COMPOSITION FOR PREPARING GRAPHENE AND METHOD FOR PREPARING GRAPHENE USING SAME

Hereinafter, in the embodiment according to one method of the present invention composition therefor and yes pin number using the same number bath more detailed as follows.

In the specification, "yes pin (graphene)" RM, a plurality of carbon atoms covalently linked to each other in the shape of a 2 dimensional film (conventional sp² Binding) meaning that the each other. The carbon atoms constituting the basic repeating units are formed as annular but 6, 5 and/or 7 further including an annular an annular also be disclosed. Yes pin 5 and/or 7 can be included in the content of an annular according to define a torus, said s402. forms. It can be single layer , these the plurality laminated layers which are formed in the insulating layer, to be a maximum 100 nm thickness.

In the specification, "yes pin number composition therefor" RM, catalyst metal and/or a stand-alone tank yes pin number employed in number, used to dope the big composition.

In the specification, "laminate" means including a plurality of layer as implies, each stage of the bath method according number according to an embodiment of the present invention, in addition to catalytic metal yes pin, further state including at least one big target film carrier film and during 1.

In the embodiment of the present invention according to one, these compositions comprise a nitrogenous organic compound represented by formula 1 quiet yes pin number; oxidation number; and acid can be:

A nitrogenous organic compound represented by a formula 1;

Oxidation number; and

Acid number yes pin including composition therefor:

<>Formula 1

During said formula 1,

X₂₁ The N (nitrogen atom) or CR₂₁ And, X₂₂ The N or CR₂₂ And, X₂₃ The N or CR₂₃ And, X₂₄ The N or CR₂₄ Implementation being.

For example, during said formula 1, X₂₁ The CR₂₁ And, X₂₂ The CR₂₂ And, X₂₃ The CR₂₃ And, X₂₄ The CR₂₄ Handler, limited to are not correct.

During said formula 1,

R₁ And R₂₁ To R₂₄ Are each independently,

Hydrogen, a substituted or unsubstituted C₁ - C₆₀ Alkyl, a substituted or unsubstituted C₃ - C₁₀ Cycloalkyl, a substituted or unsubstituted C₆ - C₆₀ Aryl and substituted or a substituted or unsubstituted C₂ - C₆₀ Heteroaryl can be selected.

For example, during said formula 1, R₁ And R₂₁ To R₂₄ Are each independently,

Hydrogen, methyl, ethyl, n - propyl, iso - propyl, n - butyl, sec - butyl, iso - butyl, tert - butyl, neopentyl n -, cyclo neopentyl, cyclohexyl, phenyl, naphthyl and pyridinyl; and

Deuterium, halogen atom, cyano, nitro, methyl, ethyl, n - propyl, iso - propyl, n - butyl, sec - butyl, iso - butyl, tert - butyl, phenyl, naphthyl and pyridinyl selected from at least one substituted, methyl, ethyl, n - propyl, iso - propyl, n - butyl, sec - butyl, iso - butyl, tert - butyl, neopentyl n -, cyclo neopentyl, cyclohexyl, phenyl, naphthyl and pyridinyl; but selected, limited to are not correct.

As another example, during said formula 1, R₁ And R₂₁ To R₂₄ Are each independently,

Hydrogen, methyl, ethyl, n - propyl, iso - propyl, n - butyl, sec - butyl, iso - butyl, tert - butyl, neopentyl n -, cyclo neopentyl, cyclohexyl, phenyl, naphthyl and pyridinyl; but selected, limited to are not correct.

For example, during said formula 1 R₁ Can be a hydrogen, limited to are not correct.

For example, during said formula 1 R₂₁ To R₂₄ Is can be a all, limited to are not correct.

For example, nitrogenous organic compound that is represented by said formula 1 represented by the formula 1A but, limited to are not correct:

Formula 1A<>

During said formula 1A,

R₁ As defined in the thereof can.

