CN113594421A - Preparation method and application of electrolyte-treated laboratory potassium metal sheet - Google Patents
Preparation method and application of electrolyte-treated laboratory potassium metal sheet Download PDFInfo
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- CN113594421A CN113594421A CN202110709931.9A CN202110709931A CN113594421A CN 113594421 A CN113594421 A CN 113594421A CN 202110709931 A CN202110709931 A CN 202110709931A CN 113594421 A CN113594421 A CN 113594421A
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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
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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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
- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- 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 preparation method and application of a metal potassium sheet for a laboratory, which is processed by electrolyte, and belongs to the technical field of potassium ion batteries. When the battery is assembled, only the film coated on the surface of the battery needs to be removed. The method can simply and quickly prepare the potassium metal sheet, the prepared potassium sheet can be stored for a long time, the problems that the existing potassium metal sheet needs to be prepared for use at present and cannot be stored for a long time can be solved, the time consumed by the preparation of the potassium ion battery can be greatly shortened, the preparation difficulty is reduced, and the scientific research and the marketization application of potassium electricity can be effectively promoted.
Description
Technical Field
The invention relates to the technical field of potassium ion batteries, in particular to a preparation method and application of a laboratory potassium metal sheet treated by electrolyte.
Background
Since the successful development of lithium ion batteries by the company sony, japan in 1990, the lithium ion batteries have already been in a steady development stage through a high-speed development of several decades. In recent years, with the increasing proliferation of portable electronic products, energy storage devices, and electric/hybrid vehicles, more energy-dense, long-cycle-life, and environmentally compatible energy storage and conversion devices have begun to be mentioned. However, the lithium ion battery is restricted by the factors of insufficient lithium resource reserves and uneven global distribution, and cannot meet the increasing energy demands of people in the future.
Potassium ion batteries are considered as a substitute for the most potential lithium ion batteries, and have recently received attention from researchers. On one hand, potassium has physical/chemical properties similar to lithium, and meanwhile, the potassium ion battery is also considered to have a rocking chair storage mechanism similar to a lithium ion battery, which provides a good foundation for the research of the potassium ion battery. Moreover, the crust reserves of potassium resources are abundant, and the relative ratio of potassium ions to lithium ions is as follows: K/Li =23000ppm/20ppm, potassium element is widely distributed in land and sea in the form of salt, and main economic bodies around the world have important sylvite ores, so that the potassium sylvite ore is low in price and is expected to become a next-generation large-scale energy storage device. Further, potassium has a redox potential similar to that of lithium, and potassium can also be electrochemically intercalated/deintercalated from graphite layers to form graphite intercalation compounds. Safety due to potassium potassizing potential (0.2V vs. K)+the/K) is higher than that of lithium (0.1V vs. Li)+Li), the potassium ion battery is also considered to have higher safety.
However, the development of the potassium ion battery is still limited by multiple factors at present in a fundamental research stage. The chemical property of potassium is extremely active, and the potassium metal is soft and sticky and is difficult to process, so the existing preparation process of the potassium metal sheet is difficult to meet the industrialization requirement of the potassium ion battery in the future. At present, most of testers are used for preparation on site, and the preparation is difficult, the quality is not high, and the time and the labor are wasted. The specification, size and thickness of the prepared potassium metal sheet are difficult to unify, which greatly limits the scientific research and the marketization application of the potassium ion battery.
Therefore, a simple, convenient, efficient and feasible method for preparing the potassium metal sheet capable of being stored for a long time is urgently needed at present so as to meet the scientific research requirements and market applications of the future potassium ion battery.
