CN111924884A - Basic ferric oxide/graphene negative electrode material and preparation method and application thereof - Google Patents
Basic ferric oxide/graphene negative electrode material and preparation method and application thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 103
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 100
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 239000007773 negative electrode material Substances 0.000 title claims abstract description 39
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 58
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 19
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 19
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 19
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims abstract description 19
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
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- 230000035484 reaction time Effects 0.000 claims abstract description 4
- 238000002242 deionisation method Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 33
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 17
- 229910001416 lithium ion Inorganic materials 0.000 claims description 17
- 239000010405 anode material Substances 0.000 claims description 7
- 238000003760 magnetic stirring Methods 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 6
- 230000002441 reversible effect Effects 0.000 abstract description 6
- 239000003513 alkali Substances 0.000 abstract description 4
- 230000001351 cycling effect Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000010406 cathode material Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000007599 discharging Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 description 7
- 229910002588 FeOOH Inorganic materials 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000002033 PVDF binder Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000009881 electrostatic interaction Effects 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000006245 Carbon black Super-P Substances 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910019850 NaxCoO2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
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- 239000012467 final product Substances 0.000 description 1
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- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
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- C01G49/02—Oxides; Hydroxides
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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Abstract
The invention relates to an alkali type ferric oxide \ graphene negative electrode material and a preparation method and application thereof, wherein the preparation method comprises the following steps: providing a graphene ethanol solution; adding ferric chloride hexahydrate into the graphene ethanol solution, and stirring until the ferric chloride hexahydrate is dissolved; adding ammonium bicarbonate, and stirring until the ammonium bicarbonate is dissolved; stirring and reacting at room temperature, and then carrying out deionization washing, centrifuging and drying on the material obtained by the reaction to obtain the basic ferric oxide/graphene negative electrode material. Compared with the prior artCompared with the prior art, the method has the advantages of easily obtained raw materials, low cost, mild preparation conditions, short reaction time, environmental protection and sustainability, and the obtained cathode material is 100 mA.g‑1The capacity of the battery can reach 600 mAh.g under charging and discharging current‑1The composite material has high reversible capacity, good cycling stability and good electrical property.
Description
Technical Field
The invention belongs to the technical field of material science and electrochemistry, and particularly relates to a basic ferric oxide/graphene negative electrode material as well as a preparation method and application thereof.
Background
With the development and progress of the automobile industry, the continuous development problem of human beings faces huge challenges. The combustion of non-renewable fuels can release various exhaust gases, leading to various problems. Therefore, it is important to find renewable and sustainable energy storage devices. The rechargeable battery is economical, environment-friendly, high in power and long in service life, and compared with non-renewable energy, the rechargeable battery realizes continuous utilization of energy. Among them, the lithium ion battery combines high energy and power, making it the first choice technology for portable electronic products, electric tools and all-electric automobiles. Lithium ion electric vehicles are adopted to replace most fuel oil vehicles, and the emission of greenhouse gases is greatly reduced. And the lithium ion is also suitable for various intelligent power grids for generating power by natural energy, including wind energy, solar geothermal energy and the like, so that energy sustainable economy is realized.
The theoretical capacity of graphite, the main commercial negative electrode material of lithium ion batteries, is only 372mAh g-1Other negative electrode materials are mainly composed of layered oxide NaxCoO2Polyanion compounds, layered oxides, etc., but this is not a limiting exampleThe compounds have poor thermal stability, and the products have toxicity, so the compounds are easy to cause environmental pollution and difficult to meet the high-capacity requirement of large-scale energy storage of electric vehicles and power grids. Therefore, the development of a new electrode material for a high-efficiency and stable lithium ion battery is very important. Basic iron oxide has been widely studied as a negative electrode of lithium ion batteries because of its attractive theoretical capacity, low cost and environmentally friendly characteristics. However, the applicant has found that basic iron oxide has disadvantages, firstly, because the final product is rod-shaped nanometer basic iron oxide, the size of the nanometer basic iron oxide is small, and the rod-shaped appearance makes the nanometer basic iron oxide more easily agglomerated, which is not favorable for adsorbing and decomposing organic matters.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the basic ferric oxide \ graphene negative electrode material and the preparation method and application thereof. The method has the advantages of easily available raw materials, low cost, mild preparation conditions, short reaction time, environmental protection and sustainability, and the obtained cathode material has high reversible capacity, good cycling stability and good electrical properties.
