CN109231172A - A kind of two-dimensional metallic oxide nano-slice and preparation method thereof - Google Patents
A kind of two-dimensional metallic oxide nano-slice and preparation method thereof Download PDFInfo
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- CN109231172A CN109231172A CN201811018977.0A CN201811018977A CN109231172A CN 109231172 A CN109231172 A CN 109231172A CN 201811018977 A CN201811018977 A CN 201811018977A CN 109231172 A CN109231172 A CN 109231172A
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- oxide nano
- salt
- frame material
- graphite alkene
- metallic oxide
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- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 50
- -1 graphite alkene Chemical class 0.000 claims abstract description 41
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 33
- 239000010439 graphite Substances 0.000 claims abstract description 33
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052751 metal Inorganic materials 0.000 claims abstract description 22
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 21
- 239000002184 metal Substances 0.000 claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 17
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 5
- 238000004146 energy storage Methods 0.000 claims abstract description 4
- 150000004706 metal oxides Chemical class 0.000 claims description 25
- 239000002135 nanosheet Substances 0.000 claims description 22
- 150000003839 salts Chemical class 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 7
- 239000010410 layer Substances 0.000 claims description 7
- 239000013049 sediment Substances 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical group [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- 239000011229 interlayer Substances 0.000 claims description 5
- 230000001376 precipitating effect Effects 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- 150000005323 carbonate salts Chemical class 0.000 claims description 4
- 238000003837 high-temperature calcination Methods 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical class [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 159000000013 aluminium salts Chemical class 0.000 claims description 2
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims description 2
- 239000001099 ammonium carbonate Substances 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- 239000000908 ammonium hydroxide Substances 0.000 claims description 2
- 229910052788 barium Inorganic materials 0.000 claims description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 2
- 159000000009 barium salts Chemical class 0.000 claims description 2
- 239000011651 chromium Substances 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 150000001868 cobalt Chemical class 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 159000000003 magnesium salts Chemical class 0.000 claims description 2
- 150000002696 manganese Chemical class 0.000 claims description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- 150000002751 molybdenum Chemical class 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 239000011733 molybdenum Substances 0.000 claims description 2
- 150000002815 nickel Chemical class 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims description 2
- 239000011135 tin Substances 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 150000003608 titanium Chemical class 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 150000003657 tungsten Chemical class 0.000 claims description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 239000010937 tungsten Substances 0.000 claims description 2
- 150000003751 zinc Chemical class 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 17
- 239000000243 solution Substances 0.000 abstract description 13
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000001354 calcination Methods 0.000 abstract description 3
- 239000012702 metal oxide precursor Substances 0.000 abstract 2
- 239000012266 salt solution Substances 0.000 abstract 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
- 239000002055 nanoplate Substances 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 4
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 4
- 239000004408 titanium dioxide Substances 0.000 description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 229960004887 ferric hydroxide Drugs 0.000 description 2
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000000347 magnesium hydroxide Substances 0.000 description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 2
- 239000011656 manganese carbonate Substances 0.000 description 2
- 229940093474 manganese carbonate Drugs 0.000 description 2
- 235000006748 manganese carbonate Nutrition 0.000 description 2
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 2
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 229940007718 zinc hydroxide Drugs 0.000 description 2
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 241000549556 Nanos Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium(II) oxide Chemical compound [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/36—Methods for preparing oxides or hydroxides in general by precipitation reactions in aqueous solutions
-
- 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
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/145—After-treatment of oxides or hydroxides, e.g. pulverising, drying, decreasing the acidity
-
- 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
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
-
- 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
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
-
- 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]
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- 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
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- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
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Abstract
The present invention relates to a kind of two-dimensional metallic oxide nano-slices and preparation method thereof.This method comprises the following steps: lamellar graphite alkene frame material particle being immersed in metal salt solution and the hygrometric state lamellar graphite alkene frame material particle comprising metal salt solution is obtained by filtration；The hygrometric state lamellar graphite alkene frame material particle precipitates in precipitant solution and filtration drying obtains lamellar graphite alkene frame material/metal oxide precursor compound；Layered graphene frame material/metal oxide precursor compound obtains two-dimensional metallic oxide nano-slice through calcining in air.Compared with prior art, the present invention has the characteristics that low cost, high universality, high efficiency, high controllability and can magnanimity preparation.The average thickness of two-dimensional metallic oxide nano-slice prepared by the present invention is 0.5-30 nanometers; width is 0.1-1000 microns; specific surface area is 20-500 meters squared per gram, can be used for the multiple fields such as energy storage and conversion, chemical catalysis, environmental protection, biomedicine.
