CN111924880A - Preparation method of carbon-coated tantalum pentoxide nanosheet - Google Patents
Preparation method of carbon-coated tantalum pentoxide nanosheet Download PDFInfo
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- CN111924880A CN111924880A CN202010695543.5A CN202010695543A CN111924880A CN 111924880 A CN111924880 A CN 111924880A CN 202010695543 A CN202010695543 A CN 202010695543A CN 111924880 A CN111924880 A CN 111924880A
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- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 title claims abstract description 46
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 38
- 239000002135 nanosheet Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 title description 5
- 229910004481 Ta2O3 Inorganic materials 0.000 claims abstract description 43
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229960003638 dopamine Drugs 0.000 claims abstract description 31
- 239000002131 composite material Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000012298 atmosphere Substances 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 52
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 34
- 239000007853 buffer solution Substances 0.000 claims description 29
- 238000003756 stirring Methods 0.000 claims description 24
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 23
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000011248 coating agent Substances 0.000 claims description 11
- 238000000576 coating method Methods 0.000 claims description 11
- MCHZKGNHFPNZDP-UHFFFAOYSA-N 2-aminoethane-1,1,1-triol;hydrochloride Chemical compound Cl.NCC(O)(O)O MCHZKGNHFPNZDP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 229910001413 alkali metal ion Inorganic materials 0.000 abstract description 5
- 239000010406 cathode material Substances 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 238000004227 thermal cracking Methods 0.000 abstract description 3
- 230000021148 sequestering of metal ion Effects 0.000 abstract 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 19
- 229910001416 lithium ion Inorganic materials 0.000 description 18
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 17
- 238000002156 mixing Methods 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 15
- 239000002105 nanoparticle Substances 0.000 description 15
- 239000010408 film Substances 0.000 description 14
- 229910052751 metal Inorganic materials 0.000 description 11
- 239000002184 metal Substances 0.000 description 11
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 10
- 238000003860 storage Methods 0.000 description 10
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 9
- 239000004202 carbamide Substances 0.000 description 9
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 8
- 229910052744 lithium Inorganic materials 0.000 description 8
- 229960000583 acetic acid Drugs 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 239000012300 argon atmosphere Substances 0.000 description 5
- 239000007773 negative electrode material Substances 0.000 description 5
- 230000002441 reversible effect Effects 0.000 description 5
- 229910001415 sodium ion Inorganic materials 0.000 description 5
- 229910000314 transition metal oxide Inorganic materials 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 4
- 229910003481 amorphous carbon Inorganic materials 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 239000004964 aerogel Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000002608 ionic liquid Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000012983 electrochemical energy storage Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 239000012362 glacial acetic acid Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- QIVUCLWGARAQIO-OLIXTKCUSA-N (3s)-n-[(3s,5s,6r)-6-methyl-2-oxo-1-(2,2,2-trifluoroethyl)-5-(2,3,6-trifluorophenyl)piperidin-3-yl]-2-oxospiro[1h-pyrrolo[2,3-b]pyridine-3,6'-5,7-dihydrocyclopenta[b]pyridine]-3'-carboxamide Chemical compound C1([C@H]2[C@H](N(C(=O)[C@@H](NC(=O)C=3C=C4C[C@]5(CC4=NC=3)C3=CC=CN=C3NC5=O)C2)CC(F)(F)F)C)=C(F)C=CC(F)=C1F QIVUCLWGARAQIO-OLIXTKCUSA-N 0.000 description 1
- -1 1-methyl 3- (2-bromoethyl) imidazole bromide Chemical compound 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000733 Li alloy Inorganic materials 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 239000000411 inducer Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000006138 lithiation reaction Methods 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000352 supercritical drying Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G35/00—Compounds of tantalum
-
- 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
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G35/00—Compounds of tantalum
- C01G35/006—Compounds containing, besides tantalum, two or more other elements, with the exception of oxygen or hydrogen
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a carbon-coated Ta2O5A preparation method of a nano sheet, belonging to the technical field of nano material preparation; in particular to a preparation method of carbon-coated and precursor thermal cracking. The method is characterized in that: mesogen (NH) synthesized by hydrothermal method4)2Ta2O3F6Taking the powder as a raw material; first coated by solutionPreparation of mesogen (NH) by dopamine process4)2Ta2O3F6@ dopamine composite; then the carbon-coated Ta is synthesized by taking the precursor as a precursor and carrying out high-temperature heat treatment in inert atmosphere2O5Nanosheets. The material has the advantages of high conductivity, high alkali metal ion storage capacity, high coulombic efficiency, quick charge and discharge, good cycle stability and the like, so that the material becomes a cathode material of an alkali metal ion battery with high potential. In addition, the preparation method provided by the invention is simple, the selected raw materials are easy to obtain, the experimental equipment is simple, the experimental period is short, and the process flow is easy to control.
