CN114284485A - V-shaped groove2O3Preparation method of/C hollow nanosphere electrode material - Google Patents
V-shaped groove2O3Preparation method of/C hollow nanosphere electrode material Download PDFInfo
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- CN114284485A CN114284485A CN202111655124.XA CN202111655124A CN114284485A CN 114284485 A CN114284485 A CN 114284485A CN 202111655124 A CN202111655124 A CN 202111655124A CN 114284485 A CN114284485 A CN 114284485A
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- 239000002077 nanosphere Substances 0.000 title claims abstract description 19
- 239000007772 electrode material Substances 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title abstract description 8
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000137 annealing Methods 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 229910001868 water Inorganic materials 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 30
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- 235000006408 oxalic acid Nutrition 0.000 claims description 10
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 9
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 239000012300 argon atmosphere Substances 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 239000002243 precursor Substances 0.000 claims description 4
- 239000008098 formaldehyde solution Substances 0.000 claims description 2
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 22
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 abstract description 17
- 229910001935 vanadium oxide Inorganic materials 0.000 abstract description 17
- 229910052799 carbon Inorganic materials 0.000 abstract description 10
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 abstract description 4
- 239000005011 phenolic resin Substances 0.000 abstract description 4
- 229920001568 phenolic resin Polymers 0.000 abstract description 4
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 6
- 239000003575 carbonaceous material Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 239000002041 carbon nanotube Substances 0.000 description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- FSJSYDFBTIVUFD-SUKNRPLKSA-N (z)-4-hydroxypent-3-en-2-one;oxovanadium Chemical compound [V]=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FSJSYDFBTIVUFD-SUKNRPLKSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
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- 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
Abstract
The invention relates to a V2O3A preparation method of a/C hollow nanosphere electrode material. The preparation method comprises the following steps: placing hollow nanospheres generated by hydrothermal reaction in a three-neck flask, adding resorcinol and formaldehyde, coating phenolic resin in a water bath process, and annealing at high temperature to form V2O3a/C hollow nanosphere structure. The preparation method is simple in preparation process and controllable, and the carbon layer thickness of the phenolic resin can be controlled by controlling the addition of the phenolic resin. The carbon-coated structure can not only increase the conductivity of the vanadium oxide, but also inhibit the collapse of the structure of the vanadium oxide electrode material in the battery cycle process.
Description
Technical Field
The invention belongs to the technical field of new energy materials, and mainly relates to a V2O3A preparation method of a/C hollow nanosphere electrode material.
Background
Vanadium oxide is one of the most common positive electrode materials in a water system zinc ion battery, and has attracted extensive attention of people due to the characteristics of larger specific capacity, various chemical valence states, rich morphology and the like. However, the vanadium oxide also has the defects of poor conductivity and easy structural collapse in the circulating process so as to influence the circulating stability of the vanadium oxide. To improve the above-mentioned disadvantages, carbon, which is a highly conductive material, is generally usedThe property substance is introduced into the vanadium oxide to increase the stability and the electric conductivity of the vanadium oxide. For example, methods for introducing a carbon source include the following methods: vanadium oxide is mixed with carbon-based materials such as: and carrying out hydrothermal compounding on the carbon nano tube and the graphite oxide to obtain the vanadium oxide/carbon composite material. Vanadium oxide is combined with resin, organic amine, MOF and converted to derivatized carbon at high temperature. Wu et al will V2O5·H2O is stirred and compounded with the graphite oxide sheet to obtain V2O5·H2O can be uniformly grown on the graphite oxide sheet (Journal of Alloys and Compounds 2021, 108388-. Fang et al seal vanadyl acetylacetonate in ZiF-8 and carbonize it to convert it to a porous carbon-coated vanadium oxide material with high Li＋Transmission efficiency (Journal of Colloid and Interface Science 2021.07251-265). Chinese patent literature (CN201810990270. X) discloses a preparation method of a vanadium oxide composite electrode material of a zinc ion battery, which comprises the following steps: (1) dissolving ammonium metavanadate in water at a certain temperature; (2) adding a carbon material, and uniformly stirring and mixing; (3) drying the vanadium oxide/carbon composite material and then carrying out high-temperature annealing; the dissolving temperature in the step (1) is 20-100 ℃; the carbon material in the step (2) is graphene, carbon nano tubes, activated carbon and a mixture of the graphene, the carbon nano tubes and the activated carbon in any proportion; in the step (3), the vanadium oxide accounts for 5-100% of the vanadium oxide/carbon composite material by mass percent; the high-temperature annealing temperature in the step (3) is 250-800 ℃, and the heat preservation time is 0.5-10 h; the method has complex reaction conditions, long reaction period and improved electrochemical performance.
