CN109378464B - Tin dioxide carbon nano composite and preparation method and application thereof - Google Patents

Tin dioxide carbon nano composite and preparation method and application thereof Download PDF

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CN109378464B
CN109378464B CN201811474688.1A CN201811474688A CN109378464B CN 109378464 B CN109378464 B CN 109378464B CN 201811474688 A CN201811474688 A CN 201811474688A CN 109378464 B CN109378464 B CN 109378464B
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dioxide carbon
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CN109378464A (en
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周东山
陆红燕
万远鑫
汪天一
薛奇
王晓亮
陈葳
江伟
季青
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Nanjing Research Institute Of Nanjing University
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    • H01M4/00—Electrodes
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    • H—ELECTRICITY
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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
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    • H—ELECTRICITY
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Abstract

The invention discloses a tin dioxide carbon nano composite and a preparation method and application thereof. The aluminum ion battery prepared by matching the tin dioxide carbon nano composite and the aluminum cathode material has high discharge capacity, high rate capability and long cycle life.

Description

Tin dioxide carbon nano composite and preparation method and application thereof
Technical Field
The invention belongs to the chemical power technology, and particularly relates to a tin dioxide carbon nano composite and a preparation method and application thereof.
Background
Lithium Ion Batteries (LIBs) have enjoyed great success in the field of energy sources for portable electronic devices, electric vehicles and power grids, however, due to the high cost of lithium, poor safety and, in particular, limited resources, the objective is to provide lithium batteries with a high capacityThe application of the prior lithium ion battery still has a plurality of problems to be solved. The present research on secondary batteries focuses on the development of low-cost, high-safety, high-energy-density batteries, such as zinc ion batteries, sodium ion batteries, magnesium ion batteries, and aluminum ion batteries. Among them, Aluminum Ion Batteries (AIBs) are attracting attention because of their low cost, abundant resources, and good safety. Al (Al)3+Due to its trivalent nature, three electrons are transferred in the electrochemical reaction, which results in a high specific capacity of the aluminum ion battery (2980Ah kg)-1). However, there are some key problems to be solved, and the most important of them is to find a suitable cathode material. Most AIB positive electrode materials exhibit low discharge capacity (about 100mAh g)-1) And the long-term cycling stability is poor (less than 200 cycles of stable cycling), and the capacity is attenuated, so that the research on the high-capacity and high-stability cathode material is still challenging.
Disclosure of Invention
The invention aims to solve the technical problem of the prior art and provides a tin dioxide carbon nano composite suitable for an aluminum ion battery anode and a preparation method thereof.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of a tin dioxide carbon nano composite comprises the following steps:
(1) taking SnCl4·5H2Dissolving the O crystal in deionized water, heating the obtained water solution to 190-230 ℃, keeping the temperature for 18-72 hours to obtain a first mixed solution, and cooling to room temperature;
(2) adding glucose into the first mixed solution cooled in the step (1), stirring and dissolving, heating to 190-230 ℃, keeping for 18-24 hours to obtain a second mixed solution, and cooling to room temperature;
(3) and (3) centrifuging the second mixed solution cooled in the step (2), taking the precipitate, cooling to room temperature, and calcining at 500-800 ℃ for 3-10 h in an argon atmosphere to obtain the tin dioxide carbon nano composite.
Wherein in the step (1), the obtained aqueous solution is prepared by mixing 1-5 g of SnCl4·5H2Dissolving the O crystal in 100-150 mL deionized water.
And (2) cooling and centrifuging the first mixed solution obtained in the step (1) to obtain white tin dioxide nano-crystalline precipitate.
In the step (2), the adding amount of the glucose and SnCl4·5H2The mass ratio of the O crystal is (10-20): (1-5), preferably 10: 1.
In the step (2), stirring is carried out to dissolve the added glucose on one hand and uniformly disperse the tin dioxide nanocrystal obtained in the step (1) in the solution on the other hand. The second mixed solution is brown to black nano-scale carbon-coated tin dioxide particle dispersion liquid.