Description
Technical field
The invention belongs to technical field of nano material, it is related to a kind of two-dimensional metallic oxide nano-slice and preparation method thereof.
Background technique
Metal oxide nano-material is because of performances such as its excellent electricity, light, heat, mechanics, in the energy, catalysis, material, ring
The fields such as border, electronics and biomedicine, which exist, is widely applied potentiality.Metal oxide nano-sheet with two-dimensional structure due to
With characteristics such as high-specific surface area, short carrier mobility distance, high activities, it is widely used in the energy, catalysis and environmental protection
Equal fields.
Due to the huge application prospect of two-dimensional metallic oxide-based nanomaterial, in recent years about metal oxide nano-sheet
The research of synthesis and pattern control is more and more, wherein how to synthesize non-laminar metal oxide nano-sheet becomes research
Focus.Currently, the synthetic method of non-laminar metal oxide nano-sheet mainly have it is several: nanocrystalline self-assembly method, two dimension
It is orientated connection method, stratiform presoma up-stripping method, two dimension pattern plate synthetic method and local chemical transfer method, wherein especially with two-dimentional mould
The most widely used hair of plate method.In numerous two dimension pattern plate agent, the graphene oxide with two-dimensional structure is due to containing largely on surface
Oxygen-containing group is convenient for that interaction occurs and is most widely used with metal precursor.
Since two dimension pattern plate agent cannot achieve real two-dimensional confinement, two dimension pattern plate method synthesis of metal oxide nanometer
The key of piece is how to allow presoma uniformly to grow the nanoparticle of thin layer on two dimension pattern plate agent surface or receive by accuracy controlling
Rice corpuscles precursor can neither generate alone nanoparticle in this process in the solution, can not grow up on template surface
Larger sized crystal or aggregation.In order to solve this problem, existing research work uses various methods, it usually needs essence
Thin regulation realizes that nanoparticle is grown on two dimension pattern plate agent surface, and this regulation usually has specificity: different metal
Need different condition and method.This makes these preparation methods all not pervasive enough, is only applicable to specific metal or certain kinds
Metal.Simultaneously as harsh reaction condition, the metal oxide nano-sheet normal yield of preparation is low, at high cost, it is difficult to big
Amount preparation.Therefore, develop it is a kind of with low cost, high universality, high efficiency, high controllability and can magnanimity preparation synthesis two dimension
The new method of metal oxide nano-sheet, be still two-dimensional metallic oxide nano-slice faced one of practical application it is important
Challenge.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of low costs, high universality, high efficiency, Gao Ke by the present invention
Control property and can magnanimity preparation two-dimensional metallic oxide nano-slice and preparation method thereof.Two-dimensional metallic oxide prepared by the present invention
Nanometer sheet can be used for the multiple fields such as energy storage and conversion, chemical catalysis, environmental protection, biomedicine.
A kind of two-dimensional metallic oxide nano-slice proposed by the present invention, the metal oxide nano-sheet have two-dimensional layer
Structure；The metal oxide nano-sheet with a thickness of 0.5-30 nanometers；The cross-section lengths of the metal oxide nano-sheet
It is 0.1-1000 microns.
In the present invention, the metal oxide nano-sheet has hole configurations, and the average pore size of hole is 0.5-10 nanometers；
The specific surface area of the metal oxide nano-sheet is 20-500 meters squared per gram.
In the present invention, in the metal oxide nano-sheet metallic element include iron, aluminium, magnesium, titanium, zinc, chromium, copper, manganese,
The mixing of one or more of barium, nickel, cobalt, zirconium, tin, silver, tungsten or molybdenum.
