Following GO deposition onto a Cu foil (25-μm-thick, 99.8% purity, Alfa Aesar), the Cu foil was loaded into a CVD furnace and heated up to 1000 °C under a pressure of 1.0 Torr while 100 s.c.c.m. hydrogen gas (H2) was introduced. The growth of graphene was then performed at 1060 °C for a certain time under a gas mixture of 2 s.c.c.m. methane gas (CH4), diluted in 300 s.c.c.m. argon gas (Ar) and 60 s.c.c.m. of H2. Finally, as prepared, the sample was cooled down to room temperature with Ar and H2 after turning off the flow of CH4. After all the process was over the Cu foil was removed from the furnace for further characterization. For Raman spectroscopy and its correlated studies, the graphene samples on the Cu foil were transferred to SiO2/Si wafers (Si(100) covered by 300-nm-thick SiO2) using a poly(methyl methacrylate) (PMMA) assisted process. Briefly, the PMMA dissolved in chlorobenzene was spin-coated onto the graphene samples at 2,000 r.p.m. for 30 s. The PMMA-coated samples were placed in a Cu etchant (CE-100, Transene Company) to remove the Cu foil. After complete etching of Cu foil, the PMMA-coated samples were scooped out of the etchant using the SiO2/Si substrates. Finally, the PMMA layer was then removed with acetone and the surface was further rinsed several times with deionized water.
Cu foil
Manufactured by Thermo Fisher Scientific
Sourced in United States
Cu foil is a thin, flat sheet of copper material. It has a high electrical and thermal conductivity. The foil is made through a rolling process to achieve the desired thickness.
Automatically generated - may contain errors
Lab products found in correlation
Ammonia borane, by Merck Group (2 mentions)
Nh4 2s2o8, by Merck Group (1 mentions)
Co3o4 nanoparticles, by Merck Group (1 mentions)
Ammonium persulfate, by Merck Group (1 mentions)
Agnws, by Merck Group (1 mentions)
Sulfur, by Merck Group (1 mentions)
Mo foil, by Thermo Fisher Scientific (1 mentions)
Vg escalab250, by VG Scientific (1 mentions)
Haucl4, by Merck Group (1 mentions)
Potassium carbonate, by Thermo Fisher Scientific (1 mentions)
Graphite rod, by Merck Group (1 mentions)
Dimethyl sulfoxide (dmso), by Thermo Fisher Scientific (1 mentions)
Carbon dioxide, by Air Liquide (1 mentions)
Chelex 100 sodium form, by Merck Group (1 mentions)
Isopropanol, by Merck Group (1 mentions)
Phosphoric acid, by Merck Group (1 mentions)
Nafion solution, by Merck Group (1 mentions)
Deuterium oxide, by Merck Group (1 mentions)
Innova afm, by Bruker (1 mentions)
Turanose, by Merck Group (1 mentions)
39 protocols using cu foil
1
Chemical Vapor Deposition of Graphene
2
Scalable CVD Synthesis of Graphene Films
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The graphene films are synthesized by the CVD method. Cu foil (Alfa Aesar, 20 μm thick, 99.9% purity) was heated to 1035 °C in an atmosphere of 100 standard cubic centimeters per minute (sccm) H2 and 500 sccm Ar at low pressure of 400 Pa. After reaching 1035 °C for 10 min, 30 sccm CH4 was introduced for 15 min to grow monolayer graphene on the surface of the Cu foil. Finally, the Cu foil with graphene on the surface was cooled to room temperature in an atmosphere of 10 sccm H2 and 500 sccm Ar. By increasing the growing pressure to 2000 Pa and extending the growth time to 20 min, three-layer graphene film was prepared. Six-layer graphene was obtained by introducing 20 sccm CH4 and 100 sccm H2 under atmospheric pressure for 10 min.
3
Low-Pressure CVD Synthesis of Single-Layer Graphene
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Single-layer graphene was synthesized by the low-pressure CVD (LPCVD) on a Cu foil (25 μm, 99.999% purity, Alfa-Aesar). Before CVD, the foil was placed in the fused quartz tube and annealed at 1000 °C in a CO2 atmosphere at 700 Torr for 30 min to remove organic contaminents49 (link). Then CO2 was switched off and the chamber was evacuated. Following this, 8 sccm of H2 was introduced to purge out CO2 and to subsequently anneal the copper surface at 1000 °C. To initiate graphene nucleation, 24 sccm of CH4 was added at total pressure of 460 mTorr. After 30 min growth, the CH4 flow was switched off and the chamber was rapidly cooled down to the room temperature.