Disclosure of Invention
The invention aims to provide a preparation method of a potassium metal sheet for a laboratory for electrolyte treatment and application thereof, and aims to provide an efficient and convenient preparation method of the potassium metal sheet by optimizing a preparation process of the potassium metal sheet so as to shorten the time consumed in the preparation process of a potassium ion battery and reduce the preparation difficulty of the potassium ion battery.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of electrolyte-treated laboratory potassium metal sheets comprises the following steps:
s1, wiping off residual kerosene on the surface of the purchased potassium metal block by using dust-free paper in a glove box filled with inert atmosphere;
s2, cutting off the oxide layer on the surface of the metal potassium block wiped clean by a stainless steel knife on the acrylic plate;
s3, transferring a set amount of electrolyte solution to be dripped on the surface of the potassium metal block pretreated in the step 2;
s4, manually rolling the potassium metal block dropwise added with the electrolyte in the step 3 to a metal sheet with a set thickness by means of a metal aluminum bar under the coating of the polyethylene film;
s5, cutting the metal sheet rolled in the step 4 into sheets with preset shapes and sizes by using a sheet punching device to obtain a potassium metal sheet;
and S6, again taking a set amount of electrolyte, dripping the electrolyte on the surface of the cut potassium metal sheet in the step 5, encapsulating the electrolyte by using a polyethylene film, and storing the electrolyte in an inert atmosphere.
The technical scheme of the invention is further improved as follows: in step 1 and step 6, the inertThe atmosphere is argon, wherein H2O and O2Are not more than 1 ppm.
The technical scheme of the invention is further improved as follows: in step 3 and step 6, the electrolyte is: 1M KPF6in DME =100% or 1M KFSI in EC: DEC =1:1 (V/V).
The technical scheme of the invention is further improved as follows: in the step 3 and the step 6, the dosage of the dropwise added electrolyte is 50-400 mu L, and the dosage of the electrolyte is controlled according to the size of the potassium metal sheet, so that the potassium metal sheet can be completely wetted.
The technical scheme of the invention is further improved as follows: in the step 4, the thickness of the metal potassium sheet is controlled by controlling the number of times of manual rolling.
The technical scheme of the invention is further improved as follows: in the step 5, the shape and the size of the potassium metal sheet are controlled by changing the shape and the size of the punching device.
The technical scheme of the invention is further improved as follows: the shape of the prepared potassium metal sheet is customized according to the form of the assembled battery.
The potassium metal sheet prepared by the preparation method of the electrolyte-treated laboratory potassium metal sheet can be applied to assembling of potassium ion batteries.
The technical scheme of the invention is further improved as follows: when the potassium ion battery is assembled, a corresponding number of the pre-encapsulated potassium metal sheets are taken out in a glove box, and the polyethylene films coated on the two side surfaces of the pre-encapsulated potassium metal sheets are removed, so that the potassium ion battery can be assembled.
The technical scheme of the invention is further improved as follows: when the button battery is assembled, the potassium metal sheet is cut into a round metal sheet with the diameter of 14mm or 16mm by using a button battery punching device.
Due to the adoption of the technical scheme, the invention has the technical progress that:
1. in the preparation process, electrolyte is dripped into the pretreated potassium metal block to wet the surface of the potassium metal block, and the potassium metal block is coated by virtue of the polyethylene film, so that the problems that the potassium metal sheet is easy to stick and difficult to process in the rolling process are really solved; in addition, the dropwise added electrolyte and the polyethylene film coated on the surface can also solve the problem that the potassium metal is easy to oxidize.
2. In order to ensure that the prepared potassium metal sheet can be stored for a long time and is convenient for subsequent experimental needs, the prepared potassium metal sheet is subjected to secondary electrolyte treatment and then is encapsulated by a polyethylene film, so that the prepared potassium metal sheet can be stored in a glove box filled with inert atmosphere for a long time and is convenient to take and use at any time.
3. The invention provides an efficient and convenient preparation method of the potassium metal sheet by optimizing the preparation method of the potassium metal sheet, shortens the time consumed by the preparation of the potassium ion battery, and reduces the preparation difficulty.
4. The invention can also flexibly regulate and control the thickness, size and shape of the metal potassium sheet, which has important significance for promoting scientific research and marketization application of potassium ion batteries.
5. The invention provides a novel preparation method of a potassium metal sheet for a laboratory, which is processed by electrolyte, aiming at the problem that the potassium metal sheet is difficult to prepare and store in the existing potassium ion battery research.
Drawings
FIG. 1 is a flow chart of the preparation process of the present invention.
