Synthesis and characterization of Y Temperature ...

1
-10000 -5000 0 5000 10000 -0,020 -0,015 -0,010 -0,005 0,000 0,005 0,010 0,015 0,020 Y123 Moment (emu/g) Magnetic Field (Oe) 50 100 150 200 250 300 -0,00035 -0,00030 -0,00025 -0,00020 -0,00015 -0,00010 -0,00005 0,00000 0,00005 50 100 150 200 250 300 ZFC Moment (emu) x=0.5 FC Temperature (K) Synthesis and characterization of Y (1-x) Nd x Ba 2 Cu 3 O 7-δ High Temperature Superconductors by Acetate Method A. C. de Léo 1 , M. P. Nascimento 2 , U. D. Chacón 2 , E. M. B. Saitovitch 2 , M. Fontes 2 , M. A. Neves 3 , A. López 1 1 Universidade do Estado do Rio de Janeiro, Instituto de Física Armando Dias Tavares, RJ, Brazil. 2 Centro Brasileiro de Pesquisas Físicas, RJ, Brazil. 3 LMDS / Universidade Federal Rural do Rio de Janeiro, RJ, Brazil. e-mail: [email protected] Abstract: The REBCO (RE = Rare Earth) powder materials have a great application on industries, especially used as fault current limiters, current leads and levitators for electrical enhances and generators. In this work is presented an efficient process and results that may contribute to improve superconducting materials of optimum quality to Melt-Textured-Growth (MTG), which are suitable for many applications. Polycrystalline bulk samples of Y (1-x) Nd x Ba 2 Cu 3 O 7-δ were obtained by a wet-chemical acetate method with x = 0, 0,1, 0,2, 0,5 and 1,0 as well as change the Yttrrium for the rare earth Neodymium until full replacements i.e., from YBCO to NdBCO. The acetate route consists of a wet chemical procedure reaction with the powder Y 2 O 3 , Nd 2 O 3 , BaCO 3 and CuO (99,9% purity) into a solution of 50% glacial acetic acid. This method improves the grain growth, is shorter than conventional solid state method without any degradation in sample parameters. The samples were submitted to X-ray powder diffraction (XRD) and the spectra obtained were fitted using Rietveld method, orthorhombic space group Pmmm was assumed, the result showed that the unitary cell average volume increases with the Neodymium doping quantity. The porosity of the samples was calculated with densities from the sample and XRD data, and the values are from 11% up to 23%, resulting into a high degree of granularity in those samples. Those result shows that are fewer necks on the samples than expected by conventional method synthesis, confirmed by SEM images of cross section and superficial surfaces. It also provides information of the grains size and homogeneity. AC electrical resistance as a function of temperature measurements and DC magnetization measurements showed that all sampleshad superconducting transition with T C >77 K, and in absence of Neodymium, the critical temperature reaches 91K. From the analysis of the results we conclude that this method is promising for obtaining optimal high temperature superconducting cuprates in order to be used for MTG. The X-ray diffractogram (after a Rietveld refinement) for samples of YBa 2 Cu 3 O 7-δ and NdBa 2 Cu 3 O 7-δ , showed orthorhombic crystal system and space group P m m m. Fig. 4 – Amplification of 2500x the straight section of the samples Y (1-x) Nd x Ba 2 Cu 3 O 7-δ : a) x=0; b) x=0.1; c) x=0.5 and d)x=1. Fig.2 – Resistivity versus temperature of the samples Y (1-x) Nd x Ba 2 Cu 3 O 7-δ : a) x=0; b) x=0.1; c) x=0.2 d) x=0.5 and e) x=1 Fig.1 – X-ray diffratogram after adjustment by Rietveld refinement of the samples. CBPF’s X-ray Laboratory, resistivity and magnetic measurements, LMDS’s Laboratory for SEM characterization. PeD ANEEL, CEMIG D, CEMIG GT, CTEEP, TAESA and TBE (D712:SUPERCABO Project) and FAPERJ for financial support. The YBa 2 Cu 3 O 7-δ compound was synthesized in 1987, and was the first superconductor which showed a critical temperature above the boiling point temperature of nitrogen. In its composition, Yttrium (Y) can be replaced by various rare earth ions, which exhibit similar properties. Samples of YBa 2 Cu 3 O 7-δ (Y-123) and NdBa 2 Cu 3 O 7-δ (Nd-123) were obtained by a liquid route of acetic acid solution in distilled water. The magnetic moment analysis performed in two steps obtained irreversibility temperatures in ZFC and FC curves for the samples. These measurements confirmed the diamagnetic property of all compounds obtained over the temperature range. Fig.3 – a) Hysteresis Loop of Y123 (absence of Nd); b) Magnetization measurements versus temperature of the samples Y 0.5 Nd 0.5 Ba 2 Cu 3 O 7-δ . The results allow one to conclude that the method of wet synthesis of acetate proposed is promising for obtaining high quality powders of superconducting RE123 system, usable as starting materials to obtain sputtering targets to thin or thick superconducting films as well for the production of bulk pieces for use as levitators or current leads. b) c) d) The resistivity versus temperature curves of AC for the samples Y-123 (a) and Nd-123 (b) are shown in Figure 2. a) b) x a (Å) b (Å) c (Å) V (Å 3 ) 0 3.858435 3.877067 11.679653 174.721 0.1 3.852419 3.879487 11.687979 174.682 0.2 3.872143 3.879525 11.705256 175.830 0.5 3.880576 3.891899 11.705530 176.786 1 3.901839 3.914003 11.725516 179.070 20 30 40 50 60 70 80 (a) 2 (degrees) (b) Intensity (a.u) (c) (d) (e) a) Table 1 – Lattice parameters and unitary cell volume of the samples. 0,000 0,005 0,010 0,015 0,020 0,025 0,000 0,005 0,010 0,015 0,020 0,025 0,030 0,00 0,01 0,02 0,03 0,04 0,05 0,00 0,01 0,02 0,03 0,04 0,05 0,06 0,07 0 25 50 75 100 125 150 175 200 225 250 275 300 0,0 0,1 0,2 0,3 0,4 0,5 x=0 T x=1 x=0.2 x=0.5 x=1 Resistivity (mm. Temperature (K) a) b) c) d) e) H c1 = 288.92 Oe

