CN108400329A - A kind of preparation method of precious metal simple substance adulterated vanadate nano-electrode material - Google Patents
A kind of preparation method of precious metal simple substance adulterated vanadate nano-electrode material Download PDFInfo
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- CN108400329A CN108400329A CN201810091299.4A CN201810091299A CN108400329A CN 108400329 A CN108400329 A CN 108400329A CN 201810091299 A CN201810091299 A CN 201810091299A CN 108400329 A CN108400329 A CN 108400329A
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- 239000000126 substance Substances 0.000 title claims abstract description 46
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000010970 precious metal Substances 0.000 title claims abstract description 40
- 239000007772 electrode material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000002070 nanowire Substances 0.000 claims abstract description 35
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 28
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical class O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 claims abstract description 24
- ZDYUUBIMAGBMPY-UHFFFAOYSA-N oxalic acid;hydrate Chemical class O.OC(=O)C(O)=O ZDYUUBIMAGBMPY-UHFFFAOYSA-N 0.000 claims abstract description 23
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 claims abstract description 22
- 239000000758 substrate Substances 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 20
- 229910052751 metal Inorganic materials 0.000 claims abstract description 20
- 239000002184 metal Substances 0.000 claims abstract description 20
- 150000003839 salts Chemical class 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 238000005342 ion exchange Methods 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000009938 salting Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 6
- 238000004090 dissolution Methods 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 24
- 229910052799 carbon Inorganic materials 0.000 claims description 24
- 239000004744 fabric Substances 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 21
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 16
- 238000004140 cleaning Methods 0.000 claims description 12
- 229910001416 lithium ion Inorganic materials 0.000 claims description 12
- 239000012266 salt solution Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- 229920000742 Cotton Polymers 0.000 claims description 10
- 206010013786 Dry skin Diseases 0.000 claims description 10
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000011068 loading method Methods 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 10
- 239000010936 titanium Substances 0.000 claims description 10
- 229910052719 titanium Inorganic materials 0.000 claims description 10
- 239000006260 foam Substances 0.000 claims description 8
- 229910052759 nickel Inorganic materials 0.000 claims description 8
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 7
- 229910000831 Steel Inorganic materials 0.000 claims description 7
- 239000010959 steel Substances 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- 150000002940 palladium Chemical class 0.000 claims description 4
- 150000003057 platinum Chemical class 0.000 claims description 4
- 239000001103 potassium chloride Substances 0.000 claims description 4
- 235000011164 potassium chloride Nutrition 0.000 claims description 4
- 229910001415 sodium ion Inorganic materials 0.000 claims description 4
- SDKPSXWGRWWLKR-UHFFFAOYSA-M sodium;9,10-dioxoanthracene-1-sulfonate Chemical compound [Na+].O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2S(=O)(=O)[O-] SDKPSXWGRWWLKR-UHFFFAOYSA-M 0.000 claims description 4
- 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 4
- 150000001621 bismuth Chemical class 0.000 claims description 3
- 150000001868 cobalt Chemical class 0.000 claims description 3
- 229910003002 lithium salt Inorganic materials 0.000 claims description 3
- 159000000002 lithium salts Chemical class 0.000 claims description 3
- 239000002086 nanomaterial Substances 0.000 claims description 3
- 159000000000 sodium salts Chemical class 0.000 claims description 3
- 150000003751 zinc Chemical class 0.000 claims description 3
- 150000002503 iridium Chemical class 0.000 claims description 2
- 150000002907 osmium Chemical class 0.000 claims description 2
- 150000003283 rhodium Chemical class 0.000 claims description 2
- 150000003303 ruthenium Chemical class 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000007164 Oryza sativa Nutrition 0.000 claims 1
- 235000009566 rice Nutrition 0.000 claims 1
- 238000002604 ultrasonography Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 11
- 229910052744 lithium Inorganic materials 0.000 description 11
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- 239000003643 water by type Substances 0.000 description 8
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 5
- 229910017052 cobalt Inorganic materials 0.000 description 5
- 239000010941 cobalt Substances 0.000 description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 229910052762 osmium Inorganic materials 0.000 description 5
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 5
- BQFYGYJPBUKISI-UHFFFAOYSA-N potassium;oxido(dioxo)vanadium Chemical compound [K+].[O-][V](=O)=O BQFYGYJPBUKISI-UHFFFAOYSA-N 0.000 description 5
- 229910052703 rhodium Inorganic materials 0.000 description 5
- 239000010948 rhodium Substances 0.000 description 5
- 229910052707 ruthenium Inorganic materials 0.000 description 5
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 description 5
- 229910052725 zinc Inorganic materials 0.000 description 5
- 239000011701 zinc Substances 0.000 description 5