Detailed Description
The invention is described in further detail below with reference to the following figures and examples:
as shown in fig. 1, experimental equipment and instruments used in the preparation method include a glove box, an acrylic plate, a stainless steel knife, a liquid-moving gun, a polyethylene film, a metal aluminum bar, a sheet punching device and the like; the method comprises the steps of rolling a potassium metal sheet to a certain thickness by using an electrolyte and a polyethylene film and then cutting the potassium metal sheet with a given shape and size by using a punching machine so as to meet the assembly requirement of the potassium ion battery.
Example 1
The electrolyte used in this example was 1M KPF6 in DME=100%。
A preparation method of electrolyte-treated laboratory potassium metal sheets comprises the following steps:
step 1, in a glove box filled with inert atmosphere (argon) (H)2O，O2<<1 ppm), taking out the potassium metal blocks, and wiping off kerosene remained on the surfaces of the potassium metal blocks by using dust-free paper;
step 2, on the acrylic plate, cutting off the oxide layer on the surface of the metal potassium block cleaned by the stainless steel knife;
step 3, using 200 microliter liquid-transfering gun to transfer a certain quantity of 1M KPF6in DME =100% is dripped on the surface of the pretreated metal potassium block;
step 4, manually rolling the metal potassium block to a metal sheet with a certain thickness by means of a metal aluminum bar under the coating of the polyethylene film;
step 5, cutting the rolled metal sheet into a metal wafer with the diameter of 14mm by using a button cell punching device to obtain a metal potassium sheet;
step 6, using 200 muL pipette to pipette a certain amount of 1M KPF again6in DME =100% was added dropwise to the surface of the cut potassium metal sheet, and the sheet was wrapped with a polyethylene film and stored under an inert atmosphere.
When the potassium ion battery is assembled, a corresponding number of pre-encapsulated potassium metal sheets are taken out of the glove box, and the polyethylene films coated on the surfaces of the two sides of the potassium metal sheets are removed, so that the potassium ion battery can be assembled.
Through comparative analysis: 1M KPF6in DME =100% treated metal potassium sheet has smooth and flat surface with metal luster, and is the same as the metal potassium sheet treated by not dripping electrolyte; after the potassium metal sheet is stored for two months, obvious oxidation phenomenon appears on the surface of the potassium metal sheet which is not added with the electrolyte, the metal luster is completely lost, and 1M KPF is added6in DME =100% treated potassium metal flake still had its more pronounced metallic luster seen.
Example 2
The electrolyte used in this example was 1M KFSI in DME = 100%.
A preparation method of electrolyte-treated laboratory potassium metal sheets comprises the following steps:
step 1In a glove box filled with inert gas (argon) (H)2O，O2<<1 ppm), taking out the potassium metal blocks, and wiping off kerosene remained on the surfaces of the potassium metal blocks by using dust-free paper;
step 2, on the acrylic plate, cutting off the oxide layer on the surface of the metal potassium block cleaned by the stainless steel knife;
step 3, using a 200-mu-L liquid-transferring gun to transfer a certain amount of 1M KFSI in DME =100% to be dripped on the surface of the pretreated metal potassium block;
step 4, manually rolling the metal potassium block to a metal sheet with a certain thickness by means of a metal aluminum bar under the coating of the polyethylene film;
step 5, cutting the rolled metal sheet into a metal wafer with the diameter of 14mm by using a button cell punching device to obtain a metal potassium sheet;
step 6, a certain amount of 1M KFSI in DME =100% was again pipetted with a 200 μ L pipette on the surface of the cut potassium metal sheet, encapsulated with a polyethylene film, and stored under an inert atmosphere.
When the potassium ion battery is assembled, a corresponding number of pre-encapsulated potassium metal sheets are taken out of the glove box, and the polyethylene films coated on the surfaces of the two sides of the potassium metal sheets are removed, so that the potassium ion battery can be assembled.
