PREPARATION OF TUNGSTEN TRIOXIDE, WO3

Method 1 :

1. In a typical synthesis, 10 mg of W powder was taken in a vial containing 10 ml of distilled

water (pH 6.5).
2. After sonication, samples prepared have been kept at different temperatures ranging from
50 to 100C in an oven at different reaction times from 12-72h.
3. Distilled water has been used throughout the experiment.
4. Afterwards the mixture was centrifuged to reclaim the precipitated sample.
5. Final product was vacuum dried.

W(s) + 3H2O (l) WO3 (s) + 3H2 (g)

Reference : A Novel Approach for the Synthesis of Tungsten Trioxide Nanostructures

Method 2 :

1. HCl (150 ml, 0.7 M) was carefully added to 500 ml of 0.1 M Na2WO4 solution until the final
pH of the clear solution reached a value of 1.6.
2. The clear solution thus obtained was autoclaved at 60C for 48 h.
3. A white precipitate appeared within 1 h.
4. After 48 h of autoclaving the white precipitate was isolated by decantation an
centrifugation, washed several times with doubly distilled water and then dried in a Petri
dish at 60C for 48 h.
5. The color of this sample did not change from first appearance to its isolation.

Reference : Synthesis of tungsten trioxide hydrates and their structural properties

Method 3 :

1. The WO nanostructures were synthesized by precipitation technique from aqueous solutions

of ammonium tungstate para pentahydrate ((NH4)10W12O41.5H2O. Wako) and nitric acid
(HNO3, Merck).
2. A pre-determined amount of the tungstate salt was dissolved in de-ionized water and the
resulting solution was brought to 80C.
3. With vigorous stirring, a warm, concentrated nitric acid was added dropwise. The amounts
of the tungstate salt and nitric acid were used such that the nal concentrations of both
reactants were in the range of 5.316.0 mM and 1.56.0 M, respectively, to study the effect
of reactant concentrations on a precipitation rate and yield of the precipitating product.
4. With continuous stirring, the mixed solution was kept at 80C for 3060 min, after which the
precipitates were allowed to settle for 1 day at room temperature.
5. The precipitate was washed by addition of a large amount of de-ionized water into the
precipitate followed by stirring for about 10 min and allowing the precipitates to settle down
overnight before decanting the liquid.
6. This washing procedure was carried out twice.
7. Finally, the precipitates were separated by ultraltration using a polymer membrane (pore
size = 0.47 mm).
8. After drying at 100C overnight, the precipitates were calcined in air at temperatures
ranging from 150 to 800C for 2 h.
9. In some experiments, the asprecipitates were dried at room temperature under vacuum
before subjected to crystal structure analysis.

Reference : Synthesis of tungsten oxide nanoparticles by acid precipitation method

PREPARATION OF NICKEL OXIDE, NiO

Method 1:

1. NiO was prepared by dissolving 0.1 M of Nickel(II) chloride hexahydrate (NiCl2.6H2O),

0.1M of hexamethylenetetramine(HMT,C6H12N4) in 50 mL deionized water.
2. Hydrothermal growth was carried out at 200C in an autoclave placed in a furnace for 4hr.
3. The obtained particles were washed with distilled water several times and dried at room
temperature in air for further characterisation.
4. The obtained particles were annealed for 1 hour at 500C.

Reference : Preparation and Characterisation of ZnO/NiO Nanocomposite Particles for Solar Cell
Applications

PREPARATION OF CoO

Method 1

1. Cobalt acetate (Co(CH3COO)24H2O), anhydrous ethanol (CH3CH2OH) and polyethylene

glycols 4000 (PEG 4000) are analytic grade reagents and purchased without further
treatment.
2. In a typical reaction, 4mmol (Co(CH3COO)24H2O) and 50mL (CH3CH2OH) were sealed in a
Teflon lined stainless steel autoclave of 100mL capacity allowing 5060% filling.
3. The autoclave was kept at 150C for 24h under continuous stirring.
4. Then, it was cooled down to room temperature.
5. The brownish black insoluble solid products in ethanol were collected by centrifugation and
washed with anhydrous ethanol for several times.
6. Finally, a high yield (>92%) of CoO particles was obtained after the products were dried in air
at room temperature.

Reference : Synthesis of CoO nanoparticles by esterification reaction under solvothermal conditions

Method 2 ( Preparation of NiO and CoO nanoparticles)

1. The nanoparticles were synthesis in two steps:

rst to prepare an M 2+ -oleate (M = Ni, Co) precursor and
second to decompose the precursor.
2. To prepare M2+ -oleate (M = Ni, Co), the reported work was followed [16].
3. Typically, 1.18 g of NiCl2.6H2O(5mM) and 1.18 g of CoCl2.6H2O (5 mM) were dissolved in a
mixture solution containing 6 ml of water, 8 ml of ethanol and 14 ml of hexane, respectively.
4. Each resulting solution was added by 3.04 g sodium oleate (10 mM) under vigorous stirring
for 4 h at 70C.
5. The precipitate was separated in a separatory funnel and washed three times with 3 ml of
water.
6. Then, the aqua Ni-oleate and wine Co-oleate were dried under vacuum condition overnight.
7. To synthesize NiO nanoparticles, about 5 mM Ni-oleate and 2 mM oleic acid were dissolved
in 15 ml of 1-octadecene.
8. The mixture was heated to 320 C with a constant heating rate of 3.3 C/min and kept at
that temperature for 30 min.
9. After the resulting solution was cooled, NiO nanoparticles were collected by addition of
excess ethanol.
10. The synthesis of CoO nanoparticles was the same with that of NiO nanoparticles.

Reference : Preparation of NiO and CoO nanoparticles using M2+ -oleate (M = Ni, Co) as precursor
PREPARATION OF WO3/g-C3N4 (Catalyst preparation)

1. The chemicals used in this work, melamine (C3H), dicyanodiamide(C2H4N4), and tungstic
anhydride powder (WO6), were reagent grade
2. Metal-free g-C3N4 powders were synthesized by heating mixed melamine an dicyanodiamide
powder in a mufe furnace.
3. In a typical synthesis, 2.0 g of melamine and 2.0 g of dicyanodiamide were well mixed using
a mortar.
4. After mixing, the powder was placed in a semi-closed alumina crucible with a cover.
5. The crucible was heated to 550C and held for 4 hr at a heating rate of 2.2Cmin-1 .
6. After the reaction, the alumina crucible was cooled to room temperature.
7. The product was then collected and ground into powder.
8. The synthesized g-C3N4 and WO3 powders were mixed using an agate mortar.
9. The mixed mass ratios in this work were as follows : g-C3N4:WO3= 8:2, 6:4, 4:6, 2:8.

Reference : Preparation of graphitic carbon nitride (g-C3N4)/WO3 composites and enhanced visible-
light-driven photodegradation of acetaldehyde gas