Patent
US 8,906,337Method for Preparing Graphene by Using Two-dimensional Confined Space between the Layers of Inorganic Layered Materials
Wensheng Yang
US
Copyright © 2026 Matter42. All rights reserved.
Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Amendments to the Claims: This listing of claims will replace all prior versions, and listings of claims in the application: Listing of Claims 1. A preparation method for graphene, comprising the following steps: (1) mix a soluble salt of a divalent metal ion M 2+, a soluble salt of a trivalent metal ion M'+, a soluble salt of a chain alkyl anion A-and a carbon source molecule C and dissolve them in deionized and C O 2-eliminated water to prepare a mixed salt solution; mix the mixed salt solution with an alkali solution under nitrogen protection and subject them to reaction and crystallization at 60 ° C to 80 ° C for 6 to 10 hours under nitrogen, filter the suspension obtained thereafter and wash the filter cake with deionized water until the pH of the filtrate is 7 to 7.5, and then dry the filter cake at 50 ° C to 60 ° C for 6 to 12 hours to obtain layered double hydroxides with an intercalated structure having a general chemical structure of: SVG 13980715.08-12-2014.HYRKVOM₄PXXIFW3.CLM.1.svg 0.19 2.41 Black and white wherein, x is 0.2-0.33, a is 0.2-6.6, and p is 0.3-3; (2) under an inert atmosphere or a reducing atmosphere, calcinate the layered double hydroxides with an intercalated structure to provide a calcinated product at a calcination temperature of 700 ° C to 950 ° C for a period of time of 0.5 to 3 hours; (3) add the calcinated product into a hydrochloric acid solution with a concentration of 5 wt% for ultrasonic treatment, and separate the solution by centrifugation and wash the precipitate obtained by centrifugation with deionized water until the pH of the filtrate is 6.5 to 7 to obtain the graphene.
The preparation method according to claim 1, wherein, in step (1), the soluble salt of the divalent metal ion M is one or more of a nitrate, a sulfate, an oxalate or a chloride of Mg or Zn; and the soluble salt of the trivalent metal ion M 'i3 is one or more of a nitrate, a sulfate, an oxalate or a chloride of Al.
The preparation method according to claim 1, wherein, the molar ratio between the divalent metal ion M₂ + and the trivalent metal ion M 'i3 is 2 to 4: 1.
The preparation method according to claim 1, wherein, in the mixed salt solution, the overall concentration of the divalent metal ion M₂ + and the trivalent metal ion M' 3+ is 0.2 to 0.5 mol/L.
The preparation method according to claim 1, wherein, in step (1), the soluble salt of the chain alkyl anion A-is one or more of sodium dodecyl sulfate, sodium dodecyl sulfonate, sodium dodecyl benzene sulfonate, potassium dodecyl sulfate, potassium dodecyl sulfonate and potassium dodecyl benzene sulfonate.
The preparation method according to claim 1, wherein, in the mixed salt solution in step (1), the number of moles of the chain alkyl anion A- is equivalent to the number of moles of the trivalent metal ion M'3 +.
The preparation method according to claim 1, wherein, in step (1), the carbon source molecule C is one or more of methyl methacrylate, n-pentane, benzene, toluene, xylene, and styrene.
The preparation method according to claim 1, wherein, in the mixed salt solution, the number of moles of the carbon source molecule C is 1 to 20 times of the number of moles of the trivalent metal ion M'3 +.
The preparation method according to claim 1, wherein, in step (1), the alkali solution is a solution prepared by dissolving sodium hydroxide or potassium hydroxide into deionized and CO 2 -eliminated water with a concentration of 2 to 5 mol/L.
The preparation method according to claim 1, wherein, the number of moles of the alkali in the alkali solution is twice of the total number of trivalent metal ion M'3 +.
The preparation method according to claim 1 nitrogen atmosphere or an argon atmosphere, and atmosphere.
The preparation method according to claim 1 between the calcinated product and the HCl solution
The preparation method according to claim 1 ultrasonic treatment is 0.5 to 2 hours.
The preparation method according to claim 1 centrifugation is 5000 to 9000 rpm.
Embodiments described in the patent, grouped by the materials and process steps they use.