A kind of preparation method of two-dimensional metallic oxide nano-slice proposed by the present invention, the specific steps are as follows:
(1): lamellar graphite alkene frame material being added in aqueous metal salt, the wet of interlayer metalline solution is obtained by filtration
State layer shape graphene frame material particle；
(2): the precipitating reagent that the hygrometric state lamellar graphite alkene frame material particle that step (1) obtains is added to excessive metal salt is molten
In liquid, after sediment is filtered, washed and dried drying, lamellar graphite alkene frame material/metal salt precipitate object compound is obtained；
(3): lamellar graphite alkene frame material/metal salt precipitate object compound that step (2) is obtained obtains two through high-temperature calcination
Tie up metal oxide nano-sheet.
In the present invention, lamellar graphite alkene frame material used is by graphene oxide three-dimensional structure and more in step (1)
The reaction of amino-polyether amine is prepared, layered graphene frame material by graphene sheet layer periodically arranged in parallel and
Interlayer links the polyamino polyetheramine strand of two adjacent sheets and micropore/mesopore orbit is constituted.
In the present invention, metal salt as described in step (1) be soluble ferric iron salt, aluminium salt, magnesium salts, titanium salt, zinc salt, chromic salts,
The mixing of one or more of mantoquita, manganese salt, barium salt, nickel salt, cobalt salt, zirconates, pink salt, silver salt, tungsten salt or molybdenum salt；The metal
The concentration of salt is 0.0001-100 mol/L.
In the present invention, the precipitating reagent of metal salt described in step (2) is water soluble alkali or soluble carbonate salt；It is described heavy
The concentration of shallow lake agent is 0.001-50 mol/L.
In the present invention, the water soluble alkali is the mixing of one or more of sodium hydroxide, potassium hydroxide or ammonium hydroxide, described
Soluble carbonate salt is the mixing of one or more of sodium carbonate, potassium carbonate or ammonium carbonate.
In the present invention, high-temperature calcination condition described in step (3) are as follows: in air at a temperature of 200-1500 DEG C, calcining
0.5-20 hours.
Two-dimensional metallic oxide nano-slice proposed by the present invention energy storage and conversion, chemical catalysis, environmental protection or
Application in the fields such as biomedicine.
The present invention has the advantage that compared with technology with current material
It (1) can be strictly by metal oxide using the two-dimensional confinement space of the graphene film interlayer of lamellar graphite alkene frame material
In the two-dimensional space that presoma growth is limited in, avoids the uncontrollable growth of presoma and further grow up, it is ensured that final
To metal oxide be two-dimensional nano piece rather than other structure.
(2) thickness for the two-dimensional metallic oxide nano-slice being prepared is by the lamellar graphite as two-dimensional nano reactor
The interlamellar spacing of alkene frame material determines, and lamellar graphite alkene frame material used has uniform, controllable graphene film interlamellar spacing,
Therefore two-dimensional metallic oxide nano-slice prepared by the present invention has controllable thickness and narrow thickness distribution.
(3) preparation method provided by the invention has extraordinary universality, can prepare various metal oxide nanos
Piece.Meanwhile preparation method provided by the invention have the characteristics that low cost, can magnanimity preparation.
Detailed description of the invention
The drawings are intended to provide a further understanding of the invention, and constitutes part of specification, with following reality
It applies mode to be used to explain the present invention together, but is not construed as limiting the invention.
Fig. 1 is bitter earth nano piece transmission electron microscope photo.
Fig. 2 is titanium dioxide nanoplate transmission electron microscope photo.
Fig. 3 is di-iron trioxide nanometer sheet transmission electron microscope photo.
Specific embodiment
Below in conjunction with attached drawing, specific embodiments of the present invention will be described in detail.It should be understood that of the invention
The one or more steps mentioned is not repelled before and after the combination step there is also other method and steps or these are clear
Other method and steps can also be inserted between the step of referring to.It should also be understood that these examples be merely to illustrate the present invention without
For limiting the scope of the invention.Unless otherwise indicated, the number of various method steps is only the purpose of identification various method steps, and
Non- arrangement order or restriction to limit each method practical range of the invention, relativeness is altered or modified, in nothing
Under conditions of substantial technological content alteration, when being also considered as the enforceable scope of the present invention.