As another example, when a nitrogenous organic compound represented by said formula 1 is represented by said formula 1A, R₁ Is,

Hydrogen, methyl, ethyl, n - propyl, iso - propyl, n - butyl, sec - butyl, iso - butyl, tert - butyl, neopentyl n -, cyclo neopentyl, cyclohexyl, phenyl, naphthyl and pyridinyl; and

Deuterium, halogen atom, cyano, nitro, methyl, ethyl, n - propyl, iso - propyl, n - butyl, sec - butyl, iso - butyl, tert - butyl, phenyl, naphthyl and pyridinyl selected from at least one substituted, methyl, ethyl, n - propyl, iso - propyl, n - butyl, sec - butyl, iso - butyl, tert - butyl, neopentyl n -, cyclo neopentyl, cyclohexyl, phenyl, naphthyl and pyridinyl; but selected, limited to are not correct.

For example, nitrogenous organic compound represented by said formula 1 benzotriazole (benzotriazole) handler, limited to are not correct.

A nitrogenous organic compound represented by said formula 1 acids together including composition when, Fe value is used as the flange. For example, nitrogenous organic compound is represented by said formula 1 include, acids are not use composition, not Fe value is lower. I.e., the use of nitrogenous organic compounds represented by said formula 1 including composition , doping cannot be disclosed.

In addition, a nitrogenous organic compound represented by said formula 1 such as, in the case of compounds including at least one nitrogen compound in at least 3, and lower nitrogen compounds included compared, for doping effects is better disclosed.

In addition, structures having a triazole compound in the, electricity power supply (negative charge) structure including a high carbon to nitrogen to voice only resonance structure (resonance structure) can be made, according to the ionic yes pin height doping effects can be.

Said oxidation number is H₂ O₂ , (NH₄ ) S₂ O₈ , Na₂ S₂ O₈ , Scaleable (oxone), HClO and HClO₄ Can be a selected one of the at least one 1, limited to are not correct. E.g., said oxidation number is H₂ O₂ Implementation being. In addition, said oxidation number is introduced into said solid form composition may be quiet yes pin number, to state a solvent such as water can be introduced dilution may be filled.

Said acid is H₂ SO₄ , HNO₃ , H₃ PO₄ , HCl, HCOOH and CH₃ A selected one of the at least one COOH can be a 1, limited to are not correct. A solvent such as water dilution state to said acids are said yes pin number can be quiet and dried. For example, 95% by weight of said acid is aqueous solution of sulfuric acid, or phosphoric acid 85% by weight can be an aqueous solution.

Copper (I) ions or copper (II) ions yes pin number said quiet composition can be further. Said yes pin number (source) copper (I) ions or copper copper - won quiet be added to the composition (II) ions can be number whenever he form number is not one. For example, quiet composition CuCl said yes pin number₂ , CuCl or Cu [(BI)₄ ] SO₄ (Cu^{2 +} Stabilizing complex) in the form of a copper salt such as copper - won can be added.

Said quiet composition yes pin number 0. 2 Wt % to 10 wt % of a nitrogenous organic compound represented by said formula 1, 1 wt % to 10 wt % oxidation number, it can be 2 wt % to 30 wt % acid and residual solvent, limited to are not correct. In the specification, said nitrogenous organic compound, based on total weight of said composition and said quiet yes pin number the content of acid oxidation number are disclosed.

For example, quiet composition said yes pin number 0. 5 Wt % or more, 1 wt % or more, 2. 5 Wt % hereinafter, but which contains a nitrogenous organic compound of said formula 1 or 2 wt % hereinafter represented, limited to are not correct.

For example, quiet composition said yes pin number, 2 wt % or more, 3 wt % or more, 9 wt % hereinafter, or 8 wt % hereinafter include oxidation number but, limited to are not correct.

For example, quiet composition said yes pin number 3 wt % or more, 5 wt % or more, 18 wt % hereinafter, or it can be 15 wt % hereinafter acid, limited to are not correct.

Said quiet composition yes pin number 0. 2 Wt % to 3 wt % of a nitrogenous organic compound, oxidation number 1 wt % to 5 wt %, 2 wt % to 10 wt % acid, 0. 1 Wt % to 1. 0 Wt % copper (I) ions or copper (II) ion and residual solvent but, limited to are not correct.