Disclosure of Invention
Based on the technical problems of the background art, a carbon material may be introduced to improve the conductive performance. V prepared by the invention2O3the/C hollow nanosphere electrode material.
The technical scheme of the invention is as follows:
according to the invention, a V2O3The preparation method of the/C hollow nanosphere electrode material comprises the following steps:
(1) adding 4mmol of ammonium metavanadate into 70ml of deionized water, stirring for 30min, adding 0.1-0.6 g of oxalic acid, stirring until the oxalic acid is dissolved, adding 1-6 ml of hydrazine hydrate, and stirring for 30 min;
(2) transferring the mixed solution obtained in the step (1) into a 100ml liner of a hydrothermal reaction kettle, cooling to room temperature after the reaction is finished at 160 ℃ for 12h, alternately centrifuging and washing water and absolute ethyl alcohol until the solution is colorless, and cooling to dry to obtain a precursor material;
(3) putting 0.2g of the precursor material obtained in the step (2) into a three-neck flask, adding 30ml of deionized water, 15ml of absolute ethyl alcohol and 0.1ml of ammonia water, carrying out ultrasonic treatment for 30min, adding 0.06g-0.96g of resorcinol, carrying out magnetic stirring for 1h, dripping 0.36 ml-0.72 ml of formaldehyde solution into the three-neck flask, reacting for 12h at 25 ℃, centrifuging, washing and drying;
(4) and (4) placing the dried product in the step (3) in an argon atmosphere at 500-800 ℃ for annealing treatment.
According to the present invention, it is preferable that the mass of oxalic acid in step (1) is 0.3 g.
According to the present invention, it is preferred that the volume of hydrazine hydrate in step (1) is 4 ml.
According to the present invention, it is preferred that the mass of resorcinol in step (3) is 0.24 g.
According to the present invention, it is preferred that the volume of formaldehyde in step (3) is 0.48 ml.
According to the present invention, it is preferable that the annealing temperature in the step (4) is 700 ℃.
The technical advantages of the invention are as follows:
(1) the preparation method is simple in preparation process and controllable, and the thickness of the carbon layer can be controlled through the content of resorcinol and formaldehyde.
(2) The invention designs a V2O3The V/C hollow nanosphere electrode material is prepared by coating vanadium oxide with phenolic resin, and performing subsequent high-temperature annealing to form V2O3the/C hollow nanosphere structure further improves the conductivity of the vanadium oxide.
Drawings
FIG. 1 shows V obtained in example 1 of the present invention2O3hollow/C nanosphere electricityXRD of the pole material.
FIG. 2 shows V obtained in example 1 of the present invention2O3Long cycle diagram of/C hollow nanosphere electrode material.
FIG. 3 shows V obtained in example 1 of the present invention2O3SEM of/C hollow nanosphere electrode material.
Fig. 4 is SEM of the hollow nanosphere electrode material prepared according to comparative example of the present invention.
Detailed Description
The present invention will be further described with reference to the following embodiments and drawings, but is not limited thereto.
Meanwhile, the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1:
4mmol ammonium metavanadate is put into 70ml deionized water, 0.3g oxalic acid is added and stirred until the ammonium metavanadate is dissolved, 4ml hydrazine hydrate is added and stirred for 30min, and then the mixture is transferred to a 100ml hydrothermal kettle and reacted for 12h at 160 ℃. Centrifugally washing and drying a hydrothermal product, putting 0.2g of the hydrothermal product into a three-neck flask, adding 30ml of deionized water, 15ml of ethanol and 0.1ml of ammonia water, carrying out ultrasonic treatment for 30min, adding 0.24g of resorcinol, magnetically stirring for 1h, dropwise adding 0.48ml of formaldehyde into the three-neck flask, reacting for 12h at 25 ℃, centrifugally washing and drying, putting the three-neck flask into an argon atmosphere, and annealing at 700 ℃ to obtain V2O3the/C hollow nanosphere electrode material.
