1. COPPER OXIDATION IN AIR ELECTROCHEMICAL REDUCTION
IN SITU
COPPER OXIDATION IN AIR
and its
ELECTROCHEMICAL REDUCTION
R. S. Huang, C. J. Lin
State Key Laboratory for Physical Chemistry of Solid Surfaces
Xiamen University, Xiamen , P. R. China
R. S. Lillard
Materials Science and Technology Division
Los Alamos National Laboratory, Los Alamos, NM 87545, USA
H. S. Isaacs
Materials Science Department
Brookhaven National Laboratory, Upton, NY 11973, USA
FUNDING U.S. Department of Energy, Basic Energy Sciences

2. Copper single crystal sphere (111) 250o C O2 30 minutes (110) 178oC
(100)
(110)
(111)
Cathcart 1956
(100)
(111)
(110)
Thickness (nm)
Time (min)
100 60
178oC

3. orientation of multi-grain samples 5 mm SEM electron backscatter
Kikuchi bands
orientation of
multi-grain samples
5 mm

4. reduction in oxidation in air Experimental 0.2 M BO3 pH 10 microscope
calomel
reference electrode
SAMPLE
counter electrode
transparent lid
transparent tape
microscope
and
annular lighting
reduction in
0.2 M BO3 pH 10
microscope
and
annular lighting
heating
element
coarse grain
Cu sample
oxidation in air

5. Air Oxidation
1 mm

6. Air Oxidation
Time (min)
350 25
Temperature ( oC )
(I)
(I)
1 mm

7. reduction in
0.2 M BO3 pH 10

8. reduction in
0.2 M BO3 pH 10
(I)
(I)
(I)

9. Current Density (mA/cm
detection of small changes
using difference imaging II
III I a c b
0.5 mm
-1.4
-0.7
-1.5 -1
-0.5 5 10 15 20
Current Density (mA/cm 2 )
Potential (V)
Time (min)
(I)
0.5mm
0.5mm b

10. * summary air borate CuO Cu2O Cu Cu+ time time Cu+ Temperature ( oC )
Time (min)
350 25
Temperature ( oC )
Cu+
CuO
Cu2O
time