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Reduced graphene oxide by chemical graphitization

by:Top-In     2020-02-10
Reduction of graphene oxide (RG-Os)
Given their potential applications in electronic and optoelectronic devices and circuits, considerable interest has been raised.
However, little is known about the chemical-induced reduction methods for graphene oxide (G-O)
In the solution and gas phase, except for the ammonia-
Although it is essential to use the vapor phase to map the hydrophilic G-
OS on pre-patterned substrate and in-situ reduction to a hydrophobic RG-Os.
In this paper, we report a new proxy reduction system (
Hydrogen acid containing acetic acid (HI–AcOH))
This allows for an efficient, one
Pan reduction of solution-phased RG-
O powder and steamphased RG-O (VRG-O)
Paper and film.
Reduced proxy system provides high quality RG-
Achieve highly conductive RG-by mass production of operating systems-OHI−AcOH. Moreover, VRG-
Ohi-acoh paper and film were prepared at low temperature (40 °C)
It was found to be suitable for flexible equipment. This one-
The Pot method is expected to promote the study of highly conductive graphene platelets. Sulfuric acid (95–97%)
Hydrogen peroxide (30 wt%)
Potassium permanganate, sodium nitrate and hydrogen acid (57 wt%)
Ammonia water (
35 weight % in water, Aldrich)
, Obtain sodium bicarbonate and acetic acid from commercial sources and use them for receiving purposes.
Perform EA on the LECO 932 primary analyzer (
Atlantic micro lab. FT-IR spectra (KBr)
Collect the instruments that use the Avatar 320 inch of the Geney heights. All UV-
Dual recording of Vis absorption spectrabeam UV-
1650 PC metering instrument (Shimadzu).
Nuclear magnetic resonance of G-O and RG-
O record samples on the spectrometer (
Brook Avance II-400)
Using MAS technology, the C core is operated at a rotation rate of 10 khz.
Nuclear magnetic resonance of RG-
O performed on a 200 MHz solid in Varian
State NMR spectrometer with 4-
Mm detector of Korea Institute of Basic Science, Daegu Center, South Korea. The direct C-
The polarization spectrum is obtained with 90 ° pulse 3.
For 8192 scans, the pulse repeat delay is 10 seconds, 5 μsec.
At 0 p, the C spectrum is referenced to TMS. p. m.
The thermal properties of graphene platelets were characterized by TGA (
TGA 1000 plus polymer lab). All RG-
O in the temperature range from room temperature to 40 ml °c, sample measurements are performed at a nitrogen flow rate of 800 min, and the ramp rate is 10 °c min. The G-
O samples are also heated from room temperature to 800 °c at 1 °c min to avoid G-
O due to rapid heating.
G offO and RG-
O afm for single layer (
Agilent Technology, Agilent 5500 AFM/SPM system).
The powder X-ray spectrum was recorded on D8-
Advanced Instruments (Germany)using Cu-Kα radiation.
Raman spectrum measurement is the use of microRaman system (
Renishaw, RM1000-In Via)
The excitation energy is 2. 41 eV (514 nm).
All XPS measurements are performed in SIGMA probes (ThermoVG)
Use monochrome Al-Kα X-
Source of radiation at 100 W
Surface analysis of graphene paper collected by optical microscope (Microscope company
, Wm0039000a S39A).
Observation of microstructure by field emission scanning electron microscope (JSM-
JEOL) 6701F/Inca energy. HR-
TEM imaging of G-O and RG-
O perform platelets and accumulate this platelets on JEOL JEM
The 2100F microscope is at 200 kilovolts.
TEM samples were prepared by disperse G-dry powderO and RG-
O homogeneous suspension is formed in distilled water and methanol, respectively.
Suspended matter is dripped on the 200 mesh copper TEM grid coated with thin amorphous carbon film.
SAED was performed in TEM.
Determine the iodine that may remain (
Ion form of iodine)
, And iodine value and iodine in RG-
O, the standard halogen ion test method is used with CIC connected to the automatic fast furnace (AQF-100).
Combustion device (AQF-
100, automatic fast Furnace)
Used for sample pretreatment.