Transcript of Synthesis and characterization of Y Temperature ...

Page 1: Synthesis and characterization of Y Temperature ...

-10000 -5000 0 5000 10000

-0,020

-0,015

-0,010

-0,005

0,000

0,005

0,010

0,015

0,020

Y123

Mo

me

nt (e

mu

/g)

Magnetic Field (Oe)

50 100 150 200 250 300

-0,00035

-0,00030

-0,00025

-0,00020

-0,00015

-0,00010

-0,00005

0,00000

0,00005

50 100 150 200 250 300

ZFC

Mo

me

nt (e

mu

)

x=0.5

FC

Temperature (K)

Synthesis and characterization of Y(1-x)NdxBa2Cu3O7-δ High

Temperature Superconductors by Acetate Method A. C. de Léo1, M. P. Nascimento2, U. D. Chacón2, E. M. B. Saitovitch2, M. Fontes2, M. A. Neves3, A. López1

1Universidade do Estado do Rio de Janeiro, Instituto de Física Armando Dias Tavares, RJ, Brazil. 2Centro Brasileiro de Pesquisas Físicas, RJ, Brazil.

3LMDS / Universidade Federal Rural do Rio de Janeiro, RJ, Brazil.

e-mail: [email protected]

Abstract: The REBCO (RE = Rare Earth) powder materials have a great application on industries, especially used as fault current limiters, current leads and levitators for electrical enhances and generators. In this work is presented an efficient process and

results that may contribute to improve superconducting materials of optimum quality to Melt-Textured-Growth (MTG), which are suitable for many applications.

Polycrystalline bulk samples of Y(1-x)NdxBa2Cu3O7-δ were obtained by a wet-chemical acetate method with x = 0, 0,1, 0,2, 0,5 and 1,0 as well as change the Yttrrium for the rare earth Neodymium until full replacements i.e., from YBCO to NdBCO. The acetate

route consists of a wet chemical procedure reaction with the powder Y2O3, Nd2O3, BaCO3 and CuO (99,9% purity) into a solution of 50% glacial acetic acid. This method improves the grain growth, is shorter than conventional solid state method without any

degradation in sample parameters.