Description
Technical Field
The invention relates to a preparation method of carbon-coated tantalum pentoxide nanosheets, belonging to the technical field of nano material preparation; in particular to a preparation method of carbon-coated and precursor thermal cracking.
Background
Electrochemical energy storage, particularly lithium ion, sodium ion and potassium ion batteries, have attracted extensive research interest in various fields as power sources for large electronic devices such as electric vehicles. The research focuses on exploring the application of electrode materials with high theoretical capacity, high power density, quick charge, low self-discharge rate, long cycle life, good safety, wide working temperature range and other excellent performances to the negative electrode of a power supply so as to improve the comprehensive performance of the battery. Due to its high theoretical capacity, transition metal oxides are excellent candidates. In lithium ion batteries, transition metal oxides as the negative electrode material provide three lithium storage mechanisms:
intercalation, namely lithium ions are inserted into or removed from a crystal skeleton in the charge and discharge process;
(II) alloying, i.e. a lithium alloy is formed during charging and is decomposed during discharging;
(III) conversion, i.e. redox reaction of lithium ions with metal oxides to form Li2O and metal/lower valent metal oxides.
The current research is mostly focused on alloying and conversion type transition metal oxides. Wherein, tantalum pentoxide (beta-Ta)2O5) Is a metal oxide in the fifth group of the periodic table of elements, has an orthorhombic structure, and has lattice parameters of a =6.198 Ȧ, b =40.29 Ȧ, and c =3.88 Ȧ. As a semiconductor material with a band gap of about 4.0eV, the material has the advantages of no toxicity, high dielectric constant, good thermal stability, good chemical stability and the like. Therefore, the material has wide application prospect in the fields of dielectric materials, anticorrosive materials, solar cell antireflection films and the like; in particular, it has shown significant visible light absorption and highly enhanced photocatalytic hydrogen production activity.
Further, Ta2O5The transition metal oxide is widely used as a typical conversion transition metal oxide in the negative electrode of a lithium ion battery; the corresponding lithiation/delithiation reversible process is shown in formula (1)
Ta2O5+8Li++8e-↔Ta2O+4Li2O (1)
Wherein each mole of Ta2O5The material can hold 8 mol of lithium ions at most, and the theoretical capacity of the material is calculated to be up to 482mAh/g, while the theoretical capacity of the current commercial graphite negative electrode is only 372 mAh/g. In the process of lithium intercalation, Ta2O5Conversion to Ta2O instead of metallic tantalum; and, the higher lithium insertion/extraction potential (-0.8/~ 1v vs Li/Li)+) The deposition of metal lithium on the surface of the cathode material can be avoided, so that the safety of the lithium ion battery is improved.
At present, Ta2O5As the negative electrode material of the alkali ion battery, there are two forms: (1) a film; and (2) nanoparticles.