In the step (3), the centrifugation condition is 500-10000 r/min.
The particle size of the obtained stannic oxide carbon nano composite particles is between 50 and 80nm, and the particle size is uniform.
The tin dioxide carbon nano composite obtained by the preparation method is also within the protection scope of the invention.
Although tin dioxide has long been used in lithium ion battery negative electrode materials, it has not been studied in aluminum ion batteries. The reason is that the electrolytes used in the two battery systems are very different. Most of the lithium ion battery electrolyte is an alkaline lithium hexafluorophosphate-carbonate system, while the electrolyte used by the aluminum ion battery is an acidic aluminum trichloride- [ EMIm ] Cl system, and has serious corrosion side reaction with the traditional oxide and sulfide electrode materials, so that most of the electrode materials suitable for the lithium ion battery system cannot be used in the aluminum ion battery. In addition, the electrochemical energy storage mechanism and the battery assembly technology are greatly different, and the application is the first application of the tin dioxide to the anode material of the aluminum ion battery, so that great innovation is achieved.
Meanwhile, the electrochemical performance of the tin dioxide in the battery cycle process is greatly improved by using a porous carbon coating method. By further optimizing the preparation process parameters, the uniformity and the particle size of the prepared product are greatly improved.
The invention also claims the application of the prepared stannic oxide carbon nano composite as a positive electrode in an aluminum ion battery.
The invention further provides an aluminum ion battery anode material which is prepared by mixing the prepared tin dioxide carbon nano composite, polyvinylidene fluoride and super phosphorus carbon black according to the mass ratio of (70-90) to (5-20), dispersing the mixture in a solvent, and coating the solvent on a light molybdenum foil with the thickness of 20-50 microns.
The solvent is N-methyl pyrrolidone; wherein the mass-volume ratio of the polyvinylidene fluoride to the N-methyl pyrrolidone is 0.5-100 mg/ml.
The preparation method comprises the following steps: weighing a tin dioxide carbon nano composite, polyvinylidene fluoride (PVDF) and Super phosphorus black (Super P), mixing, dispersing in N-methylpyrrolidone (NMP), stirring to dissolve the PVDF, uniformly mixing other materials, coating on a double-sided smooth molybdenum foil with the thickness of 20-50 microns to obtain a positive electrode foil, and cutting to directly match with an aluminum negative electrode material to form the aluminum ion battery.
The content which is not described in the technical scheme of the invention can be realized according to the conventional operation of the industry.
Has the advantages that:
the invention provides a positive tin dioxide carbon nano composite material capable of being matched with an Al negative electrode and a preparation method thereof.
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The foregoing and/or other advantages of the invention will become further apparent from the following detailed description of the invention when taken in conjunction with the accompanying drawings.
Fig. 1 is an SEM image of a tin dioxide carbon nanocomposite prepared in example 1;
fig. 2 is a BET specific surface area measurement diagram of the tin dioxide carbon nanocomposite prepared in example 1.
Detailed Description
The invention will be better understood from the following examples.
And (3) reagent sources: super phosphorus carbon black (Super P) was purchased from tex high graphite ltd, switzerland. Other reagents not described are commercially available.
Example 1 preparation of tin dioxide carbon nanocomposite
The method comprises the following steps:
(1) accurately weighing 1g of SnCl4·5H2Dissolving O crystals in 120mL of deionized water, transferring the solution into a reaction kettle, heating the solution at 190 ℃ for 18 hours to obtain a first mixed solution, taking out the first mixed solution, and cooling the first mixed solution to room temperature;
(2) accurately weighing 10g of glucose, adding the glucose into the first mixed solution, dissolving the glucose into the first mixed solution, stirring the solution to ensure that the obtained tin dioxide nanoparticles are well dispersed in the solution, placing the solution into a reaction kettle after the glucose is completely dissolved, heating the solution at 190 ℃ for 18 hours to obtain a second mixed solution, taking out the second mixed solution, and cooling the second mixed solution to room temperature;
(3) and (3) centrifuging the second mixed solution cooled in the step (2) at 1000 revolutions per minute, taking the precipitate, placing the precipitate at 500 ℃, and calcining the precipitate for 3 hours in an argon atmosphere to obtain the tin dioxide carbon nano composite.
