CN107275578B - Method for manufacturing potassium ion battery cathode by adopting nitrogen-doped porous carbon material - Google Patents
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Abstract
A method for manufacturing a potassium ion battery cathode by adopting a nitrogen-doped porous carbon material belongs to a method for manufacturing a potassium ion battery cathode. Firstly, preparing a nitrogen-doped porous carbon material, regulating and controlling technical parameters in a reaction process by adopting a simple and easily-obtained high-temperature solid-phase sintering method to prepare a nitrogen-doped porous carbon material structure, and then manufacturing a potassium ion battery cathode by adopting the nitrogen-doped porous carbon material; dissolving a nitrogen source in a solvent to form a transparent solution, adding a proper amount of carbon source into the solution, and stirring and continuously adding the solvent to fully and uniformly diffuse the nitrogen source to obtain a white product; drying the white product in a freeze dryer for 3-10 hours, transferring the dried product into a crucible, heating the product to 350-1200 ℃ at the speed of 1-10 ℃/min in an argon atmosphere in a vacuum tube furnace, preserving the heat for 3-6 hours, and separating and purifying the generated product to obtain the target product. The potassium ion battery cathode has excellent electrochemical performance, low raw material price, simple synthesis method, high controllability of operation steps and easy expanded production.
Description
Technical Field
The invention relates to a method for manufacturing a potassium ion battery cathode, in particular to a method for manufacturing a potassium ion battery cathode by adopting a nitrogen-doped porous carbon material.
Background
Lithium ion batteries have the outstanding advantages of high energy density, long cycle life, no pollution and the like, have become the mainstream of the battery market, and are beginning to be applied to driving electric vehicles. However, with the large-scale application of lithium ion batteries, the price and the resource limitation of lithium are worried more and more. In recent years, many new alternative energy storage batteries have been produced and developed rapidly, mainly including secondary batteries of sodium ions, potassium ions, magnesium ions, calcium ions and the like. The potassium ion battery has many advantages, wherein the potassium source is cheap, the content of the potassium source in the earth crust is rich, the standard reduction potential of the potassium ion battery is closest to that of the lithium ion battery, so that the energy density is high, and the electrochemical activity of the electrolyte of the potassium ion battery is high, so that the electrolyte is beneficial to the transmission of ions and electrons. At present, less negative electrode materials of the potassium ion battery are reported, wherein the carbon material has lower de-intercalation potassium potential and is easy to form dendrite to cause potential safety hazard. Therefore, the development of a novel potassium ion battery which is green and environment-friendly, has a stable structure, is suitable for an electrochemical potassium deintercalation platform and has a large specific capacity has very important significance.
Recently, nitrogen doping of carbon materials has attracted extensive attention by researchers, as nitrogen doping is an effective method for improving the electrochemical performance of carbon materials in devices such as potassium ion batteries and supercapacitors. Nitrogen doping is very attractive for the following reasons. Firstly, nitrogen atoms are smaller than carbon atoms and have strong electronegativity, and the nitrogen atom doping can enhance the combination between the doped carbon material and potassium, thereby being beneficial to the embedding of potassium ions; secondly, nitrogen is doped into a graphite carbon structure (such as a carbon nanotube) to form an effective method of N-type doping, so that the conductivity of the carbon material can be improved. Finally, nitrogen doping causes a number of defects in the carbon structure that provide more active sites for potassium storage.
However, the traditional preparation method of nitrogen-doped porous carbon mainly adopts NH3Post-treatment methods such as plasma or hydrazine introduce nitrogen atoms into the carbon material. However, most of these methods are complicated, and the content of nitrogen atoms to be doped is limited, so that uniform and controllable doping is difficult to achieve. However, the preparation method of the nitrogen-doped carbon material with good chemical component uniformity, high purity and regular microstructure has not been reported so far, which greatly restricts the further application of the potassium ion battery cathode material.
Disclosure of Invention
The invention aims to provide a method for manufacturing a potassium ion battery cathode by adopting a nitrogen-doped porous carbon material, which has the advantages of easily obtained raw materials, simple synthesis method and high controllability of operation steps.