4
Graphene Liquid Cell for In-situ TEM
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Co3O4 nanoparticles were purchased from Sigma-Aldrich.
For the fabrication of the GLC, the multilayer graphene was initially
synthesized. Using Cu foil (99.8%, Alfa Aesar) as the substrate, graphene
was synthesized by using chemical vapor deposition (CVD). Then, the
Cu foil was etched with 20% phosphoric acid (H3PO4, 85%, Junsei) for 20 min for removing impurities and oxides. As
for the conditions of CVD, the temperature was set to 1050 °C
for 30 min and stabilized for 60 min under 200 standard cubic centimeters
per minute (sccm) of hydrogen (H2) gas. Subsequently, 20
sccm of methane (CH4) gas, which acted as the carbon source,
was injected for 25 min and was later cooled to room temperature at
a rapid rate. Such a synthesized multilayer graphene was transferred
to a holey carbon Au TEM grid (quantifoil, 300 mesh, hole size = 2
μm). Ammonium persulfate (0.2 M, (NH4)2S2O8, Sigma-Aldrich) was used to etch the Cu
foil for 6 h. Then, it was washed with water to remove the (NH4)2S2O8. The GLC was prepared
by dropping 20 μL of the electrolyte mixture containing Co3O4 nanoparticles, lithium hexafluorophosphate (LiPF6), and EC/DEC (v/v = 3:7) with 10 wt % of FEC on one graphene-transferred
grid and placing another graphene-transferred grid on the top.26 (link) Liquid cells were formed during spontaneous
drying by graphene sheets by the van der Waals force.
For the fabrication of the GLC, the multilayer graphene was initially
synthesized. Using Cu foil (99.8%, Alfa Aesar) as the substrate, graphene
was synthesized by using chemical vapor deposition (CVD). Then, the
Cu foil was etched with 20% phosphoric acid (H3PO4, 85%, Junsei) for 20 min for removing impurities and oxides. As
for the conditions of CVD, the temperature was set to 1050 °C
for 30 min and stabilized for 60 min under 200 standard cubic centimeters
per minute (sccm) of hydrogen (H2) gas. Subsequently, 20
sccm of methane (CH4) gas, which acted as the carbon source,
was injected for 25 min and was later cooled to room temperature at
a rapid rate. Such a synthesized multilayer graphene was transferred
to a holey carbon Au TEM grid (quantifoil, 300 mesh, hole size = 2
μm). Ammonium persulfate (0.2 M, (NH4)2S2O8, Sigma-Aldrich) was used to etch the Cu
foil for 6 h. Then, it was washed with water to remove the (NH4)2S2O8. The GLC was prepared
by dropping 20 μL of the electrolyte mixture containing Co3O4 nanoparticles, lithium hexafluorophosphate (LiPF6), and EC/DEC (v/v = 3:7) with 10 wt % of FEC on one graphene-transferred
grid and placing another graphene-transferred grid on the top.26 (link) Liquid cells were formed during spontaneous
drying by graphene sheets by the van der Waals force.
5
Graphene Synthesis via Thermal CVD
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Graphene was synthesized using conventional thermal chemical vapor deposition (TCVD). A 25-μm-thick Cu foil (Alfa Aesar, 99.8% purity) was used as a catalytic substrate for graphene growth. The Cu foil was heated to 1050°C inside the TCVD reactor under 100 sccm flow of H2 gas at a pressure of ~5 Torr for 60 min. After this pre-annealing process, which was crucial for enlarging the Cu grains and establishing a smooth surface, CH4 (2 sccm) was introduced as a carbon feedstock with H2 gas for 25 min to obtain graphene. The CH4 gas was then turned off, and the TCVD reactor was cooled to room temperature under a flow of H2 gas. The synthesized graphene films were transferred onto SiO2 (300 nm)/Si(001) substrates by a poly(methyl methacrylate)(PMMA)-assisted wet-transfer method35 (link).
