CN113921825A - Preparation and calibration method of anti-seepage conductive graphite plate for aqueous solution battery - Google Patents

Preparation and calibration method of anti-seepage conductive graphite plate for aqueous solution battery Download PDF

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Publication number
CN113921825A
CN113921825A CN202111176291.6A CN202111176291A CN113921825A CN 113921825 A CN113921825 A CN 113921825A CN 202111176291 A CN202111176291 A CN 202111176291A CN 113921825 A CN113921825 A CN 113921825A
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graphite plate
aqueous solution
solution battery
conductive graphite
contact angle
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徐少辉
孙若晨
王连卫
熊大元
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East China Normal University
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East China Normal University
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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
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/663—Selection of materials containing carbon or carbonaceous materials as conductive part, e.g. graphite, carbon fibres
    • 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
    • H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
    • 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
    • H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
    • H01M10/38—Construction or manufacture
    • 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
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/665—Composites
    • 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
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/668—Composites of electroconductive material and synthetic resins
    • 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
    • H01M4/64—Carriers or collectors
    • H01M4/70—Carriers or collectors characterised by shape or form
    • H01M4/80—Porous plates, e.g. sintered carriers
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a preparation and calibration method of an impermeable conductive graphite plate applied to an aqueous solution battery. The preparation and calibration method of the anti-seepage conductive graphite plate comprises the following steps: firstly, melting the organic matter at high temperature (or in a pressurized environment); secondly, soaking the graphite plate material; thirdly, polishing, washing and vacuum drying; and fourthly, observing the liquid seepage prevention effect by using a contact angle measuring instrument. By means of the technical scheme, the conductive graphite plate with high conductivity and liquid seepage prevention function is produced and can be used for an aqueous solution battery. Compared with the prior art, the water solution battery conductive graphite plate manufactured by the structure can utilize the excellent conductive performance of the water solution battery to improve the energy efficiency of the water solution battery, and the graphite plate coated by the organic matter can prevent liquid seepage, can prolong the service life of the battery, and is beneficial to expanding the application range of the water solution battery.