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 229910052769 Ytterbium Inorganic materials 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- XDBSEZHMWGHVIL-UHFFFAOYSA-M hydroxy(dioxo)vanadium Chemical compound O[V](=O)=O XDBSEZHMWGHVIL-UHFFFAOYSA-M 0.000 description 4
- 238000007654 immersion Methods 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 4
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 4
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 4
- -1 Gold ion Chemical class 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 229910052797 bismuth Inorganic materials 0.000 description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 238000009830 intercalation Methods 0.000 description 3
- 230000002687 intercalation Effects 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 3
- 229910017988 AgVO3 Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000002127 nanobelt Substances 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 241001614291 Anoplistes Species 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910021581 Cobalt(III) chloride Inorganic materials 0.000 description 1
- 229910021592 Copper(II) chloride Inorganic materials 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 229910003206 NH4VO3 Inorganic materials 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 1
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000000452 restraining effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- ISIHFYYBOXJLTM-UHFFFAOYSA-N vanadium;pentasilicate Chemical compound [V].[V].[V].[V].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] ISIHFYYBOXJLTM-UHFFFAOYSA-N 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
Classifications
-
- 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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention relates to a kind of preparation methods of precious metal simple substance adulterated vanadate nano-electrode material, belong to nanometer material and electrochemical technology field.Metal salt, ammonium metavanadate, two oxalic acid hydrates, six four ammoniums of methylene are dissolved in deionized water by a certain percentage, ultrasonic dissolution obtains presoma, presoma is moved into the autoclave containing substrate and carries out hydro-thermal reaction, there is the substrate of vanadate nano wire to clean load after reaction, it is dry, there is the substrate of vanadate nano wire to be immersed in soluble precious-metal salting liquid at 10 100 DEG C load later, takes out, cleans, is dry, finally using H again2High temperature reduction method under atmosphere, the precious metal ion being inserted into vanadic acid salt deposit by ion exchange is reduced to precious metal simple substance, obtain a kind of precious metal simple substance adulterated vanadate nano-electrode material, preparation process of the present invention is simple, reaction condition is mild and the reaction time is short, overall process non-secondary pollution object generates, and the electrode material of preparation has excellent chemical property.
Description
Technical field
The present invention relates to a kind of preparation methods of precious metal simple substance adulterated vanadate nano-electrode material, belong to nano material
With electrochemical technology field
Technical background
In recent years, due to economic sustained and rapid development, market is greatly have stimulated to changes such as coal, oil, natural gases
The demand of the stone energy.Up to now, more and more big environmental pollution and the energy weary pressure of hideing are increasingly prominent, find new replace
It is increasingly urgent for the energy, development energy conservation and environmental protection tool.Therefore, development new energy is to realize sustainable economic development, is solved increasingly
The effective way of serious environmental pollution.Wherein, lithium ion battery is especially noticeable due to unique superiority, such as ring
The advantages that border close friend, high-energy density, operating temperature range be wide, memory-less effect, has gradually attracted the sight of world community.With
Application the widening to the extensive energy storage field such as electric vehicle, intelligent grid of lithium ion battery, industry is to its cost and electricity
Chemical property has higher requirement, wherein the exploitation of high performance electrode material of new generation is the key that break through to apply bottleneck.And
Positive electrode is the key that lithium ion battery development, it is not only the restraining factors and lithium-ion electric of lithium ion battery price
The important determinant of pond power density and energy density.Therefore, low cost, high power capacity, high-power lithium ion battery anode material
The exploitation of material becomes the research hotspot of recent domestic academia.Vanadate intercalation materials of li ions is due to of low cost, synthetic method
Simply, the features such as specific capacity is high becomes the hot spot of recent researches.Embedding lithium performance study shows vanadate lithium intercalation compound
Cyclical stability is still to be improved, and storage lithium ability is low and high rate performance is insufficient, this is also that vanadium base intercalation materials of li ions field is general simultaneously
All over an existing problem, to limit its commercial applications.For the limitation and challenge for solving above-mentioned.The doping of metal simple-substance
The electric conductivity of electrode can be improved, therefore people begin one's study precious metal doping vanadate and its chemical property.Sodium-ion battery
Because the price of sodium is cheap compared with lithium, also become the emphasis of research, electrode material is often similar in lithium electricity electrode material performance.