Through comparative analysis: the surface of the 1M KFSI in DME =100% treated metal potassium sheet is smooth and flat with metal luster, and is the same as the metal potassium sheet which is not treated by dropwise adding electrolyte; after the potassium metal sheet is stored for two months, the obvious oxidation phenomenon appears on the surface of the potassium metal sheet which is not added with the electrolyte, the metal luster is completely lost, and the obvious metal luster can still be seen on the potassium metal sheet which is added with 1M KFSI in DME =100% and is treated.
Example 3
The electrolyte used in this example was 1M KFSI in EC: DEC =1:1 (V/V).
A preparation method of electrolyte-treated laboratory potassium metal sheets comprises the following steps:
step 1, in a glove box filled with inert atmosphere (argon) (H)2O，O2<<1 ppm), taking out the potassium metal blockRemoving the residual kerosene on the surface of the metal potassium block by using dust-free paper;
step 2, on the acrylic plate, cutting off the oxide layer on the surface of the metal potassium block cleaned by the stainless steel knife;
step 3, using a 200-L liquid-transferring gun to transfer a certain amount of 1M KFSI in EC: DEC =1:1(V/V) to be dripped on the surface of the pretreated metal potassium block;
step 4, manually rolling the metal potassium block to a metal sheet with a certain thickness by means of a metal aluminum bar under the coating of the polyethylene film;
step 5, cutting the rolled metal sheet into a metal wafer with the diameter of 14mm by using a button cell punching device to obtain a metal potassium sheet;
and 6, using a 200-mu-L pipette to again pipette a certain amount of 1M KFSI in EC: DEC =1:1(V/V) electrolyte liquid drops on the surface of the cut potassium metal sheet, encapsulating the electrolyte liquid with a polyethylene film, and storing the electrolyte liquid under an inert atmosphere.
When the potassium ion battery is assembled, a corresponding number of pre-encapsulated potassium metal sheets are taken out of the glove box, and the polyethylene films coated on the surfaces of the two sides of the potassium metal sheets are removed, so that the potassium ion battery can be assembled.
Through comparative analysis: the surface of the potassium metal sheet treated by 1M KFSI in EC, DEC =1:1(V/V) is smooth and flat with metallic luster, and is the same as that of the potassium metal sheet not treated by dropping the electrolyte; after the potassium metal sheet is stored for two months, the obvious oxidation phenomenon appears on the surface of the potassium metal sheet which is not treated by the electrolyte, the metallic luster is completely lost, and the obvious metallic luster can still be seen on the potassium metal sheet which is treated by the electrolyte dropwise adding 1M KFSI in EC: DEC =1:1 (V/V).
In conclusion, in the preparation process, the electrolyte is dripped into the pretreated metal potassium block to wet the surface of the metal potassium block, and the metal potassium block is coated by the polyethylene film, so that the problems that the metal potassium sheet is easy to stick and difficult to process in the rolling process are really solved; the dropwise added electrolyte and the polyethylene film coated on the surface can also solve the problem that the potassium metal is easy to oxidize; the time consumed in the preparation process of the potassium ion battery is effectively shortened, and the preparation difficulty is reduced.
Finally, it should be noted that: the above examples of the present invention are merely examples for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention. Numerous obvious variations, adaptations and substitutions will occur to those skilled in the art without departing from the scope of the invention. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. A preparation method of a metal potassium sheet for a laboratory treated by electrolyte is characterized by comprising the following steps: the method comprises the following steps:
s1, wiping off residual kerosene on the surface of the purchased potassium metal block by using dust-free paper in a glove box filled with inert atmosphere;
s2, cutting off the oxide layer on the surface of the metal potassium block wiped clean by a stainless steel knife on the acrylic plate;
s3, transferring a set amount of electrolyte solution to be dripped on the surface of the potassium metal block pretreated in the step 2;
s4, manually rolling the potassium metal block dropwise added with the electrolyte in the step 3 to a metal sheet with a set thickness by means of a metal aluminum bar under the coating of the polyethylene film;
s5, cutting the metal sheet rolled in the step 4 into sheets with preset shapes and sizes by using a sheet punching device to obtain a potassium metal sheet;
and S6, again taking a set amount of electrolyte, dripping the electrolyte on the surface of the cut potassium metal sheet in the step 5, encapsulating the electrolyte by using a polyethylene film, and storing the electrolyte in an inert atmosphere.
