beside some of secondary phases such as PbO and
MgO which were assigned in the back ground in minor. The evaluated lattice parameters were estimated and refined by
and c = 3.5632 A
for undoped MgB2 sample, while a
using GSAS and Fullprof program and found to be a = 3.0817 A
and c axes exhibit length elongation with increasing lead dopant from x = 0.05 to 0.2 mole, respectively (see Fig. 1e).
It is clear that increasing in the c axis is much noticeable than increasing of a axis (see Table 1). The increasing in c/
a ratio can be explained on the bases of, first ionic size effect that lead ionic radius is larger than magnesium ionic
radius (Mg2+ = 72 pm while Pb2+ = 119 pm) and second increasing of in- and inter-plane coupling depending upon
electron-dopant effect which is due to the average charge on Pb-ion higher than that on Mg-ion depending on amount
of traces from tetra-valent lead (Pb4+) existed.
It is known that, MgB2 has AB2 structure type which is commonly found for many metals diborides. This structure,
consisting of interleaved graphite-like layers of boron and triangular layers of metal atoms. This kind of graphite-like
layers structure allows for lead-ions to insert successfully without problems in the main hexagonal structure at low
concentrations only but at higher one destroy the crystal structure.
Cava et al. [23] have been reported the minimal criteria for judging a successful chemical substitution in
magnesium diboride system which are: first the second phases should not grow systematically with propagation of
dopant ratio concentration in the solid-state solution and special care must be apply to peak indexing of impurity
phases, second the shift of lattice parameter of by more than three standard deviations in least squares lattice parameter
refinements in the series of doped samples should be seen, third the properties of superconductor should change on
doping.
In our opinion we are in fully agreement with Cava et al. [23], and we can add a fourth feature must be present in the
dopant atom as precondition factor to substitute successfully, which is atomic size of the dopant element must be
harmonize and thermodynamically compatible with the solid solution of system on doping whatever this system.
Many researchers attempted to substitute in Mg-sites on MgB2 but their trails were always failed or had some
limitations [3035]. The isoelectronic or hole-doping substitution of Mg expects to produce an increase of Tc [30].
Actually, a detrimental effect on Tc has been observed on the electron-doped Mg1xAlxB2 ternary system, but also for
the hole-doped like Mg1xLixB2 solid solution [31]. A very small increase of Tc (0.2 K) has been observed for Zn
doping [32], as well as an equivalent decrease was reported [33].

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Fig. 1. (ad) X-ray diffraction patterns recorded for pure and doped MgB2-regime: (a) x = 0.00 mole; (b) x = 0.05 mole; (c) x = 0.10 mole; (d)
x = 0.20 mole. (e) Variations of c-axis lattice parameter vs. Pb-content.

According to ref. f[30], copper should behave as a hole dopant, producing a shift of EF to higher binding energies
and an increase of the density of states N(EF), at least for concentrations as high as 25%. Claims of an increase of Tc up
to 49 K by Cu substitution have been reported [34], but they were not confirmed and the original claim withdrawn.
In fact, the synthesis of Mg1xCuxB2 has proved to be hard and, to our knowledge, no successful method for this
preparation has so far been published and even stated as impossible.
In our opinion doping MgB2 with Cu or/M2+ is difficult because of the high affinity of Cu and Mg to form cubic
inter-metallic compounds with Cu/Mg ratio ranging from 2/3 to 3. CuB binary systems are known, starting from the
composition CuB22 [35]. Phases with higher Cu/B ratio are unstable and copper diboride does not exist.
Table 1
The calculated lattice parameter, values Tc-offsets and critical current densities values (Jcs) recorded for doped and undoped MgB2 samples
Dopant ratio (mole)

)
a (A

)
c (A

Tc-offset (K)

Jc (A/cm2)

0.00
0.05
0.10
0.20

3.081(74)
3.086(56)
3.087(53)
3.088(38)

3.563(21)
3.711(74)
3.784(28)
3.830(67)