Shuquan Liang et al. (Hydrothermal synthesis of Ag/ β-AgVO3nanobelts with
Enhanced performance as a cathode material for lithium batteries,
CrystEngComm, 2013,15,9869-9873) simple hydro-thermal method is used, by by NH4VO3, AgNO3 and H2O2 conducts
Nano silver grain load β-AgVO3 nanobelt compounds, the Ag/ has been made for 24 hours in original material hydro-thermal reaction under 190 degree
β-AgVO3 nanobelts are demonstrated by very high capacitance, high rate performance and cyclical stability when as lithium-ion electric grade.But hydro-thermal
Processing method needs hydrothermal reaction kettle, and hydrothermal conditions are long, and temperature is higher.
Invention content
The present invention is in view of the problems of the existing technology, and it is an object of the present invention to provide a kind of precious metal simple substance adulterated vanadate nanometer
The preparation method of electrode material.
To achieve the goals above, the present invention uses following technical scheme：
A kind of preparation method of precious metal simple substance adulterated vanadate nano-electrode material, it is characterised in that：The preparation side
Method refers to being dissolved in metal salt, ammonium metavanadate, two oxalic acid hydrates, six four ammoniums of methylene in deionized water by a certain percentage, is surpassed
Sound dissolves to obtain presoma, and presoma is moved into the autoclave containing substrate and carries out hydro-thermal reaction, after reaction will
Load has the substrate cleaning, drying of vanadate nano wire, has the substrate of vanadate nano wire at 10-100 DEG C load later
It is immersed in soluble precious-metal salting liquid, takes out, cleans, is dry, finally using H again2High temperature reduction method under atmosphere will pass through
The metal ion that ion exchange is inserted into vanadic acid salt deposit is reduced to metal simple-substance, obtains a kind of precious metal simple substance doping vanadium
Silicate nanometer electrode material, preparation method carry out according to the following steps：
Metal salt, ammonium metavanadate, two oxalic acid hydrates, six four ammoniums of methylene are add to deionized water by a, ultrasonic dissolution
Obtain presoma, wherein a concentration of 0.2~1mol/L of ammonium metavanadate, the concentration ratio of ammonium metavanadate and metal salt is 1:6~1:
20, the concentration ratio of two oxalic acid hydrates and metal salt is 1:3~1:10, the concentration ratio of six four ammoniums of methylene and metal salt is 1:3
~1:6；
B cleans substrate, and the substrate after cleaning is put into autoclave liner；
C by after the prepared precursor solution of a steps is transferred in the autoclave liner equipped with substrate, 90~
150 DEG C of 40~120min of reaction, take out reaction kettle after room temperature natural cooling, and will react back loading has the base of vanadate nano wire
Bottom is taken out, and is rinsed with deionized water, in an oven 30~100 DEG C of dryings；
D loads after step c drying of learning from else's experience have the substrate of vanadate nano wire, in 0.01-1mol/L soluble precious-metals
In salting liquid at 10-100 DEG C impregnate 1~for 24 hours；
E takes in Step d the load after being impregnated in metal salt solution to have the substrate of metal vanadate nano wire, in tubular type
H in stove2With the heating rate of 0.5~2 DEG C/min under atmosphere, 200~700 DEG C are heated to, 2~5h is kept the temperature, will be handed over by ion
The precious metal ion inserted in vanadic acid salt deposit is reduced to precious metal simple substance, obtains a kind of precious metal simple substance doping vanadic acid
Salt nano-electrode material.
