aOvidius University of Constanta, 124 Mamaia Ave., 900527, Constanta, Romania bFaculty of Physics, The University of Bucharest, 405 Atomistilor St., PO Box
MG-11, RO – 077125, Magurele, Ilfov, Romania.
cNational Institute for Laser, Plasma and Radiation Physics, 409C Atomistilor
St., PO Box MG-36, 077125, Magurele, Ilfov, Romania
dAcademy of Romanian Scientists, Splaiul Independentei St, No. 54, 050094,
Bucharest, Romania
eCERONAV, 69A Pescarilor St., 900581, Constanta, Romania;
fNational Institute for Marine Research and Development “Grigore Antipa” 300 Mamaia Avenue, Constanta, Romania 90058
Journal of Ovonic Research 2022, 18(6),759-767; https://doi.org/10.15251/JOR.2022.186.759
To obtain ZrO2 and ZrO2+N2 thin films was used magnetron sputtering in radio frequency mode in a 10-6 mbar high vacuum deposition chamber. Silicon and carbon substrates measuring 12x15mm were used for deposition. The used magnetron system was composed of a single water-cooled cathode, provided with one circular targets of ZrO2 (2 mm thick and 50 mm in diameter) of high purity (99.95%). TDS Analysis of the films was performed. The desorbed species were observed with a QMG 220 Mass spectrometer provided with a W filament. It can be observed that in the case of the ZnO2 film, nitrogen desorption registers two maxima with signal intensity of 9.7x10- 12 and 9.0x10- 12, reached after 2000s and 4900s respectively. In the case of ZrO2+N2 film, nitrogen desorption shows a pronounced maximum with a signal intensity of 2.4x10- 11 reached after 6000s. .
The topology the ZrO2 and ZrO2+N2 samples deposited on Si substrates
have been investigated by scanning electron microscopy (SEM) using a FEI
Inspect S scanning electron microscope ( Hillsboro, Oregon, OR, USA) in
high-vacuum modes. For the ZrO2 deposition, the surface appears to have
grain-like topology, with a mean dimension of around 150 nm. These
structures do not appear for the ZrO2+N2 deposition. Instead, for the
ZrO2+N2 sample, small blisters (between 300 nm and 1.000nm) have formed
on the surface, as a consequence of injecting N2 during the deposition.
Cross-section measurements were also performed to establish the layer
thickness. The ZrO2 sample has a measured thickness of 1950nm, while the
introduction of N2 gas for the ZrO2+N2 sample had a poisoning effect on
the magnetron target that led to a decrease (5 times) in deposition
rate, giving this sample a final thickness of 365nm (compared to 1950nm)
for the same deposition The crystalline structure was investigated using
X-Ray Diffraction (XRD) method. The experimental set-up was composed of
a diffractometer equipped with a Cu-Kα X-ray sourse, with a specific
wavelength of 0.154nm, in a Bragg-Bretano type geometry. In this way, a
crystalline phase corresponding to ZrO2 with a group symmetry Fm-3m
(225)-face centered cubic was identified.
At
the same time, it is observed that the films deposited in the reactive
atmosphere show a pronounced amorphization, this most likely being due
to the retention of nitrogen which leads to the modification of the
network parameters.