6 materials3 process steps
Preparation of single-layer graphene (G₁) via intercalated layered double hydroxides (LDH-1). Magnesium nitrate hexahydrate (0.075 mol), aluminum nitrate nonahydrate (0.025 mol), sodium dodecyl sulfate (SDS, 0.025 mol), and methyl methacrylate (MMA, 0.03 mol) dissolved in 300 mL deionized CO₂-eliminated water. NaOH solution (80 mL, 2.5 mol/L) dripped in under nitrogen; mixture reacted at 80°C for 8 hours under nitrogen atmosphere; filtered, washed (pH 7.2), dried at 50°C for 12 hours to give LDH-1 with interlayer spacing 2.4 nm (003 peak by XRD and TEM). LDH-1 then calcinated and acid-treated to yield single-layer graphene G1.
1 material1 process step
Preparation of two-layer and three-layer graphene (G₂) via intercalated LDH-2. Similar procedure to Example 1 with different ratios/conditions to yield 2-to-3-layer graphene, characterized by high-resolution TEM (Fig. 6, 7, 8).
1 material1 process step
Preparation of multi-layer graphene G₃ (4 to 6 layers) via intercalated LDH-3. Similar procedure yielding multi-layer graphene, characterized by high-resolution TEM (Fig. 9, 10) and Raman spectroscopy (Fig. 11).
Materials described outside the worked examples.
graphene
layered double hydroxides with intercalated structure
[M₂+1-x M'3+x(OH)2]x+ A-x-a C·p H₂O
chain alkyl anion A- salt
carbon source molecule C
divalent metal ion M₂+ salt (Mg or Zn nitrate/sulfate/oxalate/chloride)
trivalent metal ion M'3+ salt (Al nitrate/sulfate/oxalate/chloride)
metal oxide
sodium dodecyl sulfate/sodium dodecyl sulfonate/sodium dodecyl benzene sulfonate/potassium dodecyl sulfate/potassium dodecyl sulfonate/potassium dodecyl benzene sulfonate
carbon source molecule C (methyl methacrylate/n-pentane/benzene/toluene/xylene/styrene)
sodium hydroxide/potassium hydroxide alkali solution
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
LDH-1 003 interlayer spacing | 2.4 nm | LDH-1 |
Temperature | 60–80 °C | — |
Temperature | 50–60 °C | — |
Temperature | 700–950 °C | — |
Duration | 6–10 hours | — |
Duration | 6–12 hours | — |
Duration | 0.5–3 hours | — |
Duration | 0.5–2 hours | — |
Related documents with shared materials, methods, properties, or citations.
Kohn-–Luttinger like superconductivity in twisted bilayer graphene at large twist angles
Symmetry-adapted closest Wannier modeling based on complete multipole basis set
Random State Approach to Quantum Computation of Electronic-Structure Properties
Low-energy model for doped graphene nanoribbons
Nonlinear thermal and thermoelectric transport from quantum geometry
GRAPHENE COMPOSITE AND METHOD OF PRODUCING THE SAME
Strain-Tunable Harmonic Responses in Valley-Polarized Bilayer Graphene
Role of ultrafast electron-optical-phonon interactions in high harmonic generation from graphene
Moiré-driven equilibrium of perturbations in moiré systems
Shaping Maximally Localized Wannier Functions via Discrete Adiabatic Transport
METHODS OF IMPROVING SINTERING OF PCD USING GRAPHENE
Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Amendments to the Claims: This listing of claims will replace all prior versions, and listings of claims in the application: Listing of Claims 1. A preparation method for graphene, comprising the following steps: (1) mix a soluble salt of a divalent metal ion M 2+, a soluble salt of a trivalent metal ion M'+, a soluble salt of a chain alkyl anion A-and a carbon source molecule C and dissolve them in deionized and C O 2-eliminated water to prepare a mixed salt solution; mix the mixed salt solution with an alkali solution under nitrogen protection and subject them to reaction and crystallization at 60 ° C to 80 ° C for 6 to 10 hours under nitrogen, filter the suspension obtained thereafter and wash the filter cake with deionized water until the pH of the filtrate is 7 to 7.5, and then dry the filter cake at 50 ° C to 60 ° C for 6 to 12 hours to obtain layered double hydroxides with an intercalated structure having a general chemical structure of: SVG 13980715.08-12-2014.HYRKVOM₄PXXIFW3.CLM.1.svg 0.19 2.41 Black and white wherein, x is 0.2-0.33, a is 0.2-6.6, and p is 0.3-3; (2) under an inert atmosphere or a reducing atmosphere, calcinate the layered double hydroxides with an intercalated structure to provide a calcinated product at a calcination temperature of 700 ° C to 950 ° C for a period of time of 0.5 to 3 hours; (3) add the calcinated product into a hydrochloric acid solution with a concentration of 5 wt% for ultrasonic treatment, and separate the solution by centrifugation and wash the precipitate obtained by centrifugation with deionized water until the pH of the filtrate is 6.5 to 7 to obtain the graphene.