First, some researchers have prepared Ta on a metal substrate2O5The film is used as a self-supporting electrode, and the use of an adhesive and carbon black as a conductive agent is avoided due to good electric adhesion with a substrate. Fu et al in the article "Characterisation of Amorphous Ta2O5film as a novel anode material' prepared amorphous Ta with thickness of about 135nm on stainless steel substrate by reaction pulse laser deposition technology2O5Thin film, the electrochemical performance of which in a lithium ion battery is reported for the first time, at a current density of 5mA/cm2The reversible capacity is about 400mAh/g, the capacity is slightly reduced after 1100 cycles, and the reduction amount of each cycle<0.13 percent. Dang et al in the paper "Lithium implantation/desorption Characteristics of Nanostructured Amorphous Tantalum Oxide Film" prepared by electron beam evaporation on copper foil to form nanoporous Amorphous Ta with a thickness and porosity of 195nm and 46%, respectively2O5And a thin film electrode. When the current density is 0.1C, the reversible capacity is about 350 mAh/g; when the current density reached 1C, the capacity was about 252 mAh/g, and the associated capacity loss was about 4% after 100 cycles. The researchers believe that Ta is produced2O5The film has amorphous structure, is porous and has a large specific surfaceThe area characteristics are beneficial to the insertion/extraction process of lithium ions and are helpful to bear the stress related to volume expansion or contraction. Xia et al in the article "Oxygen-determination Ta2O5 nanoporous films as self-supported electrodes for lithium micro batteries" applied electrochemical anodic oxidation technique to nano porous Ta2O5The thickness of the film is increased from hundreds of nanometers to 2.5um, so that the mass load of the film is greatly improved; and heat-treating under argon atmosphere to obtain crystalline and amorphous Ta2O5A film. 3D porous amorphous Ta2O5The theoretical lithium storage capacity of the film is about 480 mAh/g; under the current density of 1C, the reversible capacity of the material reaches 363 mAh/g; further experimental results show significant stability after 8000 cycles at a current density of 5C. The oxygen vacancy and the nano-porous structure are shown to improve the conductivity of the film and promote the diffusion of lithium ions in the negative electrode.
In addition, some studies have focused on Ta2O5The nano particles are used as the negative electrode material of the alkali ion battery. Manukumar et al, paper "Mesoporous Ta2O5In the nanoparticles as an inorganic material for lithium ion batteries and an organic photo catalyst for hydrogen evolution ", 1-methyl 3- (2-bromoethyl) imidazole bromide ionic liquid is used as a porous inducer, and an ionic liquid assisted hydrothermal method is adopted to prepare a nano-composite material with a specific surface area of 236.1 m by a subsequent calcination process (800 ℃/3 h)2(g) mesoporous amorphous Ta having a particle size of 40nm2O5And (3) nanoparticles. Electrochemical test results show that under the current density of 0.1C, the reversible capacity is 180 mAh/g, and after 50 cycles, the coulombic efficiency is close to 100%. In addition, this group followed the "Ionic liquid-assisted hydraulic synthesis of Ta2O5The nanoparticles for lithium-ion batteries applications "synthesized by the method have fine particle size (25 nm), good porosity (average pore diameter of 21 nm) and large specific surface area (23.11 m)2High crystallinity Ta of/g)2O5And (3) nanoparticles. Due to Ta2O5The material has higher lithium storage capacityAmount (190 mAh/g); in addition, at the current density of 0.1C, the coulombic efficiency is still close to 100% after 150 cycles, and good cycle stability is shown. Pan et al, in the article "structural distributed Ta2O5In aerogel for high-rate and high-level Li-ion and Na-ion storage through surface redox reaction, porous three-dimensional interconnected Ta is prepared by adopting a solvothermal method2O5Nano aerogel and subjecting it to CO2And supercritical drying and calcining are carried out, so that the lithium ion and sodium ion battery cathode material with high speed and good stability is prepared. The results show that amorphous Ta has a current density of 100 and 5000mA/g, respectively2O5The lithium ion storage capacity of the aerogel is 280 mAh/g and 94mAh/g respectively, and the sodium ion storage capacity is 100 mAh/g and 44mAh/g respectively; in addition, after the lithium ion battery is cycled for 20000 times under the current density of 5000mA/g and the sodium ion battery is cycled for 1000 times under the current density of 1000mA/g, the electrochemical performance is kept stable, and the capacity is not obviously attenuated.