The purpose of the invention is realized as follows: the preparation method of the potassium ion battery negative electrode comprises the following steps: firstly, preparing a nitrogen-doped porous carbon material, regulating and controlling technical parameters in a reaction process by adopting a simple and easily-obtained high-temperature solid-phase sintering method to prepare a nitrogen-doped porous carbon material structure, and then manufacturing a potassium ion battery cathode by adopting the nitrogen-doped porous carbon material.
The preparation method of the potassium ion battery cathode comprises the following specific steps:
(1) dispersing the prepared nitrogen-doped porous carbon material, the conductive carbon black and the binding agent polyvinylidene fluoride in an N-methyl pyrrolidone solution according to the mass ratio of 70: 20: 10 to prepare slurry, and uniformly coating the slurry on a copper foil current collector; drying the coated electrode slice in a forced air drying oven at 50 +/-20 ℃ to obtain the electrode slice;
(2) cutting the obtained electrode plate into a circular electrode with the diameter of 14 mm, pressing the electrode plate by using a powder press, then placing the electrode plate in a vacuum oven for drying at 120 ℃ for 12 hours, and then transferring the electrode plate into a special glove box for placing for 24 hours to obtain a potassium ion battery electrode plate; the powder press was at a pressure of 15 mpa.
The preparation method of the nitrogen-doped porous carbon material comprises the following steps:
(1) dissolving a nitrogen source in a solvent, wherein the mass ratio of the nitrogen source to the solvent is 1: 2-5, and preparing a transparent solution; adding a carbon source into the solution, wherein the mass ratio of the solution to the carbon source is 1: 0.8-2, and forming a white substance;
(2) drying the white substance in a freeze dryer for 3-10 hours to obtain an initial product;
(3) and (3) heating the initial product obtained in the step (2) to 350-1200 ℃ at the speed of 1-10 ℃/min in an argon atmosphere in a vacuum tube furnace, preserving the heat for 3-6 hours, and then separating and purifying to obtain the nitrogen-doped porous carbon material.
The nitrogen source is ammonium salt, ammonium carbonate ((NH)4)2CO3) Ammonium hydrogen carbonate (NH)4HCO3) Ammonium chloride (NH)4Cl) or urea (CO (NH)2)2) One of (1); preferably, the nitrogen source is ammonium chloride (NH)4Cl) or urea (CO (NH)2)2)。
The solvent is deionized water or ethanol.
The carbon source is a modified highly water-soluble polymer (polyacrylic resin).
And (4) performing separation and purification in the step (3) by centrifugation or suction filtration through a Buchner funnel, and repeatedly washing with deionized water.
Testing the electrode plates of the potassium ion battery:
assembling the electrode plates, the diaphragm and the potassium plate into a button cell by a conventional method in an argon-filled environment, and testing constant-current charge-discharge capacity and cycle performance;
and (3) test results: under the current condition of 50 milliampere/gram, the first discharge capacity and the second discharge capacity of the nitrogen-doped porous carbon material are 1153 and 533 milliampere hour/gram respectively, and the subsequent capacity tends to be stable and fully shows high specific capacity.
Has the advantages that: by adopting the scheme, the nitrogen-doped porous carbon material is prepared for the first time, the used raw materials are easy to obtain, the preparation method is simple, the operation is easy, and the product has high purity, narrow particle size distribution and regular appearance and is easy for large-scale industrial production. Meanwhile, the structural material shows excellent electrochemical performance as a potassium ion battery cathode material, overcomes the defect of low specific capacity of the traditional carbon cathode material for a commercial potassium ion battery, has excellent cycling stability which is not possessed by the traditional transition metal oxide cathode material, and has a guiding effect on the development of a novel potassium ion battery.
The advantages are that: the raw materials used are easy to obtain, the synthesis method is simple, the controllability of the operation steps is high, and the obtained product has high purity and uniform particle size and is easy to expand production. Meanwhile, the porous structure material is used as a negative electrode material of a potassium ion battery and shows excellent electrochemical performance.
Description of the drawings:
FIG. 1 is a powder X-ray powder diffraction pattern diagram of a nitrogen-doped porous carbon material in example 1 of the present invention.