The metal salt is one kind in sylvite, molysite, sodium salt, bismuth salt, zinc salt, cobalt salt, mantoquita, lithium salts.
The substrate is one kind in carbon cloth or cotton or titanium sheet or stainless steel steel wire or nickel foam.
The soluble precious-metal salt is one in gold salt, silver salt, platinum salt, ruthenium salt, rhodium salt, palladium salt, osmium salt, iridium salt
Kind.
The precious metal simple substance adulterated vanadate nano material can be used for lithium ion, sodium-ion battery as electrode material
In.
As a result of above technical scheme, a kind of synthesis side of precious metal simple substance adulterated vanadate nano-electrode material
Method is first obtained vanadate nano wire, then vanadate nano wire is placed in precious metal salt solution and is impregnated, and will pass through ion exchange
The precious metal ion being inserted into vanadic acid salt deposit is reduced to precious metal simple substance, obtains a kind of precious metal simple substance adulterated vanadate
Nano-electrode material, reaction condition of the present invention is mild and the reaction time is short, and the product prepared is grown in lower-cost conductive base
Simple for process on bottom, easy to operate, overall process non-secondary pollution object generates, and the precious metal simple substance adulterated in the present invention is inserted into vanadium
In silicate layer, the doping of precious metal simple substance can increase the electric conductivity of electrode material.Therefore a kind of precious metal simple substance of the present invention is mixed
Miscellaneous vanadate nano-electrode material has prodigious development prospect in lithium ion, sodium-ion battery material.
Specific implementation mode
The present invention is described in further detail with reference to embodiment.
Embodiment 1
A is by potassium chloride (KCl), ammonium metavanadate (NH4VO3), two oxalic acid hydrate (H2C2O4 2H2O), six four ammoniums of methylene
(C6H12N4) be added in 17.5ml deionized waters, ultrasonic mixing is made into mixed liquor and obtains presoma, and wherein ammonium metavanadate is dense
Degree is 0.2mol/L, a concentration of 1.2mol/L of potassium chloride, a concentration of 0.4mol/L of two oxalic acid hydrates, six four ammoniums of methylene
A concentration of 0.4mol/L；
B cleans carbon cloth, and the carbon cloth after cleaning is put into 20ml autoclave liners；
C is by after the prepared precursor solution of a steps is transferred in the autoclave liner equipped with carbon cloth, at 90 DEG C
40min is reacted, takes out reaction kettle after room temperature natural cooling, will react back loading has the carbon cloth of potassium vanadate nano wire to take out, and uses
Deionized water is rinsed, 30 DEG C of dryings in an oven；
D loads after step c drying of learning from else's experience have the carbon cloth of potassium vanadate nano wire, 10 DEG C in 0.01mol/L gold salt solution
Lower immersion 1h；
E takes in Step d the load after being impregnated in gold salt solution to have the carbon cloth of potassium vanadate nano wire, the H in tube furnace2
With the heating rate of 0.5 DEG C/min under atmosphere, 200 DEG C are heated to, 2h is kept the temperature, will be inserted into potassium vanadate layer by ion exchange
Gold ion is reduced to elemental gold, obtains a kind of elemental gold doping potassium vanadate nano-electrode material.
