Title : Hydrothermal synthesis of CdSe

Hydrothermal
synthesis of transitionDendrite
HyperBranched
hierarchical dendrites using ionic liquid asDetail Experimental
metal sulfideProcedure
dendrites or microspheres
template
with functional imidazolium salt
Material/Chemical Used:
1. [C16mim]Cl
2. Cd(NO3)24H2O
3. Deionized water
4. Na2SeO35H2O
5. N2H4H2O
1.25 mL)

(0.2 g)
(0.077 g)
(7.5 mL)
(0.04 g)
(80%,

EquipmentUsed:
1. Teflon-lined autoclave
2. Centrifuge
Test Conducted:
1. X-Ray Diffraction (XRD)
2. Scanning Electron Microscopy
(SEM)
3. Transmission Electron Microscopy
(TEM)
4. High Resolution TEM (HRTEM)
5. UV-vis absorption spectrometer
6. Energy-dispersive spectrometer
(EDS)
Experimental Procedure:
1. All chemicals were analytical-grade and
used without further purification.
2. According to the literature [8],
[C16mim]Cl was fabricated and its
structure is shown below:

3. In the synthesis, Cd(NO3)24H2O (0.077

g) was dissolved into deionized water
(7.5 mL) and put into a Teflon-lined
autoclave.
4. then, Na2SeO35H2O (0.04 g) and
[C16mim]Cl (0.2 g) were added in the
solution with stirring for 10 min.
5. finally, N2H4H2O (80%, 1.25 mL) was

Material/Chemical Used:
1. [BMIM][SCN]
2. MCl2 (M= Cd, Co, Cu) or
M(CH3COO)2
(M= Pb, Zn)
1mmol
3. [BMIM][SCN]
2mmol
4. Distilled water
(10 ml)
5. Ethanol
( 5ml )
Equipment Used:
1. 50ml Teflon-lined stainless-steel
autoclave

Template-free synthesis of CuSCN and

CU2S Crystallites with a facile
hydrothermal method at different
temperatures.
Material/Chemical Used:
1. 2 mmol ionic liquid ([BMIM]SCN)
2. 1 mmol copper chloride (CuCl2)
3. 10ml of distilled water
4. Ethanol (washing purposes)

Equipment Used:
1. 50ml Teflon-lined stainless-steel
autoclave.

Test Conducted:
1. X-Ray Diffraction (XRD)
2. Scanning Electron
Microscopy (SEM).
3. Energy dispersive X-ray
Spectroscopy (EDX)

Test Conducted:
1. X-ray powder diffraction (XRD)
2. The scanning electron microscope
(SEM)
3. Energy dispersive X-ray
spectroscopy (EDS)
4. UV-vis absorption spectrometer

Experimental Procedure:
1. All chemicals used in our
experiment were analytical-grade
and without further purification.
2. The 1-butyl-3-methlyimidazole
thiocyanate ([BMIM][SCN]) was
prepared according to the
literature.
3. The preparation of transition-metal
sulfide dendrites or microspheres
involves the precipitation ofM2+
(M= Cd, Pb, Zn, Co, Cu) and SCN
at a consequent hydrothermal
treatment at 200 C for 24 h.
4. A typical procedure of transitionmetal sulfide is as follows: 1mmol
corresponding MCl2 (M= Cd, Co,
Cu) or M(CH3COO)2 (M= Pb, Zn)
and 2mmol [BMIM][SCN] were
dissolved in distilled water (10 ml),

Experimental Procedure:
1. All chemicals used in our
experiment were of
analytical-grade and used without
further purification;
2. 1-butyl-3 methlyimidazole
thiocyanate ([BMIM]SCN) was
prepared according to the literature.
3. In a typical procedure of preparing
Cu2S microspheres,2 mmol ionic
liquid ([BMIM]SCN) and 1 mmol
copper chloride (CuCl2) were
dissolved in two beakers containing
10ml of distilled water.
4. Two clear solutions were mixed
together
with addition of 5 ml ethanol and
vigorous magnetic stirring at room
temperature.

Nanorod/Nanowires Detail Experimental Procedure

Effect of ionic liquid amount (C8H15BrN2)
on the morphology of Bi2Te3 nanoplates
synthesized via a microwave-assisted
heating approach.

Electrodeposition of nanocrystalline silver

films and nanowires from the ionic liquid 1ethyl-3-methylimidazolium
trifluoromethylsulfonate

An active nano-supported interface

designed from gold nanoparticles
embedded on ionic liquid for depositing
DNA.