Fig. 2 is a scanning electron micrograph of nitrogen-doped porous carbon according to example 1 of the present invention.
Fig. 3 is a charge-discharge curve diagram of the nitrogen-doped porous carbon material at a constant current density of 50 ma/g in example 1 of the present invention.
Detailed Description
The preparation method of the potassium ion battery negative electrode comprises the following steps: firstly, preparing a nitrogen-doped porous carbon material, regulating and controlling technical parameters in a reaction process by adopting a simple and easily-obtained high-temperature solid-phase sintering method to prepare a nitrogen-doped porous carbon material structure, and then manufacturing a potassium ion battery cathode by adopting the nitrogen-doped porous carbon material.
The preparation method of the potassium ion battery cathode comprises the following specific steps:
(1) dispersing the prepared nitrogen-doped porous carbon material, conductive carbon black, graphite and a binder polyvinylidene fluoride in an N-methyl pyrrolidone solution according to the mass ratio of 70: 20: 10 to prepare slurry, and uniformly coating the slurry on a copper foil current collector; drying the coated electrode slice in a forced air drying oven at 50 +/-20 ℃ to obtain the electrode slice;
(2) cutting the obtained electrode plate into a circular electrode with the diameter of 14 mm, pressing the electrode plate by using a powder press, then placing the electrode plate in a vacuum oven for drying at 120 ℃ for 12 hours, and then transferring the electrode plate into a special glove box for placing for 24 hours to obtain a potassium ion battery electrode plate; the powder press was at a pressure of 15 mpa.
The preparation method of the nitrogen-doped porous carbon material comprises the following steps:
(1) dissolving a nitrogen source in a solvent, wherein the mass ratio of the nitrogen source to the solvent is 1: 2-5, and preparing a transparent solution; adding a carbon source into the solution, wherein the mass ratio of the solution to the carbon source is 1: 0.8-2, and forming a white substance;
(2) drying the white substance in a freeze dryer for 3-10 hours to obtain an initial product;
(3) and (3) heating the initial product obtained in the step (2) to 350-1200 ℃ at the speed of 1-10 ℃/min in an argon atmosphere in a vacuum tube furnace, preserving the heat for 3-6 hours, and then separating and purifying to obtain the nitrogen-doped porous carbon material.
The nitrogen source is ammonium salt, ammonium carbonate ((NH)4)2CO3) Ammonium hydrogen carbonate (NH)4HCO3) Ammonium chloride (NH)4Cl) or urea (CO (NH)2)2) Preferably, the nitrogen source is ammonium chloride (NH)4Cl) or urea (CO (NH)2)2)；
The solvent is deionized water or ethanol;
the carbon source is a modified highly water-soluble polymer (polyacrylic resin).
And (4) performing separation and purification in the step (3) by centrifugation or suction filtration through a Buchner funnel, and repeatedly washing with deionized water.
Testing the electrode plates of the potassium ion battery:
assembling the electrode plates, the diaphragm and the potassium plate into a button cell by a conventional method in an argon-filled environment, and testing constant-current charge-discharge capacity and cycle performance;
and (3) test results: under the current condition of 50 milliampere/gram, the first discharge capacity and the second discharge capacity of the nitrogen-doped porous carbon material are 1153 and 533 milliampere hour/gram respectively, and the subsequent capacity tends to be stable and fully shows high specific capacity.
Example 1: preparation and structural characterization of nitrogen-doped porous carbon material
Take 0.3g NH4Placing Cl into a beaker, adding 1ml of deionized water, carrying out ultrasonic oscillation to prepare a transparent solution, adding 1.2g of a highly water-soluble polymer (polyacrylic resin) into the transparent solution, and carrying out ultrasonic stirring while adding; finally, deionized water was slowly added until a fluffy white substance was formed. The material was transferred to a lyophilizer and dried for 10 hours to give a white powder. After drying, taking a proper amount of powder, placing the powder in a crucible, heating the powder to 850 ℃ at the speed of 3 ℃/min under the argon atmosphere in a vacuum tube furnace, preserving the heat for 5 hours, and removing a generated black productRepeatedly washing with ionized water, vacuum filtering with Buchner funnel, and drying to obtain black powder, which is processed by Bruker D8ADVANCE Germany X-ray powder diffractometer with Cu K α ray (wavelength)
The scanning pace is 0.08 degree/second) is identified as a disordered carbon material (figure 1), the nitrogen-doped porous carbon material has a broadened diffraction peak at about 24 degrees, and no other impurity peak appears corresponding to a (002) plane of a graphite type structure.