Embodiment 2
A is by iron chloride (FeCl3 6H2O), ammonium metavanadate (NH4VO3), two oxalic acid hydrate (H2C2O4 2H2O), six methylenes
Four ammonium (C of base6H12N4) be added in 17.5ml deionized waters, ultrasonic mixing is made into mixed liquor and obtains presoma, wherein metavanadic acid
A concentration of 1mol/L of ammonium, a concentration of 20mol/L of molysite, a concentration of 2mol/L of two oxalic acid hydrates, six four ammoniums of methylene
A concentration of 3mol/L；
B cleans cotton, and the cotton after cleaning is put into 20ml autoclave liners；
C is by after the prepared precursor solution of a steps is transferred in the autoclave liner equipped with cotton, 150
DEG C reaction 120min, take out reaction kettle after room temperature natural cooling, by react back loading have ferric vandate cotton take out, spend from
Sub- water rinses, 100 DEG C of dryings in an oven；
D loads after step c drying of learning from else's experience have the carbon cloth of vanadic acid Fe nanowire, in 1mol/L silver salt solutions at 100 DEG C
Impregnate 1h；
E takes in Step d the load after being impregnated in silver salt solution to have the carbon cloth of vanadic acid Fe nanowire, the H in tube furnace2
With the heating rate of 2 DEG C/min under atmosphere, 700 DEG C are heated to, keeps the temperature 5h, the silver that will be inserted by ion exchange in vanadic acid iron layer
Ion reduction is elemental silver, obtains a kind of simple substance Ag doping ferric vandate nano-electrode material.
Embodiment 3
A is by sodium chloride (NaCl), ammonium metavanadate (NH4VO3), two oxalic acid hydrate (H2C2O4 2H2O), six four ammoniums of methylene
(C6H12N4) be added in 17.5ml deionized waters, ultrasonic mixing is made into mixed liquor and obtains presoma, and wherein ammonium metavanadate is dense
Degree is 0.5mol/L, a concentration of 5mol/L of sodium salt, a concentration of 1mol/L of two oxalic acid hydrates, the concentration of six four ammoniums of methylene
For 1mol/L；
B cleans titanium sheet, and the titanium sheet after cleaning is put into 20ml autoclave liners；
C is by after the prepared precursor solution of a steps is transferred in the autoclave liner equipped with titanium sheet, at 90 DEG C
80min is reacted, takes out reaction kettle after room temperature natural cooling, will react back loading has the titanium sheet of sodium vanadate nano wire to take out, and uses
Deionized water is rinsed, 80 DEG C of dryings in an oven；
D loads after step c drying of learning from else's experience have the carbon cloth of sodium vanadate nano wire, in 0.1mol/L platinum salt solution at 50 DEG C
Impregnate 1h；
E takes in Step d the load after being impregnated in platinum salt solution to have the carbon cloth of sodium vanadate nano wire, the H in tube furnace2
With the heating rate of 1 DEG C/min under atmosphere, 500 DEG C are heated to, keeps the temperature 3h, the platinum that will be inserted by ion exchange in sodium vanadate layer
Ion reduction is simple substance platinum, obtains a kind of simple substance platinum dopant sodium vanadate electrode material.
Embodiment 4
A is by bismuth nitrate (Bi (NO3)3 5H2O), ammonium metavanadate (NH4VO3), two oxalic acid hydrate (H2C2O42H2O), six Asias
Four ammonium (C of methyl6H12N4) be added in 17.5ml deionized waters, ultrasonic mixing is made into mixed liquor and obtains presoma, wherein inclined vanadium
A concentration of 0.2mol/L of sour ammonium, a concentration of 1.2mol/L of bismuth salt, a concentration of 0.4mol/L of two oxalic acid hydrates, six methylenes
A concentration of 0.4mol/L of four ammonium of base；
B cleans stainless steel steel wire, and the stainless steel steel wire after cleaning is put into 20ml autoclave liners；
C will be transferred to through the prepared precursor solution of a steps in the autoclave liner equipped with stainless steel steel wire
Afterwards, 40min is reacted at 90 DEG C, takes out reaction kettle after room temperature natural cooling, and reaction back loading is had into vanadic acid bismuth nano-wire not
The steel steel wire that becomes rusty takes out, and is rinsed with deionized water, in an oven 30 DEG C of dryings；
D loads after step c drying of learning from else's experience have the carbon cloth of vanadic acid bismuth nano-wire, 10 DEG C in 0.01mol/L ruthenium salting liquids
Lower immersion 1h；
E takes in Step d the load after being impregnated in ruthenium salting liquid to have the carbon cloth of vanadic acid bismuth nano-wire, the H in tube furnace2
With the heating rate of 1 DEG C/min under atmosphere, 250 DEG C are heated to, keeps the temperature 3h, the ruthenium that will be inserted by ion exchange in pucherite layer
Ion reduction is simple substance ruthenium, obtains a kind of simple substance ruthenium doping pucherite nano-electrode material.