The performance of the basic iron oxide is improved by utilizing the advantages of high specific surface area, high stability, high conductivity and the like of the graphene. Wherein the graphene is a single layer sp2Carbon lattice with maximum surface area 2630m2g-1It has excellent electrochemical properties due to its excellent carrier mobility, mechanical stability and thermochemical stability. However, the exfoliated graphene is easy to be piled again, so that the capacitance and the conductivity of the exfoliated graphene are limited, basic iron oxide is uniformly supported on the surface of a graphene sheet to generate a synergistic effect, the conductivity of the material after compounding can be improved, the agglomeration degree is reduced, and the material has better cycle stability, high reversible capacity, thermal stability and mechanical strength. The graphene-based substrate material can assist in the growth of the material while providing conductivity, and provides structural support for the entire material. Based on the background, the negative electrode of the basic ferric oxide/graphene prepared by the invention has high reversible capacity and more stable structureSkeleton, good cycling stability and green sustainable.
The purpose of the invention can be realized by the following technical scheme:
the invention provides a preparation method of a basic ferric oxide/graphene negative electrode material, which comprises the following steps:
s1: providing a graphene ethanol solution;
s2: adding ferric chloride hexahydrate into the graphene ethanol solution, and stirring until the ferric chloride hexahydrate is dissolved;
s3: adding ammonium bicarbonate, and stirring until the ammonium bicarbonate is dissolved;
s4: stirring and reacting at room temperature, and then carrying out deionization washing, centrifuging and drying on the material obtained by the reaction to obtain the basic ferric oxide/graphene negative electrode material.
The invention compounds basic ferric oxide and graphene by mixing ferric chloride hexahydrate (FeCl)3·6H2O) and ammonium hydrogen carbonate (NH)4HCO3) The reaction better generates basic iron oxide (FeOOH), and when the basic iron oxide is mixed with graphene, the basic iron oxide can be well combined with oxygen-containing groups on graphene sheets through electrostatic interaction. Since graphene has a high specific surface area, electrical conductivity, and excellent chemical stability, the two can be effectively combined very stably. The composite material has higher specific surface area and more electron transmission channels, has more excellent electrical properties, and is expected to be applied to lithium ion batteries as a negative electrode material.
Preferably, the mass ratio of the ferric chloride hexahydrate to the ammonium bicarbonate to the graphene in the graphene ethanol solution is 6:5:5-10, so that the basic iron oxide can be better attached to the graphene sheet, the agglomeration degree of the basic iron oxide on the graphene is reduced, and a better polymerization and conduction basis is provided for the comprehensive performance of the composite material.
Preferably, the mass ratio of the ferric chloride hexahydrate to the ammonium bicarbonate to the graphene in the graphene ethanol solution is 6:5: 7.
Preferably, the graphene ethanol solution contains graphene with the mass concentration of 6mg/ml-12 mg/ml.
Preferably, the graphene ethanol solution contains graphene with the mass concentration of 8.46 mg/ml.
Preferably, the ammonium bicarbonate is used to react with ferric chloride hexahydrate to form basic iron oxide.
Preferably, the graphene ethanol solution is obtained by replacing a graphene aqueous solution.
Preferably, the stirring in step S2, step S3 and step S4 is magnetic stirring, respectively.
Preferably, in step S4, the reaction time is 8 h.
Preferably, the drying in step S4 is vacuum drying at 40 ℃.
The second aspect of the invention provides the basic iron oxide/graphene negative electrode material obtained by the preparation method.