FIG. 1 is a powder X-ray powder diffraction pattern of nitrogen-doped porous carbon; where the left ordinate is the relative Intensity (Intensity) and the abscissa is the diffraction angle (2 θ).
The morphology of the nitrogen-doped porous carbon nanoparticles is observed by adopting a JSF-6700 scanning electron microscope, and as shown in figure 2, the nitrogen-doped porous carbon mainly consists of nanoparticles with the particle size distribution of about 200nm, and is uniform in size and narrow in size distribution.
And (3) electrochemical performance testing: respectively weighing a nitrogen-doped carbon material, conductive graphite and polyvinylidene fluoride according to the weight ratio of 70: 20: 10, mixing a binder polyvinylidene fluoride and an N-methyl pyrrolidone solution solvent according to a certain ratio, then carrying out ball milling for 2 hours, adding an active material and a binder solution into a ball milling tank according to a certain ratio, and carrying out ball milling for 2 hours to obtain electrode slurry; uniformly coating the slurry on a copper foil current collector; drying the coated electrode slice in a forced air drying oven at 50 +/-20 ℃; cutting the obtained electrode slice according to a preset size, pressing the electrode slice by using a powder press (the pressure is 15 MPa), drying the electrode slice in a vacuum oven at 120 ℃ for 12 hours, and then transferring the electrode slice into a glove box to be placed for 24 hours for use; and assembling the electrode plates, the diaphragm and the potassium plate into a button cell by a conventional method in a glove box filled with argon, and carrying out constant-current charging and discharging capacity. The electrochemical performance is shown in fig. 3.
Example 2: take 0.3g NH4Putting Cl into a beaker, adding 1ml of deionized water, performing ultrasonic oscillation to prepare a transparent solution, adding 1.2g of highly water-soluble polymer (polyacrylic resin) into the transparent solution one gram by one gram, and performing ultrasonic stirring while adding; finally slowly addDeionized water was added until a fluffy white mass was formed. The above material was transferred to a freeze dryer and dried for 10 hours to obtain a white dry powder. And after drying, putting a proper amount of powder into a crucible, heating to 650 ℃ at the speed of 3 ℃/min under the argon atmosphere in a vacuum tube furnace, preserving the heat for 5 hours, repeatedly washing the generated black product by deionized water, performing suction filtration by using a Buchner funnel, and drying to obtain a black powder product.
The obtained superfine powder is an amorphous carbon structure of a nitrogen-doped porous carbon material, and the product is composed of nano particles with the average particle size of about 170 nm.
Example 3: 0.5g of CO (NH) was taken2)2Putting into a beaker, adding 1ml of deionized water, ultrasonically oscillating to prepare a transparent solution, adding 1g of highly water-soluble polymer (polyacrylic resin) into the transparent solution, and ultrasonically stirring while adding; finally, deionized water was slowly added until a fluffy white substance was formed. Transferring the above materials to a freeze dryer, and drying for 10 hr to obtain white powder. After drying, taking a proper amount of the black powder, putting the black powder into a crucible, heating the crucible to 650 ℃ at the speed of 3 ℃/min under the argon atmosphere in a vacuum tube furnace, preserving the heat for 5 hours, repeatedly washing the generated black product by deionized water, and performing suction filtration and drying by a Buchner funnel to obtain a black powder product.
The obtained superfine powder is an amorphous carbon structure of a nitrogen-doped porous carbon material and consists of nano particles with the average particle size of about 200 nm.