In conclusion, Ta2O5The pseudocapacitance characteristic of the capacitor not only is beneficial to improving the storage capacity of the alkali metal ions, but also can realize the rapid charging function. Although Ta is amorphous for the crystalline state2O5Although there is a controversy for improving the storage capacity of alkali metal ions, the nano-and porous materials can provide more active sites and shorten the ion diffusion distance, which is well accepted by researchers.
The invention provides a carbon-coated Ta2O5A method for preparing a nanosheet; firstly, tantalum powder, hydrofluoric acid, acetic acid and urea are used as raw materials, and mesogen (NH) is prepared by a hydrothermal method4)2Ta2O3F6Taking the material as a precursor; secondly, obtaining (NH) by coating dopamine4)2Ta2O3F6@ dopamine composite; finally, heat treatment is carried out under argon atmosphere (inert oxygen-free atmosphere) to prepare the carbon-coated Ta2O5And (3) nanoparticles. Ta promoted by pseudocapacitance and conversion type alkali metal storage mechanism2O5Nano materialThe lithium ion battery has the advantages of high capacity, high coulombic efficiency, quick charge and discharge, good cycle stability and the like; in addition, carbon coating can improve the conductivity of the composite material. Thus, carbon-coated Ta2O5The nano-sheet becomes an electrochemical energy storage negative electrode material with potential and wide application.
Disclosure of Invention
The invention aims to provide carbon-coated Ta2O5The preparation method of the nano-sheet enables the material to be used as an efficient energy storage material. Also provides a mesogen (NH)4)2Ta2O3F6Carbon coating and heat treatment of the material.
The processing scheme is as follows:
(1) mesogen (NH)4)2Ta2O3F6Preparation of the material:
the method is characterized in that metal tantalum powder, hydrofluoric acid with the mass fraction of 40%, analytically pure acetic acid, urea and deionized water are used as raw materials. The method comprises the following steps: (1) hydrofluoric acid and metal tantalum powder are mixed according to a molar ratio (3-12): 1, mixing, and fully stirring until the metal tantalum powder is dissolved; (2) deionized water and glacial acetic acid are mixed according to the volume ratio (0.17-6): 1, uniformly mixing; gradually dripping the acetic acid solution into the mixed solution obtained in the step (1) to obtain a milky mixed solution; (3) according to the molar ratio of (0.25-2) urea to metal tantalum powder: 1, weighing urea, adding the urea into the milky white solution system obtained in the step (2), and uniformly stirring. (4) Transferring the solution system into a lining of a hydrothermal reaction kettle, screwing down the reaction kettle, transferring the reaction kettle into a drying oven, heating to 160-210 ℃, and reacting for 3-48 h; (5) after the reaction is finished, naturally cooling the reaction kettle to room temperature, then centrifugally separating the product to obtain white precipitate, repeatedly washing the white precipitate with ethanol and water, centrifuging until the filtrate is neutral, and finally drying to obtain white (NH)4)2Ta2O3F6A material.
(2) Mesogen (NH)4)2Ta2O3F6Preparation of @ dopamine composite material:
with tris (hydroxymethyl) aminomethaneHydrochloride, dopamine hydrochloride, analytically pure concentrated hydrochloric acid and deionized water are used as raw materials. The method comprises the following steps: (1) preparing a buffer solution: firstly, mixing trihydroxymethyl aminomethane hydrochloride and deionized water according to a molar volume ratio (mol: V) of (0.5-2) mol: mixing at a ratio of 10L and stirring thoroughly until a clear solution is obtained, which is named solution A; then, analytically pure concentrated hydrochloric acid and deionized water are mixed according to the volume ratio of (0.25-1): 1, weighing and mixing, stirring to obtain a hydrochloric acid solution which is uniformly mixed and named as a solution B; and gradually dropwise adding the solution B into the solution A until the pH value of the solution A reaches 8-9, thus obtaining the buffer solution. (2) Coating dopamine: white mesogen (NH)4)2Ta2O3F6The mass volume ratio of the powder to the dopamine hydrochloride to the buffer solution (w: w: V) is (1-5) g: (0.5-2) g: 1L of the mixture is weighed; dissolving dopamine hydrochloride in a buffer solution, and fully stirring until the solution is uniform and light yellow; then grinding the fine mesogen (NH)4)2Ta2O3F6Slowly adding the powder into the dopamine hydrochloride buffer solution, fully stirring at room temperature for 12-48 h, carrying out suction filtration on the slurry, and transferring the obtained powder into an oven to dry at 50-100 ℃ for 12-36 h; cooling to obtain mesogen (NH)4)2Ta2O3F6@ dopamine composite.
