CN114620769A - Preparation method of component-adjustable mesoporous metal oxide two-dimensional sheet - Google Patents
Preparation method of component-adjustable mesoporous metal oxide two-dimensional sheet Download PDFInfo
- Publication number
- CN114620769A CN114620769A CN202210292463.4A CN202210292463A CN114620769A CN 114620769 A CN114620769 A CN 114620769A CN 202210292463 A CN202210292463 A CN 202210292463A CN 114620769 A CN114620769 A CN 114620769A
- Authority
- CN
- China
- Prior art keywords
- solution
- nitrate
- ion
- mesoporous
- metal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 33
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000000243 solution Substances 0.000 claims abstract description 52
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000002244 precipitate Substances 0.000 claims abstract description 14
- 229940096992 potassium oleate Drugs 0.000 claims abstract description 12
- MLICVSDCCDDWMD-KVVVOXFISA-M potassium;(z)-octadec-9-enoate Chemical compound [K+].CCCCCCCC\C=C/CCCCCCCC([O-])=O MLICVSDCCDDWMD-KVVVOXFISA-M 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 11
- 239000012298 atmosphere Substances 0.000 claims abstract description 10
- 150000001768 cations Chemical class 0.000 claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- 239000002184 metal Substances 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 30
- 229910021645 metal ion Inorganic materials 0.000 claims description 16
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 12
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 12
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 11
- 238000001354 calcination Methods 0.000 claims description 10
- 239000000758 substrate Substances 0.000 claims description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 9
- -1 iron ion Chemical class 0.000 claims description 8
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 6
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 6
- 238000010000 carbonizing Methods 0.000 claims description 5
- OBOSXEWFRARQPU-UHFFFAOYSA-N 2-n,2-n-dimethylpyridine-2,5-diamine Chemical compound CN(C)C1=CC=C(N)C=N1 OBOSXEWFRARQPU-UHFFFAOYSA-N 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000005341 cation exchange Methods 0.000 claims description 3
- 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 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 238000000197 pyrolysis Methods 0.000 claims description 3
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 claims description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 2
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229910001429 cobalt ion Inorganic materials 0.000 claims description 2
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910001437 manganese ion Inorganic materials 0.000 claims description 2
- 229910001453 nickel ion Inorganic materials 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- 239000002585 base Substances 0.000 claims 1
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims 1
- 239000012299 nitrogen atmosphere Substances 0.000 abstract description 10
- 238000004108 freeze drying Methods 0.000 abstract description 9
- 238000003756 stirring Methods 0.000 abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 9
- 239000002135 nanosheet Substances 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract 1
- 230000005540 biological transmission Effects 0.000 description 13
- 238000001000 micrograph Methods 0.000 description 12
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
- 229910017135 Fe—O Inorganic materials 0.000 description 5
- 238000003917 TEM image Methods 0.000 description 4
- 229910000859 α-Fe Inorganic materials 0.000 description 4
- 229910000420 cerium oxide Inorganic materials 0.000 description 3
- 229910017052 cobalt Inorganic materials 0.000 description 3
- 239000010941 cobalt Substances 0.000 description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229940049964 oleate Drugs 0.000 description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 3
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910007541 Zn O Inorganic materials 0.000 description 1
- 229910007567 Zn-Ni Inorganic materials 0.000 description 1
- 229910007614 Zn—Ni Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/218—Yttrium oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/224—Oxides or hydroxides of lanthanides
- C01F17/235—Cerium oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/006—Compounds containing, besides cobalt, two or more other elements, with the exception of oxygen or hydrogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
Abstract
The invention provides a preparation method of a mesoporous metal oxide two-dimensional sheet with adjustable components, which comprises the following steps: dispersing graphene oxide in a potassium oleate aqueous solution, and performing ultrasonic stirring to uniformly disperse the graphene oxide; slowly adding a metal cation solution, shaking to precipitate, and then washing with water; and freeze-drying the obtained precipitate, pyrolyzing the precipitate in a nitrogen atmosphere, and empty-burning the graphene oxide template in an air atmosphere to obtain the metal oxide mesoporous two-dimensional sheet. The invention can prepare a plurality of mesoporous metal oxide two-dimensional sheets, has simple method and adjustable components, and can be used as a plurality of unitary metal oxides and binary to high-entropy metal oxides. Overcomes the defects that the prior method only can prepare single metal oxide nanosheets and is complicated, the appearance is uncontrollable and the mesoporous structure is not obvious, and expands the method for preparing mesoporous metal oxide two-dimensional slices.