2. The method for preparing the electrolyte-treated laboratory potassium metal sheet according to claim 1, wherein the electrolyte-treated laboratory potassium metal sheet is prepared by the following steps: in the step 1 and the step 6, the inert atmosphere is argon, wherein H2O and O2Are all less than 1 ppm.
3. A method as claimed in claim 1The preparation method of the metal potassium sheet for the laboratory treated by the electrolyte is characterized by comprising the following steps: in step 3 and step 6, the electrolyte is: 1M KPF6in DME =100% or 1M KFSI in EC: DEC =1:1 (V/V).
4. The method for preparing the electrolyte-treated laboratory potassium metal sheet according to claim 1, wherein the method comprises the following steps: in the step 3 and the step 6, the dosage of the dropwise added electrolyte is 50-400 mu L, and the dosage of the electrolyte is controlled according to the size of the potassium metal sheet, so that the potassium metal sheet can be completely wetted.
5. The method for preparing the electrolyte-treated laboratory potassium metal sheet according to claim 1, wherein the electrolyte-treated laboratory potassium metal sheet is prepared by the following steps: in the step 4, the thickness of the metal potassium sheet is controlled by controlling the number of times of manual rolling.
6. The method for preparing the electrolyte-treated laboratory potassium metal sheet according to claim 1, wherein the electrolyte-treated laboratory potassium metal sheet is prepared by the following steps: in the step 5, the shape and the size of the potassium metal sheet are controlled by changing the shape and the size of the punching device.
7. The method for preparing the electrolyte-treated laboratory potassium metal sheet according to claim 1, wherein the electrolyte-treated laboratory potassium metal sheet is prepared by the following steps: the shape of the prepared potassium metal sheet is customized according to the form of the assembled battery.
8. The potassium metal sheet prepared by the method for preparing electrolyte-treated laboratory potassium metal sheet according to any one of claims 1 to 7 can be used for assembling potassium ion batteries.
9. Use of an electrolyte treated laboratory potassium metal flake according to claim 8, characterized in that: when the potassium ion battery is assembled, a corresponding number of the pre-encapsulated potassium metal sheets are taken out in a glove box, and the polyethylene films coated on the two side surfaces of the pre-encapsulated potassium metal sheets are removed, so that the potassium ion battery can be assembled.
10. Use of an electrolyte treated laboratory potassium metal flake according to claim 8, characterized in that: when the button battery is assembled, the potassium metal sheet is cut into a round metal sheet with the diameter of 14mm or 16mm by using a button battery punching device.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104377349A (en) * | 2013-08-14 | 2015-02-25 | 苏州宝时得电动工具有限公司 | Lithium-embedded electrode material, preparation method thereof, electrode, and battery |
| CN104993094A (en) * | 2015-05-26 | 2015-10-21 | 广东烛光新能源科技有限公司 | Preparation method of metallic lithium strip and metallic lithium strip prepared by the same |
| CN109830656A (en) * | 2019-01-09 | 2019-05-31 | 清华大学 | A kind of preparation method of the lithium anode with solid-liquid compound interface layer |
| CN111653723A (en) * | 2020-05-22 | 2020-09-11 | 南京理工大学 | Preparation method and application method of metal sodium sheet and metal potassium sheet |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104377349A (en) * | 2013-08-14 | 2015-02-25 | 苏州宝时得电动工具有限公司 | Lithium-embedded electrode material, preparation method thereof, electrode, and battery |
| CN104993094A (en) * | 2015-05-26 | 2015-10-21 | 广东烛光新能源科技有限公司 | Preparation method of metallic lithium strip and metallic lithium strip prepared by the same |
| CN109830656A (en) * | 2019-01-09 | 2019-05-31 | 清华大学 | A kind of preparation method of the lithium anode with solid-liquid compound interface layer |
| CN111653723A (en) * | 2020-05-22 | 2020-09-11 | 南京理工大学 | Preparation method and application method of metal sodium sheet and metal potassium sheet |
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