Claims (3)
1. A method for manufacturing a potassium ion battery cathode by adopting a nitrogen-doped porous carbon material is characterized by comprising the following steps: the preparation method of the potassium ion battery negative electrode comprises the following steps: firstly, preparing a nitrogen-doped porous carbon material, regulating and controlling technical parameters in a reaction process by adopting a simple and easily-obtained high-temperature solid-phase sintering method to prepare a nitrogen-doped porous carbon material structure, and then manufacturing a potassium ion battery cathode by adopting the nitrogen-doped porous carbon material;
the method comprises the following specific steps:
(1) dispersing the prepared nitrogen-doped porous carbon material, the conductive carbon black and the binding agent polyvinylidene fluoride in an N-methyl pyrrolidone solution according to the mass ratio of 70: 20: 10 to prepare slurry, and uniformly coating the slurry on a copper foil current collector; drying the coated electrode slice in a forced air drying oven at 50 +/-20 ℃ to obtain the electrode slice;
(2) cutting the obtained electrode plate into a circular electrode with the diameter of 14 mm, pressing the electrode plate by using a powder press, then placing the electrode plate in a vacuum oven for drying at 120 ℃ for 12 hours, and then transferring the electrode plate into a special glove box for placing for 24 hours to obtain a potassium ion battery electrode plate; the pressure of the powder press is 15 MPa;
the preparation method of the nitrogen-doped porous carbon material comprises the following steps:
(1) dissolving a nitrogen source in a solvent, wherein the mass ratio of the nitrogen source to the solvent is 1: 2-5, and preparing a transparent solution; adding a carbon source into the solution, wherein the mass ratio of the solution to the carbon source is 1: 0.8-2, and forming a white substance;
(2) drying the white substance in a freeze dryer for 3-10 hours to obtain an initial product;
(3) heating the initial product obtained in the step (2) to 350-1200 ℃ at the speed of 1-10 ℃/min in an argon atmosphere in a vacuum tube furnace, preserving the temperature for 3-6 hours, and then separating and purifying to obtain the nitrogen-doped porous carbon material;
the nitrogen source is ammonium salt, ammonium carbonate ((NH)4）2CO3) Ammonium hydrogen carbonate (NH)4HCO3) Ammonium chloride (NH)4Cl) or urea (CO (NH)2)2) One of (1);
the carbon source is a modified highly water-soluble polymer, namely: polyacrylic acid resin.
2. The method for manufacturing the potassium ion battery cathode by adopting the nitrogen-doped porous carbon material as claimed in claim 1, is characterized in that: the solvent is deionized water or ethanol.
3. The method for manufacturing the potassium ion battery cathode by adopting the nitrogen-doped porous carbon material as claimed in claim 1, is characterized in that: and (3) separating and purifying by centrifugation or suction filtration of a Buchner funnel, and repeatedly washing by deionized water.
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| CN107555412A (en) * | 2017-09-07 | 2018-01-09 | 江苏福瑞士电池科技有限公司 | A kind of preparation method of N doping porous carbon and its application on lithium ion battery |
| CN107768645B (en) * | 2017-11-28 | 2020-07-14 | 吉林大学 | Porous nitrogen-doped carbon nanosheet composite negative electrode material and preparation method thereof |
| CN108598419A (en) * | 2018-04-24 | 2018-09-28 | 珠海光宇电池有限公司 | A kind of lithium carbon compound cathode piece and preparation method thereof and lithium secondary battery |
| CN109301220A (en) * | 2018-10-10 | 2019-02-01 | 东北大学秦皇岛分校 | A kind of N doping hard carbon material, preparation method and its kalium ion battery as cathode |
| CN109768235A (en) * | 2018-12-24 | 2019-05-17 | 肇庆市华师大光电产业研究院 | A kind of lithium ion battery negative material and preparation method thereof |
| CN109742384B (en) * | 2019-01-07 | 2021-05-11 | 中国矿业大学 | Method for using biomass porous carbon as potassium ion battery cathode |
| CN111682205A (en) * | 2020-05-30 | 2020-09-18 | 中国海洋大学 | Method for preparing bubble-cushion-like porous carbon material with assistance of double-salt crystal template and potassium storage application of bubble-cushion-like porous carbon material |
| CN113381018B (en) * | 2021-04-20 | 2022-08-16 | 南昌航空大学 | Nitrogen-fluorine atom doped three-dimensional porous carbon electrode material, preparation method and application thereof |
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