CN109244441B - non-Newtonian fluid Na-K alloy electrode and preparation method and application thereof - Google Patents
non-Newtonian fluid Na-K alloy electrode and preparation method and application thereof Download PDFInfo
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/40—Alloys based on alkali metals
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a non-Newtonian fluid Na-K alloy electrode, a preparation method thereof and application of the non-Newtonian fluid Na-K alloy electrode as a negative electrode material of an alkali metal secondary battery, wherein the method comprises the following steps: under the protection of inert gas, stacking K metal and Na metal physically to perform alloying reaction of the K metal and the Na metal to obtain Na-K liquid alloy; under the protection of inert gas, mixing and stirring the liquid Na-K alloy and the powder particles to form a non-Newtonian fluid Na-K alloy composite material, and then coating the material on a carrier to obtain the non-Newtonian fluid Na-K alloy electrode. The electrode comprises a carrier and a non-Newtonian fluid Na-K alloy composite material coated on the carrier. The electrode has the characteristics of high coulombic efficiency, no dendritic crystal growth, stable structure and the like, can be used as a potassium metal cathode and a sodium metal cathode simultaneously, and can obviously improve the energy density and the cycling stability of the whole battery when being matched with positive electrode materials such as sulfur, Prussian blue and the like.
Description
Technical Field
The invention relates to the technical field of negative electrode materials of alkali metal secondary batteries, in particular to a non-Newtonian fluid Na-K alloy electrode, a preparation method thereof and application of the non-Newtonian fluid Na-K alloy electrode as a negative electrode material of an alkali metal secondary battery.
Background
With the development of technology and the popularization of electronic products, the conventional battery cannot meet the requirements. The alkali metal battery as a novel energy storage device has the characteristics of large reserve, low preparation cost, wide electrochemical window and the like, and has wide application prospect in the fields of mobile communication, electric automobiles, energy storage and the like. The alkali metal negative electrode has higher specific capacity compared with the traditional carbon material, metal oxide and the like. However, the alkali metal cathode is easy to generate dendrite, which causes short circuit of the battery and potential safety hazard, and limits the large-scale application of the battery. The liquid alloy represented by Na-K alloy can completely inhibit the growth of dendrite, and becomes a new research direction of non-dendrite electrode materials. In addition, the Na-K liquid alloy has the characteristics of low toxicity, wide stable temperature (existing in a liquid state at normal temperature even at-12.6 ℃), and the like. However, the liquid Na-K alloy has a large surface tension and is difficult to wet on the surface of the current collector, which seriously hinders the commercial application of the liquid Na-K alloy. Therefore, the research on the liquid metal electrode with stable structure at normal temperature has important significance for the application development of the alkali metal secondary battery.
Researches show that the wettability of the liquid Na-K alloy on the carbon paper can be improved by high-temperature treatment (>420 ℃), and meanwhile, more liquid Na-K alloy can be captured by the porous structure substrate, so that the problem of the fluidity of the Na-K liquid alloy is solved. However, at room temperature, the surface tension of the liquid Na-K alloy is recovered, so that the liquid Na-K alloy exposed on the surface of the composite electrode falls off, and particularly, the internal alloy is extruded under the action of external force to form the exposed alloy. Thus simple carbon supported liquid Na-K alloys cannot essentially solve the problem of interface stability.
Therefore, changing the fluid properties of the liquid Na-K alloy is the key to essentially solve the problem of structural stability of the liquid Na-K alloy electrode. However, at present, no research is conducted at home and abroad aiming at changing the fluid property of the liquid Na-K alloy. Therefore, from changing the fluid property of the liquid Na-K alloy, the key problem of continuously solving the large-scale application of the liquid Na-K alloy negative electrode is to construct a stable electrode and electrolyte interface.
Disclosure of Invention
In view of the problems in the background art, the present invention aims to provide a non-newtonian fluid Na-K alloy electrode, a method for preparing the same, and an application of the non-newtonian fluid Na-K alloy electrode as a negative electrode material of an alkali metal secondary battery, wherein the method can change the easy-flowing physical properties of the Na-K fluid alloy to prepare a dendrite-free negative electrode of the alkali metal battery with strong stability.