The third aspect of the invention provides application of the basic ferric oxide/graphene negative electrode material in preparation of a lithium ion battery negative electrode material.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention prepares the basic ferric oxide/graphene anode material in FeCl by a simple magnetic stirring method3·6H2O and NH4HCO3In the reaction process, basic iron oxide is generated; in which Fe is produced3+Cations are well combined with oxygen-containing groups on the graphene sheets through electrostatic interaction; the assembly of the graphene structure and the in-situ uniform polymerization of the basic iron oxide on the bottom surface of the graphene can be completed in one step, and the method is simple and convenient;
2. the method adopts a simple magnetic stirring method, the reaction conditions are room temperature and 8 hours, and compared with other methods, the method has the advantages of short time, high temperature avoidance, environmental protection and sustainability;
3. the graphene contained in the graphene ethanol solution is 8.46mg/ml in mass concentration, high in concentration and small in addition amount, and can have more excellent electrical properties;
4. the invention uses FeCl3·6H2O、NH4HCO3And graphene are used as raw materials to prepare the composite material, so that the raw materials are easy to obtain, designability is realized, and the cost is low;
5. the basic ferric oxide/graphene negative electrode material prepared by the method has good electrical properties, high reversible capacity, good cycle stability, greenness and sustainability, and has wide application prospects in the field of lithium ion batteries.
Drawings
Fig. 1 is an SEM topography of the basic iron oxide \ graphene negative electrode material obtained in example 1 as a negative electrode material of a lithium ion battery.
Fig. 2 is a cycle performance diagram of the basic iron oxide \ graphene negative electrode material obtained in example 1 as a negative electrode material of a lithium ion battery, in which FeOOH/GO represents the basic iron oxide \ graphene negative electrode material obtained in example 1, and pure FeOOH represents basic iron oxide.
Fig. 3 is a rate performance graph of the basic iron oxide \ graphene negative electrode material obtained in example 1 as a negative electrode material of a lithium ion battery, and FeOOH/GO in the graph represents the basic iron oxide \ graphene negative electrode material obtained in example 1.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
Preparing an alkali type ferric oxide/graphene anode material:
(1) replacing the graphene aqueous solution with 50ml of graphene ethanol solution, wherein the mass concentration of graphene is 8.46mg/ml, and taking 40ml of graphene ethanol solution;
(2) mixing ferric chloride hexahydrate (FeCl)3·6H2O) adding the mixture into the graphene oxide ethanol solution, and magnetically stirring until the graphene oxide ethanol solution is dissolved;
(3) mixing ammonium hydrogen carbonate (NH)4HCO3) Adding into the above solution, magnetically stirring to dissolve, adding ferric chloride hexahydrate (FeCl)3·6H2O), ammonium hydrogen carbonate (NH)4HCO3) And graphene in a mass ratio of 6:5: 7.
(4) carrying out magnetic stirring reaction on the solution for 8 hours;
(5) and repeatedly washing and centrifuging the material obtained by the reaction by using deionized water, and finally drying the material in vacuum to obtain the basic ferric oxide/graphene negative electrode material. As shown in fig. 1, elliptical basic iron oxide particles with a particle size of about 300nm are uniformly dispersed on graphene, the loading capacity of the particles reaches 87%, and meanwhile, due to the fact that the particles have high specific surface area, high conductivity and high chemical stability, the composite material can have more electron transmission channels, has more excellent electrical properties, and can be used as a negative electrode material of a lithium ion battery.
(6) The obtained negative electrode material is used as a negative electrode material of a lithium ion battery to assemble a lithium ion button type half battery, the composite material, carbon black (Super-P) and polyvinylidene fluoride (PVDF) are mixed according to the weight ratio of 7:2:1, then the mixture is uniformly coated on pure copper foil (99.6%) by a coating method to prepare a negative electrode, and a pure lithium sheet is used as a counter electrode. Electrochemical tests are carried out by using the button type half cell, and the cycle performance graph and the rate performance graph are respectively shown in figures 2 and 3. As can be seen from FIG. 2, the negative electrode material prepared by the present invention has a high reversible capacity of 100mA · g-1The capacity of the battery can reach 600 mAh.g under charging and discharging current-1(ii) a As can be seen from FIG. 3, the cathode material prepared by the method has good cycling stability and has wide application prospect in the field of lithium ion batteries.
