CN113206234B - Lithium metal composite cathode based on antimony tin oxide modified carbon framework and preparation method thereof - Google Patents
Lithium metal composite cathode based on antimony tin oxide modified carbon framework and preparation method thereof Download PDFInfo
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- CN113206234B CN113206234B CN202110480146.0A CN202110480146A CN113206234B CN 113206234 B CN113206234 B CN 113206234B CN 202110480146 A CN202110480146 A CN 202110480146A CN 113206234 B CN113206234 B CN 113206234B
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Abstract
The invention belongs to the field of lithium battery cathodes, and particularly discloses a lithium metal composite cathode based on an antimony tin oxide modified carbon framework and a preparation method thereof, wherein the preparation method comprises the following steps: modifying the carbon frame by antimony tin oxide to obtain a modified carbon frame; and combining the metal lithium with the modified carbon framework to obtain the lithium metal composite cathode based on the antimony oxide tin modified carbon framework. According to the invention, the carbon frame is modified by the antimony tin oxide, the antimony tin oxide is easily adsorbed on the surface of the carbon frame, the wettability between the metal lithium and the carbon frame can be improved, the metal lithium and the modified carbon frame can be tightly combined, the stable lithium metal composite cathode is obtained, the process is simple and environment-friendly, subsequent heat treatment is not required, the equipment requirement is low, the cost is low, and mass production is easy.
Description
Technical Field
The invention belongs to the field of lithium battery cathodes, and particularly relates to a lithium metal composite cathode based on an antimony tin oxide modified carbon framework and a preparation method thereof.
Background
The lithium metal cathode has high theoretical capacity (as high as 3860 mAh/g) and lowest electrochemical potential (-3.040V relative to a standard hydrogen electrode), and can meet the requirements of human beings on a high-energy-density lithium battery. However, the lithium metal negative electrode has problems of dendrite growth, high reactivity, large volume expansion, and the like. The conductive carbon material is used as the frame of the lithium negative electrode, so that the deposition of metal lithium can be effectively accommodated, and the volume expansion of the metal lithium can be inhibited, so that the comprehensive performance of the battery is improved.
At present, the preparation method of the carbon frame/metal lithium composite negative electrode mainly comprises an electrochemical deposition method and a molten metal lithium pouring method. By adopting an electrochemical deposition method, the initial deposition of lithium is difficult to control, the phenomenon of uneven lithium deposition is easy to occur, metal lithium needs to be pre-deposited by preparing a sacrificial battery for pre-circulation, the sacrificial battery is disassembled and discarded after the pre-deposition is finished, and a great amount of labor and cost are wasted in the process. The molten metal lithium pouring method is simple in preparation process, easy to operate and free of 'sacrificing batteries', and metal lithium is uniformly distributed in the frame, but the wettability between the metal lithium and the carbon frame is poor, so that the surface of the carbon frame needs to be modified. The surface modification method of the carbon frame mainly comprises an electroplating method and a chemical vapor deposition method. However, these modification methods have some disadvantages, such as high equipment requirement, high preparation cost, requirement of subsequent heat treatment, or use of toxic and harmful organic substances, and these disadvantages greatly limit the preparation and application of the carbon frame/lithium composite negative electrode. Therefore, there is a need for a carbon frame/lithium composite anode that is inexpensive, environmentally friendly, simple and easy to operate, and a method for preparing the same.
Disclosure of Invention
Aiming at the defects or improvement requirements in the prior art, the invention provides a lithium metal composite cathode based on an antimony tin oxide modified carbon framework and a preparation method thereof, aiming at modifying the carbon framework to enable metal lithium and the modified carbon framework to be tightly combined to obtain a stable lithium metal composite cathode, and the preparation method is simple in process and environment-friendly.
In order to achieve the above object, according to an aspect of the present invention, a method for preparing a lithium metal composite anode based on an antimony tin oxide modified carbon framework is provided, which comprises the following steps:
modifying the carbon frame by antimony tin oxide to obtain a modified carbon frame; and combining the metal lithium with the modified carbon framework to obtain the lithium metal composite cathode based on the antimony oxide tin modified carbon framework.