A preparation method of a non-Newtonian fluid Na-K alloy electrode comprises the following steps:
1) under the protection of inert gas, stacking K metal and Na metal physically to perform alloying reaction of the K metal and the Na metal to obtain Na-K liquid alloy;
2) under the protection of inert gas, mixing and stirring the liquid Na-K alloy prepared in the step 1) and powder particles to form a non-Newtonian fluid Na-K alloy composite material, and then coating the non-Newtonian fluid Na-K alloy composite material on a carrier to form a non-Newtonian fluid Na-K alloy coating, so as to obtain the non-Newtonian fluid Na-K alloy electrode.
In the step 1), the amounts of K and Na are in a certain proportion, and the mass ratio of K metal to Na metal is 70-86: 14-30, preferably 75-81: 19 to 25, more preferably 77 to 79: 21 to 23.
The K metal and the Na metal are pure K and pure Na.
The K metal and the Na metal need to be cut to remove surface oxides before use.
In the step 2), the powder particles are carbon nanospheres, copper oxide nanopowder or silicon nanopowder.
The preparation of the nano carbon spheres comprises the following steps: uniformly mixing glucose and an aqueous solution containing sodium alkyl benzene sulfonate (surfactant), pouring the mixture into a hydrothermal tank, carrying out hydrothermal treatment at 170-190 ℃ for 10-14 hours (preferably at 180 ℃ for 12 hours), and washing to obtain the carbon nanospheres. The dosage ratio of the glucose to the aqueous solution containing sodium alkyl benzene sulfonate is 0.5 g-2.5 g: 400 mL-600 mL (preferably 1 g: 500mL), wherein the mass percent of the sodium alkyl benzene sulfonate in the aqueous solution containing the sodium alkyl benzene sulfonate is 0.5-2% (preferably 1%).
The preparation of the copper oxide nano powder comprises the following steps: uniformly mixing copper dichloride dihydrate with an aqueous solution containing sodium alkyl benzene sulfonate (surfactant), pouring the mixture into a hydrothermal tank, carrying out hydrothermal treatment at 150-170 ℃ for 9-13 hours (preferably at 160 ℃ for 11 hours), and washing to obtain the copper oxide nano powder.
The dosage ratio of the copper dichloride dihydrate to the sodium alkyl benzene sulfonate-containing aqueous solution is 1.5 g-3.5 g: 800 mL-1200 mL (preferably 2.5 g: 1000mL), wherein the mass percent of the sodium alkyl benzene sulfonate in the aqueous solution containing the sodium alkyl benzene sulfonate is 0.5-2% (preferably 1%).
The preparation of the silicon nano powder comprises the following steps: uniformly mixing silicon oxide powder with an aqueous solution containing sodium alkyl benzene sulfonate (surfactant), pouring the mixture into a hydrothermal tank, carrying out hydrothermal treatment at 170-190 ℃ for 10-14 hours (preferably at 180 ℃ for 12 hours), and washing to obtain the silicon nano powder.
The dosage ratio of the silicon oxide powder to the aqueous solution containing sodium alkyl benzene sulfonate is 1 g-2.8 g: 800 mL-1200 mL (preferably 1.8 g: 1000mL), wherein the mass percent of the sodium alkyl benzene sulfonate in the aqueous solution containing the sodium alkyl benzene sulfonate is 0.5-2% (preferably 1%).
The non-Newtonian fluid Na-K alloy composite material is similar to paint-like alloy and can be coated on a carrier by a tool such as a brush.
The amount of the liquid Na-K alloy and the amount of the powder particles are in a certain proportion, and the mass ratio of the liquid Na-K alloy to the powder particles is 0.1-5: 1, more preferably 0.1 to 3: 1, more preferably 0.256 to 1.28: 1.
the support may be any solid support. The material can be divided into a conductive carrier and a non-conductive carrier according to conductivity, a one-dimensional carrier, a two-dimensional carrier and a three-dimensional carrier according to dimensionality, and a metal carrier, an organic carrier and an inorganic carrier according to materials. Preferably a two-dimensional thin film conductive support of a certain thickness, most preferably a two-dimensional thin film carbon material of a certain thickness and area. The non-Newtonian fluid Na-K alloy itself has good conductivity and therefore does not limit the carrier properties.
The thickness of the carrier is 0.1mm to 10mm, more preferably 0.5mm to 5mm, and most preferably 1mm to 2 mm.
The area of the carrier is 0.1cm2～10cm2More preferably 0.2cm2～2cm2Most preferably 0.5cm2～1.5cm2The length and width of the material is not limited, and a square or a circle is preferable.