Embodiment 5
A is by zinc acetate (C4H6O4Zn), ammonium metavanadate (NH4VO3), two oxalic acid hydrates (H2C2O42H2O), six methylenes
Four ammonium of base (C6H12N4) is added in 17.5ml deionized waters, and ultrasonic mixing is made into mixed liquor and obtains presoma, wherein metavanadic acid
A concentration of 1mol/L of ammonium, a concentration of 20mol/L of zinc salt, a concentration of 2mol/L of two oxalic acid hydrates, six four ammoniums of methylene
A concentration of 3mol/L；
B cleans nickel foam, and the nickel foam after cleaning is put into 20ml autoclave liners；
C by after the prepared precursor solution of a steps is transferred in the autoclave liner equipped with nickel foam,
150 DEG C of reaction 120min, take out reaction kettle after room temperature natural cooling, and will react back loading has the nickel foam of Zinc vanadate to take out,
It is rinsed with deionized water, in an oven 100 DEG C of dryings；
D loads after step c drying of learning from else's experience have the nickel foam of Zinc vanadate nano wire, 100 DEG C in 1mol/L rhodium salting liquids
Lower immersion 1h；
E takes in Step d the load after being impregnated in rhodium salting liquid to have the nickel foam of Zinc vanadate nano wire, in tube furnace
H2With the heating rate of 2 DEG C/min under atmosphere, 300 DEG C are heated to, 5h is kept the temperature, will be inserted into vanadic acid zinc layers by ion exchange
Rhodium ion is reduced to simple substance rhodium, obtains a kind of simple substance rhodium doping Zinc vanadate electrode material.
Embodiment 6
A is by cobalt chloride (CoCl3 6H2O), ammonium metavanadate (NH4VO3), two oxalic acid hydrate (H2C2O4 2H2O), six methylenes
Four ammonium (C of base6H12N4) be added in 17.5ml deionized waters, ultrasonic mixing is made into mixed liquor and obtains presoma, wherein metavanadic acid
A concentration of 0.2mol/L of ammonium, a concentration of 1.2mol/L of cobalt salt, a concentration of 0.4mol/L of two oxalic acid hydrates, six methylene
A concentration of 0.4mol/L of four ammoniums；
B cleans carbon cloth, and the carbon cloth after cleaning is put into 20ml autoclave liners；
C is by after the prepared precursor solution of a steps is transferred in the autoclave liner equipped with carbon cloth, at 90 DEG C
40min is reacted, takes out reaction kettle after room temperature natural cooling, will react back loading has the carbon cloth of vanadic acid cobalt nanowire to take out, and uses
Deionized water is rinsed, 30 DEG C of dryings in an oven；
D loads after step c drying of learning from else's experience have the carbon cloth of vanadic acid cobalt nanowire, in 0.1mol/L palladium salt solution at 50 DEG C
Impregnate 1h；
E takes in Step d the load after being impregnated in palladium salt solution to have the carbon cloth of vanadic acid cobalt nanowire, the H in tube furnace2
With the heating rate of 0.5 DEG C/min under atmosphere, 200 DEG C are heated to, 2h is kept the temperature, will be inserted into vanadic acid cobalt layers by ion exchange
Palladium ion is reduced to simple substance palladium, obtains a kind of simple substance palladium doping vanadic acid cobalt electrode material.