The samples were submitted to X-ray powder diffraction (XRD) and the spectra obtained were fitted using Rietveld method, orthorhombic space group Pmmm was assumed, the result showed that the unitary cell average volume increases with the

Neodymium doping quantity.

The porosity of the samples was calculated with densities from the sample and XRD data, and the values are from 11% up to 23%, resulting into a high degree of granularity in those samples. Those result shows that are fewer necks on the samples than

expected by conventional method synthesis, confirmed by SEM images of cross section and superficial surfaces. It also provides information of the grains size and homogeneity.

AC electrical resistance as a function of temperature measurements and DC magnetization measurements showed that all sampleshad superconducting transition with TC >77 K, and in absence of Neodymium, the critical temperature reaches 91K. From

the analysis of the results we conclude that this method is promising for obtaining optimal high temperature superconducting cuprates in order to be used for MTG.

The X-ray diffractogram (after a Rietveld

refinement) for samples of YBa2Cu3O7-δ

and NdBa2Cu3O7-δ, showed orthorhombic

crystal system and space group P m m m.

Fig. 4 – Amplification of 2500x the straight section of the samples Y(1-x)NdxBa2Cu3O7-δ : a) x=0;

b) x=0.1; c) x=0.5 and d)x=1.

Fig.2 – Resistivity versus temperature of the samples Y(1-x)NdxBa2Cu3O7-δ : a) x=0; b) x=0.1; c) x=0.2

d) x=0.5 and e) x=1

Fig.1 – X-ray diffratogram after

adjustment by Rietveld refinement of

the samples.

CBPF’s X-ray Laboratory, resistivity and magnetic measurements, LMDS’s Laboratory for SEM characterization. PeD ANEEL, CEMIG D,

CEMIG GT, CTEEP, TAESA and TBE (D712:SUPERCABO Project) and FAPERJ for financial support.

The YBa2Cu3O7-δ compound was synthesized in 1987, and was the first

superconductor which showed a critical temperature above the boiling point

temperature of nitrogen. In its composition, Yttrium (Y) can be replaced by

various rare earth ions, which exhibit similar properties. Samples of

YBa2Cu3O7-δ (Y-123) and NdBa2Cu3O7-δ (Nd-123) were obtained by a liquid

route of acetic acid solution in distilled water.

The magnetic moment analysis performed in two steps obtained

irreversibility temperatures in ZFC and FC curves for the samples. These

measurements confirmed the diamagnetic property of all compounds

obtained over the temperature range.

Fig.3 – a) Hysteresis Loop of Y123 (absence of Nd); b) Magnetization measurements versus

temperature of the samples Y0.5Nd0.5Ba2Cu3O7-δ.

The results allow one to conclude that the method of wet synthesis of

acetate proposed is promising for obtaining high quality powders of

superconducting RE123 system, usable as starting materials to obtain

sputtering targets to thin or thick superconducting films as well for the

production of bulk pieces for use as levitators or current leads.

b)

c) d)

The resistivity versus temperature curves of AC for the samples Y-123 (a)

and Nd-123 (b) are shown in Figure 2.

a) b)

x

a (Å) b (Å) c (Å) V (Å3)

0

3.858435

3.877067

11.679653

174.721

0.1

3.852419

3.879487

11.687979

174.682

0.2

3.872143

3.879525

11.705256

175.830

0.5

3.880576

3.891899

11.705530

176.786

1

3.901839

3.914003

11.725516

179.070

20 30 40 50 60 70 80

(a)

2 (degrees)

(b)

Inte

nsity (

a.u

)

(c)

(d)

(e)

a)

Table 1 – Lattice parameters and unitary cell volume of the samples.

0,0000,0050,0100,0150,0200,025

0,0000,0050,0100,0150,0200,0250,030

0,000,010,020,030,040,05

0,000,010,020,030,040,050,060,07

0 25 50 75 100 125 150 175 200 225 250 275 300

0,00,10,20,30,40,5

x=0

T

x=1

x=0.2

x=0.5

x=1

Re

sis

tivity (

mm

.

Temperature (K)

a)

b)

c)

d)

e)

Hc1= 288.92 Oe