Description
Technical Field
The invention belongs to the field of materials and inorganic chemistry, in particular to a method for preparing a metal oxide two-dimensional sheet, and particularly relates to a method for preparing a component-adjustable metal oxide two-dimensional sheet.
Background
The metal oxide is cheap, easy to prepare, environment-friendly and widely applied to the fields of catalysis, energy storage and the like. To expose more active centers, nanocrystallization is currently the most common strategy, and therefore a large number of metal oxides with specific micro-morphologies, including nanoparticles, two-dimensional platelets, and the like, are currently prepared. The mesoporous two-dimensional metal oxide sheet can expose more active sites, and the mesopores are more beneficial to material transmission and show better mass transfer and reaction kinetics, so that the mesoporous two-dimensional metal oxide sheet has better application prospect.
The template sacrifice method is a new method for preparing a two-dimensional mesoporous metal oxide sheet, and at present, metal cations are often physically adsorbed on the surface of graphene oxide by the traditional method, and then the graphene oxide template is removed by calcination in the air atmosphere, and at the moment, the metal cations are converted into two-dimensional metal oxides. However, the method can only prepare a plurality of single-component two-dimensional mesoporous metal oxide sheets, and the sheets have the advantages of unadjustable appearance, small size, irregular mesoporous size and easy occurrence of large-area agglomeration.
In a word, the existing mesoporous two-dimensional metal oxide nanosheet preparation method is single, and only a few single-component two-dimensional mesoporous metal oxide nanosheets can be prepared. And the prepared two-dimensional sheet has unadjustable appearance, smaller size and irregular mesoporous size. Therefore, it is necessary to develop a method capable of preparing a mesoporous metal oxide two-dimensional sheet having a tunable composition.
Disclosure of Invention
The invention aims to provide a preparation method of a component-adjustable mesoporous metal oxide two-dimensional sheet.
The invention provides a preparation method of a mesoporous metal oxide two-dimensional sheet with adjustable components, which comprises the following steps:
(1) dispersing substrate graphene oxide in a potassium oleate aqueous solution, and performing ultrasonic treatment to uniformly disperse the substrate graphene oxide;
(2) slowly adding metal cations into the solution obtained in the step (1) for cation exchange, and washing after precipitation;
(3) drying the precipitate obtained in the step (2), then pyrolyzing at high temperature in an inert gas atmosphere, and finally carrying out air firing in an oxidizing atmosphere to prepare a two-dimensional metal oxide nanosheet with adjustable components;
wherein, the metal cation in the step (2) is one or more of iron ion, manganese ion, cobalt ion, zinc ion, nickel ion, cerium ion, aluminum ion or yttrium ion.
In the invention, in the step (1), the oxygen content of the substrate graphene oxide is 40-50%.
In the invention, in the step (1), the oxygen content of the substrate graphene oxide is 40-50%.
In the invention, the metal ion solution in the step (2) is ferric nitrate solution.
In the invention, the metal ion solution in the step (2) is a cerium nitrate solution.
In the invention, the metal ion solution in the step (2) is an aluminum chloride solution.
In the invention, the metal ion solution in the step (2) is yttrium chloride solution.
In the invention, the metal ion solution in the step (2) is a mixed solution composed of ferric nitrate and cobalt nitrate with a molar ratio of 1: 1.
In the invention, the metal ion solution in the step (2) is prepared by mixing the following components in a molar ratio of 1: 1:1, and a mixed solution of ferric nitrate, manganese nitrate and cobalt nitrate.
In the invention, the metal ion solution in the step (2) is prepared by mixing the following components in a molar ratio of 1: 1: 1:1 of ferric nitrate, manganese nitrate, cobalt nitrate and zinc nitrate.
In the invention, the metal ion solution in the step (2) is prepared by mixing the following components in a molar ratio of 1: 1: 1: 1:1 of ferric nitrate, manganese nitrate, cobalt nitrate, zinc nitrate and nickel nitrate.
In the invention, oleate is converted into ordered metal oxide during the high-temperature pyrolysis of the inert gas in the step (3).
In the invention, the mesoporous metal oxide prepared in the step (3) has a two-dimensional structure, a large number of mesopores and adjustable components.
In the present invention, the cation ratio of the mixed metal cation solvent is an equimolar ratio.