(3) Carbon coated Ta2O5Preparing a nano sheet:
the heat treatment scheme is as follows; using mesogens (NH)4)2Ta2O3F6The @ dopamine composite material is used as a precursor, the temperature is raised to 900-1100 ℃ at the heating rate of 1-10 ℃/min in inert atmosphere (argon, oxygen-free), the temperature is kept for 0.5-5 h, and carbon-coated Ta can be obtained after cooling2O5Nanosheets.
The working principle of the invention is as follows:
mesogen (NH)4)2Ta2O3F6The @ dopamine composite material is subjected to cracking reaction (mesogen (NH) under the conditions that the temperature is 900-1100 ℃ and the argon atmosphere (inert oxygen-free atmosphere)4)2Ta2O3F6The material and dopamine can be respectively thermally cracked into Ta in high-temperature inert atmosphere2O5Nanoparticles and amorphous carbon) to produce carbon-coated Ta2O5And (3) nanoparticles.
The invention has the advantages that:
carbon coated Ta2O5The nano-particles have the characteristics of small particle size, high specific surface area, porous microstructure, high purity and the like. The preparation method of the material is simple, the experimental period is short, the operation is easy, and the raw materials are easy to obtain. In addition, the prepared carbon-coated Ta2O5The nano particles have the advantages of high lithium ion storage capacity, high coulombic efficiency, rapid charge-discharge characteristics, excellent cycle stability and the like, and can be used as a negative electrode material of an alkali metal ion battery.
Drawings
FIG. 1 is carbon coated Ta prepared in example 12O5XRD pattern of the nano-sheet.
FIG. 2 is carbon coated Ta prepared in example 12O5SEM photograph of nanoplatelets.
FIG. 3 is carbon coated Ta prepared in example 12O5Raman spectra of the nanosheets.
FIG. 4 is carbon coated Ta prepared in example 12O5TEM photograph of nanosheets.
Detailed Description
The technical solution of the present invention is not limited to the specific examples listed below, and includes any combination of the specific embodiments.
Example 1:
preparation of carbon-coated Ta in this embodiment2O5The method of nanosheet is as follows:
(1) mesogen (NH)4)2Ta2O3F6Preparation of @ dopamine composite material:
takes trihydroxymethyl aminomethane hydrochloride, dopamine hydrochloride, analytically pure concentrated hydrochloric acid and deionized water as raw materials. The method comprises the following steps: (1) preparing a buffer solution: will be provided withThe tris hydrochloride and deionized water are mixed according to a molar volume ratio (mol: V) of 1 mol: mixing at a ratio of 13L and stirring thoroughly until a clear solution is obtained, which is named solution A; then, analytically pure concentrated hydrochloric acid and deionized water are mixed according to the volume ratio of 0.5: 1, weighing and mixing, stirring to obtain a hydrochloric acid solution which is uniformly mixed and named as a solution B; and gradually dropwise adding the solution B into the solution A until the pH value reaches 8.5 to obtain a buffer solution. (2) coating dopamine: white mesogen (NH)4)2Ta2O3F6The mass volume ratio of the powder to the dopamine hydrochloride to the buffer solution (w: w: V) is 2.5 g: 1 g: 1L of the mixture is weighed; dissolving dopamine hydrochloride in a buffer solution, and fully stirring until the solution is uniform and light yellow; then grinding the fine mesogen (NH)4)2Ta2O3F6Slowly adding the powder into the dopamine hydrochloride buffer solution, fully stirring at room temperature for 20 hours, carrying out suction filtration on the slurry, and transferring the obtained powder into an oven to dry at 60 ℃ for 20 hours; cooling to obtain mesogen (NH)4)2Ta2O3F6@ dopamine composite.