Material/Chemical Used:
1. Bismuth nitrate (Bi(NO3)35H2O,
(0.5 mmol),
2. Telluride powder (Te, 0.75 mmol)
3. potassium hydroxide (KOH, 0.3 g)
4. 1-butyl-3-methylimidazolium bromide
(C8H15BrN2, 1 g)
5. 15mL of ethylene glycol

Equipment Used:
1. microwave oven
2. centrifuge

Test Conducted:
1. X-ray diffraction (XRD)
2. Field emission scanning electron
microscope (FE-SEM)
3. transmission electron microscope
(TEM)

Experimental Procedure:
1. All reagents were commercially
available and used without further
purification.
2. In a typical procedure, bismuth
nitrate (Bi(NO3)35H2O, 0.5 mmol),
telluride powder (Te, 0.75 mmol),
potassium hydroxide (KOH, 0.3 g)
and an ionic liquid 1-butyl-3methylimidazolium bromide
(C8H15BrN2, 1 g) were dissolved in
15mL of ethylene glycol.
3. After vigorous magnetic stirring for 2
h, the solution was put into the
microwave oven and heated for 10
min.
4. Microwave assisted reactions were
conducted

Material/Chemical Used:
1. 1-ethyl-3-methylimidazolium
trifluoromethylsulfonate [EMIm]TfO
2. Silver trifluoromethylsulfonate
3. Acetone
4. Isopropanol
5. nuclear track-etched polycarbonate
membranes (Millipore) with pore
diameters of 100 nm.
6. Platinum wire (Alfa, 99.99%)
7. Silver wire (Alfa, 99.99%)
Equipment Used:
1. Verstat 263A
Potentiostat/Galvanostat (Princeton
Applied Research)
2. Electrochemical cell made of
polytetrafluoroethylene (Teflon)
Test Conducted:
1. Field emission scanning electron
microscope (FE-SEM)
2. X-ray diffraction (XRD)
Experimental Procedure:
1. The electrodeposition of silver was
studied in the water and air stable
ionic liquid 1-ethyl-3methylimidazolium
trifluoromethylsulfonate
[EMIm]TfO with high purity (Merck).
2. The ionic liquid was used as received
without further purification or drying.
3. The viscosity and conductivity of the
employed ionic liquid at 20 C were
reported to be 45mPa s and
8.6mScm1, respectively.
4. Silver trifluoromethylsulfonate (Alfa,
99%)was used as a source of silver
due to its high solubility in the
employed ionic liquid.

Material/Chemical Used:
1. Calf thymus DNA (ct-DNA)
2. [BMIM]BF4 (>99%)
3. TrisHCl buffer solution (THB).
4. 0.1 M H2SO4
Equipment Used:
1. Electrochemistry workstation (CHI660A, CHI, USA)
2. Three-electrode cell with a glassy
carbon electrode (GCE)
3. platinum wire auxiliary electrode
4. saturated calomel electrode (SCE)
reference electrode
Test Conducted:
1. electrochemical measurements and
impedance spectroscopy
2. X-ray photoelectron spectroscopy
(XPS)
3. Atomic force microscopy (AFM)
4. Scanning electron microscope (SEM)

Experimental Procedure:
1. Calf thymus DNA (ct-DNA) was
purchased from Sigma.
2. [BMIM]BF4 (>99%) was obtained
from J&K Chemical Ltd. They were
used as received without further
purification.
3. All other chemicals were of analytical
grade.
4. Solution of DNA was freshly prepared
in 5 mM pH 7.4 TrisHCl buffer
solution (THB).
5. All solutions were prepared using
doubly distilled water.
6. All electrochemical measurements
and impedance spectroscopy were
performed on an electrochemistry

5.

6.

7.

8.

9.

in an 800W microwave oven, with a

2.45GHz working frequency.
In all experiments, the microwave
oven was cycled as follows: on for 40
s, off for 60 s.
At the end of the reaction, a great
amount of black precipitate was
obtained.
After cooling to room temperature,
the precipitates were centrifuged,
washed with water and absolute
ethanol in sequence, and dried under
vacuum at 60 C for 12 h.
The phase structure characterization
of the samples was examined by Xray diffraction
(XRD) in the 2 range 2080 using
Cu-K X-ray source ( = 0.15418 nm)
with voltage
and current of 40 kV and 100 mA,
respectively.
The morphology of as-prepared
samples was observed by a field
emission scanning electron
microscope (FE-SEM,JEOL S4800) and
transmission electron microscope
(TEM, JEOL JEM 2100).