SEM characterization of the tin dioxide carbon nanocomposite revealed that the tin dioxide had a particle size of about 50nm, a small particle size and high uniformity, as shown in FIG. 1. The BET specific surface area test of the above tin oxide carbon nanocomposite revealed that the specific surface area of the particles was about 204.8m2g-1See fig. 2.
Example 2 application of tin dioxide carbon nanocomposite in aluminum ion batteries
Application 1: 160mg of the tin dioxide carbon nano composite prepared in example 1, 20mg of PVDF and 20mg of Super P are accurately weighed, dispersed in 1.5mL of NMP, magnetically stirred for 24 hours and coated on a double-sided light molybdenum foil with the thickness of 20 micrometers to obtain the required positive electrode foilAnd cutting to obtain the positive pole piece. High-purity Al wafer (thickness of 0.02mm) is used as a negative electrode, and ionic liquid (molar ratio AlCl)3:[EMIm]Cl-1.3: 1) as an electrolyte, a GF/D glass fiber septum manufactured by Whatman was used, and the electrolyte was placed in a glove box ([ O ] filled with argon gas2]<0.1ppm,[H2O]<0.1ppm) into CR2032 coin cells, each containing 50 microliters of electrolyte. (in the application, the mass ratio of the stannic oxide carbon nano composite, the polyvinylidene fluoride and the super phosphorus carbon black is 80:10:10)
Application 2: and (3) accurately weighing 140mg of the tin oxide carbon nano composite prepared in the embodiment 1, 10mg of PVDF and 20mg of Super P, dispersing the tin oxide carbon nano composite, 10mg of PVDF and 20mg of Super P in 1.5mL of NMP, magnetically stirring the mixture for 24 hours, coating the mixture on a double-sided smooth molybdenum foil with the thickness of 20 micrometers to obtain a required positive electrode foil, and cutting the positive electrode foil to obtain a positive electrode piece. High-purity Al wafer (thickness of 0.02mm) is used as a negative electrode, and ionic liquid (molar ratio AlCl)3:[EMIm]Cl-1.3: 1) was used as an electrolyte, and a GF/D glass fiber septum manufactured by Whatmann was used in a glove box ([ O ] filled with argon gas2]<0.1ppm,[H2O]<0.1ppm) into CR2032 coin cells, each containing 50 microliters of electrolyte. (in the application, the mass ratio of the stannic oxide carbon nano composite to the polyvinylidene fluoride to the super-phosphorus carbon black is 70:10:20)
Application 3: and accurately weighing 180mg of the tin dioxide carbon nano composite prepared in the example 1, 5mg of PVDF and 5mg of Super P, dispersing in 1.5mL of NMP, magnetically stirring for 24h, coating on a double-sided light molybdenum foil with the thickness of 20 microns to obtain a required positive electrode foil, and cutting to obtain the positive electrode piece. High-purity Al wafer (thickness of 0.02mm) is used as a negative electrode, and ionic liquid (molar ratio AlCl)3:[EMIm]Cl-1.3: 1) was used as an electrolyte, and a GF/D glass fiber septum manufactured by Whatmann was used in a glove box ([ O ] filled with argon gas2]<0.1ppm,[H2O]<0.1ppm) into CR2032 coin cells, each containing 50 microliters of electrolyte. (in the application, the mass ratio of the stannic oxide carbon nano composite, the polyvinylidene fluoride and the super phosphorus carbon black is 90:5:5)
The performance of the prepared aluminum ion battery is detected by adopting a battery test system, the test voltage window is 0-2V, and the result is shown in table 1. (coulombic efficiency means the ratio of discharge capacity to charge capacity; stable cycle number means the number of times the battery is charged and discharged stably and maintains discharge capacity of more than 100mAh/g, one cycle is counted after one charge and discharge process is completed; discharge capacity 1 means the discharge capacity of the battery under the current density of 100 mA/g; discharge capacity 2 means the discharge capacity of the battery under the current density of 200 mA/g; mass ratio means the tin dioxide carbon nano composite: polyvinylidene fluoride: super-phosphorus carbon black)
TABLE 1
Figure BDA0001891899090000051
As can be seen from the data in the table: the highest discharge capacity of the battery is achieved at a mass ratio of 80:10:10, so a slurry formulation process with a mass ratio of 80:10:10 should be preferred (i.e. application 1 is the best application).