In the step 2), the non-Newtonian fluid Na-K alloy electrode is 0.001gcm according to the calculation of the electrode area-2～10gcm-2More preferably 0.01gcm-2～5gcm-2Most preferably 0.05gcm-2～0.2gcm-2。
The inert gas in the steps 1) and 2) is argon, and preferably high-purity argon. The water content is less than 0.1ppm in the inert gas filled environment.
The obtained non-Newtonian fluid Na-K alloy keeps liquid state at normal temperature, does not have dendritic crystal growth condition, and can be used as a K ion battery cathode material and a Na ion battery cathode material at the same time.
The non-Newtonian fluid Na-K alloy electrode comprises a carrier and non-Newtonian fluid Na-K alloy loaded on the carrier. The non-Newtonian fluid Na-K alloy/nano carbon composite material is in a paint shape, has the characteristic of coating, is not limited by the area of a carrier, and can be used for preparing a larger-size electrode.
The non-Newtonian fluid Na-K alloy composite material has strong tensile and bending resistance and can be used as a flexible battery cathode.
The non-Newtonian fluid Na-K alloy electrode is applied as a negative electrode material of an alkali metal secondary battery.
Compared with the prior art, the invention has the following advantages and outstanding effects:
the invention aims to prepare a dendrite-free liquid alloy cathode electrode with a stable structure. The invention has the following two characteristics: 1) the conventional liquid Na-K alloy with liquid property is easy to fall off from the surface of an electrode because of strong surface tension, so that the electrode structure is unstable. The invention provides a method for constructing a non-Newtonian fluid Na-K alloy, which essentially solves the problem of the binding force between the conventional liquid Na-K alloy and an electrode and can be directly coated on the surfaces of carriers with various shapes. 2) The conventional liquid Na-K alloy is liquid and needs to be absorbed in the carrier, and the liquid Na-K alloy is difficult to deform along with the carrier and is easy to fall off from the carrier in the process of bending and stretching the carrier. The non-Newtonian fluid Na-K alloy provided by the invention changes the property of a flowable liquid state into a coating, has the capabilities of resisting stretching, bending and the like, and can be applied to a flexible battery. In addition, due to the non-Newtonian fluid state characteristic, the coating can be coated on a large-area carrier, and is suitable for large-scale production of enterprises.
The non-Newtonian fluid Na-K alloy electrode has the characteristics of high coulombic efficiency, no dendritic crystal growth, stable structure and the like, can be used as a potassium metal cathode and a sodium metal cathode simultaneously, and can obviously improve the energy density and the cycle stability of a full battery when being matched with positive electrode materials such as sulfur, Prussian blue and the like.
Drawings
FIG. 1 is a schematic diagram of the large area coating of a non-Newtonian fluid Na-K alloy prepared in example 1;
FIG. 2 is a schematic diagram of tensile properties test of the non-Newtonian fluid Na-K alloy prepared in example 1, wherein (a), (b) and (c) in FIG. 2 show different tensile states, and the arrows in (a) in FIG. 2 indicate the non-Newtonian fluid Na-K alloy coating;
FIG. 3 is a graph showing the cycle curves of a conventional Na-K alloy electrode and a non-Newtonian fluid Na-K alloy electrode obtained in example 1 after the electrode is assembled into a symmetrical electrode.
Detailed Description
The present invention will be described in detail with reference to examples, but the present invention is not limited thereto.
Example 1
Under the protection of inert gas argon, K metal and Na metal need to be cut to remove surface oxides before use, 0.1g of K metal and 0.028g of Na metal are stacked in a glove box and react for a while to form liquid Na-K alloy. 1g of glucose and 500mL of aqueous solution containing 1 mass percent of surfactant (sodium alkyl benzene sulfonate) are uniformly mixed, poured into a hydrothermal tank, heated at 180 ℃ for 12 hours, and cleaned to obtain the carbon nanospheres. Mixing 0.128g of liquid Na-K alloy and 0.5g of nano carbon spheres, continuously stirring until a viscous mixture is formed, forming non-Newtonian fluid Na-K alloy (namely the non-Newtonian fluid Na-K alloy composite material), and then coating the non-Newtonian fluid Na-K alloy composite material on the surface of a copper sheet to form a non-Newtonian fluid Na-K alloy coating, thus preparing the non-Newtonian fluid Na-K alloy electrode.