37.2
33.1
27.3
16.6

2.8  l06
3.1  l07
4.2  l08
2.7  l07

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1055

For these reasons, attempts to synthesise Mg1xCuxB2 solid solutions by a simple addition of Cu to MgB2, followed
by thermal treatments in argon atmosphere, were not successful.
Our results emphasis the mentioned literatures and confirmed it but in case of lead Pb2+ which is considered
isoelectronic dopant we succeeded to prepare lead-doped-MgB2 depending on both of Mg and Pb has very low melting
point which are 648.6 and 327.5 8C, respectively, and converted into vapour at temperature over 648.6 8C while, boron
has very high melting point 2180 8C, so MgB2 and its variant Pb-doped samples are produced through diffusion
reaction mechanism of Mg and Pb ions vapour into boron matrix in an isolated system.
3.2. Microstructure properties
Fig. 2ad explains SEM-images through ab-plane for Pb-doped-Mg1xPbxB2 and pure MgB2 with boron particle
size <50 mm. From the analysis of SEM-images and EDX elemental analysis for many spots on each sample we
deduced the following facts:
First (MgO/or PbO phases) does not noticeable at the inter grain-layers especially in sample with lower Pbconcentration x = 0.05 mole while sample (d) with maximum dopant ratio (x = 0.2 mole) it begins to appear in
between layers in very small aggregation.
Second the average estimated grain size is in between 0.43 and 1.6 mm.
Third lead atoms diffused regularly as shiny spots through over the samples with x = 0.05 and 0.1 mole while
distributed in random state in case of x = 0.2 mole. This observations and facts also very clear in our XRD
patterns impurity phases begin to appear clearly with considerable intensities in sample (c and d) see Fig. 1.
From these micrographs beside EDX analysis, one can conclude that, MgB2 is the major phase with high degree of
homogeneity which appears in degree of gray colouration.
Impurity phases like (MgO and PbO) were not noticeable on the morphological analysis of samples at low
concentration from doping but by accurate examinations of interior of the bulk by cutting many sectors in the same
pellet, it was observed that there are small traces and aggregations from MgO and PbO located on the boundaries
between grains of MgB2 regime.
These results obtainable from SEM enhance, why Tcs-offsets in DC-resistivity measurement decreases as Pbdopant concentration increases.
3.3. Superconducting measurements
Fig. 3ad shows the DC-electrical resistivity measured as a function of absolute temperature for undoped MgB2 and
lead-doped family Mg1xPbxB2 (x = 0.05, 0.10 and 0.2 mole).
It is clear that, the Tcs-offsets decrease regularly (37.2, 33.1, 27.3 and 16.6 K) as Pb-dopant concentration x
increases from x = 0 to 0.2 mole, respectively (see Table 1and Fig. 3f).
From these results, the depression of Tcs-offsets is mainly due to two factors first is the hole band filling caused by
divalent/or higher valent Pb-dopant [36,37] and the second factor is increasing the impurity phases concentration as x
increases as shown in Fig. 1. It is clear that the sample with lower Tc-offset (Tc = 18 K) is recorded for higher lead
concentration (x = 0.2 mole) and higher impurity phases (see Fig. 1d). Furthermore, existence of MgO-impurity phase
which is insulator oxide [29] inhibits the supercurrents especially if it is present in between the grains of MgB2 as
proved in SEM examinations. In our work MgO/PbO were detected as secondary phases in both XRD and SEM
pictures.
The critical current densities Jcs were found to be 2.8, 31, 420 and 27 MA/cm2 for pure and Pb-doped samples
x = 0.0, 0.05, 0.1 and 0.2 mole, respectively, at 5 K and H = 2 T.
These results are considered quiet good for powder samples composites if it is compared with the Jcs values
reported in literatures [3842]. The highest values Jcs reported were ranged in between 2000 and 9000 MA/cm2 and
usually recorded for wires and tapes sheathed by hard magnetic sheath such as iron or nickel [4142]. These forms are
so difficult to process tapes by mechanical deformation and the role of Fe or Ni might benefit in case of Jc
measurements but these ferromagnetics can locally suppress superconductivity. Our results are in full agreement with
these information such that, the samples of maximum doping ratio x = 0.2 mole recorded Jc = 27 MA/cm2 which