Ion Chromatography (
761 small IC)
Used for the determination of iodine, iodine value and iodine content in the sample solution after combustion steps.
Certified halogen ion standard (each 1,000 p. p. m. solution)
It was obtained from the otchi company.
Purified with milliliters of pure waterQ plus system (Millipore Co. )
And filter the solution by 0.
45 μm membrane filter and degassing.
Oxygen and nitrogen are used for combustion at a flow rate of 400 and 200 ml minutes, respectively.
The pyrolysis is divided into two steps.
Step 1 increase the sample temperature in the Shell oven to 700-900 °c.
The second step increases the temperature of the sample to 800-1,000 °c with O in the Shell oven.
This test is 0. 10 g of RG-
O and 30% HO absorption solution. An IonPac AS9-
SC analysis column (Dionex)IonPac AG9-
SC guard column (Dionex)
The conductivity detector was used.
The eluate consists of a mixture of 1. 8mm NaCO and 1. 7 mM NaHCO.
The flow rate is 1.
5 ml min, the sample quantity is 100 μ l.
The diluted alkali absorption solution was then analyzed by ion chromatography and the concentration of halogen elements in the absorption solution was determined using the standard curve.
If the concentration of the halogen element of the absorbing solution is higher than the calibration range, it is appropriately diluted to the concentration within that range.
The contact points were measured using the SEO Phoenix 300 microscope at five different points.
Conductivity is four-
Probe conductivity test meter (MCP-T600;
Mitsubishi Chemical)
The sample is pressed into particles or paper form at room temperature. G-
O powder from natural graphite (Bay Carbon, SP-1 graphite)
Improved Hummers and orfenman methods using HSO, NaNO and KMnO.
In a typical program, 4. 0 g of G-
O scattered in 1.
5 liters of acetic acid.
Ultrasonic treatment of this dispersion is performed using Branson 1510 ultrasonic bath cleaner until it becomes clear. HI (80. 0 ml)
Then add and store the mixture for 40 hours at 40 °c by constant stirring.
The product is separated by filtration and washed with saturated sodium bicarbonate (5×100 ml)
Distilled water (5×100 ml)and acetone (2×100 ml)
And then vacuum dry overnight at room temperature to produce RG-O (2. 83 g)(). The RG-
O powder from G-
O use the Wallace method to hydrate ammonia. G-
O powder is dispersed in D. I.
Mix well with water.
Then cast from G-by solvent-O solutions (10. 0 ml)
On a clean glass petri dish (diameter, 5. 0 cm).
Water evaporates slowly on a clean bench for 2 days at room temperature, and then vacuum dries overnight at 50 °c, such (
Rectangle and circle). The G-
O place the paper in a 300 ml jar with 2.
HI 0 ML and 5.
0 ml of acetic acid.
The lid of the jar is sealed with vacuum grease and placed on the oil bath at 40 °c for 24 hours.
Subsequently, VRG-
O rinse the paper with saturated sodium bicarbonate solution, water and methanol and dry at room temperature.
Color of VRG-
O after treatment with HI steam, the paper changes from matte brown to metallic gray, indicating that the material is reduced, as shown in. The VRG-
O papers are also prepared using literature methods. The VRG-
O films are manufactured using improved methods reported elsewhere. A dilute G-
O vacuum filtration of suspended solids using a mixed cellulose ester membrane with a 25 nm hole (Millipore). The G-
O films are allowed to dry at room temperature at a 1 and attach to the substrate for the night. 0 kg weight.
The weight is removed and the membrane is dissolved in acetone to leave G-
O film on substrate. The G-
The O film is then rinsed with methanol and carefully transferred to the PET film. The G-
O/PET film is placed in a 300 ml jar with 2.
HI 0 ML and 5.
0 ml of acetic acid.
The lid of the jar is sealed with vacuum grease and placed in an oil bath at 40 °c for 24 hours.
Subsequently, VRG-
O/PET film is washed with saturated baking soda, water and methanol and dried at room temperature.
Color of VRG-
O/PET film changed from light brown to light black.
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