Embodiment 7
A is by copper chloride (CuCl2 2H2O), ammonium metavanadate (NH4VO3), two oxalic acid hydrate (H2C2O4 2H2O), six methylenes
Four ammonium (C of base6H12N4) be added in 17.5ml deionized waters, ultrasonic mixing is made into mixed liquor and obtains presoma, wherein metavanadic acid
A concentration of 1mol/L of ammonium, a concentration of 20mol/L of mantoquita, a concentration of 2mol/L of two oxalic acid hydrates, six four ammoniums of methylene
A concentration of 3mol/L；
B cleans cotton, and the cotton after cleaning is put into 20ml autoclave liners；
C is by after the prepared precursor solution of a steps is transferred in the autoclave liner equipped with cotton, 150
DEG C reaction 120min, take out reaction kettle after room temperature natural cooling, by react back loading have copper vanadate cotton take out, spend from
Sub- water rinses, 100 DEG C of dryings in an oven；
D loads after step c drying of learning from else's experience have the carbon cloth of vanadic acid copper nano-wire, 10 DEG C in 0.01mol/L osmium salting liquids
Lower immersion 1h；
E takes in Step d the load after being impregnated in osmium salting liquid to have the carbon cloth of vanadic acid copper nano-wire, the H in tube furnace2
With the heating rate of 2 DEG C/min under atmosphere, 300 DEG C are heated to, keeps the temperature 5h, the osmium that will be inserted by ion exchange in vanadic acid layers of copper
Ion reduction is simple substance osmium, obtains a kind of simple substance osmium doping copper vanadate nano-electrode material.
Embodiment 8
A is by lithium nitrate (LiNO3), ammonium metavanadate (NH4VO3), two oxalic acid hydrate (H2C2O4 2H2O), six methylene four
Ammonium (C6H12N4) be added in 17.5ml ionized waters, ultrasonic mixing is made into mixed liquor and obtains presoma, wherein ammonium metavanadate
A concentration of 0.5mol/L, a concentration of 5mol/L of lithium salts, a concentration of 1mol/L of two oxalic acid hydrates, six four ammoniums of methylene it is dense
Degree is 1mol/L；
B cleans titanium sheet, and the titanium sheet after cleaning is put into 20ml autoclave liners；
C is by after the prepared precursor solution of a steps is transferred in the autoclave liner equipped with titanium sheet, at 90 DEG C
80min is reacted, takes out reaction kettle after room temperature natural cooling, will react back loading has the titanium sheet of lithium vanadate nano wire to take out, and uses
Deionized water is rinsed, 80 DEG C of dryings in an oven；
D loads after step c drying of learning from else's experience have the carbon cloth of lithium vanadate nano wire, in 1mol/L ytterbium salting liquids at 100 DEG C
Impregnate 1h；
E takes in Step d the load after being impregnated in cerium solution to have the carbon cloth of lithium vanadate nano wire, the H in tube furnace2
With the heating rate of 1 DEG C/min under atmosphere, 500 DEG C are heated to, keeps the temperature 3h, the ytterbium that will be inserted by ion exchange in vanadic acid lithium layer
Ion reduction is simple substance ytterbium, obtains a kind of simple substance ytterbium doping lithium vanadate electrode material.