(2) Carbon coated Ta2O5Preparing a nano sheet:
using mesogens (NH)4)2Ta2O3F6The @ dopamine composite material is taken as a precursor, heated to 1000 ℃ at the heating rate of 5 ℃/min under the inert atmosphere (argon, oxygen-free), kept for 2h, cooled along with the furnace, and then the carbon-coated Ta can be obtained2O5Nanosheets.
(NH) used in the present example4)2Ta2O3F6The preparation method of the precursor comprises the following steps:
the method is characterized in that metal tantalum powder, hydrofluoric acid with the mass fraction of 40%, analytically pure acetic acid, urea and deionized water are used as raw materials. The method comprises the following steps: (1) hydrofluoric acid and metal tantalum powder are mixed according to a molar ratio (3-12): 1, mixing, and fully stirring until the metal tantalum powder is dissolved; (2) deionized water and glacial acetic acid are mixed according to the volume ratio (0.17-6): 1 mixing allHomogenizing; gradually dripping the acetic acid solution into the mixed solution obtained in the step (1) to obtain a milky mixed solution; (3) according to the molar ratio of (0.25-2) urea to metal tantalum powder: 1, weighing urea, adding the urea into the milky white solution system obtained in the step (2), and uniformly stirring. (4) Transferring the solution system into a lining of a hydrothermal reaction kettle, screwing down the reaction kettle, transferring the reaction kettle into a drying oven, heating to 160-210 ℃, and reacting for 3-48 h; (5) after the reaction is finished, naturally cooling the reaction kettle to room temperature, then centrifugally separating the product to obtain white precipitate, repeatedly washing the white precipitate with ethanol and water, centrifuging until the filtrate is neutral, and finally drying to obtain white (NH)4)2Ta2O3F6And (3) powder.
Coating the prepared carbon with Ta2O5The nanosheet is subjected to X-ray diffraction phase analysis (XRD), and an XRD spectrogram obtained by testing is shown in figure 1. The main XRD characteristic peak can be combined with beta-Ta2O5Diffraction peaks of (JCPDS 00-025-0922) are matched; this indicates mesogen (NH)4)2Ta2O3F6The @ dopamine composite material is used as a precursor to generate Ta with high crystallinity through thermal cracking at 1000 ℃ in an argon atmosphere2O5And (4) phase(s).
FIG. 2 is the prepared carbon coated Ta2O5Scanning Electron Microscope (SEM) images of the nanoparticles; the experimental result shows that the prepared Ta2O5The material is granular, and the particle size of the material is 50-250 nm. FIG. 2(b) shows Ta2O5The surface of the nano particles is wrapped with a layer of film.
Coating the prepared carbon with Ta2O5The nanoparticles were raman characterized and the results are shown in figure 3. The spectrum shows Raman peaks corresponding to D and G of amorphous carbon, which indicates mesomorphism (NH)4)2Ta2O3F6@ dopamine composite material is subjected to high-temperature heat treatment (1000 ℃/2 h) in argon atmosphere, then dopamine is thermally cracked to generate amorphous carbon, and the amorphous carbon is wrapped in Ta2O5Outside the particle.
FIG. 4 is the prepared carbon coated Ta2O5A Transmission Electron Microscope (TEM) image of the nanoparticles; the experimental results show that Ta2O5The width of the nano sheet is 50-150 nm, and the surface of the nano sheet is wrapped with a layer of uniform carbon film (shown in fig. 4(a) and (b)); FIG. 4(c) is Ta2O5The distance between crystal planes of a high resolution image (HRTEM) of the nanosheet is measured to be 0.4nm, which corresponds to a (001) crystal plane.