Modifying potassium oleate on the surfaces of various substrates, adding cations, generating a target oleate precursor on the surface of the substrate in situ through cation exchange, pyrolyzing oleate at high temperature in a nitrogen atmosphere to obtain graphene oxide-loaded two-dimensional metal oxide, and burning off a graphene oxide template in the air atmosphere to obtain the mesoporous metal oxide two-dimensional sheet. The metal oxide nanosheet is of a two-dimensional structure, has a large number of mesopores, and is adjustable in component.
The invention has the beneficial effects that: the invention can prepare various mesoporous two-dimensional unitary metal oxide sheets and binary to high-entropy mesoporous two-dimensional unitary metal oxide sheets. The existing method can only coat on a single substrate, and most of the coated carbon is disordered and has low graphitization degree and limited application value. Therefore, the invention develops a method for coating the ordered mesoporous graphene on the substrate.
Drawings
FIG. 1 is a transmission electron micrograph of a mesoporous two-dimensional iron oxide sheet prepared in example 1;
FIG. 2 is a transmission electron micrograph of a mesoporous two-dimensional cerium oxide sheet prepared in example 2;
FIG. 3 is a transmission electron microscope image of the mesoporous two-dimensional aluminum oxide sheet prepared in example 3;
FIG. 4 is a transmission electron micrograph of a mesoporous two-dimensional yttrium oxide sheet prepared in example 4;
FIG. 5 is a transmission electron microscope image of a mesoporous two-dimensional cobalt ferrite sheet prepared in example 5;
FIG. 6 is a transmission electron microscope image of a mesoporous two-dimensional Mn-Co-Fe-O sheet prepared in example 6;
FIG. 7 is a transmission electron microscope image of a mesoporous two-dimensional Mn-Co-Zn-Fe-O sheet prepared in example 7;
FIG. 8 is a transmission electron micrograph of a mesoporous two-dimensional Mn-Co-Zn-Ni ferrite sheet obtained in example 7.
Detailed Description
The invention is further illustrated by the following examples.
Example 1
(1) Dispersing 20-50 mg of graphene oxide in 20 ml of 0.25 mol/L potassium oleate solution, performing ultrasonic treatment for 30 minutes, and stirring for two hours to uniformly disperse the graphene oxide;
(2) slowly adding 2.5 ml of 1 mol/L ferric nitrate solution into the solution obtained in the step (1), shaking to precipitate the ferric nitrate solution, and then washing with water for three times;
(3) freeze-drying the precipitate obtained in the step (2) to keep the morphology, and then carrying out 400-500 ℃ in a nitrogen atmosphereoC is carbonized for 2 to 4 hours, and then air 400-450oAnd C, calcining for 6-12 hours to remove the graphene oxide template.
FIG. 1 is a transmission electron microscope image of the mesoporous two-dimensional iron oxide sheet prepared in example 1, and the result shows that the two-dimensional iron oxide sheet has a good ordered mesoporous structure.
Example 2
(1) Dispersing 20-50 mg of graphene oxide in 20 ml of 0.25 mol/L potassium oleate solution, performing ultrasonic treatment for 30 minutes, and stirring for two hours to uniformly disperse the graphene oxide;
(2) slowly adding 2.5 ml of 1 mol/L cerium nitrate solution into the solution obtained in the step (1), shaking to precipitate, and then washing with water for three times;
(3) freeze-drying the precipitate obtained in the step (2) to keep the morphology, and then carrying out 400-500 ℃ in a nitrogen atmosphereoC is carbonized for 2 to 4 hours, and then air 400-450oAnd C, calcining for 6-12 hours to remove the graphene oxide template.
Fig. 2 is a transmission electron microscope image of the mesoporous two-dimensional cerium oxide sheet prepared in example 2, and the result shows that the two-dimensional cerium oxide sheet has a very good ordered mesoporous structure.
Example 3
(1) Dispersing 20-50 mg of graphene oxide in 20 ml of 0.25 mol/L potassium oleate solution, performing ultrasonic treatment for 30 minutes, and stirring for two hours to uniformly disperse the graphene oxide;
(2) slowly adding 2.5 ml of 1 mol/L aluminum chloride solution into the solution obtained in the step (1), shaking to precipitate, and then washing with water for three times;
(3) freeze-drying the precipitate obtained in the step (2) to keep the morphology, and then carrying out 400-500 ℃ in a nitrogen atmosphereoC is carbonized for 2 to 4 hours, and then air 400-450oAnd C, calcining for 6-12 hours to remove the graphene oxide template.