The preparation of 1. bitter earth nano piece of embodiment
(1): 0.1 gram of lamellar graphite alkene frame material being added in the magnesium nitrate solution that 10 milliliters of concentration are 1 mol/L, impregnates
The hygrometric state lamellar graphite alkene frame material particle containing magnesium nitrate solution is obtained by filtration afterwards；
(2): it is 0.5 mol/L that 100 milliliters of concentration, which are added, in the hygrometric state lamellar graphite alkene frame material particle that step (1) is obtained
Sodium hydroxide solution in, sediment be filtered, washed and dried it is dry after obtain graphene frame material/magnesium hydroxide compound；
(3): graphene frame material/magnesium hydroxide compound that step (2) is obtained is calcined 2 hours in air at 500 DEG C,
Obtain final bitter earth nano piece.
The characterization result of gained bitter earth nano piece is shown in attached drawing 1.
The preparation of 2. titanium dioxide nanoplate of embodiment
(1): 0.1 gram of lamellar graphite alkene frame material being added in the aqueous solution of titanyle sulfate that 10 milliliters of concentration are 0.1 mol/L
Material, is obtained by filtration the hygrometric state lamellar graphite alkene frame material particle of sulfur acid oxygen titanium solution after immersion；
(2): it is 1 mol/L that 100 milliliters of concentration, which are added, in the hygrometric state lamellar graphite alkene frame material particle that step (1) is obtained
In sodium hydroxide solution, sediment obtains graphene frame material/titanium hydroxide compound after being filtered, washed and dried drying；
(3): graphene frame material/titanium hydroxide compound that step (2) is obtained is calcined 2 hours in air at 700 DEG C,
Obtain final titanium dioxide nanoplate.
The characterization result of gained titanium dioxide nanoplate is shown in attached drawing 2.
The preparation of 3. di-iron trioxide nanometer sheet of embodiment
(1): 0.1 gram of lamellar graphite alkene frame material being added in the ferrum sulfuricum oxydatum solutum that 10 milliliters of concentration are 5 mol/Ls, impregnates
The hygrometric state lamellar graphite alkene frame material particle of sulfur acid ferrous solution is obtained by filtration afterwards；
(2): it is 1 mol/L that 100 milliliters of concentration, which are added, in the hygrometric state lamellar graphite alkene frame material particle that step (1) is obtained
In ammonia spirit, sediment obtains graphene frame material/ferric hydroxide composite after being filtered, washed and dried drying；
(3): graphene frame material/ferric hydroxide composite that step (2) is obtained is calcined 5 hours for 400 DEG C in air, is obtained
To final di-iron trioxide nanometer sheet.
The characterization result of gained di-iron trioxide nanometer sheet is shown in attached drawing 3.
The preparation of 4. manganese dioxide nano-plates of embodiment
(1): 0.1 gram of lamellar graphite alkene frame material, leaching being added in the manganese nitrate solution that 20 milliliters of concentration are 0.5 mol/L
The hygrometric state lamellar graphite alkene frame material particle containing manganese nitrate solution is obtained by filtration after bubble；
(2): it is 1 mol/L that 100 milliliters of concentration, which are added, in the hygrometric state lamellar graphite alkene frame material particle that step (1) is obtained
In sodium carbonate liquor, sediment obtains graphene frame material/manganese carbonate compound after being filtered, washed and dried drying；
(3): graphene frame material/manganese carbonate compound that step (2) is obtained is calcined 2 hours in air at 800 DEG C, is obtained
To final manganese dioxide nano-plates.