For example, quiet composition said yes pin number 0. 2 Wt % or more, 0. 5 Wt % hereinafter, or 0. Copper (I) ions or copper (II) ions but 4 wt % hereinafter, limited to are not correct. Or, 3 g/L copper (I) said yes pin number yes pin number quiet composition bath composition (II) detachable to ions or copper ions, copper (I) ions or copper (II) ion collision yes pin number bath but additionally, limited to are not correct.

Said solvent composition yes pin number can be quiet water. I.e., yes pin number said quiet composition contains a nitrogenous organic compound, an aqueous solution of oxide and acid be a number. However, said composition without limited to solvent, oxidation and acid number can be homogeneously dispersing specially if the number is not one. The, said in addition to the solvent can be water, any other liquid can be compatible further comprises water. Or, said homogeneously to disperse a nitrogenous organic compound further comprises an organic solvent situby 2 can be.

Quiet composition further comprises said number yes pin number can be added. Known in the present invention is is provided to said number will be added. For example, dispersion number, positive number, stabilizing number and their combination. Adding the content of said yes pin number 3 wt % to 20 wt % based on total weight of said number quiet composition may be in the range disclosed.

Said yes pin number represented by said formula 1 quiet composition contains a nitrogenous organic compound, oxidation number, acid and solvent is mixed to in situ (in non-situ) may also be used but, nitrogenous organic compound represented by said formula 1, oxidation number, number acid and a solvent composition after mixing high pressure liquid coolant, disapproval use storage composition prepared by the number. In particular, a nitrogenous organic compound represented by said formula 1, oxidation number, number acid and a solvent composition after mixing high pressure liquid coolant, when storing by said number prepared by the composition, said composition further includes a number number number and preservation of stable quiet yes pin number dispersion can be added. In addition, oxidation number yes pin number as said quiet composition H₂ O₂ When a including, quiet composition said H said yes pin number₂ O₂ Controlled oxidation of stabilizing further comprises 100 weight number number can be.

The nitrogenous organic compound represented by said formula 1 can be included in the dopant. The nitrogenous organic compound represented by said formula 1 surface of and/or may be physically coupling, chemically and/or physically coupling constituting a layer may also be used but, is not limited. I.e., if Fe value may be , represented by said formula 1 contains a nitrogenous organic compound binding sites, binding method is not one number.

AuCl₃ When such as metal salt to doping, but Fe lower resistance value, which has a lower can be. While, HNO₃ When acid such as doping, Fe to a predetermined value, but added transmission can be maintained, long-lasting effect of these doping may be discontinuous disclosed.

However, when using a nitrogenous organic compound represented by said formula 1 doping, Fe to a predetermined value, and to maintain a lower transmittance than the , lower Fe value is can be obtained.

A nitrogenous organic compound represented by said formula 1 exceeds 0 to 300 Ω / sq hereinafter doped with, e.g., 100 to 230 Ω / sq and to shorten value.

In the embodiment according to one of the present invention, said formula 1 can be used to replace existing ITO electrode doped with a nitrogenous organic compound used but, limited to are not correct. Specifically, said transparent electrode, more specifically transparent electrode for touch panel can be used. In addition, specifically, said serving as electrodes for solar cell can be.

In the embodiment shown in Figure 1 shows a number of method to determine the bath also are disclosed. Hereinafter, in the embodiment according to the method of the present invention are described with reference to one number tank also 1 as follows.

Yes pin (110) on one surface of the carrier film (120) to bind to.

Carrier film (120) is yes pin (110) which can support a transfer for hereinafter, yes pin (110) to keep the shape of can be protected against damage if, kinds and number one is not. For example, carrier film (120) is ten peelings off tape or polymer support can be a, is not limited. Said at room temperature-resistant but ten peelings off tape adhesion, lose the adhesiveness at a temperature higher than a predetermined properties. Said polymer support such as polymethylmethacrylate (Polymethylmethacrylate: PMMA) composition comprises a poly yes pin (110) on one surface of the polymer precursor solution is formed, an organic solvent can be a stand-alone when desired number.