The non-Newtonian fluid Na-K alloy prepared in example 1 is more viscous and can be coated. FIG. 1 is a schematic diagram of the large-area coating of the non-Newtonian fluid Na-K alloy prepared in example 1, which shows that the alloy can be coated on the surface of a carrier in a large area. FIG. 2 is a schematic diagram of the tensile properties of the non-Newtonian fluid Na-K alloy prepared in example 1, which shows that the alloy has very strong tensile properties.
Example 2
Under the protection of inert gas argon, K metal and Na metal need to be cut to remove surface oxides before use, 0.2g of K metal and 0.056g of Na metal are stacked in a glove box and reacted for a period of time to form liquid Na-K alloy. 2.5g of copper dichloride dihydrate and 1000mL of aqueous solution containing 1 percent of surfactant (sodium alkyl benzene sulfonate) by mass are uniformly mixed, poured into a hydrothermal tank, and then are subjected to hydrothermal treatment at 160 ℃ for 11 hours, and then are cleaned to obtain the copper oxide nano powder. And mixing 0.256g of liquid Na-K alloy and 0.2g of copper oxide nano powder, continuously stirring until a viscous mixture is formed, namely forming the non-Newtonian fluid Na-K alloy, and then coating the non-Newtonian fluid Na-K alloy on the surface of carbon cloth to obtain the non-Newtonian fluid Na-K alloy electrode.
The performance of the obtained electrode was similar to that of example 1.
Example 3
Under the protection of inert gas argon, K metal and Na metal need to be cut to remove surface oxides before use, 0.2g of K metal and 0.056g of Na metal are stacked in a glove box and reacted for a period of time to form liquid Na-K alloy. 1.8g of silicon oxide powder and 1000mL of aqueous solution containing 1 mass percent of surfactant (sodium alkyl benzene sulfonate) are uniformly mixed, poured into a hydrothermal tank, subjected to hydrothermal treatment at 180 ℃ for 12 hours, and cleaned to obtain the silicon nano powder. And mixing 0.256g of liquid Na-K alloy and 0.4g of silicon nano powder, continuously stirring until a viscous mixture is formed, namely forming the non-Newtonian fluid Na-K alloy, and then coating the non-Newtonian fluid Na-K alloy on the surface of a plastic film to obtain the non-Newtonian fluid Na-K alloy electrode.
The performance of the obtained electrode was similar to that of example 1.
Performance testing
The non-Newtonian fluid Na-K alloy electrode and the carbon cloth 400-degree adsorption liquid Na-K alloy electrode prepared in the embodiments 1-3 are respectively used as a counter electrode and a working electrode of the button cell, and the electrolyte is 1M KPF6(or 1M NaPF6) In the electrolyte, the current density was 1mA cm-2The circulating electric quantity is 1mAh cm-2Measuring K (in a symmetrical electrode system in an environment of 25 +/-1 DEG COr Na) the overpotential of the metal negative electrode.
The performance test results are as follows:
the Na-K alloy composite electrodes of examples 1, 2 and 3 were measured at 1mAcm-2The current density is circulated for 360 times, the overvoltage can be stabilized within 15mV, 13mV and 19mV respectively, the voltage platform is stable without obvious fluctuation, and the potential fluctuation of the carbon cloth 400-degree adsorption liquid Na-K alloy electrode is severe. In addition, the coulombic efficiency of 100 electrode cycles can be respectively maintained above 99.2%, 98.6% and 99.4%. Therefore, the prepared non-Newtonian fluid Na-K alloy composite electrode is low in overvoltage, good in circulation stability and high in coulomb efficiency. The curve of the non-Newtonian fluid Na-K alloy composite electrode prepared in example 1 is shown in FIG. 3, and the curve of the common Na-K alloy electrode is also shown in FIG. 3, wherein the curve is obtained by assembling the non-Newtonian fluid Na-K alloy composite electrode into a symmetrical electrode under different multiplying factors.
The non-Newtonian fluid Na-K alloy has a better stable structure compared with the common liquid Na-K alloy, maintains the liquid non-dendritic crystal characteristic, changes the easy flowing property of the liquid Na-K alloy and ensures the stability of the electrode structure.
Therefore, the non-Newtonian fluid Na-K alloy electrode has the characteristics of high coulombic efficiency, obvious dendritic crystal growth inhibition, stable interface structure and the like, has great significance in metal negative electrode modification of the alkali metal secondary battery, and is beneficial to large-scale application of the alkali metal negative electrode without dendritic crystals.