The preparation of 5. Zinc oxide nano sheet of embodiment
(1): 0.1 gram of lamellar graphite alkene frame material, leaching being added in the zinc nitrate solution that 10 milliliters of concentration are 0.5 mol/L
The hygrometric state lamellar graphite alkene frame material particle containing zinc nitrate solution is obtained by filtration after bubble；
(2): it is 1 mol/L that 100 milliliters of concentration, which are added, in the hygrometric state lamellar graphite alkene frame material particle that step (1) is obtained
In potassium hydroxide solution, sediment obtains graphene frame material/zinc hydroxide compound after being filtered, washed and dried drying；
(3): graphene frame material/zinc hydroxide compound that step (2) is obtained is small in 600 DEG C of calcinings 0.5 in air
When, obtain final Zinc oxide nano sheet.
Claims (10)
1. a kind of two-dimensional metallic oxide nano-slice, it is characterised in that the metal oxide nano-sheet has two-dimensional layer knot
Structure；The metal oxide nano-sheet with a thickness of 0.5-30 nanometers；The cross-section lengths of the metal oxide nano-sheet are
0.1-1000 microns.
2. two-dimensional metallic oxide nano-slice according to claim 1, it is characterised in that the metal oxide nano-sheet
With hole configurations, the average pore size of hole is 0.5-10 nanometers；The specific surface area of the metal oxide nano-sheet is 20-
500 meters squared per grams.
3. two-dimensional metallic oxide nano-slice according to claim 1, it is characterised in that the metal oxide nano-sheet
Middle metallic element includes one or more of iron, aluminium, magnesium, titanium, zinc, chromium, copper, manganese, barium, nickel, cobalt, zirconium, tin, silver, tungsten or molybdenum
Mixing.
4. a kind of preparation method of two-dimensional metallic oxide nano-slice as described in claim 1, it is characterised in that specific steps
It is as follows:
(1): lamellar graphite alkene frame material being added in aqueous metal salt, the wet of interlayer metalline solution is obtained by filtration
State layer shape graphene frame material particle；
(2): the precipitating reagent that the hygrometric state lamellar graphite alkene frame material particle that step (1) obtains is added to excessive metal salt is molten
In liquid, after sediment is filtered, washed and dried drying, lamellar graphite alkene frame material/metal salt precipitate object compound is obtained；
(3): lamellar graphite alkene frame material/metal salt precipitate object compound that step (2) is obtained obtains two through high-temperature calcination
Tie up metal oxide nano-sheet.
5. the preparation method of two-dimensional metallic oxide nano-slice according to claim 4, it is characterised in that institute in step (1)
It is to be reacted to be prepared with polyamino polyetheramine by graphene oxide three-dimensional structure with lamellar graphite alkene frame material, it is described
Lamellar graphite alkene frame material is linked the polyamino of two adjacent sheets by graphene sheet layer and interlayer periodically arranged in parallel
Polyetheramine strand and micropore/mesopore orbit are constituted.
6. the preparation method of two-dimensional metallic oxide nano-slice according to claim 4, it is characterised in that institute in step (1)
The metal salt stated is soluble ferric iron salt, aluminium salt, magnesium salts, titanium salt, zinc salt, chromic salts, mantoquita, manganese salt, barium salt, nickel salt, cobalt salt, zirconium
The mixing of one or more of salt, pink salt, silver salt, tungsten salt or molybdenum salt；The concentration of the metal salt be 0.0001-100 moles/
It rises.
7. the preparation method of two-dimensional metallic oxide nano-slice according to claim 4, it is characterised in that institute in step (2)
The precipitating reagent for stating metal salt is water soluble alkali or soluble carbonate salt；The concentration of the precipitating reagent is 0.001-50 mol/L.
8. the preparation method of two-dimensional metallic oxide nano-slice according to claim 7, it is characterised in that the solubility
Alkali is the mixing of one or more of sodium hydroxide, potassium hydroxide or ammonium hydroxide, and the soluble carbonate salt is sodium carbonate, potassium carbonate
Or one or more of ammonium carbonate mixing.
9. the preparation method of two-dimensional metallic oxide nano-slice according to claim 4, it is characterised in that institute in step (3)
State high-temperature calcination condition are as follows: in air at a temperature of 200-1500 DEG C, calcine 0.5-20 hours.
10. a kind of two-dimensional metallic oxide nano-slice as described in claim 1 is in energy storage and conversion, chemical catalysis, ring
Application in border protection or field of biomedicine.
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