FIG. 3 is a transmission electron microscope image of the mesoporous two-dimensional aluminum oxide sheet prepared in example 3, and the result shows that the two-dimensional aluminum oxide sheet has a good ordered mesoporous structure.
Example 4
(1) Dispersing 20-50 mg of graphene oxide in 20 ml of 0.25 mol/L potassium oleate solution, performing ultrasonic treatment for 30 minutes, and stirring for two hours to uniformly disperse the graphene oxide;
(2) slowly adding 2.5 ml of 1 mol/L yttrium chloride solution into the solution obtained in the step (1), shaking to precipitate the yttrium chloride solution, and then washing with water for three times;
(3) freeze-drying the precipitate obtained in the step (2) to keep the morphology, and then carrying out 400-500 ℃ in a nitrogen atmosphereoC is carbonized for 2 to 4 hours, and then air 400-450oAnd C, calcining for 6-12 hours to remove the graphene oxide template.
FIG. 4 is a transmission electron microscope image of the mesoporous two-dimensional yttrium oxide sheet prepared in example 4, and the result shows that the two-dimensional yttrium oxide sheet has a good ordered mesoporous structure.
Example 5
(1) Dispersing 20-50 mg of graphene oxide in 20 ml of 0.25 mol/L potassium oleate solution, performing ultrasonic treatment for 30 minutes, and stirring for two hours to uniformly disperse the graphene oxide;
(2) slowly adding 2.5 ml of 1 mol/L mixed solution of ferric nitrate and cobalt nitrate (the molar ratio is 1: 1) into the solution obtained in the step (1), shaking to precipitate the mixed solution, and then washing with water for three times;
(3) freeze-drying the precipitate obtained in the step (2) to keep the morphology, carbonizing the precipitate at 400-500 ℃ for 2-4 hours in a nitrogen atmosphere, and calcining the precipitate at 400-450 ℃ for 6-12 hours in air to remove the graphene oxide template.
Fig. 5 is a transmission electron microscope image of the mesoporous two-dimensional cobalt ferrite sheet prepared in example 5, and the result shows that the two-dimensional cobalt ferrite sheet has a very good ordered mesoporous structure.
Example 6
(1) Dispersing 20-50 mg of graphene oxide in 20 ml of 0.25 mol/L potassium oleate solution, performing ultrasonic treatment for 30 minutes, and stirring for two hours to uniformly disperse the graphene oxide;
(2) slowly adding 2.5 ml of 1 mol/L mixed solution of ferric nitrate, manganese nitrate and cobalt nitrate (the molar ratio is 1: 1: 1) into the solution obtained in the step (1), shaking to precipitate the mixed solution, and then washing with water for three times;
(3) freeze-drying the precipitate obtained in the step (2) to keep the morphology, then carbonizing at 400-450 ℃ for 2-4 hours in a nitrogen atmosphere, and then calcining at 400-450 ℃ for 6-12 hours in air to remove the graphene oxide template.
FIG. 6 is a transmission electron microscope image of the mesoporous two-dimensional Mn-Co-Fe-O sheet prepared in example 6, and the result shows that the two-dimensional Mn-Co-Fe-O sheet has a good ordered mesoporous structure.
Example 7
(1) Dispersing 20-50 mg of graphene oxide in 20 ml of 0.25 mol/L potassium oleate solution, performing ultrasonic treatment for 30 minutes, and stirring for two hours to uniformly disperse the graphene oxide;
(2) slowly adding 2.5 ml of 1 mol/L mixed solution of ferric nitrate, zinc nitrate, manganese nitrate and cobalt nitrate (the molar ratio is 1: 1: 1: 1) into the solution obtained in the step (1), shaking to precipitate the mixed solution, and then washing with water for three times;
(3) freeze-drying the precipitate obtained in the step (2) to keep the morphology, then carbonizing at 400-450 ℃ for 2-4 hours in a nitrogen atmosphere, and then calcining at 400-450 ℃ for 6-12 hours in air to remove the graphene oxide template.
FIG. 7 is a transmission electron microscope image of the mesoporous two-dimensional MnCoFeZnOe sheet prepared in example 7, and the result shows that the two-dimensional MnCoFeOx sheet has a very good ordered mesoporous structure.