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Fig. 2. (ad) SE-micrographs pictures recorded for pure and doped MgB2-regime with different amplification factors and particle sizes <50 mm: (a)
x = 0.00 mole; (b) x = 0.05 mole; (c) x = 0.10 mole; (d) x = 0.20 mole.

brake the trend of increasing Jc values which in our opinion due to impurity phases MgO (which is insulator) and PbO
make as electrons traps restrict and suppress the flow of supercurrent and consequently Jcs values decrease.
3.4. Mechanical properties
The mechanical tensile strength as a function of displacement of the actuator (stroke mm) at the fracture at 290 K
were carried out see Figs. 4 and 5), it is clear that, the maximum average of tensile strength increases as Pb-content
increase and the maximum tensile average 31.7 MPa was for the sample with Pb-content = 0.2 mole, which means
increasing of Pb-content plays an important role as softener element for magnesium diboride regime. Moreover extra
lead particles (x-values) dispersed regularly in the matrix of MgB2 making it more ductile material and consequently
the stroke increases from x = 0.0 mole (stroke 0.06 mm) to x = 0.2 mole (stroke 0.24 mm) this means existence of
lead as softener dopant duplicate the value of stoke more than four times. A similar behaviour was obtainable with one
of authors themselves during investigations of mechanical properties of highly lead content-BPSCCO [43].

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Fig. 3. (ad) DC-electrical resistivity as a function of absolute temperatures for pure and doped MgB2-regime: (a) x = 0.00 mole; (b) x = 0.05 mole;
(c) x = 0.10 mole; (d) x = 0.20 mole. (e) Variations of Jcs values measured vs. Pb-content. (f) Variations of Tcs values measured vs. Pb-content.

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K.M. Elsabawy, E.E. Kandyel / Materials Research Bulletin 42 (2007) 10511060

Fig. 4. Strokestress curves recorded at R.T. for pure and doped MgB2-regime: (a) x = 0.00 mole; (b) x = 0.05 mole; (c) x = 0.10 mole; (d) x = 0.20
mole.

Fig. 5. The average fracture stresses (MPa) recorded vs. Pb-content.

Table 2 displays the crushing pressures recorded for pure and variant lead doped magnesium diboride regime. As
clear from the table there is directly proportional relation between the crushing pressure as mechanical deformation
effect and the amount of lead content induced in the sample. This result indicated that lead plays a good role as softener
and consequently ductility of the doped-MgB2 samples increases. A similar behaviour was noticeable with [43] when
they applied lead dopings to improve mechanical properties of BPSCCO regime.
Table 2
Crushing pressure vs. lead dopant ratio at room temperature
Sample

Temperature of mold (8C)

Crushing pressure (tonnes/cm2)

MgB2
Mg0.95Pb0.05B2
Mg0.90Pb0.10B2
Mg0.80Pb0.20B2

33
33.6
33.8
34.2

10.6
11.3
11.8
12.2

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4. Conclusions
Structural analysis proved that lead can substitutes successfully on MgB2 at low concentration only which is nearly
equal to the maximum solubility limit of lead n  0.2 mole. This result emphasises that substitution on MgB2 system
is stilling too limited and needs many precautions to be successful.
The crystalline lattice constants exhibit noticeable length elongation in case of c-axis as x increases while a, b-axes
were nearly constant. SE-microscopic analysis indicated that lead ions diffuse regularly through surface and bulk in
case of (x = 0.05 and 0.1 mole) and grain size was estimated to be in between 0.43 and 1.6 mm. Critical current
densities (Jcs values) recorded an reasonable increase as Pb-content increase (from x = 0 to x = 0.1 mole) while
recorded a slight decrease for sample with maximum lead content (x = 0.2 mole). The mechanical tensile strength of
the samples was clearly improved linearly as Pb-content increase recording maximum tensile 31.7 MPa for sample
with x = 0.2 mole.
Acknowledgements
The authors would like to thank Prof. M.A. Sekkina for his careful reading of the manuscript and his conclusive
remarks. Also thanks a lot for Prof. M. Jansen at (Max Planck Institute for solid state research-Stuttgart-Germany) for
his technical support in some of parts inside this article.
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