Example 2:
this example differs from example 1 in that:
(1) mesogen (NH)4)2Ta2O3F6Preparation of @ dopamine composite material:
takes trihydroxymethyl aminomethane hydrochloride, dopamine hydrochloride, analytically pure concentrated hydrochloric acid and deionized water as raw materials. The method comprises the following steps: (1) preparing a buffer solution: firstly, mixing trihydroxymethyl aminomethane hydrochloride and deionized water according to a molar volume ratio (mol: V) of 1 mol: mixing at a ratio of 5L, stirring thoroughly until a clear solution is obtained, and naming the clear solution as solution A; then, analytically pure concentrated hydrochloric acid and deionized water are mixed according to the volume ratio of 1: 1, weighing and mixing, stirring to obtain a hydrochloric acid solution which is uniformly mixed and named as a solution B; and then gradually dropwise adding the solution B into the solution A until the pH value of the solution reaches 9, thus obtaining the buffer solution. (2) coating dopamine: white mesogen (NH)4)2Ta2O3F6The mass volume ratio of the powder to the dopamine hydrochloride to the buffer solution (w: w: V) is 5 g: 2 g: 1L of the mixture is weighed; dissolving dopamine hydrochloride in a buffer solution, and fully stirring until the solution is uniform and light yellow; then grinding the fine mesogen (NH)4)2Ta2O3F6Slowly adding the powder into the dopamine hydrochloride buffer solution, fully stirring at room temperature for 48 hours, carrying out suction filtration on the slurry, and transferring the obtained powder into an oven to dry at 100 ℃ for 12 hours; cooling to obtain mesogen (NH)4)2Ta2O3F6@ dopamine composite.
(2) Carbon coated Ta2O5Preparing a nano sheet:
using mesogens (NH)4)2Ta2O3F6The @ dopamine composite material is taken as a precursor, is heated to 900 ℃ at the heating rate of 1 ℃/min under the inert atmosphere (argon, oxygen-free), is kept for 5 hours, and is cooled along with the furnace to obtain the carbon-coated Ta2O5Nanosheets. The rest is the same as in example 1.
Example 3:
this example differs from example 1 in that:
(1) mesogen (NH)4)2Ta2O3F6Preparation of @ dopamine composite material:
takes trihydroxymethyl aminomethane hydrochloride, dopamine hydrochloride, analytically pure concentrated hydrochloric acid and deionized water as raw materials. The method comprises the following steps: (1) preparing a buffer solution: firstly, mixing trihydroxymethyl aminomethane hydrochloride and deionized water according to a molar volume ratio (mol: V) of 1 mol: 20L were mixed and stirred well until a clear solution was obtained, which was designated as solution A. Then, analytically pure concentrated hydrochloric acid and deionized water are mixed according to the volume ratio of 0.25: 1, weighing and mixing, stirring to obtain a hydrochloric acid solution which is uniformly mixed and named as a solution B; and then gradually dropwise adding the solution B into the solution A until the pH value of the solution reaches 8 to obtain a buffer solution. (2) coating dopamine: white mesogen (NH)4)2Ta2O3F6The mass volume ratio of the powder to the dopamine hydrochloride to the buffer solution (w: w: V) is 1 g: 0.5 g: 1L of the mixture is weighed; dissolving dopamine hydrochloride in a buffer solution, and fully stirring until the solution is uniform and light yellow; then grinding the fine mesogen (NH)4)2Ta2O3F6Slowly adding the powder into the dopamine hydrochloride buffer solution, fully stirring at room temperature for 12 hours, carrying out suction filtration on the slurry, and transferring the obtained powder into an oven to dry at 50 ℃ for 36 hours; cooling to obtain mesogen (NH)4)2Ta2O3F6@ dopamine composite.
(2) Carbon coated Ta2O5Preparing a nano sheet:
using mesogens (NH)4)2Ta2O3F6The @ dopamine composite material is taken as a precursor, is heated to 1100 ℃ at the heating rate of 10 ℃/min under the inert atmosphere (argon, oxygen-free), is kept for 0.5h, and is cooled along with the furnace to obtain the carbon-coated Ta2O5Nanosheets. The rest is the same as in example 1.