Example 3
The preparation of the tin dioxide carbon nano composite comprises the following steps:
(1) accurately weighing 1g of SnCl4·5H2Dissolving O crystal in 120mL of pure water, transferring the solution into a reaction kettle, heating the solution at 210 ℃ for 36 hours to obtain a first mixed solution, taking out the first mixed solution, and cooling the first mixed solution to room temperature;
(2) accurately weighing 10g of glucose, adding the glucose into the first mixed solution, dissolving the glucose in the first mixed solution, stirring the solution to well disperse the obtained tin dioxide nanoparticles in the solution, placing the solution into a reaction kettle after the glucose is completely dissolved, heating the solution at 210 ℃ for 36 hours to obtain a second mixed solution, taking out the second mixed solution, and cooling the second mixed solution to room temperature;
(3) and (3) centrifuging the second mixed solution cooled in the step (2) at 1000 revolutions per minute, taking the precipitate, placing the precipitate at 500 ℃, and calcining the precipitate for 3 hours in an argon atmosphere to obtain the tin dioxide carbon nano composite.
Example 4
The preparation of the tin dioxide carbon nano composite comprises the following steps:
(1) accurately weighing 1g of SnCl4·5H2Dissolving the O crystal in 120mL of pure water, transferring the solution into a reaction kettle,heating at 230 deg.C for 72 hr to obtain a first mixed solution, taking out, and cooling to room temperature;
(2) accurately weighing 10g of glucose, adding the glucose into the first mixed solution, dissolving the glucose in the first mixed solution, stirring the solution to well disperse the obtained tin dioxide nanoparticles in the solution, placing the solution into a reaction kettle after the glucose is completely dissolved, heating the solution at 230 ℃ for 72 hours to obtain a second mixed solution, taking out the second mixed solution, and cooling the second mixed solution to room temperature;
(3) and (3) centrifuging the second mixed solution cooled in the step (2) at 1000 revolutions per minute, taking the precipitate, placing the precipitate at 500 ℃, and calcining the precipitate for 3 hours in an argon atmosphere to obtain the tin dioxide carbon nano composite.
Example 5
The procedure was as in example 1, except that:
in the step (1), 3g of SnCl is weighed4·5H2O crystal dissolved in 150mL of pure water;
in the step (2), 15g of glucose or sucrose is accurately weighed and added into the first mixed solution.
Example 6
The procedure was as in example 1, except that:
in the step (1), 5g of SnCl is weighed4·5H2O crystal dissolved in 150mL of pure water;
in the step (2), 15g of glucose or sucrose is accurately weighed and added into the first mixed solution.
Example 7
The procedure was as in example 1, except that:
in the step (3), the calcination temperature is 650 ℃ and the calcination time is 5 hours.
Example 8
The procedure was as in example 1, except that:
in the step (3), the calcination temperature is 800 ℃ and the calcination time is 10 hours.