Example 2:
4mmol ammonium metavanadate is put into 70ml deionized water, 0.3g oxalic acid is added and stirred until the ammonium metavanadate is dissolved, 4ml hydrazine hydrate is added and stirred for 30min, and then the mixture is transferred to a 100ml hydrothermal kettle and reacted for 12h at 160 ℃. Centrifugally washing and drying a hydrothermal product, putting 0.2g of the hydrothermal product into a three-neck flask, adding 30ml of deionized water, 15ml of ethanol and 0.1ml of ammonia water, carrying out ultrasonic treatment for 30min, adding 0.12 g of resorcinol, magnetically stirring for 1h, dropwise adding 0.36ml of formaldehyde into the three-neck flask, reacting for 12h at 25 ℃, centrifugally washing and drying, putting the obtained product into an argon atmosphere, and annealing at 700 ℃ to obtain V2O3the/C hollow nanosphere electrode material.
Example 3:
4mmol ammonium metavanadate is put into 70ml deionized water, 0.3g oxalic acid is added and stirred until the ammonium metavanadate is dissolved, 4ml hydrazine hydrate is added and stirred for 30min, and then the mixture is transferred to a 100ml hydrothermal kettle and reacted for 12h at 160 ℃. Centrifugally washing and drying a hydrothermal product, putting 0.2g of the hydrothermal product into a three-neck flask, adding 30ml of deionized water, 15ml of ethanol and 0.1ml of ammonia water, carrying out ultrasonic treatment for 30min, adding 0.48 g of resorcinol, magnetically stirring for 1h, dropwise adding 0.60 ml of formaldehyde into the three-neck flask, reacting for 12h at 25 ℃, centrifugally washing and drying, putting the obtained product into an argon atmosphere, and annealing at 700 ℃ to obtain V2O3the/C hollow nanosphere electrode material.
Example 4:
4mmol ammonium metavanadate is put into 70ml deionized water, 0.3g oxalic acid is added and stirred until the ammonium metavanadate is dissolved, 4ml hydrazine hydrate is added and stirred for 30min, and then the mixture is transferred to a 100ml hydrothermal kettle and reacted for 12h at 160 ℃. Centrifugally washing and drying a hydrothermal product, putting 0.2g of the hydrothermal product into a three-neck flask, adding 30ml of deionized water, 15ml of ethanol and 0.1ml of ammonia water, carrying out ultrasonic treatment for 30min, adding 0.96g of resorcinol, mechanically stirring for 1h, dropwise adding 0.72ml of formaldehyde into the three-neck flask, reacting for 12h at 25 ℃, centrifugally washing and drying, putting the three-neck flask into an argon atmosphere, and annealing at 700 ℃ to obtain V2O3the/C hollow nanosphere electrode material.
Comparative example:
4mmol ammonium metavanadate is put into 70ml deionized water, 0.3g oxalic acid is added and stirred until the ammonium metavanadate is dissolved, 4ml hydrazine hydrate is added and stirred for 30min, and then the mixture is transferred to a 100ml hydrothermal kettle and reacted for 12h at 160 ℃. And (4) centrifugally washing and drying the hydrothermal product.
Claims (6)
1. According to the invention, a V2O3The preparation method of the/C hollow nanosphere electrode material comprises the following steps:
(1) adding 4mmol ammonium metavanadate into 70ml deionized water, stirring for 30min, adding 0.1 g-0.6 g oxalic acid, stirring for dissolving, adding 1 ml-6 ml hydrazine hydrate, stirring for 30 min;
(2) transferring the mixed solution obtained in the step (1) into a 100mL liner of a hydrothermal reaction kettle, reacting at 160 ℃ for a period of time, cooling to room temperature after the reaction is finished, alternately centrifuging and washing water and absolute ethyl alcohol until the solution is colorless, and cooling to dry to obtain a precursor material;
(3) putting 0.2g of the precursor material obtained in the step (2) into a three-neck flask, adding 30ml of deionized water, 15ml of absolute ethyl alcohol and 0.1ml of ammonia water, carrying out ultrasonic treatment for 30min, adding 0.06g-0.96g of resorcinol, carrying out magnetic stirring for 1h, dripping 0.36 ml-0.72 ml of formaldehyde solution into the three-neck flask, reacting for 12h at 25 ℃, centrifuging, washing and drying;
(4) and (3) annealing the dried product in 500-800 deg.c in argon atmosphere.