Yes pin (110) carrier film (120) stack of nitrogenous organic compound represented by said formula 1, including acid oxidation number and quiet yes pin number composition by doping doping yes pin (130) to obtain.

A nitrogenous organic compound represented by said formula 1, and acid of oxidation number, type, such as a use form and content these yes pin quiet composition number reference each other.

Said doping yes pin (130) doped method to obtain a number can be obtained if the format is not one. E.g., said step yes pin (110) carrier film (120) can be produced by impregnating composition comprising said stack of quiet yes pin number. Or, said step yes pin (110) carrier film (120) can be made quiet yes pin number lamination formed by spraying the composition. Said doping yes pin (130) to 60 minutes to obtain a 3 can be performed. For example, quiet yes pin number 3 to 60 minutes said composition, e.g., 3 to 15 minutes, 5 to 10 minutes yes pin (110) a doping disclosed. 3 Minutes 60 minutes time collects yes pin (110) or user obtained sufficiently doped doped yes pin (130) and to shorten value can be dielectric window. Said quiet time can then if yes pin number composition can be properly controlled.

Doping yes pin (130) target film (140) is transferred to a substrate.

Said target film (140) doping yes pin (130) for application of the device can be a part of, said device specifically be a electrode of the one surface.

Doping yes pin (130) target film (140) for transferred to, yes pin (110) carrier film (120) the laminate of a target film (140) after bonded, carrier film (120) number a stationary substrate. For example, carrier film (120) when ten peelings off the adhesive tape, said tape ten peelings off lose the adhesiveness at a temperature higher than apply a force to a predetermined doping yes pin (130) from said ten peelings off tape is stripped off substrate. For example, carrier film (120) when a polymer support, said organic solvent to a variation of the applied polymer support doping yes pin (130) can be a stand-alone number from.

In the embodiment shown in Figure 2 shows a method to determine the number of bath also are disclosed. Hereinafter, the method of the present invention are described with reference to the number one in the embodiment according to bath also 2 as follows.

Yes pin (210) target film on one surface of (240) to bind to.

Target film (240) these of Figure 1 description of target film (140) the description of the reference substrate.

Yes pin (210) target film (240) the stack of nitrogenous organic compound, oxide and acid number yes pin number including quiet composition by doping doping yes pin (230) to obtain.

Said nitrogenous organic compound, oxide and acid number of, type, such as a use form and content these yes pin quiet composition number reference each other.

Said doping yes pin (230) of Figure 1 to obtain account of the doping yes pin (130) to obtain a description is given of a reference substrate.

In the embodiment shown in Figure 3 shows a method to determine the number another aspect of bath also are disclosed. Hereinafter, in the embodiment according to the method of the present invention are described with reference to one number tank also 3 as follows.

But that does not itself shown, catalytic metal (350) pre-each other.

Catalytic metal (350) is growing location can be used. Catalytic metal (350) can be grown not only the shape of the number one. For example, catalytic metal (350) sheet, be a substrate or film.

Catalytic metal (350) copper (Cu), nickel (Ni), cobalt (Co), iron (Fe), platinum (Pt), gold (Au), is (Ag), aluminum (Al), chromium (Cr), magnesium (Mg), manganese (Mn), molybdenum (Mo), rhodium (Rh), silicon (Si), tantalum (Ta), titanium (Ti), tungsten (W), uranium (U), vanadium (V), palladium (Pd), yttrium (Y), zirconium (Zr), germanium (Ge) and alloys thereof can be a selected one of the at least one 1, limited to are not correct.

Catalytic metal (350) may be a single-seed layer, at least one layer of the multilayer substrate can be outermost layer 2.

Catalytic metal (350) for pretreating a process with the catalytic metal (350) number into a foreign particles on the surface of a stand-alone, hydrogen gas can be used. In addition, catalytic metal using an acid or alkali solution or the like (350) by washing the surface of the, yes pin reduce deficiency can be formed. Catalytic metal (350) for cleaning the surface of the stage may be needed can be omitted.

Catalytic metal (350) of at least one of yes pin (310) formed on the substrate.

Said catalytic metal (350) of at least one of yes pin (310) specific forming method is not limited. For example, chemical vapor deposition method includes steps of said (Chemical Vapor Deposition: CVD), thermal chemical vapor deposition (Thermal Chemical Vapor Deposition: TCVD), rapid thermal chemical vapor deposition (Rapid Thermal Chemical Vapor Deposition: PTCVD), inductively coupled plasma chemical vapor deposition (Inductive Coupled Plasma Chemical Vapor Deposition: ICP non-CVD), atoms can be bake is such as the layer evaporation law (Atomic Layer Deposition: ATLD). Said step of number but by way of example, chemical vapor deposition is cited.

Chemical vapor deposition with the catalytic metal container which is disposed in the vapor carbon source which can be again by cooling said vessel, said catalyst metal surfaces in growing method yes pin sheet are disclosed.

Said gaseous carbon source is carbon monoxide, ethane, ethylene, ethanol, acetylene, propane, butane, butadiene, pentane, pentene, 1 petroleum cracking process, hexane, cyclohexane, benzene, toluene or a mixture of 2 or more of them can be. The gaseous carbon source at a high temperature carbon atoms and hydrogen atoms apart from each other. Carbon atoms separated heated catalytic metal (350) is deposited, catalytic metal (350) while cooled yes pin (310) formed therein.

Yes pin (310) with the catalytic metal (350) can be formed on at least. In the embodiment of the present invention 3 also shown in one such as catalytic metal (350) on one surface of the yes pin (310) but formed, and are not limited to, catalytic metal (350) yes pin on both sides of (310) are formed in the disapproval.

Catalytic metal (350) not having yes pin (310) on one surface of the carrier film (320) formed on the substrate.

Carrier film (320) account of the carrier film of Figure 1 (120) description is given with reference to the other.

Carrier film (320), yes pin (310) and catalytic metal (350) a nitrogenous organic compound lamination, oxidation catalytic metal composition including quiet yes pin number and acid number (350) industry a number simultaneously yes pin (310) by doping doping yes pin (330) to obtain.

Catalytic metal (350) industry a number simultaneously yes pin (310) since a doping, doping yes pin (330) the diameter number number can be a high pressure liquid coolant. I.e., and a stand-alone catalytic metal number, then compared doping method, said method during the tank due to the number of steps is, doping number tank reduces the cost. In addition, quiet yes pin number by using said composition, doping yes pin (330) of lower metal interconnection value can be obtained.

Said catalytic metal (350) industry a number simultaneously yes pin (310) by doping doping yes pin (330) to 60 minutes to obtain a 3 can be performed. For example, quiet yes pin number 3 to 60 minutes said composition, e.g., 3 to 15 minutes, 5 to 10 minutes a catalyst metal (350) industry a number simultaneously yes pin (310) a doping disclosed. 3 Minutes 60 minutes time collects catalytic metal (350) while substantially completely stand-alone yes pin number (310) or user obtained sufficiently doped doped yes pin (330) and to shorten value can be dielectric window. Said quiet time can then if yes pin number composition can be properly controlled.

Quiet yes pin number said catalytic metal composition (350) 50g 500 to 1000 ml per dose can be used.

Doping yes pin (330) a target film (340) is transferred to a substrate.

Doping yes pin (330) target film (340) for transferred to, yes pin (310) carrier film (320) target film stack (340) which bind to the method of Figure 1 description reference each other.

Target film (340) of Figure 1 account of the target film (140) with reference to the other.

In the embodiment shown in Figure 4 shows a method to determine the number of bath also are disclosed. Hereinafter, the method of the present invention are described with reference to the number one in the embodiment according to bath also 4 as follows.

But that does not itself shown, catalytic metal (450) pre-each other.

Catalytic metal (450) for pretreating a step of Figure 3 description is catalytic metal (350) pretreating a description is given of the reference substrate.

Catalytic metal (450) of at least one of yes pin (410) formed on the substrate.

Catalytic metal (450) of at least one of yes pin (410) of Figure 3 forming account of the catalytic metal (350) of at least one of yes pin (310) to form a description is given of a reference substrate.

Yes pin (410) with the catalytic metal (450) can be formed on at least. In the embodiment of the present invention 4 also shown in one such as catalytic metal (450) yes pin on both sides of (410) formed but, the which are not limited to, catalytic metal (450) only one side of yes pin (410) are formed in the disapproval.

Catalytic metal (450) not having yes pin (410) on one surface of the carrier film (320) formed on the substrate.

Carrier film (420) account of the carrier film of Figure 1 (120) description is given with reference to the other.

Catalytic metal (450) number a stationary substrate.

Catalytic metal (450) industry specific method steps a number but not limited. For example, be a electrochemical and exfoliating.

Electrochemical exfoliating the electrolyte solution and the catalyst metal laminate organometalloid applies a voltage to said laminate, said catalytic metal from said as to method are disclosed. The catalytic metal is separated both said electrochemical exfoliating yes pin causes both faces can be used.

Said electrolyte solution is NaOH, Na₂ CO₃ , Na₃ PO₄ , Na₂ SiO₃ 1 Sodium silicate and more species selected ones but, is not limited.

Said voltage is 3 to 30V handler, not limited.

Carrier film (420) and yes pin (410) nitrogenous organic compound as a lamination, oxidation number and acid composition including quiet yes pin number yes pin (410) by doping doping yes pin (430) to obtain.

Quiet yes pin number by using said composition, doping yes pin (430) of lower metal interconnection value can be obtained.

Said yes pin (410) by doping doping yes pin (430) to obtain account of the yes pin of Figure 1 (110) by doping doping yes pin (130) to obtain a description is given of a reference substrate.

Doping yes pin (430) a target film (440) is transferred to a substrate.

Doping yes pin (430) target film (440) for transferred to, yes pin (410) carrier film (420) target film stack (440) that bind to the method of Figure 1 description reference each other.

Target film (440) of Figure 1 account of the target film (140) with reference to the other.

Or more, also with reference to the 1 to 4, are described but number bath method, this method of the present invention limited to number tank and not the

Hereinafter, the present invention broadcast receiver through more detailed in the embodiment. In the embodiment for the present invention is to exemplify these only which, in the embodiment of the present invention is one which means that the number by these range is provided to the person with skill in the art of the present invention to not nontrivial disclosed.

In the embodiment 1

Of CVD (CVD furnace) to 35 °C-gate into a Cu plate. (Furnace) to about 1000 °C CH in said₄ 5 Minutes at a rate of about 30 sccm flow me. Then, H₂ Atmosphere, 600 °C up at a rate of 60 °C/min, cooled to room temperature to speed of 40 °C/min, Cu on weight percent.

3 Wt % Cu and laminate of benzotriazole, 3 wt % of H₂ O₂ , 9 Wt % of H₂ SO₄ 40 Minutes Cu is immersed in water including composition during industry a number of 2VM and simultaneously, by doping doping are obtained.

Comparison example 1

The number in the range of 0.1 and 3 wt % 3 wt % of benzotriazole instead of benzo imidazole , doped the same method in the embodiment 1 are obtained.

<Benzoimidazole>

Evaluation example

In the embodiment 1 and comparison example 1 to each table value according to said value and Fe Fe prepared by the number 1 and 5 have shown to also change.

Automatic (available from ENG multi brush) Fe value is automatically selected for measuring point by using the average value measured at a point 143 of cotton resistance, measured values from the average of 8 times in every point 7 times or are disclosed.

With reference to the table 1, a nitrogenous organic compound represented by said formula 1, oxidation number and acid together including the use composition, which contains a nitrogenous organic compound doping, to make it possible to Fe value has been confirmed. In addition, a stand-alone catalytic metal number at the same time, reduce cotton resistance by doping can confirm it.

With reference to the table 1, a nitrogenous organic compound represented by said formula 1, at least one aqueous oxidation number and acid together including, T easy vector obtained cotton resistance can be lowered.