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Prime pagine RA2010FUS:Copia di Layout 1 - ENEA - Fusione

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094<br />

progress report<br />

2010<br />

Intensity (Arb. units)<br />

1200<br />

800<br />

400<br />

As grown<br />

Annealed<br />

42 43<br />

(200) MgO<br />

0<br />

35 45 55<br />

2θ (deg)<br />

Figure 4.8 – X–ray <strong>di</strong>ffraction θ–2θ scan of MgO<br />

film grown on Pd–buffered Ni–Cu–W. The<br />

spectra refer to the as–grown sample (full<br />

dots) and after annealing at 800 °C in vacuum<br />

(empty dots). In the inset, a detail of (200)MgO<br />

peaks. The thickness of MgO, Pd and Ni–Cu–W<br />

is 120 nm, 10 nm and 50 mm, respectively<br />

Realtive–peak–to–peak<br />

intensity (Arb. units)<br />

2×10 3<br />

a)<br />

(200) Pd<br />

b)<br />

(200) Ni–Cu–W<br />

Zr<br />

Y<br />

O<br />

Ce<br />

Ni<br />

Pd<br />

0 400 800<br />

oriented (fig. 4.8). The MgO layer is adequate for the<br />

deposition of a cap layer before YBCO deposition as tested by<br />

the heat treatment at 800 °C in vacuum.<br />

Oxidation behaviour of the Ni–W and CeO 2<br />

interface: role of<br />

Pd inter–layer<br />

Considering that oxidation at the substrate interface could<br />

influence the epitaxial growth and the mechanical stability of<br />

the whole coating architecture, the role of the Pd interlayer at<br />

the interface between NiW and CeO 2<br />

/YSZ/CeO 2<br />

buffer layer<br />

structure has been stu<strong>di</strong>ed by x–ray techniques and electron<br />

Auger spectroscopy. Extended x–ray absorption fine structure<br />

(EXAFS) analyses reveal that the inter–<strong>di</strong>ffusion process<br />

between the Pd layer and the substrate mo<strong>di</strong>fies the substrate<br />

interface composition due to the formation of an ordered<br />

Ni–Pd alloy even at temperatures as low as 600°C. At high<br />

temperatures, the oxidation mechanism is dependent on the Pd<br />

layer thickness, and competition between the NiO and the<br />

NiWO 4<br />

formation is observed. Oxidation also affects the CeO 2<br />

interface with the substrate. Auger electron spectroscopic (AES)<br />

analyses, reported in figure 4.9, reveal that the interface region<br />

is more extended than that of samples in vacuum annealed,<br />

and that outward migration of Ni and Pd in the CeO 2<br />

layer<br />

occurs. The CeO 2<br />

layer contamination results to be reduced as<br />

the Pd layer increases. The lower CeO 2<br />

contamination and the<br />

lower NiO formation could be associated to the good adhesion<br />

obtained in coated conductor samples with a Pd interlayer.<br />

4×10 3 400 800 1200 1600<br />

Realtive–peak–to–peak<br />

intensity (Arb. units)<br />

0<br />

0<br />

8×10 4<br />

4×10 4<br />

Sputtering time (s)<br />

c)<br />

Zr<br />

Y<br />

O<br />

Ce<br />

Ni<br />

Pd<br />

0<br />

0 400 800 1200 1600<br />

Sputtering time (s)<br />

Figure 4.9 – AES depth profiles for CeO 2 /YSZ<br />

samples deposited on Ni–W substrate buffered<br />

with a 50 nm Pd over layer annealed at 800 °C<br />

a) in vacuum and b) in 10 mTorr of oxygen back<br />

ground pressure. c) AES depth profiles for<br />

CeO 2 /YSZ samples deposited on Ni–W<br />

substrate buffered with a 200 nm Pd over layer<br />

annealed at 800 °C in 10 mTorr of oxygen back<br />

ground pressure. W signal is multiplied for 50<br />

Low fluorine YBCO MOD<br />

In this low fluorine method, only the Ba precursor is introduced<br />

in the coating solution as a trifluoroacetate, while other<br />

precursors are (Cu and Y)–acetate treated with an excess of<br />

propionic acid. The reaction path for YBCO formation was<br />

investigated by x–ray photoelectron spectroscopy (XPS) and<br />

<strong>di</strong>ffraction (XRD). From these analyses it resulted that the<br />

YBCO formation occurs through a rather complex mechanism<br />

involving hydrolysis of both Y and Ba fluorides and the<br />

reaction with CuO. However, this path is probably hindered by<br />

a competing reaction taking place at the same temperature<br />

range as YBCO formation (around 700–800°C). In figure 4.10,<br />

the evolution of the reaction path can be derived through<br />

x–ray <strong>di</strong>ffraction θ–2θ patterns. Within the 700–795°C<br />

temperature range the YBCO phase coexists with both<br />

Y 2<br />

Cu 2<br />

O and BaF 2<br />

phases. At 795°C, the XRD spectrum<br />

shows the presence of sharp and intense (00l) reflection of<br />

YBCO together with other <strong>di</strong>stinct peaks ascribable to the<br />

presence of residual Y 2<br />

Cu 2<br />

O 5<br />

phase, while BaF 2<br />

phase<br />

<strong>di</strong>sappears.<br />

Transport properties improvement in low fluorine YBCO MOD with artificial pinning sites<br />

The possibility of enhancing the pinning efficiency by means of artificial pinning sites created by ad<strong>di</strong>tion of<br />

BaZrO 3<br />

(BZO) has been investigated in YBa 2<br />

Cu 3<br />

O 7–x<br />

(YBCO) films grown by metallorganic decomposition<br />

(MOD) methods. YBCO and BZO coating solutions were prepared and subsequently mixed in molar ratios<br />

correspon<strong>di</strong>ng to 5, 7.5, 10, 15 mol.% BZO. A marked increase in the J c<br />

(0) value has been measured in MOD

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