The preparation method according to claim 1, wherein, in step (1), the soluble salt of the divalent metal ion M is one or more of a nitrate, a sulfate, an oxalate or a chloride of Mg or Zn; and the soluble salt of the trivalent metal ion M 'i3 is one or more of a nitrate, a sulfate, an oxalate or a chloride of Al.
The preparation method according to claim 1, wherein, the molar ratio between the divalent metal ion M₂ + and the trivalent metal ion M 'i3 is 2 to 4: 1.
The preparation method according to claim 1, wherein, in the mixed salt solution, the overall concentration of the divalent metal ion M₂ + and the trivalent metal ion M' 3+ is 0.2 to 0.5 mol/L.
The preparation method according to claim 1, wherein, in step (1), the soluble salt of the chain alkyl anion A-is one or more of sodium dodecyl sulfate, sodium dodecyl sulfonate, sodium dodecyl benzene sulfonate, potassium dodecyl sulfate, potassium dodecyl sulfonate and potassium dodecyl benzene sulfonate.
The preparation method according to claim 1, wherein, in the mixed salt solution in step (1), the number of moles of the chain alkyl anion A- is equivalent to the number of moles of the trivalent metal ion M'3 +.
The preparation method according to claim 1, wherein, in step (1), the carbon source molecule C is one or more of methyl methacrylate, n-pentane, benzene, toluene, xylene, and styrene.
The preparation method according to claim 1, wherein, in the mixed salt solution, the number of moles of the carbon source molecule C is 1 to 20 times of the number of moles of the trivalent metal ion M'3 +.
The preparation method according to claim 1, wherein, in step (1), the alkali solution is a solution prepared by dissolving sodium hydroxide or potassium hydroxide into deionized and CO 2 -eliminated water with a concentration of 2 to 5 mol/L.
The preparation method according to claim 1, wherein, the number of moles of the alkali in the alkali solution is twice of the total number of trivalent metal ion M'3 +.
The preparation method according to claim 1 nitrogen atmosphere or an argon atmosphere, and atmosphere.
The preparation method according to claim 1 between the calcinated product and the HCl solution
The preparation method according to claim 1 ultrasonic treatment is 0.5 to 2 hours.
The preparation method according to claim 1 centrifugation is 5000 to 9000 rpm.
Embodiments described in the patent, grouped by the materials and process steps they use.
6 materials3 process steps
Preparation of single-layer graphene (G₁) via intercalated layered double hydroxides (LDH-1). Magnesium nitrate hexahydrate (0.075 mol), aluminum nitrate nonahydrate (0.025 mol), sodium dodecyl sulfate (SDS, 0.025 mol), and methyl methacrylate (MMA, 0.03 mol) dissolved in 300 mL deionized CO₂-eliminated water. NaOH solution (80 mL, 2.5 mol/L) dripped in under nitrogen; mixture reacted at 80°C for 8 hours under nitrogen atmosphere; filtered, washed (pH 7.2), dried at 50°C for 12 hours to give LDH-1 with interlayer spacing 2.4 nm (003 peak by XRD and TEM). LDH-1 then calcinated and acid-treated to yield single-layer graphene G1.
1 material1 process step
Preparation of two-layer and three-layer graphene (G₂) via intercalated LDH-2. Similar procedure to Example 1 with different ratios/conditions to yield 2-to-3-layer graphene, characterized by high-resolution TEM (Fig. 6, 7, 8).