Claims (9)
1. A preparation method of a non-Newtonian fluid Na-K alloy electrode is characterized by comprising the following steps:
1) under the protection of inert gas, stacking K metal and Na metal physically to perform alloying reaction of the K metal and the Na metal to obtain Na-K liquid alloy;
2) under the protection of inert gas, mixing and stirring the liquid Na-K alloy prepared in the step 1) and powder particles to form a non-Newtonian fluid Na-K alloy composite material, and then coating the non-Newtonian fluid Na-K alloy composite material on a carrier to form a non-Newtonian fluid Na-K alloy coating to obtain a non-Newtonian fluid Na-K alloy electrode;
the powder particles are carbon nanospheres, copper oxide nano powder or silicon nano powder.
2. The method for preparing a non-Newtonian fluid Na-K alloy electrode according to claim 1, wherein in step 1), the ratio of the mass of the K metal to the mass of the Na metal is 70-86: 14 to 30.
3. The method for preparing a non-Newtonian fluid Na-K alloy electrode according to claim 2, wherein in step 1), the ratio of the mass of the K metal to the mass of the Na metal is 75-81: 19 to 25.
4. The method for preparing a non-Newtonian fluid Na-K alloy electrode according to claim 3, wherein in step 1), the ratio of the mass of the K metal to the mass of the Na metal is 77-79: 21 to 23.
5. The method for preparing a non-Newtonian fluid Na-K alloy electrode according to claim 1, wherein in step 1), the K metal and the Na metal are cut to remove surface oxides before use.
6. The method for preparing a non-Newtonian fluid Na-K alloy electrode according to claim 1, wherein in the step 2), the preparation of the nano carbon spheres comprises: uniformly mixing glucose and an aqueous solution containing sodium alkyl benzene sulfonate, pouring the mixture into a hydrothermal tank, carrying out hydrothermal treatment at 170-190 ℃ for 10-14 hours, and cleaning to obtain nano carbon spheres;
the preparation of the copper oxide nano powder comprises the following steps: uniformly mixing copper dichloride dihydrate with an aqueous solution containing sodium alkyl benzene sulfonate, pouring the mixture into a hydrothermal tank, carrying out hydrothermal treatment at the temperature of between 150 and 170 ℃ for 9 to 13 hours, and cleaning the mixture to obtain copper oxide nano powder;
the preparation of the silicon nano powder comprises the following steps: and uniformly mixing the silicon oxide powder with an aqueous solution containing sodium alkyl benzene sulfonate, pouring the mixture into a hydrothermal tank, carrying out hydrothermal treatment at 170-190 ℃ for 10-14 hours, and cleaning to obtain the silicon nano powder.
7. The method for preparing the non-Newtonian fluid Na-K alloy electrode according to claim 1, wherein in the step 2), the mass ratio of the liquid Na-K alloy to the powder particles is 0.1-5: 1.
8. the non-Newtonian fluid Na-K alloy electrode prepared by the preparation method according to any one of claims 1 to 7.
9. Use of the non-newtonian fluid Na-K alloy electrode according to claim 8 as negative electrode material for alkali metal secondary batteries.
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| CN108063219A (en) * | 2017-11-23 | 2018-05-22 | 浙江大学 | A kind of high efficiency liquid alkali metal alloy electrode and its preparation method and application |
| CN108400316A (en) * | 2018-02-11 | 2018-08-14 | 浙江大学 | Selfreparing oxidation film coats Na-K liquid alloy electrodes and its preparation method and application |
| CN108448063A (en) * | 2017-12-07 | 2018-08-24 | 苏州大学 | A kind of guard method of alkali metal secondary battery metal negative electrode |
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| CN103378355A (en) * | 2012-04-12 | 2013-10-30 | 中国科学院物理研究所 | Alkali metal secondary battery as well as negative active substance, negative material and negative electrode thereof, and preparation method of negative active substance |
| CN108063219A (en) * | 2017-11-23 | 2018-05-22 | 浙江大学 | A kind of high efficiency liquid alkali metal alloy electrode and its preparation method and application |
| CN108448063A (en) * | 2017-12-07 | 2018-08-24 | 苏州大学 | A kind of guard method of alkali metal secondary battery metal negative electrode |
| CN108400316A (en) * | 2018-02-11 | 2018-08-14 | 浙江大学 | Selfreparing oxidation film coats Na-K liquid alloy electrodes and its preparation method and application |
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