Example 8
(1) Dispersing 20-50 mg of graphene oxide in 20 ml of 0.25 mol/L potassium oleate solution, performing ultrasonic treatment for 30 minutes, and stirring for two hours to uniformly disperse the graphene oxide;
(2) slowly adding 2.5 ml of 1 mol/L mixed solution of ferric nitrate, zinc nitrate, nickel nitrate, manganese nitrate and cobalt nitrate (the molar ratio is 1: 1: 1: 1: 1) into the solution obtained in the step (1), shaking to precipitate the mixed solution, and then washing with water for three times;
(3) freeze-drying the precipitate obtained in the step (2) to keep the morphology, then carbonizing at 400-450 ℃ for 2-4 hours in a nitrogen atmosphere, and then calcining at 400-450 ℃ for 6-12 hours in air to remove the graphene oxide template.
FIG. 8 is a transmission electron microscope image of the mesoporous two-dimensional high-entropy Mn-Co-Ni-Fe-Zn-O sheet prepared in example 8, and the result shows that the two-dimensional high-entropy Mn-Co-Ni-Fe-O sheet has a very good ordered mesoporous structure.
Claims (10)
1. The preparation method of the mesoporous metal oxide two-dimensional sheet with adjustable components is characterized by comprising the following specific steps:
(1) dispersing substrate graphene oxide in a potassium oleate aqueous solution, and performing ultrasonic treatment to uniformly disperse the substrate graphene oxide;
(2) slowly adding metal cations into the solution obtained in the step (1) for cation exchange, and washing after precipitation;
(3) drying the precipitate obtained in the step (2), then carrying out high-temperature pyrolysis in an inert gas atmosphere, and finally carrying out air firing in an oxidizing atmosphere to prepare a mesoporous metal oxide two-dimensional sheet with adjustable components;
wherein, the metal cation in the step (2) is one or more of iron ion, manganese ion, cobalt ion, zinc ion, nickel ion, cerium ion, aluminum ion or yttrium ion; the high-temperature pyrolysis condition of the inert gas in the step (3) is N2In the atmosphere, 400- oCCarbonizing for 2-4 hours; the oxidizing atmosphere in the step (3) is air atmosphere, 400-oCalcining for 6-12 hours under C.
2. The method according to claim 1, wherein the oxygen content of the base graphene oxide in step (1) is 40-50%.
3. The method according to claim 1, wherein the metal ion solution in the step (2) is an iron nitrate solution.
4. The method according to claim 1, wherein the metal ion solution in step (2) is a cerium nitrate solution.
5. The method according to claim 1, wherein the metal ion solution in the step (2) is an aluminum chloride solution.
6. The method according to claim 1, wherein the metal ion solution in step (2) is a yttrium chloride solution.
7. The method according to claim 1, wherein the metal ion solution in the step (2) is a mixed solution of ferric nitrate and cobalt nitrate in a molar ratio of 1: 1.
8. The method according to claim 1, wherein the metal ion solution in the step (2) is a solution having a molar ratio of 1: 1:1 of ferric nitrate, manganese nitrate and cobalt nitrate.
9. The method according to claim 1, wherein the metal ion solution in the step (2) is a solution having a molar ratio of 1: 1: 1:1 of ferric nitrate, manganese nitrate, cobalt nitrate and zinc nitrate.
10. The method according to claim 1, wherein the metal ion solution in the step (2) is a solution having a molar ratio of 1: 1: 1: 1:1 of ferric nitrate, manganese nitrate, cobalt nitrate, zinc nitrate and nickel nitrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210292463.4A CN114620769A (en) | 2022-03-24 | 2022-03-24 | Preparation method of component-adjustable mesoporous metal oxide two-dimensional sheet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210292463.4A CN114620769A (en) | 2022-03-24 | 2022-03-24 | Preparation method of component-adjustable mesoporous metal oxide two-dimensional sheet |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114620769A true CN114620769A (en) | 2022-06-14 |
Family
ID=81903890
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210292463.4A Pending CN114620769A (en) | 2022-03-24 | 2022-03-24 | Preparation method of component-adjustable mesoporous metal oxide two-dimensional sheet |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114620769A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104163453A (en) * | 2014-07-21 | 2014-11-26 | 复旦大学 | Preparation method of highly-ordered nano particle superlattice material |
| CN104860306A (en) * | 2015-06-19 | 2015-08-26 | 海门容汇通用锂业有限公司 | Method for preparing highly ordered mesoporous grapheme materials |