1 material1 process step
Preparation of multi-layer graphene G₃ (4 to 6 layers) via intercalated LDH-3. Similar procedure yielding multi-layer graphene, characterized by high-resolution TEM (Fig. 9, 10) and Raman spectroscopy (Fig. 11).
Materials described outside the worked examples.
graphene
layered double hydroxides with intercalated structure
[M₂+1-x M'3+x(OH)2]x+ A-x-a C·p H₂O
chain alkyl anion A- salt
carbon source molecule C
divalent metal ion M₂+ salt (Mg or Zn nitrate/sulfate/oxalate/chloride)
trivalent metal ion M'3+ salt (Al nitrate/sulfate/oxalate/chloride)
metal oxide
sodium dodecyl sulfate/sodium dodecyl sulfonate/sodium dodecyl benzene sulfonate/potassium dodecyl sulfate/potassium dodecyl sulfonate/potassium dodecyl benzene sulfonate
carbon source molecule C (methyl methacrylate/n-pentane/benzene/toluene/xylene/styrene)
sodium hydroxide/potassium hydroxide alkali solution
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
LDH-1 003 interlayer spacing | 2.4 nm | LDH-1 |
Temperature | 60–80 °C | — |
Temperature | 50–60 °C | — |
Temperature | 700–950 °C | — |
Duration | 6–10 hours | — |
Duration | 6–12 hours | — |
Duration | 0.5–3 hours | — |
Duration | 0.5–2 hours | — |
Related documents with shared materials, methods, properties, or citations.
Kohn-–Luttinger like superconductivity in twisted bilayer graphene at large twist angles
Symmetry-adapted closest Wannier modeling based on complete multipole basis set
Random State Approach to Quantum Computation of Electronic-Structure Properties
Low-energy model for doped graphene nanoribbons
Nonlinear thermal and thermoelectric transport from quantum geometry
GRAPHENE COMPOSITE AND METHOD OF PRODUCING THE SAME
Strain-Tunable Harmonic Responses in Valley-Polarized Bilayer Graphene
Role of ultrafast electron-optical-phonon interactions in high harmonic generation from graphene
Moiré-driven equilibrium of perturbations in moiré systems
Shaping Maximally Localized Wannier Functions via Discrete Adiabatic Transport
METHODS OF IMPROVING SINTERING OF PCD USING GRAPHENE
Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Amendments to the Claims: This listing of claims will replace all prior versions, and listings of claims in the application: Listing of Claims 1. A preparation method for graphene, comprising the following steps: (1) mix a soluble salt of a divalent metal ion M 2+, a soluble salt of a trivalent metal ion M'+, a soluble salt of a chain alkyl anion A-and a carbon source molecule C and dissolve them in deionized and C O 2-eliminated water to prepare a mixed salt solution; mix the mixed salt solution with an alkali solution under nitrogen protection and subject them to reaction and crystallization at 60 ° C to 80 ° C for 6 to 10 hours under nitrogen, filter the suspension obtained thereafter and wash the filter cake with deionized water until the pH of the filtrate is 7 to 7.5, and then dry the filter cake at 50 ° C to 60 ° C for 6 to 12 hours to obtain layered double hydroxides with an intercalated structure having a general chemical structure of: SVG 13980715.08-12-2014.HYRKVOM₄PXXIFW3.CLM.1.svg 0.19 2.41 Black and white wherein, x is 0.2-0.33, a is 0.2-6.6, and p is 0.3-3; (2) under an inert atmosphere or a reducing atmosphere, calcinate the layered double hydroxides with an intercalated structure to provide a calcinated product at a calcination temperature of 700 ° C to 950 ° C for a period of time of 0.5 to 3 hours; (3) add the calcinated product into a hydrochloric acid solution with a concentration of 5 wt% for ultrasonic treatment, and separate the solution by centrifugation and wash the precipitate obtained by centrifugation with deionized water until the pH of the filtrate is 6.5 to 7 to obtain the graphene.
The preparation method according to claim 1, wherein, in step (1), the soluble salt of the divalent metal ion M is one or more of a nitrate, a sulfate, an oxalate or a chloride of Mg or Zn; and the soluble salt of the trivalent metal ion M 'i3 is one or more of a nitrate, a sulfate, an oxalate or a chloride of Al.
The preparation method according to claim 1, wherein, the molar ratio between the divalent metal ion M₂ + and the trivalent metal ion M 'i3 is 2 to 4: 1.
The preparation method according to claim 1, wherein, in the mixed salt solution, the overall concentration of the divalent metal ion M₂ + and the trivalent metal ion M' 3+ is 0.2 to 0.5 mol/L.
The preparation method according to claim 1, wherein, in step (1), the soluble salt of the chain alkyl anion A-is one or more of sodium dodecyl sulfate, sodium dodecyl sulfonate, sodium dodecyl benzene sulfonate, potassium dodecyl sulfate, potassium dodecyl sulfonate and potassium dodecyl benzene sulfonate.
The preparation method according to claim 1, wherein, in the mixed salt solution in step (1), the number of moles of the chain alkyl anion A- is equivalent to the number of moles of the trivalent metal ion M'3 +.
The preparation method according to claim 1, wherein, in step (1), the carbon source molecule C is one or more of methyl methacrylate, n-pentane, benzene, toluene, xylene, and styrene.
The preparation method according to claim 1, wherein, in the mixed salt solution, the number of moles of the carbon source molecule C is 1 to 20 times of the number of moles of the trivalent metal ion M'3 +.
The preparation method according to claim 1, wherein, in step (1), the alkali solution is a solution prepared by dissolving sodium hydroxide or potassium hydroxide into deionized and CO 2 -eliminated water with a concentration of 2 to 5 mol/L.
The preparation method according to claim 1, wherein, the number of moles of the alkali in the alkali solution is twice of the total number of trivalent metal ion M'3 +.
The preparation method according to claim 1 nitrogen atmosphere or an argon atmosphere, and atmosphere.
The preparation method according to claim 1 between the calcinated product and the HCl solution
The preparation method according to claim 1 ultrasonic treatment is 0.5 to 2 hours.
The preparation method according to claim 1 centrifugation is 5000 to 9000 rpm.
Embodiments described in the patent, grouped by the materials and process steps they use.
6 materials3 process steps
Preparation of single-layer graphene (G₁) via intercalated layered double hydroxides (LDH-1). Magnesium nitrate hexahydrate (0.075 mol), aluminum nitrate nonahydrate (0.025 mol), sodium dodecyl sulfate (SDS, 0.025 mol), and methyl methacrylate (MMA, 0.03 mol) dissolved in 300 mL deionized CO₂-eliminated water. NaOH solution (80 mL, 2.5 mol/L) dripped in under nitrogen; mixture reacted at 80°C for 8 hours under nitrogen atmosphere; filtered, washed (pH 7.2), dried at 50°C for 12 hours to give LDH-1 with interlayer spacing 2.4 nm (003 peak by XRD and TEM). LDH-1 then calcinated and acid-treated to yield single-layer graphene G1.
1 material1 process step
Preparation of two-layer and three-layer graphene (G₂) via intercalated LDH-2. Similar procedure to Example 1 with different ratios/conditions to yield 2-to-3-layer graphene, characterized by high-resolution TEM (Fig. 6, 7, 8).
1 material1 process step
Preparation of multi-layer graphene G₃ (4 to 6 layers) via intercalated LDH-3. Similar procedure yielding multi-layer graphene, characterized by high-resolution TEM (Fig. 9, 10) and Raman spectroscopy (Fig. 11).
Materials described outside the worked examples.
graphene
layered double hydroxides with intercalated structure
[M₂+1-x M'3+x(OH)2]x+ A-x-a C·p H₂O
chain alkyl anion A- salt
carbon source molecule C
divalent metal ion M₂+ salt (Mg or Zn nitrate/sulfate/oxalate/chloride)
trivalent metal ion M'3+ salt (Al nitrate/sulfate/oxalate/chloride)
metal oxide
sodium dodecyl sulfate/sodium dodecyl sulfonate/sodium dodecyl benzene sulfonate/potassium dodecyl sulfate/potassium dodecyl sulfonate/potassium dodecyl benzene sulfonate
carbon source molecule C (methyl methacrylate/n-pentane/benzene/toluene/xylene/styrene)
sodium hydroxide/potassium hydroxide alkali solution
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
LDH-1 003 interlayer spacing | 2.4 nm | LDH-1 |
Temperature | 60–80 °C | — |
Temperature | 50–60 °C | — |
Temperature | 700–950 °C | — |
Duration | 6–10 hours | — |
Duration | 6–12 hours | — |
Duration | 0.5–3 hours | — |
Duration | 0.5–2 hours | — |
Related documents with shared materials, methods, properties, or citations.
