What is ZrO2?
In this study, ZrO2 nanomaterials were produced as powders
or thin films through solution-based processes, i.e., a hydrothermal method
assisted by microwave irradiation and solution combustion synthesis. The
microwave-synthesized powder was further calcinated at 800 ◦C for 15 min under
atmospheric conditions. The ZrO2 nanomaterials were characterized by XRD, Raman
spectroscopy, SEM coupled with energy dispersive X-ray spectroscopy (EDS) and
focused ion beam (FIB) and TEM. The thermal behavior of the nanopowder produced
under microwave irradiation was investigated through in situ XRD, and these
powders had their optical properties assessed through PL and PLE at RT. The
ZrOx thin films produced by the solution combustion synthesis were further
tested as capacitors. The ZrO2 nanoparticle synthesis route was adapted from
ref. In a typical synthesis, 50 mL of an aqueous (aq.) solution of 0.2 M of
zirconium (IV) oxynitrate hydrate is mixed with 50 mL of an aq. Solution of 0.4
M sodium hydroxide (Labchem, CAS: 1310-73-2, NaOH). The reagents were used
without any further purification. The 100 mL solution was left to stir for 30
min. The molar ratio of zirconium precursor and sodium hydroxide was kept at
1:2. Microwave synthesis was then carried out with a CEM microwave digestion
system, Matthews, NC, USA (MARS one), and the applied microwave parameters were
1000 W, 230 ± 10 ◦C and 25 min. Afterward, the previous solution was equally
distributed into Teflon vessels of 75 mL (each vessel containing 20 mL of
solution). Subsequently, the centrifugation of the resultant nanopowder was
performed for 3 min at 4750 rpm and washed three times alternately with
deionized water and isopropyl alcohol (IPA). Finally, the nanopowder was dried
in a desiccator at 60 ◦C for five h. The yield was around 0.77 g of
nanopowder/batch.
Several studies have reported the
production of ZrO2 nanomaterials
Several studies have reported the production of ZrO2
nanomaterials using sol-gel, particularly solution combustion synthesis, which
is included in the sol-gel method. Solution combustion synthesis is an
attractive technique for the preparation of ZrO2 nanopowders and thin films,
owing to its simplicity, energy and time savings, cost-effectiveness,
versatility, higher purity compared with conventional sol-gel methods, low
synthesis temperatures, and compatibility with flexible substrates and large
scale production. The synthesis of ZrO2 nanomaterials using the hydrothermal
method assisted by microwave irradiation has also been growing exponentially
over recent years, mainly due to its several advantages, such as volumetric
heating (the entire volume of solution is evenly heated instead of relying on
heat diffusion processes across the reaction vessels). The reaction times can
be shorter as it is possible to synthesize nanostructures in just a few
minutes. Furthermore, it also allows accurate control of particle morphology
and size by adjusting the microwave parameters. Upon optimization of the
synthesis parameters, such as temperature, pH, time, and zirconium oxide
precursors (e.g., zirconyl chloride, zirconyl hydroxide, zirconyl nitrate
hydrate, and zirconium alkoxides), different ZrO2 phases can be obtained.
Solution-based ZrO2 nanomaterials are a highly appealing alternative to
physical methods due to their process simplicity, high throughput, reduced
equipment cost since no vacuum-based systems are required, and the possibility
to fabricate optoelectronic devices, even at low temperatures and by using
green solvents. As indicated, a broad range of solution-based synthesis methods
have been developed to prepare ZrO2 nanomaterials; however, solution combustion
synthesis and hydrothermal synthesis/microwave irradiation are typically
preferred, so these techniques are presented in this work. The same zirconium
precursor (zirconium (IV) oxynitrate hydrate) was used in both synthesis
techniques.
Several studies have already
reported the dielectric properties of the ZrO2
Several studies have already reported the dielectric
properties of the ZrOx films produced by different solution-based processes.
For instance, Seon et al. fabricated ZrO2 films via a non-hydrolytic sol-gel
route at low temperatures, using 2-methoxyethanol (2-ME) as a solvent, with
further annealing at 300 ◦C. The solution precursors chosen were zirconium
chloride and zirconium isopropoxide, which were prepared in equimolar amounts
and acted as a metal halide and a metal alkoxide. A breakdown voltage greater
than 4 MV cm−1, a high dielectric constant (near 10), and a low leakage current
density of 5 × 10−8 A cm−2 at a field of 1 MV cm−1 were obtained. Another study
by Gong et al. showed that a low-temperature annealing treatment at 160 ◦C
could produce high-quality amorphous ZrO2 dielectric films via a low-cost
solution process. This study prepared a solution using zirconium (IV)
acetylacetonate as zirconium precursor and N-dimethylformamide as a solvent.
Hydrolysis and condensation reactions occurred during stirring of the solution
for 32 h at 90 ◦C. The films exhibited a leakage current of 3.6 × 10−5 A cm−2
at −3 V, a capacitance of ~117.1 nF cm−2, and a dielectric constant 7.8, both
at 1 KHz. Wang et al. also fabricated high-κ ZrO2-dielectric films using a lightwave
(LW) irradiation-induced chloride-based low-temperature solution route. Results
demonstrated a great capacitance of 270 nF cm−2, a high dielectric constant of
14.1 (at 100 Hz), and a low leakage current of 7.6 × 10−8 A cm−2, under 2
MV/cm. The superior performance was attributed to the effective formation of
the metal-oxygen (M-O) framework that eliminated oxygen defects. Another study
by Jung et al. demonstrated the fabrication of ultrathin ZrOx films by deep
ultraviolet irradiation, which revealed a leakage current density as low as
10−11 A cm−2 at 1 MV/cm, a capacitance of 260 nF cm−2 (at 1 MHz), high
dielectric constant (22) and good breakdown voltage (around 6 MV/cm). In
addition, Luo et al. prepared high-quality ZrO2 films using an oxygen-doped
precursor solution (ODS). The ODS-ZrO2 films showed a low leakage current
density of 10−7 A cm−2 (at 2 MV/cm), high breakdown electric field (7.0 MV/cm),
and dielectric constant 19.5. However, the challenge still relies on
fabricating metal-oxide films with a high-quality surface (a smooth surface
with a dense network) at a low temperature and through a simple approach to
guarantee a low leakage current density and high breakdown field.
Price of ZrO2
ZrO2 particle size and purity will affect the product’s
Price, and the purchase volume can also affect the cost of ZrO2. A large amount
of large amount will be lower. The Price of ZrO2 is on our company’s official
website.
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