The tin dioxide carbon nanocomposites prepared in examples 1 and 3 to 8 were treated as the positive electrode, the high purity Al plate (thickness 0.02mm) as the negative electrode, and the ionic liquid (molar ratio AlCl) as the negative electrode according to application 1 of example 23:[EMIm]Cl-1.3: 1) was used as an electrolyte, and a GF/D glass fiber septum manufactured by Whatman was used in an argon-filled glove box ([ O ]2]<0.1ppm,[H2O]<0.1ppm) into CR2032 coin cells, each containing 50 microliters of electrolyte.
The performance of the prepared aluminum ion battery is detected by adopting a battery test system, the test voltage window is 0-2V, and the result is shown in Table 2. (coulombic efficiency means the ratio of discharge capacity to charge capacity; stable cycle number means the number of times the battery is stably charged and discharged and maintains discharge capacity of 100mAh/g or more, one cycle is counted in the process of completing one charge and discharge; discharge capacity 1 means the discharge capacity of the battery at a current density of 100 mA/g; discharge capacity 2 means the discharge capacity of the battery at a current density of 200 mA/g)
TABLE 2
Figure BDA0001891899090000071
As can be seen from the data in the table: 1g SnCl4·5H2O crystals are preferably dissolved in 120mL of pure water; 10g of glucose is preferred; the comparison of the hydrothermal reaction temperature of 190, 210 and 230 ℃ and 190 ℃ is preferred; the hydrothermal reaction time is preferably 18h, 36 h, 72h and 18 h; comparative calcination temperatures of 500, 650, 800 ℃, 500 ℃ are preferred; comparative calcination times of 3, 5, 10h, 3h are preferred. In summary, the following steps: 1g SnCl4·5H2The preparation process of dissolving O crystal in 120mL of pure water, 10g of glucose, hydrothermal at 190 ℃ for 18h and calcining at 500 ℃ for 3h is the best example, namely example 1.
The present invention provides a tin dioxide carbon nano composite, a preparation method thereof, and thinking and a method for applying the same, and a plurality of methods and ways for implementing the technical scheme, and the above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, a plurality of improvements and embellishments can be made without departing from the principle of the present invention, and these improvements and embellishments should also be regarded as the protection scope of the present invention. All the components not specified in the present embodiment can be realized by the prior art.

Claims (2)

1. A preparation method of an aluminum ion battery anode material is characterized by comprising the following steps: mixing a tin dioxide carbon nano composite, polyvinylidene fluoride and super phosphorus carbon black according to a mass ratio of 80:10:10, dispersing the mixture in a solvent, and then coating the solvent on a light molybdenum foil with the thickness of 20-50 microns;
the preparation method of the tin dioxide carbon nano composite comprises the following steps:
(1) 1g of SnCl is taken4·5H2Dissolving the O crystal in 120mL of deionized water, heating the obtained water solution to 190 ℃, keeping the temperature for 18 hours to obtain a first mixed solution, and cooling the first mixed solution to room temperature;
(2) adding 10g of glucose into the first mixed solution cooled in the step (1), stirring and dissolving, heating to 190 ℃, keeping for 18 hours to obtain a second mixed solution, and cooling to room temperature;
(3) centrifuging the second mixed solution cooled in the step (2) at 1000 revolutions per minute, taking the precipitate, cooling to room temperature, then placing at 500 ℃ and calcining for 3 hours in an argon atmosphere to obtain the tin dioxide carbon nano composite, wherein the particle size of the tin dioxide carbon nano composite is 50nm, and the specific surface area of the tin dioxide carbon nano composite is 204.8m2 g-1。
2. The method for preparing the positive electrode material for the aluminum-ion battery according to claim 1, wherein the solvent is N-methylpyrrolidone; wherein the mass-volume ratio of the polyvinylidene fluoride to the N-methyl pyrrolidone is 0.5-100 mg/ml.
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CN107482218A (en) * 2017-07-18 2017-12-15 中国科学院化学研究所 A kind of three-dimensional hollow material and preparation method thereof and the application in electrochemical energy storing device

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