Kohn-–Luttinger like superconductivity in twisted bilayer graphene at large twist angles
Symmetry-adapted closest Wannier modeling based on complete multipole basis set
Random State Approach to Quantum Computation of Electronic-Structure Properties
Low-energy model for doped graphene nanoribbons
Nonlinear thermal and thermoelectric transport from quantum geometry
GRAPHENE COMPOSITE AND METHOD OF PRODUCING THE SAME
Strain-Tunable Harmonic Responses in Valley-Polarized Bilayer Graphene
Role of ultrafast electron-optical-phonon interactions in high harmonic generation from graphene
Moiré-driven equilibrium of perturbations in moiré systems
Shaping Maximally Localized Wannier Functions via Discrete Adiabatic Transport
METHODS OF IMPROVING SINTERING OF PCD USING GRAPHENE
Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Amendments to the Claims: This listing of claims will replace all prior versions, and listings of claims in the application: Listing of Claims 1. A preparation method for graphene, comprising the following steps: (1) mix a soluble salt of a divalent metal ion M 2+, a soluble salt of a trivalent metal ion M'+, a soluble salt of a chain alkyl anion A-and a carbon source molecule C and dissolve them in deionized and C O 2-eliminated water to prepare a mixed salt solution; mix the mixed salt solution with an alkali solution under nitrogen protection and subject them to reaction and crystallization at 60 ° C to 80 ° C for 6 to 10 hours under nitrogen, filter the suspension obtained thereafter and wash the filter cake with deionized water until the pH of the filtrate is 7 to 7.5, and then dry the filter cake at 50 ° C to 60 ° C for 6 to 12 hours to obtain layered double hydroxides with an intercalated structure having a general chemical structure of: SVG 13980715.08-12-2014.HYRKVOM₄PXXIFW3.CLM.1.svg 0.19 2.41 Black and white wherein, x is 0.2-0.33, a is 0.2-6.6, and p is 0.3-3; (2) under an inert atmosphere or a reducing atmosphere, calcinate the layered double hydroxides with an intercalated structure to provide a calcinated product at a calcination temperature of 700 ° C to 950 ° C for a period of time of 0.5 to 3 hours; (3) add the calcinated product into a hydrochloric acid solution with a concentration of 5 wt% for ultrasonic treatment, and separate the solution by centrifugation and wash the precipitate obtained by centrifugation with deionized water until the pH of the filtrate is 6.5 to 7 to obtain the graphene.
The preparation method according to claim 1, wherein, in step (1), the soluble salt of the divalent metal ion M is one or more of a nitrate, a sulfate, an oxalate or a chloride of Mg or Zn; and the soluble salt of the trivalent metal ion M 'i3 is one or more of a nitrate, a sulfate, an oxalate or a chloride of Al.
The preparation method according to claim 1, wherein, the molar ratio between the divalent metal ion M₂ + and the trivalent metal ion M 'i3 is 2 to 4: 1.
The preparation method according to claim 1, wherein, in the mixed salt solution, the overall concentration of the divalent metal ion M₂ + and the trivalent metal ion M' 3+ is 0.2 to 0.5 mol/L.
The preparation method according to claim 1, wherein, in step (1), the soluble salt of the chain alkyl anion A-is one or more of sodium dodecyl sulfate, sodium dodecyl sulfonate, sodium dodecyl benzene sulfonate, potassium dodecyl sulfate, potassium dodecyl sulfonate and potassium dodecyl benzene sulfonate.
The preparation method according to claim 1, wherein, in the mixed salt solution in step (1), the number of moles of the chain alkyl anion A- is equivalent to the number of moles of the trivalent metal ion M'3 +.
The preparation method according to claim 1, wherein, in step (1), the carbon source molecule C is one or more of methyl methacrylate, n-pentane, benzene, toluene, xylene, and styrene.
The preparation method according to claim 1, wherein, in the mixed salt solution, the number of moles of the carbon source molecule C is 1 to 20 times of the number of moles of the trivalent metal ion M'3 +.