More preferably, the modified carbon frame is obtained by dispersing antimony tin oxide powder in a solvent to obtain an antimony tin oxide suspension, and dropping the antimony tin oxide suspension onto the carbon frame to physically adsorb antimony tin oxide on the carbon frame.
More preferably, the particle size of the antimony tin oxide powder is 5nm to 500nm.
More preferably, the particle size of the antimony tin oxide powder is 20nm to 200nm.
More preferably, the modified carbon frame comprises antimony tin oxide accounting for 5wt% to 80wt% of the modified carbon frame.
More preferably, the modified carbon frame comprises antimony tin oxide accounting for 20wt% -40 wt% of the modified carbon frame.
More preferably, the antimony tin oxide powder is ultrasonically dispersed in water or an ethanol solvent to obtain an antimony tin oxide suspension.
More preferably, the lithium metal composite negative electrode based on the antimony oxide tin modified carbon framework is obtained by directly contacting molten lithium metal with the modified carbon framework and absorbing the lithium metal into the modified carbon framework by a siphon effect.
Preferably, molten metal lithium is dripped into the modified carbon framework, and the metal lithium and antimony tin oxide on the surface of the modified carbon framework undergo redox reaction, so that the metal lithium and the modified carbon framework are tightly combined, and the lithium metal composite negative electrode based on the antimony tin oxide modified carbon framework is obtained.
As a further preference, according to another aspect of the present invention, there is provided an antimony tin oxide modified carbon framework-based lithium metal composite anode prepared by the above preparation method.
Generally, compared with the prior art, the above technical solution conceived by the present invention mainly has the following technical advantages:
1. according to the invention, the carbon frame is modified by the antimony tin oxide, the antimony tin oxide is easily adsorbed on the surface of the carbon frame, the wettability between the metal lithium and the carbon frame can be improved, and further the metal lithium and the modified carbon frame can be tightly combined to obtain the stable lithium metal composite cathode, the process is simple and environment-friendly, the subsequent heat treatment is not required, the equipment requirement is low, the cost is low, and the mass production is easy.
2. The antimony tin oxide adopted by the invention is an oxide with stable chemical properties and low price, and the preparation process is mature, so that nanoparticles with different sizes can be easily prepared; meanwhile, the invention drops the suspension of antimony tin oxide prepared from antimony tin oxide powder on the carbon frame, so that the antimony tin oxide is physically adsorbed on the carbon frame, the whole process is simple, and the antimony tin oxide can be uniformly adhered on the carbon frame in a large amount.
3. According to the invention, the particle size of the adopted antimony tin oxide powder is researched, and when the particle size of antimony tin oxide is too small, agglomeration is easy to occur, so that the antimony tin oxide powder is not beneficial to being uniformly adsorbed on a carbon frame; when the size of the antimony tin oxide particles is too large, the active contact surface of the subsequent antimony tin oxide and the metal lithium is too small, so that the oxidation-reduction reaction is not facilitated to occur, and the combination of the metal lithium and the modified carbon framework is not tight enough.
4. According to the invention, the content of antimony tin oxide in the modified carbon frame is researched, if the proportion of antimony tin oxide is too small, the content of the product of the in-situ reaction of antimony tin oxide and the carbon frame is small, and the product is not enough to induce the metal lithium to be fully poured; if the ratio of antimony tin oxide is too large, a large amount of Li will be formed once the antimony tin oxide modified carbon framework contacts with molten lithium metal 2 An O-oxide layer, which hinders further reaction of the lithium metal with the antimony tin oxide.
Drawings
Fig. 1 is an XRD spectrum of lithium metal composite negative electrode based on antimony tin oxide modified carbon framework, antimony tin oxide, carbon framework prepared in example 1 of the present invention;
fig. 2 is a cross-sectional SEM image of an antimony tin oxide modified carbon framework based lithium metal composite anode prepared in example 2 of the present invention;
fig. 3 is a cross-sectional SEM image of an antimony tin oxide modified carbon framework-based lithium metal composite anode prepared in example 3 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The embodiment of the invention provides a preparation method of a lithium metal composite cathode based on an antimony tin oxide modified carbon framework, which comprises the following steps:
s1, modifying a carbon frame through antimony tin oxide to obtain a modified carbon frame;
specifically, antimony tin oxide powder is ultrasonically dispersed in water or an ethanol solvent to obtain an antimony tin oxide suspension; dropwise adding the antimony tin oxide suspension on a carbon frame, and drying to enable antimony tin oxide to be physically adsorbed on the carbon frame to obtain a modified carbon frame; the kind of the carbon framework is not limited, and carbon fiber, carbon nanotube, carbon nanosheet, etc. can be used.
The particle size of the antimony tin oxide powder is preferably 5nm to 500nm, more preferably 20nm to 200nm.
Preferably, antimony tin oxide accounts for 5wt% to 80wt%, and more preferably 20wt% to 40wt% of the modified carbon frame.
And S2, pouring molten metal lithium into the modified carbon framework, and cooling to obtain the lithium metal composite cathode based on the antimony oxide tin modified carbon framework.
Specifically, metallic lithium is heated to be molten under a protective atmosphere such as argon, and then the molten metallic lithium is bonded to the modified carbon framework by one of the following two methods: 1) Directly contacting molten metal lithium with the modified carbon framework, absorbing the metal lithium into the modified carbon framework through a siphon effect, and cooling to obtain the lithium metal composite cathode based on the antimony oxide tin modified carbon framework; 2) Dropwise adding molten metal lithium into the modified carbon framework, and carrying out oxidation-reduction reaction on the molten metal lithium and antimony tin oxide on the surface of the modified carbon framework to generate Li 3 SbO 4 、Li 8 SnO 6 、Li 7 Sn 3 、Li 3 Sb and the like, so that the metal lithium is tightly combined with the modified carbon framework to obtain the lithium metal composite negative electrode based on the antimony oxide tin modified carbon framework.
The following are specific examples:
example 1
Ultrasonically dispersing 200nm antimony tin oxide powder in ethanol to prepare an antimony tin oxide suspension; dripping the suspension liquid on carbon fibers, and drying to prepare an antimony tin oxide modified carbon frame, wherein the content of antimony tin oxide is 80wt%; and placing the carbon fiber framework modified by the antimony tin oxide on the surface of molten metal lithium, absorbing the metal lithium into the modified carbon framework through siphonage, and cooling to obtain the lithium metal composite cathode based on the carbon framework modified by the antimony tin oxide. The XRD patterns of the lithium metal composite cathode based on the antimony oxide tin modified carbon framework, untreated antimony oxide tin and the carbon framework are shown in figure 1, and the relative strength of the XRD characteristic peak of the lithium metal composite cathode is obviously higher.
Example 2
Ultrasonically dispersing 5nm antimony tin oxide in water to prepare an antimony tin oxide suspension; dripping the suspension liquid on carbon fiber, and drying to prepare an antimony tin oxide modified carbon frame, wherein the content of antimony tin oxide is 5wt%; and (2) dropwise adding molten metal lithium on the surface of the carbon fiber framework modified by the antimony oxide tin, enabling the metal lithium to penetrate into the modified carbon fiber framework through gravity, cooling, and obtaining the lithium metal composite negative electrode based on the carbon fiber framework modified by the antimony oxide tin, wherein the cross-section SEM image of the lithium metal composite negative electrode is shown in figure 2, and the structure of the carbon fiber framework can be observed and is tightly integrated with the metal lithium.
Example 3
Ultrasonically dispersing 50nm antimony tin oxide in water to prepare an antimony tin oxide suspension; dripping the suspension liquid on carbon fibers, and drying to prepare an antimony tin oxide modified carbon frame, wherein the content of antimony tin oxide is 20wt%; and (3) dropwise adding molten metal lithium on the surface of the carbon fiber framework modified by the antimony oxide tin, enabling the metal lithium to penetrate into the modified carbon fiber framework through gravity, cooling, and obtaining the lithium metal composite negative electrode based on the carbon fiber framework modified by the antimony oxide tin, wherein the cross-section SEM image of the lithium metal composite negative electrode is shown in figure 3, and the structure of the carbon fiber framework can be observed and is tightly integrated with the metal lithium.
Example 4
Ultrasonically dispersing 500nm antimony tin oxide in water to prepare an antimony tin oxide suspension; dripping the suspension liquid on carbon fibers, and drying to prepare an antimony tin oxide modified carbon frame, wherein the content of antimony tin oxide is 40wt%; and dropwise adding molten metal lithium on the surface of the carbon fiber framework modified by the antimony oxide tin, permeating the metal lithium into the modified carbon framework through gravity, and cooling to obtain the antimony oxide tin modified carbon framework/lithium composite negative electrode.
It will be understood by those skilled in the art that the foregoing is only an exemplary embodiment of the present invention, and is not intended to limit the invention to the particular forms disclosed, since various modifications, substitutions and improvements within the spirit and scope of the invention are possible and within the scope of the appended claims.
Claims (8)
1. A preparation method of a lithium metal composite negative electrode based on an antimony tin oxide modified carbon framework is characterized by comprising the following steps:
modifying the carbon frame by antimony tin oxide to obtain a modified carbon frame; specifically, dispersing antimony tin oxide powder in a solvent to obtain an antimony tin oxide suspension, and dropwise adding the antimony tin oxide suspension on a carbon frame to enable antimony tin oxide to be physically adsorbed on the carbon frame to obtain a modified carbon frame; the grain size of the antimony tin oxide powder is 5 nm-500 nm;
and combining the metal lithium with the modified carbon framework to obtain the lithium metal composite cathode based on the antimony oxide tin modified carbon framework.
2. The method for preparing an antimony tin oxide modified carbon frame-based lithium metal composite negative electrode according to claim 1, wherein the antimony tin oxide powder has a particle size of 20nm to 200nm.
3. The method for preparing a lithium metal composite anode based on an antimony tin oxide modified carbon frame according to claim 1, wherein the antimony tin oxide accounts for 5wt% to 80wt% of the modified carbon frame.
4. The method for preparing the lithium metal composite negative electrode based on the antimony tin oxide modified carbon framework as claimed in claim 3, wherein the antimony tin oxide accounts for 20wt% to 40wt% of the modified carbon framework.
5. The method for preparing the lithium metal composite negative electrode based on the antimony oxide tin modified carbon framework according to claim 1, wherein antimony oxide tin powder is ultrasonically dispersed in water or an ethanol solvent to obtain an antimony oxide tin suspension.
6. The method for preparing the lithium metal composite negative electrode based on the antimony oxide tin modified carbon framework as claimed in any one of claims 1 to 5, wherein molten metal lithium is directly contacted with the modified carbon framework, and the metal lithium is absorbed into the modified carbon framework through a siphon effect, so as to obtain the lithium metal composite negative electrode based on the antimony oxide tin modified carbon framework.
7. The method for preparing the lithium metal composite negative electrode based on the antimony oxide tin modified carbon framework as claimed in any one of claims 1 to 5, wherein molten metallic lithium is dripped into the modified carbon framework, and the metallic lithium and antimony oxide tin on the surface of the modified carbon framework undergo redox reaction, so that the metallic lithium is tightly combined with the modified carbon framework, thereby obtaining the lithium metal composite negative electrode based on the antimony oxide tin modified carbon framework.
8. A lithium metal composite negative electrode based on an antimony tin oxide modified carbon framework is characterized by being prepared by the preparation method of any one of claims 1 to 7.
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| KR100346542B1 (en) * | 1999-01-25 | 2002-07-26 | 삼성에스디아이 주식회사 | Lithium secondary battery |
| JP2014235884A (en) * | 2013-06-03 | 2014-12-15 | 株式会社リコー | Nonaqueous electrolyte electricity-storage device, and method for manufacturing the same |
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| CN108365200A (en) * | 2018-02-11 | 2018-08-03 | 清华大学 | A kind of preparation method of compound lithium an- ode |
| CN108470882A (en) * | 2018-03-30 | 2018-08-31 | 江汉大学 | Tin oxide is modified carbon cloth base lithium and sodium metal negative electrode and preparation method thereof |
| KR102187992B1 (en) * | 2018-12-18 | 2020-12-08 | 한양대학교 산학협력단 | Anode for lithium secondary battery comprising lithiophilic coating layer, method for producing the same, and lithium secondary battery comprising the same |
| CN112103472A (en) * | 2019-06-17 | 2020-12-18 | 上海汽车集团股份有限公司 | Metal lithium composite material and preparation method thereof |
| CA3155063A1 (en) * | 2019-09-20 | 2021-03-25 | Li-S Energy Limited | Flexible lithium-sulfur batteries |
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