Example 2
Preparing an alkali type ferric oxide/graphene anode material:
(1) replacing the graphene aqueous solution with 50ml of graphene ethanol solution, wherein the mass concentration of graphene is 6mg/ml, and taking 40ml of graphene ethanol solution;
(2) mixing ferric chloride hexahydrate (FeCl)3·6H2O) adding the mixture into the graphene oxide ethanol solution, and magnetically stirring until the graphene oxide ethanol solution is dissolved;
(3) mixing ammonium hydrogen carbonate (NH)4HCO3) Adding into the above solution, magnetically stirring to dissolve, adding ferric chloride hexahydrate (FeCl)3·6H2O), ammonium hydrogen carbonate (NH)4HCO3) And graphene in a mass ratio of 6:5: 5.
(4) carrying out magnetic stirring reaction on the solution for 8 hours;
(5) and repeatedly washing and centrifuging the material obtained by the reaction by using deionized water, and finally drying the material in vacuum to obtain the basic ferric oxide/graphene negative electrode material.
Example 3
Preparing an alkali type ferric oxide/graphene anode material:
(1) replacing the graphene aqueous solution with 50ml of graphene ethanol solution, wherein the mass concentration of graphene is 12mg/ml, and taking 40ml of graphene ethanol solution;
(2) mixing ferric chloride hexahydrate (FeCl)3·6H2O) adding the mixture into the graphene oxide ethanol solution, and magnetically stirring until the graphene oxide ethanol solution is dissolved;
(3) mixing ammonium hydrogen carbonate (NH)4HCO3) Adding into the above solution, magnetically stirring to dissolve, adding ferric chloride hexahydrate (FeCl)3·6H2O), ammonium hydrogen carbonate (NH)4HCO3) And graphene in a mass ratio of 6:5: 10.
(4) carrying out magnetic stirring reaction on the solution for 8 hours;
(5) and repeatedly washing and centrifuging the material obtained by the reaction by using deionized water, and finally drying the material in vacuum to obtain the basic ferric oxide/graphene negative electrode material.
The embodiments described above are intended to facilitate the understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A preparation method of basic ferric oxide/graphene negative electrode material is characterized by comprising the following steps:
s1: providing a graphene ethanol solution;
s2: adding ferric chloride hexahydrate into the graphene ethanol solution, and stirring until the ferric chloride hexahydrate is dissolved;
s3: adding ammonium bicarbonate, and stirring until the ammonium bicarbonate is dissolved;
s4: stirring and reacting at room temperature, and then carrying out deionization washing, centrifuging and drying on the material obtained by the reaction to obtain the basic ferric oxide/graphene negative electrode material.
2. The preparation method of the basic ferric oxide/graphene negative electrode material as claimed in claim 1, wherein the mass ratio of the ferric chloride hexahydrate, the ammonium bicarbonate and the graphene in the graphene ethanol solution is 6:5: 5-10.
3. The preparation method of the basic ferric oxide/graphene negative electrode material as claimed in claim 2, wherein the mass ratio of the ferric chloride hexahydrate, the ammonium bicarbonate and the graphene in the graphene ethanol solution is 6:5: 7.
4. The preparation method of the basic ferric oxide/graphene negative electrode material as claimed in claim 1, wherein the graphene ethanol solution contains graphene with a mass concentration of 6mg/ml to 12 mg/ml.
5. The method for preparing the basic ferric oxide/graphene negative electrode material as claimed in claim 4, wherein the graphene ethanol solution contains graphene with a mass concentration of 8.46 mg/ml.
6. The method for preparing basic ferric oxide/graphene anode material according to claim 1, wherein the ammonium bicarbonate is used for reacting with ferric chloride hexahydrate to generate basic ferric oxide.
7. The preparation method of the basic ferric oxide/graphene anode material as claimed in claim 1, wherein the graphene ethanol solution is obtained by replacing graphene aqueous solution.
8. The preparation method of the basic iron oxide/graphene anode material according to claim 1, wherein any one or more of the following conditions are adopted:
(1) magnetic stirring is adopted for stirring in the step S2, the step S3 and the step S4 respectively;
(2) in the step S4, the reaction time is 8 h;
(3) the drying in step S4 is performed by vacuum drying at 40 ℃.
9. The basic iron oxide/graphene negative electrode material obtained by the preparation method according to any one of claims 1 to 8.
10. The application of the basic iron oxide/graphene negative electrode material of claim 9 in preparing a negative electrode material of a lithium ion battery.
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