6
Synthesis of Graphene on Ag Nanowires
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First, a 0.5 wt.% solution of commercially available Ag NWs (Sigma Aldrich, diameter: 60 nm and length: 10 μm) in isopropyl alcohol was spin-coated onto a hydrophilic-treated SiO2 (300 nm)/Si(001) substrate at a rotational speed of 3000 rpm for 30 s, and then immediately heated to 150 °C for 5 min to remove the solvent. Next, graphene was synthesized using a conventional thermal chemical vapor deposition (TCVD) system. A 25 μm-thick Cu foil (Alfa Aesar, 99.8% purity) was utilized as a catalytic substrate for the synthesis of graphene. The Cu foil was loaded into the TCVD chamber and pre-annealed at 1050 °C with introducing H2 (200 sccm) under a pressure of ~3.6 Torr for 2 h in order to reduction and surface flattening of the Cu catalytic substrate. After the pre-annealing process, the graphene was immediately synthesized through the introduction of CH4 (2 sccm) and H2 (200 sccm) for 80 min. Following the growth of the graphene, the TCVD reactor was cooled down to room temperature with H2.
7
Graphene Synthesis via LPCVD
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A poly-crystal graphene monolayer was grown using a low-pressure chemical vapor deposition (LPCVD) method on a Cu foil (0.025 mm thick, Alfa Aesar, Waltham, MA, USA) Cu foil was immersed in nitric acid in deionized water (DI) for 40 s and then washed in DI to remove the native oxide. The Cu was immediately loaded into an LPCVD chamber and annealed at 1000 °C (heating rate 15 °C/min) for 30 min in a hydrogen atmosphere (100 sccm). Then graphene was grown at 1000 °C, 60 min, and total pressure was 100 torr (CH4:H2 = 1:100). After growth, as grown graphene on Cu was cooled down to room temperature under vacuum.
8
CVD Synthesis of MoS2 and Graphene Films
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We first synthesized MoS2 film via CVD using precursor powders, including MoO3 (99.999%, Advanced Chemicals, Altona, Australia) and sulfur (99.9% Sigma Aldrich, St. Louis, MO, USA). Each precursor was placed into two ceramic crucibles. A MoO3 crucible was placed at the center of a 1 inch quartz tube, and a sulfur crucible was positioned upstream of the MoO3 crucible. A Si/SiO2 substrate was loaded downstream of the MoO3 crucible. Then, the furnace was heated to 650 °C and maintained at this temperature for 40 min with a flow of Ar (50 sccm) under 0.3 Torr. After finishing the reaction, natural cooling was performed with 200 sccm of Ar flow. Graphene monolayer film was also synthesized on Cu foil (Alfa Aesar, Haverhill, MA, USA) via identical CVD. The specific synthetic process is explained in our previous report [13 (link)].
9
Graphene Transfer Onto SiO2/Si Substrate
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The specific uses for the reagent listed in Supplementary Table S1 . Graphene was grown on Cu foil (99.8%, Alfa Aesar, Ward Hill, MA, United States) by chemical vapor deposition (CVD). Detailed synthesis methods are described elsewhere (Jeong et al., 2022 (link)). Graphene was transferred onto SiO2/Si substrates using the conventional wet transfer method (Lee et al., 2023 (link)). The graphene/Cu foil surface was coated with polymethyl methacrylate (PMMA) C4 solution (Microchem, Newton, MA, United States) in a two-step spin-coating process with rotation speeds of 500 rpm for 10 s and 3,000 rpm for 30 s. The Cu foil was then etched with CE-100 Cu etchant (Transene, Danver, MA, United States). After the Cu foil was etched, the PMMA/graphene layer was rinsed with deionized (DI) water to remove residual Cu etchant. This layer was then transferred to a SiO2/Si substrate and dried overnight at room temperature. Finally, the PMMA layer was removed by immersing the PMMA-coated substrate in acetone for 2 h, rinsed with isopropyl alcohol, and dried with blown N2.
10
Graphene Synthesis via CVD
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A typical CVD system for the fabrication of graphene is shown in the Supplementary Information SF2 . The substrate used for the graphene fabrication is Cu foil (99.8% purity from Alfa Aesar). A 25 μm thick Cu foil substrate was cleaned by acetone, isopropanol and followed by acetic acid to remove native oxide. The cleaned Cu foil was dried with nitrogen gas and then loaded into the CVD system. The CVD reaction chamber (50 mm OD quartz tube) was evacuated to 2 mBar, and then backfilled to ambient pressure with 6% H2/Ar gas. After that, the temperature was increased to 1000 °C with 6% H2/Ar gas flow of 100 sccm and the chamber pressure maintained at 20 mBar. The Cu foil was annealed at these conditions for 30 min. The graphene growth was performed by flowing 5% CH4/Ar together with 6% H2/Ar gases for 20 min with flow rates of 100 sccm and 210 sccm, respectively. Finally, the CH4/Ar flow was turned off to finish the graphene deposition and the Cu foil was cooled down naturally.
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