The preparation method according to claim 1, wherein, in step (1), the alkali solution is a solution prepared by dissolving sodium hydroxide or potassium hydroxide into deionized and CO 2 -eliminated water with a concentration of 2 to 5 mol/L.
The preparation method according to claim 1, wherein, the number of moles of the alkali in the alkali solution is twice of the total number of trivalent metal ion M'3 +.
The preparation method according to claim 1 nitrogen atmosphere or an argon atmosphere, and atmosphere.
The preparation method according to claim 1 between the calcinated product and the HCl solution
The preparation method according to claim 1 ultrasonic treatment is 0.5 to 2 hours.
The preparation method according to claim 1 centrifugation is 5000 to 9000 rpm.
Embodiments described in the patent, grouped by the materials and process steps they use.
6 materials3 process steps
Preparation of single-layer graphene (G₁) via intercalated layered double hydroxides (LDH-1). Magnesium nitrate hexahydrate (0.075 mol), aluminum nitrate nonahydrate (0.025 mol), sodium dodecyl sulfate (SDS, 0.025 mol), and methyl methacrylate (MMA, 0.03 mol) dissolved in 300 mL deionized CO₂-eliminated water. NaOH solution (80 mL, 2.5 mol/L) dripped in under nitrogen; mixture reacted at 80°C for 8 hours under nitrogen atmosphere; filtered, washed (pH 7.2), dried at 50°C for 12 hours to give LDH-1 with interlayer spacing 2.4 nm (003 peak by XRD and TEM). LDH-1 then calcinated and acid-treated to yield single-layer graphene G1.
1 material1 process step
Preparation of two-layer and three-layer graphene (G₂) via intercalated LDH-2. Similar procedure to Example 1 with different ratios/conditions to yield 2-to-3-layer graphene, characterized by high-resolution TEM (Fig. 6, 7, 8).
1 material1 process step
Preparation of multi-layer graphene G₃ (4 to 6 layers) via intercalated LDH-3. Similar procedure yielding multi-layer graphene, characterized by high-resolution TEM (Fig. 9, 10) and Raman spectroscopy (Fig. 11).
Materials described outside the worked examples.
graphene
layered double hydroxides with intercalated structure
[M₂+1-x M'3+x(OH)2]x+ A-x-a C·p H₂O
chain alkyl anion A- salt
carbon source molecule C
divalent metal ion M₂+ salt (Mg or Zn nitrate/sulfate/oxalate/chloride)
trivalent metal ion M'3+ salt (Al nitrate/sulfate/oxalate/chloride)
metal oxide
sodium dodecyl sulfate/sodium dodecyl sulfonate/sodium dodecyl benzene sulfonate/potassium dodecyl sulfate/potassium dodecyl sulfonate/potassium dodecyl benzene sulfonate
carbon source molecule C (methyl methacrylate/n-pentane/benzene/toluene/xylene/styrene)
sodium hydroxide/potassium hydroxide alkali solution
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
LDH-1 003 interlayer spacing | 2.4 nm | LDH-1 |
Temperature | 60–80 °C | — |
Temperature | 50–60 °C | — |
Temperature | 700–950 °C | — |
Duration | 6–10 hours | — |
Duration | 6–12 hours | — |
Duration | 0.5–3 hours | — |
Duration | 0.5–2 hours | — |
Related documents with shared materials, methods, properties, or citations.
Kohn-–Luttinger like superconductivity in twisted bilayer graphene at large twist angles
Symmetry-adapted closest Wannier modeling based on complete multipole basis set
Random State Approach to Quantum Computation of Electronic-Structure Properties
Low-energy model for doped graphene nanoribbons
Nonlinear thermal and thermoelectric transport from quantum geometry
GRAPHENE COMPOSITE AND METHOD OF PRODUCING THE SAME
Strain-Tunable Harmonic Responses in Valley-Polarized Bilayer Graphene
Role of ultrafast electron-optical-phonon interactions in high harmonic generation from graphene
Moiré-driven equilibrium of perturbations in moiré systems
Shaping Maximally Localized Wannier Functions via Discrete Adiabatic Transport
METHODS OF IMPROVING SINTERING OF PCD USING GRAPHENE