5. All electrochemical measurements

were performed using a Verstat 263A
Potentiostat/Galvanostat (Princeton
Applied Research) controlled by
PowerCV and PowerStep software.
6. The experiments were carried out
under air with a relative humidity of
about 50% at 20 C.
7. In cyclic voltammograms measured
on gold there is no evidence for
electrochemically active water on a
timescale of about 1 h under air.
8. Gold substrates from Arrandee (gold
films of 200300 nm thickness
deposited on chromium-covered
borosilicate glass) and
glassy carbon substrates (Alfa) were
used as working electrodes,
respectively.
9. Directly before use, the gold
substrates were very carefully heated
in a hydrogen flame to red glow.
10.Glassy carbon substrates were
cleaned for 10 min in an ultrasonic
bath in acetone followed by refluxing
in isopropanol.
11.For Ag-nanowires synthesis, nuclear
track-etched polycarbonate
membranes (Millipore) with pore
diameters of 100 nm were used as
templates.
12.The back side of the membrane was
sputtered by a roughly 100nm thick
gold film to serve as a working
electrode.
13.The Au-coated side was placed onto
a copper plate connected to the
potentiostat.
14.The electrochemical cell made of
polytetrafluoroethylene (Teflon)was
clamped over a Teflon covered Viton

workstation (CHI-660A, CHI, USA).

7. All electrochemical experiments
employed a
three-electrode cell with a glassy
carbon electrode (GCE) as working
electrode, and a platinum wire
auxiliary electrode and a saturated
calomel electrode (SCE) reference
electrode.
8. Experiments were carried out at 20
2C.
9. Scanning electron microscope (SEM)
image was obtained on a JEOL 6500F
scanning electron microanalyser
(NEC).
10.X-ray photoelectron spectroscopy
(XPS) spectra were recorded on a
spectrometer using Mg K X-ray
radiation.
11.Atomic force microscopy (AFM) image
were recorded on a SPA 300HV with
silicon tip in
tapping mode at room temperature.

DNA deposition
1. A GCE (3 mm in diameter) was
polished repeatedly with 1.0,0.3, and
0.05 m alumina slurry, followed by
successive ultrasonic cleaning in
acetone and doubly distilled water for
5 min.
2. The cleaned GCE was treated by
cyclic voltammetry scanned in the
0.1 M H2SO4 solution between 0 and
+1.0 V at a scan rate of 50 mV s-1 for
10 cycles.
3. Then, the electrode was immersed in
pure
[BMIM]BF4 solution for 10 h at 4 8C.
4. After thoroughly rinsed with water,
electrodeposition process was

o-ring onto the other side of the

membrane, thus yielding an exposed
surface area of 0.6cm2.
15.A platinum wire (Alfa, 99.99%) and a
silver wire (Alfa, 99.99%) were used
as counter and reference electrodes,
respectively.
16.The electrode potential of the
reference electrode was calibrated in
several experiments vs.
ferrocene/ferrocinium. Its electrode
potential exhibits sufficient stability
throughout the experiments.
17.The redox couple
ferrocene/ferrocinium has a value of
+320mV vs. Ag reference.
18.A high resolution field emission
scanning electron microscope (Carl
Zeiss DSM 982 Gemini) was utilized
to investigate the surface
morphology of the deposited films
and energy dispersive X-ray analysis
was used to determine the film
composition.
19.The X-ray diffractograms of the
deposited silver samples were
recorded using a Siemens D-5000
diffractometer with Co K radiation.

accomplished with cyclic

voltammetry scanning between
-0.2 and +1.0 V at a scan rate of 50
mV s1 for 15 cycles from a fresh
solution containing
3 mM
HAuCl4 and 0.1 M KCl.
5. The Au nanoparticles and [BMIM]BF4
modified electrode was obtained and
denoted as NG/RTIL/GCE.
6. The ct-dsDNA deposition on
NG/RTIL/GCE was conducted in 0.1
mg ml1 ct-dsDNA solution and 5%
(v/v) [BMIM]BF4 under controlled dc
potential of 0.5 V for 15 min, it is
denoted as ct-DNA/NG/RTIL/GCE.