A Gallium Phosphate Piezo-Microbalance System for High-Temperature Mass Relaxation Studies of Metal
OxidesPhilipp Simonsa,b,c, Ho-Il Jia,d, Timothy C. Davenporta,d, and Sossina M. Haile*a,d,e
a Materials Science, California Institute of Technology, Pasadena, CA 91125, USAb Department of Information Technology and Electrical Engineering, ETH Zurich, 8092 Zurich, Switzerland
c Department of Mechanical and Process Engineering, ETH Zurich, 8092 Zurich, Switzerlandd Materials Science and Engineering, Northwestern University, Evanston, IL 60208, USA
e Applied Physics, Northwestern University, Evanston, IL 60208, USA
Supplementary Information
The 10PCO powder was prepared by dissolving 22.7 g (52.3 mmol) of Ce(NO3)3·6H2O (Alfa
Aesar, 99.5%) and 2.53 g (5.81 mmol) of Pr(NO3)3·6H2O (Alfa Aesar, 99.99%) in 250 mL of
water. To this solution 25.5 g (87.1 mmol) of EDTA (Alfa Aesar, 99%) and 16.7 g (87.1 mmol)
of citric acid (Alfa Aesar, 99.5+%) was added. Subsequently, 60 mL of concentrated NH4OH
(Aldrich) was slowly added to form a homogeneous green solution which was stirred for 24
hr at 65 °C. The resulting gel was heated at 5 °C min-1 to 170 °C with a dwell for 5 hr, forming
a black foam that was ground into a powder. The powder was then heated at 5 °C min-1 to
350 °C with a dwell for 15 hr, followed by 5 °C min-1 to 950 °C with a dwell for 10 hr to form
10PCO as a red powder.
Figure S1. Scanning phase contrast images of 10PCO films deposited on (left) Ti-bearing Pt
electrodes and (right) Ti free electrodes.
20 30 40 50 60 70
10PCO (Ti-free)
10PCO (Ti-bearing)
(400)(222)
(311)
(220)(200)
Inten
sity /
a.u.
2 / o
(111)
XRD holder
Figure S2: XRD patterns of 10PCO films with Ti-free (red line) and Ti-bearing (green line)
electrodes after mass relaxation characterization. The XRD pattern of the XRD holder is
displayed as a black line for reference.
0 4 8 12 16
5458500
5459000
5459500
5460000Fr
eque
ncy
/ Hz
Time / h
Frequency / Hz Exponential Fit pO2 / atm
1E-5
1E-4
0,001
0,01
0,1
pO2 /
atm
Figure S3: Long term frequency profile of the piezocrystal with Ti adhesion layer (black) as
well as the oxygen partial pressure (red) as a function of time throughout the entire
measurement campaign. An exponential fit is performed to the base line drift, fitted through
all measurements at which ultra-high purity argon is supplied through the chamber. Fitted
function: f (t )=5.458900 ⋅106Hz+862.616Hz ⋅exp (−2.707 ⋅10−5t ). Temperature: T = 700°C.
Figure S4. Long term frequency profile of the piezocrystal without Ti adhesion layer (black)
as well as the oxygen partial pressure (red) as a function of time, throughout the entire
measurement campaign.
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