| CN106315515A (en) * | 2016-08-04 | 2017-01-11 | 河北大学 | Metal-oxide two-dimensional material and preparing method and application thereof |
| CN108355632A (en) * | 2018-03-16 | 2018-08-03 | 中国科学院山西煤炭化学研究所 | A kind of oxide nano-slice and preparation method thereof and composite catalyst |
| CN109852835A (en) * | 2019-01-23 | 2019-06-07 | 南京工业大学 | A kind of preparation method of graphene/copper nanocomposite |
| US20190375653A1 (en) * | 2018-06-06 | 2019-12-12 | West Virginia University | Hierarchical Cellular Mesoporous Metal-Oxide Composites |
-
2022
- 2022-03-24 CN CN202210292463.4A patent/CN114620769A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104163453A (en) * | 2014-07-21 | 2014-11-26 | 复旦大学 | Preparation method of highly-ordered nano particle superlattice material |
| CN104860306A (en) * | 2015-06-19 | 2015-08-26 | 海门容汇通用锂业有限公司 | Method for preparing highly ordered mesoporous grapheme materials |
| CN106315515A (en) * | 2016-08-04 | 2017-01-11 | 河北大学 | Metal-oxide two-dimensional material and preparing method and application thereof |
| CN108355632A (en) * | 2018-03-16 | 2018-08-03 | 中国科学院山西煤炭化学研究所 | A kind of oxide nano-slice and preparation method thereof and composite catalyst |
| US20190375653A1 (en) * | 2018-06-06 | 2019-12-12 | West Virginia University | Hierarchical Cellular Mesoporous Metal-Oxide Composites |
| CN109852835A (en) * | 2019-01-23 | 2019-06-07 | 南京工业大学 | A kind of preparation method of graphene/copper nanocomposite |
Non-Patent Citations (1)
| Title |
|---|
| 李银峰等: "《碳纳米材料制备及其应用研究》", 中国科学技术大学出版社, pages: 184 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108128774A (en) | A kind of preparation method of high-purity porous charcoal | |
| CN109665525B (en) | Preparation method of dumbbell-shaped iron-nitrogen double-doped porous carbon | |
| CN113753959A (en) | Lanthanum ferrite perovskite material and preparation method and application thereof | |
| CN112010361A (en) | Preparation method for synthesizing heteroatom-doped nickel sulfide with various shapes by using metal organic framework | |
| CN107824208B (en) | Preparation method of nickel-containing methanation catalyst | |
| CN109192961B (en) | Preparation method of positive electrode material | |
| CN111330620A (en) | Intercalation type graphite-like carbon nitride composite material, preparation method and application thereof | |
| CN110697708A (en) | Nitrogen-doped porous carbon material for lithium ion capacitor and efficient preparation method of low-temperature co-molten solvent activated biomass waste of nitrogen-doped porous carbon material | |
| CN108525637B (en) | Carbon template method modified calcium-based carbon dioxide adsorbent and preparation method thereof | |
| CN113422028A (en) | Preparation method of battery positive electrode composite material | |
| CN114620769A (en) | Preparation method of component-adjustable mesoporous metal oxide two-dimensional sheet | |
| CN111774063B (en) | Ammonium perchlorate thermal decomposition catalytic material and preparation method thereof | |
| CN111450842B (en) | Preparation method of micro-flower structure black lead-copper ore phase metal oxide electrocatalyst, electrocatalyst and application thereof | |
| CN110451498B (en) | Graphene-boron nitride nanosheet composite structure and preparation method thereof | |
| CN111874900A (en) | Metal coordination block copolymer, preparation method and application thereof | |
| CN108745405B (en) | Carbon nitride/nitrogen doped hollow mesoporous carbon/bismuth trioxide ternary Z-shaped photocatalyst and preparation method thereof | |
| CN114751369B (en) | MnCo 2 O 4.5 -MgH 2 Composite hydrogen storage material and preparation method thereof | |
| CN111533121B (en) | Preparation method of porous graphite hollow hemisphere with high specific surface area | |
| CN112875766B (en) | Method for preparing ternary cathode material by microwave heating solution method with carbon source added | |
| CN113078302B (en) | Method for preparing sodium-ion battery composite negative electrode material by using large-interlayer-distance two-dimensional layered graphene-like loaded metal sulfide | |
| CN107715883A (en) | A kind of Ni3The preparation method of FeN@graphenes/marine alga aeroge elctro-catalyst | |
| CN115246633A (en) | Hollow structure g-C 3 N 4 Material, preparation method and application thereof | |
| CN113808859A (en) | Preparation method of two-dimensional layered MXene composite TiN electrode material | |
| CN111470547A (en) | NCM @ Al2O3Preparation method for modifying/rCO material | |
| CN115676858B (en) | Preparation method of flaky porous silicon steel grade magnesium oxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |