CN110775965A - Chemical vapor deposition process for preparing high-molecular nano composite material - Google Patents
Chemical vapor deposition process for preparing high-molecular nano composite material Download PDFInfo
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- CN110775965A CN110775965A CN201911216324.8A CN201911216324A CN110775965A CN 110775965 A CN110775965 A CN 110775965A CN 201911216324 A CN201911216324 A CN 201911216324A CN 110775965 A CN110775965 A CN 110775965A
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- 239000000463 material Substances 0.000 title claims abstract description 34
- 238000005229 chemical vapour deposition Methods 0.000 title claims abstract description 15
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 239000011889 copper foil Substances 0.000 claims abstract description 97
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 91
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 84
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 57
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 52
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 28
- 239000007789 gas Substances 0.000 claims abstract description 26
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000001257 hydrogen Substances 0.000 claims abstract description 25
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 25
- 238000000576 coating method Methods 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 21
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 21
- 238000000151 deposition Methods 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 229910052786 argon Inorganic materials 0.000 claims abstract description 17
- 239000011248 coating agent Substances 0.000 claims abstract description 17
- 239000000758 substrate Substances 0.000 claims abstract description 17
- 230000008021 deposition Effects 0.000 claims abstract description 11
- 230000001681 protective effect Effects 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000010949 copper Substances 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims abstract description 5
- 229910001385 heavy metal Inorganic materials 0.000 claims abstract description 3
- 239000011159 matrix material Substances 0.000 claims abstract description 3
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 48
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 25
- 239000011259 mixed solution Substances 0.000 claims description 24
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 22
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 16
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 16
- 229920000642 polymer Polymers 0.000 claims description 11
- 239000004408 titanium dioxide Substances 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 5
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 4
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 2
- 239000010410 layer Substances 0.000 abstract description 23
- 125000004429 atom Chemical group 0.000 abstract description 8
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 abstract description 8
- 125000004432 carbon atom Chemical group C* 0.000 abstract description 4
- 239000003575 carbonaceous material Substances 0.000 abstract description 4
- 239000002356 single layer Substances 0.000 abstract description 4
- 150000001721 carbon Chemical group 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/186—Preparation by chemical vapour deposition [CVD]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/02—Single layer graphene
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The invention discloses a chemical vapor deposition process for preparing a high-molecular nano composite material, which relates to the technical field of high-molecular composite materials, and specifically comprises the steps of taking a nickel-loaded copper foil as a matrix, and carrying out nickel coating and heat treatment; gasifying a carbon source, taking a mixed gas of argon and hydrogen as a protective gas, depositing under a certain temperature condition, cooling at a speed of 10K/s after deposition is finished, and taking down the deposited graphene layer when the substrate is cooled to 200 ℃; and removing heavy metals from the taken graphene material, and then carrying out thermal reduction on the graphene material and the nano titanium dioxide together to prepare the graphene nano titanium dioxide composite material. The method adopts copper foil as a base material for generating the graphene carbon material, loads 15% of Ni on the copper foil, activates the loaded Ni through heat treatment, enables the loaded Ni atoms and the surrounding Cu atoms to be fused into a whole, and generates the complete single-layer graphene material through the combination mechanism that the Cu atoms adsorb the carbon atoms and the Ni atoms catalyze the carbon atoms.
Description
Technical Field
The invention relates to the technical field of polymer composites, in particular to a chemical vapor deposition process for preparing a polymer nanocomposite.
Background
Carbon materials have been the subject of intense research in recent years. The carbon material is a material containing carbon as a main element. Among all carbon materials, a material entirely composed of carbon element is a very special material having a very large potential for application and development. The carbon element can form three covalent bonds due to the fact that the outermost layer has four valence electrons, meanwhile, one free moving valence electron is reserved, and bonding towards the same plane in three different directions means that the carbon atom is used as the center and can extend infinitely in a certain plane to form a large plane, and the single-layer plane is an abstract prototype of the graphene material. Each carbon atom in the graphene material retains one valence electron, so that the whole material has rich electron storage capacity and very excellent performances in the aspects of conduction catalysis and the like.
However, graphene is used as a two-dimensional structure material, and in the preparation process of the graphene, the produced graphene molecules are difficult to be separated into single layers without damaging the graphene structure, or the stripped graphene material becomes wrinkled and deformed, so that the performance of the generated graphene material is poor.
Disclosure of Invention
The present invention aims at providing a chemical vapor deposition process for preparing polymer nano composite materials, so as to solve the problems in the background technology.
A chemical vapor deposition process for the preparation of a polymeric nanocomposite, the process comprising the steps of:
taking a loaded nickel copper foil as a matrix, wherein the preparation step of the loaded nickel copper foil comprises nickel coating and heat treatment, the heat treatment operation is specifically to carry out heat treatment on the obtained loaded nickel copper foil at 865-875 ℃ for 5-8min, and naturally cooling to normal temperature;
gasifying a carbon source, taking a mixed gas of argon and hydrogen as a protective gas, depositing under a certain temperature condition, cooling at a speed of 10K/s after deposition is finished, and taking down the deposited graphene layer when the substrate is cooled to 200 ℃;
removing organic matters and heavy metals from the taken graphene material;
and step four, preparing the graphene-nano inorganic substance composite material.
As a preferred scheme, the nickel coating operation in the first step specifically comprises: and (2) washing and naturally airing the copper foil by ethanol and deionized water in sequence, then placing the copper foil in a mixed solution of nickel nitrate with the mass fraction of 15% for soaking for 24h, fishing out and naturally airing, then placing the copper foil with the surface adsorbing the nickel nitrate in a hydrogen atmosphere, and keeping the temperature at 550-580 ℃ for 25-30min to obtain the nickel-loaded copper foil.
Preferably, the nickel-loaded copper foil obtained in the first step comprises 5-8% of Ni and 92-95% of Cu.
Preferably, the carbon source in the second step is one of methane, propylene or ethanol, and the deposition temperature is 1050-.
As a preferable scheme, the flow of the carbon source in the second step is 8-15ml/min, the flow of argon is 90-110ml/min, and the flow of hydrogen is 15-20 ml/min.
As a preferable scheme, the graphene layer removal in the second step is specifically: heating methyl methacrylate to 160-170 ℃, coating the methyl methacrylate on the substrate, uniformly coating the periphery of the copper foil during coating, coating the rest area after cooling and hardening the methyl methacrylate, uniformly moving from one side to the other side during coating, and uncovering the whole methyl methacrylate layer after cooling and hardening the methyl methacrylate.
As a preferable scheme, the operation in the third step is specifically: placing methyl methacrylate with graphene into acetone, slightly shaking the solution for 5-8min, dropwise adding 5% hydrogen peroxide liquid into the mixed solution, slightly shaking the solution for 2-3min, then dropwise adding 10% hydrochloric acid solution into the system, slightly shaking for 3-4min, filtering the mixed solution, washing and drying to obtain the graphene film.
As a preferable scheme, the operation in the fourth step is specifically: and calcining the mixture of the graphene oxide powder and the titanium dioxide at 250 ℃ in the atmosphere of He gas to obtain the graphene titanium dioxide material.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, a copper foil is used as a base material for generating graphene, 15% of Ni is loaded on the copper foil through an impregnation method, and the loaded Ni is activated through heat treatment, so that loaded Ni atoms and surrounding Cu atoms are fused into a whole, wherein the Cu atoms can adsorb a large amount of carbon atoms, and the Ni atoms can play a catalytic role to connect the carbon atoms into bonds, so that a complete single-layer graphene material is generated.
Drawings
FIG. 1 is a flow chart of a chemical vapor deposition process for preparing a polymer nanocomposite.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
Taking a copper foil with the thickness of 3cm multiplied by 3cm, washing the copper foil with ethanol and deionized water in sequence, naturally airing the copper foil, then placing the copper foil in a mixed solution of nickel nitrate with the mass fraction of 15%, soaking the copper foil for 24 hours, and naturally airing the copper foil after fishing out; placing the copper foil with the surface adsorbed with the nickel nitrate in a hydrogen atmosphere, and keeping the temperature at 550 ℃ for 25min to obtain a nickel-loaded copper foil; carrying out heat treatment on the obtained nickel-loaded copper foil at 865 ℃ for 5min, and naturally cooling to normal temperature;
gasifying methane at 1050 ℃ by taking methane as a carbon source, wherein the flow rate of the methane is 8ml/min, the flow rate of argon is 90ml/min, and the flow rate of hydrogen is 15 ml/min; taking a mixed gas of argon and hydrogen as a protective gas, depositing under a certain temperature condition, cooling at a speed of 10K/s after deposition is finished, and taking down the deposited graphene layer when the substrate is cooled to 200 ℃; taking down the graphene layer, specifically heating methyl methacrylate to 160 ℃, coating methyl methacrylate on a substrate, coating the periphery of a copper foil, after methyl methacrylate is hardened for about 15min, coating the rest area, moving the copper foil from one side to the other side at a constant speed in the coating process, standing for 20min, and after methyl methacrylate is completely cooled and hardened, uncovering the whole methyl methacrylate layer;
placing methyl methacrylate with graphene in acetone, slightly shaking the solution for 5min, dropwise adding 5% hydrogen peroxide liquid into the mixed solution, slightly shaking the solution for 2min, then dropwise adding 10% hydrochloric acid solution into the system, slightly shaking for 3min, filtering the mixed solution, washing and drying to obtain a graphene film;
and calcining the mixture of the graphene oxide powder and the nano titanium dioxide at 250 ℃ in the atmosphere of He gas to obtain the graphene titanium dioxide material.
Example two
Taking a copper foil with the thickness of 3cm multiplied by 3cm, washing the copper foil with ethanol and deionized water in sequence, naturally airing the copper foil, then placing the copper foil in a mixed solution of nickel nitrate with the mass fraction of 15%, soaking the copper foil for 24 hours, and naturally airing the copper foil after fishing out; placing the copper foil with the surface adsorbed with the nickel nitrate in a hydrogen atmosphere, and keeping the temperature at 580 ℃ for 30min to obtain a nickel-loaded copper foil; carrying out heat treatment on the obtained nickel-loaded copper foil at 875 ℃ for 8min, and naturally cooling to normal temperature;
using propylene as a carbon source, gasifying the carbon source at 700 ℃, wherein the flow of the carbon source is 15ml/min, the flow of argon is 110ml/min, and the flow of hydrogen is 20 ml/min; taking a mixed gas of argon and hydrogen as a protective gas, depositing under a certain temperature condition, cooling at a speed of 10K/s after deposition is finished, and taking down the deposited graphene layer when the substrate is cooled to 200 ℃; the graphene layer is taken down specifically, methyl methacrylate is heated to 170 ℃, then methyl methacrylate is coated on the substrate, the periphery of the copper foil is coated when the copper foil is coated, when the methyl methacrylate is hardened for about 15min, the rest area is coated, the copper foil is moved at a constant speed from one side to the other side in the coating process, the copper foil is kept stand for 30min, and after the methyl methacrylate is completely cooled and hardened, the whole methyl methacrylate layer is uncovered;
placing methyl methacrylate with graphene in acetone, slightly shaking the solution for 8min, dropwise adding 5% by mass of hydrogen peroxide liquid into the mixed solution, slightly shaking the solution for 3min, then dropwise adding 10% by mass of hydrochloric acid solution into the system, slightly shaking for 4min, filtering the mixed solution, washing and drying to obtain a graphene film;
calcining the mixture of the graphene oxide powder and the nano titanium dioxide at 250 ℃ in the atmosphere of He gas to obtain the graphene titanium dioxide material
EXAMPLE III
Taking a copper foil with the thickness of 3cm multiplied by 3cm, washing the copper foil with ethanol and deionized water in sequence, naturally airing the copper foil, then placing the copper foil in a mixed solution of nickel nitrate with the mass fraction of 15%, soaking the copper foil for 24 hours, and naturally airing the copper foil after fishing out; placing the copper foil with the surface adsorbed with the nickel nitrate in a hydrogen atmosphere, and keeping the temperature at 560 ℃ for 26min to obtain a nickel-loaded copper foil; carrying out heat treatment on the obtained nickel-loaded copper foil at 867 ℃ for 6min, and naturally cooling to normal temperature;
gasifying the carbon source in ethanol at 1050 ℃ by taking the carbon source as the carbon source, wherein the flow of the carbon source is 10ml/min, the flow of argon is 100ml/min, and the flow of hydrogen is 18 ml/min; taking a mixed gas of argon and hydrogen as a protective gas, depositing under a certain temperature condition, cooling at a speed of 10K/s after deposition is finished, and taking down the deposited graphene layer when the substrate is cooled to 200 ℃; the graphene layer is taken down specifically, methyl methacrylate is heated to 165 ℃, then methyl methacrylate is coated on the substrate, the periphery of the copper foil is coated when the copper foil is coated, when the methyl methacrylate is hardened for about 15min, the rest area is coated, the copper foil is moved at a constant speed from one side to the other side in the coating process, the copper foil is kept stand for 25min, and after the methyl methacrylate is completely cooled and hardened, the whole methyl methacrylate layer is uncovered;
placing methyl methacrylate with graphene in acetone, slightly shaking the solution for 6min, dropwise adding 5% by mass of hydrogen peroxide liquid into the mixed solution, slightly shaking the solution for 3min, then dropwise adding 10% by mass of hydrochloric acid solution into the system, slightly shaking for 3min, filtering the mixed solution, washing and drying to obtain a graphene film;
and calcining the mixture of the graphene oxide powder and the nano titanium dioxide at 250 ℃ in the atmosphere of He gas to obtain the graphene titanium dioxide material.
Example four
Taking a copper foil with the thickness of 3cm multiplied by 3cm, washing the copper foil with ethanol and deionized water in sequence, naturally airing the copper foil, then placing the copper foil in a mixed solution of nickel nitrate with the mass fraction of 15%, soaking the copper foil for 24 hours, and naturally airing the copper foil after fishing out; placing the copper foil with the surface adsorbed with the nickel nitrate in a hydrogen atmosphere, and keeping the temperature at 570 ℃ for 28min to obtain a nickel-loaded copper foil; carrying out heat treatment on the obtained nickel-loaded copper foil at 865-875 ℃ for 7min, and naturally cooling to normal temperature;
gasifying the carbon source in ethanol at 840 ℃, wherein the flow of the carbon source is 14ml/min, the flow of argon is 105ml/min, and the flow of hydrogen is 18 ml/min; taking a mixed gas of argon and hydrogen as a protective gas, depositing under a certain temperature condition, cooling at a speed of 10K/s after deposition is finished, and taking down the deposited graphene layer when the substrate is cooled to 200 ℃; the graphene layer is taken down specifically, methyl methacrylate is heated to 165 ℃, then methyl methacrylate is coated on the substrate, the periphery of the copper foil is coated when the copper foil is coated, when the methyl methacrylate is hardened for about 15min, the rest area is coated, the copper foil is moved at a constant speed from one side to the other side in the coating process, the copper foil is kept stand for 30min, and after the methyl methacrylate is completely cooled and hardened, the whole methyl methacrylate layer is uncovered;
placing methyl methacrylate with graphene in acetone, slightly shaking the solution for 5.5min, dropwise adding 5% by mass of hydrogen peroxide liquid into the mixed solution, slightly shaking the solution for 2.5min, then dropwise adding 10% by mass of hydrochloric acid solution into the system, slightly shaking for 3.5min, filtering the mixed solution, washing and drying to obtain a graphene film;
and calcining the mixture of the graphene oxide powder and the nano titanium dioxide at 250 ℃ in the atmosphere of He gas to obtain the graphene titanium dioxide material.
EXAMPLE five
Taking a copper foil with the thickness of 3cm multiplied by 3cm, washing the copper foil with ethanol and deionized water in sequence, naturally airing the copper foil, then placing the copper foil in a mixed solution of nickel nitrate with the mass fraction of 15%, soaking the copper foil for 24 hours, and naturally airing the copper foil after fishing out; placing the copper foil with the surface adsorbed with the nickel nitrate in a hydrogen atmosphere, and keeping the temperature at 570 ℃ for 27min to obtain a nickel-loaded copper foil; carrying out heat treatment on the obtained nickel-loaded copper foil at 865-875 ℃ for 7min, and naturally cooling to normal temperature;
gasifying the carbon source in methane at 1090 ℃ by taking the methane as the carbon source, wherein the flow of the carbon source is 12ml/min, the flow of argon is 105ml/min, and the flow of hydrogen is 18 ml/min; taking a mixed gas of argon and hydrogen as a protective gas, depositing under a certain temperature condition, cooling at a speed of 10K/s after deposition is finished, and taking down the deposited graphene layer when the substrate is cooled to 200 ℃; the graphene layer is taken down specifically, methyl methacrylate is heated to 168 ℃, then methyl methacrylate is coated on the substrate, the periphery of the copper foil is coated when the copper foil is coated, when the methyl methacrylate is hardened for about 15min, the rest area is coated, the copper foil is moved at a constant speed from one side to the other side in the coating process, the copper foil is kept stand for 28min, and after the methyl methacrylate is completely cooled and hardened, the whole methyl methacrylate layer is uncovered;
placing methyl methacrylate with graphene in acetone, slightly shaking the solution for 7min, dropwise adding 5% hydrogen peroxide liquid into the mixed solution, slightly shaking the solution for 3min, then dropwise adding 10% hydrochloric acid solution into the system, slightly shaking for 3min, filtering the mixed solution, washing and drying to obtain a graphene film;
and calcining the mixture of the graphene oxide powder and the nano titanium dioxide at 250 ℃ in the atmosphere of He gas to obtain the graphene titanium dioxide material.
EXAMPLE six
Taking a copper foil with the thickness of 3cm multiplied by 3cm, washing the copper foil with ethanol and deionized water in sequence, naturally airing the copper foil, then placing the copper foil in a mixed solution of nickel nitrate with the mass fraction of 15%, soaking the copper foil for 24 hours, and naturally airing the copper foil after fishing out; placing the copper foil with the surface adsorbed with the nickel nitrate in a hydrogen atmosphere, and keeping the temperature at 570 ℃ for 26min to obtain a nickel-loaded copper foil; carrying out heat treatment on the obtained nickel-loaded copper foil at 865-875 ℃ for 7min, and naturally cooling to normal temperature;
using propylene as a carbon source, gasifying the carbon source at 690 ℃, wherein the flow of the carbon source is 10ml/min, the flow of argon is 100ml/min, and the flow of hydrogen is 18 ml/min; taking a mixed gas of argon and hydrogen as a protective gas, depositing under a certain temperature condition, cooling at a speed of 10K/s after deposition is finished, and taking down the deposited graphene layer when the substrate is cooled to 200 ℃; taking down the graphene layer, specifically heating methyl methacrylate to 1165 ℃, coating the methyl methacrylate on the substrate, coating the periphery of the copper foil, after the methyl methacrylate is hardened for about 15min, coating the rest area, moving the copper foil from one side to the other side at a constant speed in the coating process, standing for 25min, and after the methyl methacrylate is completely cooled and hardened, uncovering the whole methyl methacrylate layer;
placing methyl methacrylate with graphene in acetone, slightly shaking the solution for 6min, dropwise adding 5% by mass of hydrogen peroxide liquid into the mixed solution, slightly shaking the solution for 2min, then dropwise adding 10% by mass of hydrochloric acid solution into the system, slightly shaking for 4min, filtering the mixed solution, washing and drying to obtain a graphene film;
and calcining the mixture of the graphene oxide powder and the nano titanium dioxide at 250 ℃ in the atmosphere of He gas to obtain the graphene titanium dioxide material.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (8)
1. A chemical vapor deposition process for the preparation of a polymer nanocomposite, 1. the process comprises the steps of:
taking a loaded nickel copper foil as a matrix, wherein the preparation step of the loaded nickel copper foil comprises nickel coating and heat treatment, the heat treatment operation specifically comprises the steps of carrying out heat treatment on the obtained loaded nickel copper foil at 865-875 ℃ for 5-8min, and naturally cooling to normal temperature;
gasifying a carbon source, taking a mixed gas of argon and hydrogen as a protective gas, depositing under a certain temperature condition, cooling at a speed of 10K/s after deposition is finished, and taking down the deposited graphene layer when the substrate is cooled to 200 ℃;
removing organic matters and heavy metals from the taken graphene material;
and step four, preparing the graphene-nano inorganic substance composite material.
2. The chemical vapor deposition process for preparing a polymer nanocomposite material according to claim 1, wherein the nickel-coating operation in the first step specifically comprises: washing the copper foil with ethanol and deionized water in sequence, naturally airing, then placing the copper foil in a mixed solution of nickel nitrate with the mass fraction of 15% for soaking for 24h, fishing out, naturally airing, then placing the copper foil with the surface adsorbing the nickel nitrate in a hydrogen atmosphere, and keeping the temperature at 550-580 ℃ for 25-30min to obtain the nickel-loaded copper foil.
3. The chemical vapor deposition process for preparing polymer nano composite material according to claim 1, wherein the nickel-loaded copper foil obtained in the first step comprises 5-8% of Ni and 92-95% of Cu by mass.
4. The chemical vapor deposition process as claimed in claim 1, wherein the carbon source in the second step is one of methane, propylene and ethanol, and the deposition temperature is 1050-.
5. The chemical vapor deposition process for preparing polymer nanocomposite material according to claim 1, wherein the flow rate of the carbon source in the second step is 8-15ml/min, the flow rate of argon is 90-110ml/min, and the flow rate of hydrogen is 15-20 ml/min.
6. The chemical vapor deposition process for preparing a polymer nanocomposite as claimed in claim 1, wherein the specific operation of removing the graphene layer in the second step is to heat methyl methacrylate to 160-170 ℃, then coat methyl methacrylate on the substrate, uniformly coat the periphery of the copper foil during coating, coat the remaining region after cooling and hardening of methyl methacrylate, move the coating process from one side to the other side at a constant speed, and uncover the entire methyl methacrylate layer after cooling and hardening of methyl methacrylate.
7. The chemical vapor deposition process for preparing polymer nano composite material according to claim 1, wherein the operations in the third step are as follows: placing methyl methacrylate with graphene into acetone, slightly shaking the solution for 5-8min, dropwise adding 5% hydrogen peroxide liquid into the mixed solution, slightly shaking the solution for 2-3min, then dropwise adding 10% hydrochloric acid solution into the system, slightly shaking for 3-4min, filtering the mixed solution, washing and drying to obtain the graphene film.
8. The chemical vapor deposition process for preparing polymer nano composite material according to claim 1, wherein the fourth step is specifically operated as follows: and calcining the mixture of the graphene oxide powder and the titanium dioxide at 250 ℃ in the atmosphere of He gas to obtain the graphene titanium dioxide material.
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| CN201911216324.8A CN110775965A (en) | 2019-12-02 | 2019-12-02 | Chemical vapor deposition process for preparing high-molecular nano composite material |
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| CN201911216324.8A CN110775965A (en) | 2019-12-02 | 2019-12-02 | Chemical vapor deposition process for preparing high-molecular nano composite material |
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Application publication date: 20200211 |