2. According to the present invention, it is preferable that the mass of oxalic acid in step (1) is 0.3 g.
3. According to the present invention, it is preferred that the volume of hydrazine hydrate in step (1) is 4 ml.
4. According to the present invention, it is preferred that the mass of resorcinol in step (3) is 0.24 g.
5. According to the present invention, it is preferred that the volume of formaldehyde in step (3) is 0.48 ml.
6. According to the present invention, it is preferable that the annealing temperature in the step (4) is 700 ℃.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101700909A (en) * | 2009-11-25 | 2010-05-05 | 中国科学技术大学 | Method of preparing intelligent energy-saving vanadium dioxide by hydrothermal method |
| CN102674457A (en) * | 2012-06-15 | 2012-09-19 | 武汉大学 | Preparation method for vanadium trioxide doped powder material |
| CN105304885A (en) * | 2014-07-15 | 2016-02-03 | 北京理工大学 | Aluminum secondary battery vanadium oxide positive material and preparation method thereof |
| CN106800311A (en) * | 2017-02-10 | 2017-06-06 | 中国科学院化学研究所 | A kind of vanadium pentoxide hollow microsphere and preparation method thereof and the application in lithium ion battery |
| CN108110244A (en) * | 2017-12-20 | 2018-06-01 | 湖南工业大学 | A kind of hollow nucleocapsid vanadic anhydride anode material for lithium-ion batteries of tremelliform and preparation method thereof |
| CN108461725A (en) * | 2018-03-07 | 2018-08-28 | 武汉理工大学 | Vanadium trioxide hollow microsphere of carbon confinement and its preparation method and application |
| CN109292819A (en) * | 2018-11-12 | 2019-02-01 | 中国科学院上海硅酸盐研究所 | A kind of method that step hydro-thermal prepares vanadium trioxide powder |
| CN110002423A (en) * | 2019-01-22 | 2019-07-12 | 齐鲁工业大学 | A kind of preparation method of phenolic resin base hollow carbon balls |
| CN112062156A (en) * | 2020-09-12 | 2020-12-11 | 南昌大学 | Preparation method of supercapacitor electrode material vanadium trioxide/carbon |
-
2021
- 2021-12-31 CN CN202111655124.XA patent/CN114284485A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101700909A (en) * | 2009-11-25 | 2010-05-05 | 中国科学技术大学 | Method of preparing intelligent energy-saving vanadium dioxide by hydrothermal method |
| CN102674457A (en) * | 2012-06-15 | 2012-09-19 | 武汉大学 | Preparation method for vanadium trioxide doped powder material |
| CN105304885A (en) * | 2014-07-15 | 2016-02-03 | 北京理工大学 | Aluminum secondary battery vanadium oxide positive material and preparation method thereof |
| CN106800311A (en) * | 2017-02-10 | 2017-06-06 | 中国科学院化学研究所 | A kind of vanadium pentoxide hollow microsphere and preparation method thereof and the application in lithium ion battery |
| CN108110244A (en) * | 2017-12-20 | 2018-06-01 | 湖南工业大学 | A kind of hollow nucleocapsid vanadic anhydride anode material for lithium-ion batteries of tremelliform and preparation method thereof |
| CN108461725A (en) * | 2018-03-07 | 2018-08-28 | 武汉理工大学 | Vanadium trioxide hollow microsphere of carbon confinement and its preparation method and application |
| CN109292819A (en) * | 2018-11-12 | 2019-02-01 | 中国科学院上海硅酸盐研究所 | A kind of method that step hydro-thermal prepares vanadium trioxide powder |
| CN110002423A (en) * | 2019-01-22 | 2019-07-12 | 齐鲁工业大学 | A kind of preparation method of phenolic resin base hollow carbon balls |
| CN112062156A (en) * | 2020-09-12 | 2020-12-11 | 南昌大学 | Preparation method of supercapacitor electrode material vanadium trioxide/carbon |
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Application publication date: 20220405 |