Claims (5)
1. a kind of preparation method of precious metal simple substance adulterated vanadate nano-electrode material, it is characterised in that：The preparation method
Refer to being dissolved in metal salt, ammonium metavanadate, two oxalic acid hydrates, six four ammoniums of methylene in deionized water by a certain percentage, ultrasound
Dissolving obtains presoma, and presoma is moved into the autoclave containing substrate and carries out hydro-thermal reaction, will be born after reaction
The substrate cleaning, drying of vanadate nano wire are loaded with, have the substrate of vanadate nano wire to be soaked at 10-100 DEG C load later
Bubble takes out, cleans, is dry, finally using H again in soluble precious-metal salting liquid2High temperature reduction method under atmosphere, will by from
Son exchanges the metal ion being inserted into vanadic acid salt deposit and is reduced to metal simple-substance, obtains a kind of precious metal simple substance doping vanadic acid
Salt nano-electrode material, preparation method carry out according to the following steps：
Metal salt, ammonium metavanadate, two oxalic acid hydrates, six four ammoniums of methylene are add to deionized water by a, and ultrasonic dissolution obtains
The concentration ratio of presoma, wherein a concentration of 0.2~1mol/L of ammonium metavanadate, ammonium metavanadate and metal salt is 1:6~1:20, two
The concentration ratio of oxalic acid hydrate and metal salt is 1:3~1:10, the concentration ratio of six four ammoniums of methylene and metal salt is 1:3~1:6；
B cleans substrate, and the substrate after cleaning is put into autoclave liner；
C is by after the prepared precursor solution of a steps is transferred in the autoclave liner equipped with substrate, 90~150
DEG C 40~120min of reaction, takes out reaction kettle after room temperature natural cooling, will react back loading has the substrate of vanadate nano wire
It takes out, is rinsed with deionized water, in an oven 30~100 DEG C of dryings；
Load after step c is dried is had the substrate of vanadate nano wire by d, molten in 0.01-1mol/L soluble precious-metal salt
In liquid at 10-100 DEG C impregnate 1~for 24 hours；
E takes in Step d the load after being impregnated in metal salt solution to have the substrate of metal vanadate nano wire, in tube furnace
H2With the heating rate of 0.5~2 DEG C/min under atmosphere, 200~700 DEG C are heated to, 2~5h is kept the temperature, will be inserted by ion exchange
The precious metal ion entered in vanadic acid salt deposit is reduced to precious metal simple substance, obtains a kind of precious metal simple substance adulterated vanadate and receives
Rice electrode material.
2. a kind of preparation method of precious metal simple substance adulterated vanadate nano-electrode material according to claim 1, special
Sign is：The metal salt is one kind in sylvite, molysite, sodium salt, bismuth salt, zinc salt, cobalt salt, mantoquita, lithium salts.
3. a kind of preparation method of precious metal simple substance adulterated vanadate nano-electrode material according to claim 1, special
Sign is：The substrate is one kind in carbon cloth or cotton or titanium sheet or stainless steel steel wire or nickel foam.
4. a kind of preparation method of precious metal simple substance adulterated vanadate nano-electrode material according to claim 1, special
Sign is：The soluble precious-metal salt is one kind in gold salt, silver salt, platinum salt, ruthenium salt, rhodium salt, palladium salt, osmium salt, iridium salt.
5. a kind of preparation method of precious metal simple substance adulterated vanadate nano-electrode material according to claim 1, special
Sign is：The precious metal simple substance adulterated vanadate nano material can be used for lithium ion, sodium-ion battery as electrode material
In.
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| CN111048778A (en) * | 2019-10-28 | 2020-04-21 | 宁波职业技术学院 | Doped modified lithium ion battery vanadate anode material and preparation method thereof |
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| CN111048778A (en) * | 2019-10-28 | 2020-04-21 | 宁波职业技术学院 | Doped modified lithium ion battery vanadate anode material and preparation method thereof |
| CN111410235A (en) * | 2020-03-26 | 2020-07-14 | 厦门大学 | Application of ultrathin ferric vanadate nanosheets in sodium ion battery and sodium ion capacitor |
| CN111589444A (en) * | 2020-04-30 | 2020-08-28 | 昆明理工大学 | Noble metal quantum dot and preparation method and application thereof |
| CN114084905A (en) * | 2021-10-10 | 2022-02-25 | 中国计量大学 | Preparation method of oxygen-enriched defect potassium-embedded ammonium vanadate nanoarray cathode material |
| CN114084905B (en) * | 2021-10-10 | 2024-01-05 | 中国计量大学 | Preparation method of potassium-embedded ammonium vanadate nano-array positive electrode material with oxygen-enriched defect |
| CN114917917A (en) * | 2022-06-07 | 2022-08-19 | 合肥工业大学 | Cu for preparing acetophenone by oxidation method x Co 1-x V 2 O 6 Catalyst, preparation method and application |
| CN114917917B (en) * | 2022-06-07 | 2023-10-13 | 合肥工业大学 | Cu for preparing acetophenone by oxidation method x Co 1-x V 2 O 6 Catalyst, preparation method and application |
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Application publication date: 20180814 |