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Synthesis of VO2

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30 views4 pages

Synthesis of VO2

Uploaded by

rishitheweird
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Synthesis of VO2

VO2
Vanadium(IV) oxide or vanadium dioxide is an inorganic compound with the formula VO2. It
is a dark blue solid. Vanadium(IV) dioxide is amphoteric, dissolving in non-oxidising acids to
give the blue vanadyl ion, [VO]2+ and in alkali to give the brown [V4O9]2− ion, or at high
pH [VO4]4−. At temperatures below Tc = 340 K (67 °C), VO2 has a monoclinic crystal
structure.

Materials
Vanadium pentaoxide (V2O5, 99 %), oxalic acid dihydrate (C2H2O4⋅2H2O, 99 %), hydrogen
peroxide (H2O2, 30 wt%), ethanol and deionized water

Approach
To synthesize VO2, we utilize a bottom up approach.
What is a bottom up approach?
In this method, materials are synthesized by building them from molecular or atomic
precursors, forming more complex structures through chemical reactions. The vanadium
pentoxide (V₂O₅) is dissolved and chemically processed with H₂O₂ and oxalic acid, leading
to the formation of vanadium oxide nanoparticles through controlled reactions and thermal
treatments.
In our case:
1. We start with molecular precursors (V₂O₅ and H₂O₂).
2. These precursors undergo chemical transformations (with oxalic acid as a reducing agent).
3. The material evolves into more complex structures (orange-yellow sol, blue-green
precursor, and finally VO₂(M) nanomaterials).
4. The annealing step crystallizes the material into the desired phase (VO₂ M-phase), a
critical part of bottom-up methods.

Sol is aged for one day Addition of oxalic acid


dihydrate
Sol containing of H202
and V2O5 Orange red sol is prepared
Annealing at Solution is kept in
Black powder of 550°C vacuum drying oven
M-phase VO2 is Formation of blue green
Top-up obtained precursor powders
approach
In a top-down approach, the synthesis begins with a bulk material, which is then broken
down into smaller structures, typically by physical or mechanical methods like milling,
etching, or lithography.
Since we are starting with molecular precursors and building up to the nanostructured VO₂
powders through chemical processes, this is clearly a bottom-up synthesis approach.

Process
1. Initial Reaction of V₂O₅ with H₂O₂ (Orange-Yellow Transparent Sol)
We prepare a 30 ml of solution of concentration 20% weight. We weigh 0.3 g of V2O5 and add
it to the solution. We stir it magnetically in an ice water bath to obtain a homogeneous
orange-yellow transparent sol.

Reaction of V₂O₅ with H₂O₂ to form Orange-Yellow Transparent Sol


-V₂O₅ + H₂O₂ → [V(O₂)]ⁿ⁺ (Orange-Yellow Sol):
When vanadium pentoxide (V₂O₅) reacts with hydrogen peroxide (H₂O₂), it forms
peroxovanadate complexes. These complexes are often yellow to orange-yellow in color,
which accounts for the color of the transparent sol.
Why we use Ice Bath?
The ice water bath is used to control the temperature and prevent the decomposition of the
hydrogen peroxide. At lower temperatures, the peroxovanadate species remain stable, and the
reaction proceeds without unwanted side reactions. H₂O₂ is quite reactive and can
decompose easily at higher temperatures, which would reduce its effectiveness in reacting
with V₂O₅.
2. Formation of Orange-Red Gel (Aging for 1 Day)
The orange-yellow transparent sol is aged for 1 day until it changed to orange-red gel.

- [V(O₂)]ⁿ⁺ (Orange-Yellow) → Reduced Vanadium Complex (Orange-Red Gel)


- As the reaction mixture aged, the peroxovanadate complex gradually hydrolyzes, leading to
the formation of an orange-red gel. This gel contains vanadium species in lower oxidation
states, possibly involving partial reduction of vanadium from V⁵⁺ to V⁴⁺.
3. Addition of C₂H₂O₄·2H₂O (Oxalic Acid Dihydrate)

We will weigh 0.623 g of C2H2O4⋅2H2O and add it to the orange-red gel. We will stir it and
heat to 80◦C to generate a clear blue solution
Reaction with Oxalic Acid
- V⁵⁺/V⁴⁺ + C₂H₂O₄ → VO²⁺ (Blue Solution)
When oxalic acid (C₂H₂O₄·2H₂O) is added, it acts as a reducing agent. The oxalate anion
reduces the vanadium in the gel further, leading to the formation of lower oxidation state
vanadium compounds, including V⁴⁺ species like VO²⁺. This reduction causes the color to
change from orange-red to blue, which is characteristic of vanadyl ion (VO²⁺).
The solution is then transferred to a vacuum drying oven.
4. Vacuum Drying (Blue-Green Precursor Powders)

The solution is kept at 80°C for over 12 hours.


During vacuum drying at 80°C, the blue solution undergoes further evasporation and
concentration to obtain the blue green precursor powders. The formation of blue-green
powders suggests the presence of mixed vanadium oxide phases, possibly including hydrated
or intermediate oxide forms such as VO₂·xH₂O or V₂O₃. No chemical changes
5. Annealing at 550°C to Obtain VO₂(M)
We take a fixed amount of precursor powders and anneal it at 550 ◦C for 10 min with heating
rate of 10 ◦C/min in to obtain black VO2(M) powders.
When the blue-green precursor is annealed at 550°C, the thermal energy causes the precursor
to decompose, driving off residual water and organic components from oxalic acid. The high
temperature also induces the final reduction of vanadium to V⁴⁺, resulting in the formation of
VO₂ (M-phase), which is black in color. The heating rate of 10°C/min ensures a controlled
transformation to the desired monoclinic phase (VO₂ M), known for its thermochromic
properties.

Conclusion
 Vanadium pentoxide (V₂O₅) is dissolved and chemically processed with H₂O₂ and
oxalic acid, leading to the formation of vanadium oxide nanoparticles through
controlled reactions and thermal treatments.
 In this work, spherical VO2(M) nanoparticles were synthesized by a simple and
efficient sol-gel method combined with post-annealing.
 Upon annealing, the reduction is completed, and the material transforms into the black
monoclinic VO₂(M-phase).

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