Example 4:
this example differs from example 1 in that:
(1) mesogen (NH)4)2Ta2O3F6Preparation of @ dopamine composite material:
takes trihydroxymethyl aminomethane hydrochloride, dopamine hydrochloride, analytically pure concentrated hydrochloric acid and deionized water as raw materials. The method comprises the following steps: (1) preparing a buffer solution: firstly, mixing trihydroxymethyl aminomethane hydrochloride and deionized water according to a molar volume ratio (mol: V) of 1 mol: 15L were mixed and stirred well until a clear solution was obtained, which was designated as solution A. Then, analytically pure concentrated hydrochloric acid and deionized water are mixed according to the volume ratio of 0.75: 1, weighing and mixing, stirring to obtain a hydrochloric acid solution which is uniformly mixed and named as a solution B; and then, gradually dropwise adding the solution B into the solution A until the pH value of the solution reaches 8.7 to obtain a buffer solution. (2) Coating dopamine: white mesogen (NH)4)2Ta2O3F6The mass volume ratio of the powder to the dopamine hydrochloride to the buffer solution (w: w: V) is 3 g: 1.5 g: 1L of the mixture is weighed; dissolving dopamine hydrochloride in a buffer solution, and fully stirring until the solution is uniform and light yellow; then grinding the fine mesogen (NH)4)2Ta2O3F6Slowly adding the powder into the dopamine hydrochloride buffer solution, fully stirring at room temperature for 24 hours, carrying out suction filtration on the slurry, and transferring the obtained powder into an oven to dry at 80 ℃ for 24 hours; cooling to obtain mesogen (NH)4)2Ta2O3F6@ dopamine composite.
(2) Carbon coated Ta2O5Preparing a nano sheet:
using mesogens (NH)4)2Ta2O3F6The @ dopamine composite material is taken as a precursor, heated to 1000 ℃ at the heating rate of 2 ℃/min in inert atmosphere (argon, oxygen-free), kept for 3h, cooled along with the furnace, and then the carbon-coated Ta can be obtained2O5Nanosheets. The rest is the same as in example 1.
Claims (1)
1. Carbon-coated Ta2O5The preparation method of the nano-sheet is characterized by comprising the following steps: mesogen (NH) synthesized by hydrothermal method4)2Ta2O3F6The material is used as a raw material, (1) mesogen (NH) is prepared by a solution coating dopamine process4)2Ta2O3F6@ dopamine composite; the process flow is as follows: firstly, gradually dripping a hydrochloric acid solution (analytically pure concentrated hydrochloric acid and deionized water according to the volume ratio of (0.25-1): 1) into a trihydroxymethyl aminomethane hydrochloride solution (the molar volume ratio of the trihydroxymethyl aminomethane hydrochloride to the deionized water is (0.5-2) mol: 10L) until the pH value of the solution reaches 8-9, namely preparing a buffer solution, and then, adding white mesocrystal (NH)4)2Ta2O3F6The mass volume ratio of the powder to the dopamine hydrochloride to the buffer solution (w: w: V) is (1-5) g: (0.5-2) g: 1L of the mixture is weighed; then dissolving dopamine hydrochloride in a buffer solution, and fully stirring until the solution is uniform and light yellow; then grinding the fine mesogen (NH)4)2Ta2O3F6Slowly adding the powder into the dopamine hydrochloride buffer solution, and fully stirring at room temperature for 12-48 h; carrying out suction filtration on the slurry, and transferring the obtained powder into an oven to dry for 12-36 h at 50-100 ℃; cooling again; (2) with mesogen (NH)4)2Ta2O3F6The @ dopamine composite material is used as a precursor, the temperature is increased to 900-1100 ℃ at the heating rate of 1-10 ℃/min in an inert atmosphere (argon, oxygen-free), and the temperature is kept for 0.5-5 h; after cooling, the carbon-coated Ta can be obtained2O5Nanosheets.
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Application publication date: 20201113 |