Description

Preparation and calibration method of anti-seepage conductive graphite plate for aqueous solution battery
Technical Field
The invention belongs to the field of aqueous solution battery energy storage, and relates to a method for permeating organic matters into a graphite plate and a method for measuring the effect of an impermeable solution by using a contact angle.
Background
The vigorous development of the green energy economy has prompted the evolutionary development of large-scale renewable energy acquisition and storage systems. Compared with lithium ion batteries which dominate the market, aqueous batteries are safer than non-aqueous lithium ion, sodium ion and potassium ion batteries of currently used organic electrolytes, and aqueous electrolytes also show great competitiveness, (1) the cost is low, no oxygen and dry assembly lines are needed, and the electrolyte and manufacturing cost are reduced; (2) environmental benefits, due to the non-volatility of water, exhibiting non-toxicity and non-flammability; (3) the ability to charge rapidly and with high power density due to the high ionic conductivity of aqueous media; (4) the high resistance to electrical and mechanical mishandling, i.e. the conditions after rapid discharge, bending, cutting and cleaning, does not cause any catastrophic consequences. Although various types of aqueous batteries have been successfully produced so far, aqueous ion secondary batteries still have a great space for development and progress. In particular, in recent years, with the development of materials and the improvement of electrochemical performance, water-based batteries have been receiving attention as an ideal energy storage device to select, particularly, for large-scale energy storage.
Carbon-based materials are often used as current collectors in the preparation of water-based batteries, such as graphite rods or graphite plates, but in the practice of assembling batteries, it is found that the aqueous solution gradually seeps out of the battery along with the pores of the graphite rods or graphite plates, so that (1) the working aqueous solution is reduced, the solution dries up, and the battery performance is rapidly attenuated; (2) the leaked aqueous solution destroys the electrodes, short-circuiting the battery; (3) the leaked aqueous solution can corrode the surface of the battery and other devices, and the battery is finally scrapped. The problem of how to improve and control the liquid seepage of the graphite rod or the graphite plate is a problem which needs to be solved in the process. Meanwhile, the problem of liquid seepage is a long process, the water solution gradually seeps out through the pores of the graphite rod or the graphite plate, and how to detect and monitor the liquid seepage process is also a problem. Based on the practical problems, the method is provided for preventing the leakage process of the aqueous solution by permeating a certain amount of non-conductive organic matters into the pores of the conductive graphite rod or the graphite plate, and determining the leakage effect of the aqueous solution by utilizing the contact angle with the aqueous solution and the change of the contact angle with time.
Disclosure of Invention
The invention aims to provide a preparation and calibration method of an impermeable conductive graphite plate for an aqueous solution battery, which solves the technical problems in the prior art. The invention makes organic matter permeate into the pores of the conductive graphite rod or the graphite plate to block the seepage process of the aqueous solution, and judges the seepage effect of the graphite rod or the graphite plate on the aqueous solution by utilizing the size of the contact angle with the aqueous solution and the change of the contact angle with time.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for preventing the leakage of aqueous solution by permeating organic substance into the pores of conductive graphite rod or graphite plate features that the high-temp fusing and pressurizing method of organic substance is used, and the impervious conductive graphite plate is prepared by such steps as preparing a conductive graphite plate with high electric conductivity and impervious liquid function, increasing the contact angle of aqueous solution from 45 deg. to over 100 deg. and decreasing the variation of contact angle with time. By means of the technical scheme, the conductive graphite plate with high conductivity and liquid seepage prevention function can be used for an aqueous solution battery.
A preparation and calibration method of an impermeable conductive graphite plate for an aqueous solution battery comprises the following steps:
(1) cutting a graphite plate into small pieces of 1cm multiplied by 1cm as a base material, ultrasonically cleaning the small pieces in ethanol and deionized water, and then drying the small pieces for 24 hours at the temperature of 60 ℃;
(2) the preparation of the organic matter by high-temperature melting (60-90 ℃) can be realized in the atmospheric environment, and the high-temperature melting (60-90 ℃) of the organic matter can also be realized in the pressurized environment;
(3) soaking the graphite plate cleaned in the step (1) in the organic matter prepared in the step (2) for 4-60min to form an organic matter infiltration layer on the surface of the graphite plate, and then drying at room temperature;
(4) cutting off redundant organic matters on the surface by using a scraper, and judging the surface treatment process of the organic matters by taking the conductivity of the measured graphite plate as a standard;
(5) cleaning the conductive graphite plate composite material infiltrated by the organic matters obtained in the step (4), and drying at 60 ℃ for 24 h;
(6) the effect of liquid permeation prevention was observed with a contact angle measuring instrument. And measuring the contact angles of different solutions and the graphite plate and the change process along with time to judge the liquid seepage prevention effect of the graphite plate.
In the step (2), the organic substance may be a polymer organic material such as PVDF, paraffin, PVA, or the like.
In the step (2) and the step (3), the graphite plate is treated by a high-temperature molten organic matter, which can be in an atmospheric environment or a pressurized environment, and the soaking time is 4 to 60 minutes.
In the step (2) and the step (3), the graphite plate is treated by high-temperature molten organic matters, and the soaking time is 4 to 60 minutes.
In the step (5), the impermeable conductive graphite plate is dried for 24 hours at 60 ℃ in the cleaning process.
In the step (6), the contact angle measuring instrument is used for observing the liquid seepage prevention effect, and the seepage prevention function of the conductive graphite plate is quantified through the change slope of the contact angle and the change slope of the contact angle along with time.
Compared with the prior art, the invention has the following beneficial effects:
the method for heating and melting the organic matter to soak the graphite plate effectively realizes that the organic matter permeates into the pores of the conductive graphite rod or the graphite plate to prevent the leakage of the aqueous solution, and has the advantages of simple operation, low cost and good reproducibility.
The method for synthesizing the graphite plate by heating and melting the organic matters to soak the graphite plate and infiltrating the organic matters under pressure is convenient to operate and uniform in infiltration of the organic matters.
The organic matter treated graphite plate prepared by the invention has the effect of preventing the leakage of the aqueous solution, and is quantitatively calibrated by measuring the contact angle of the electrode and the aqueous solution by using a contact angle measuring instrument and the change of the contact angle along with time. The method simply and visually calibrates the anti-seepage effect.
Drawings
FIG. 1 is a diagram of an apparatus for processing graphite plates.
In the figure, 1-glass container; 2-molten paraffin; 3-graphite plates; 4-gas circuit switch; 5-a gas path leading to the mechanical pump;
fig. 2 is a high magnification optical microscope photograph of an untreated graphite plate (top left) and a graphite plate (bottom right) after immersion in heated molten paraffin for 4 minutes (top right), 10 minutes (bottom left) and 20 minutes.
Fig. 3 is a graph showing the amount of paraffin infiltrated into the graphite plate as a function of soaking time.
Figure 4 is a plot of the amount of conductivity of the graphite plate after paraffin penetration as a function of soak time.
Fig. 5 shows the results of the contact angle test for an aqueous solution of untreated graphite plates (left panel) and after 60 minutes (right panel).
Fig. 6 shows the test results of the contact angle of the graphite plate with an aqueous solution after being soaked in the heated molten paraffin for 12 minutes (left panel) and the contact angle after 60 minutes (right panel).
Fig. 7 shows a high magnification optical micrograph of the graphite plate after pressure infiltration with paraffin (top), and the contact angle of an aqueous solution on the surface of this graphite plate (bottom).
FIG. 8 is a contact angle change curve of the surface of the treated graphite plate after the graphite plate is pressurized and infiltrated with paraffin and the aqueous solution is in 150 seconds.
Fig. 9 shows the contact angle change curves of untreated graphite plates (upper panel) and paraffin-treated graphite plates (lower panel) in an aqueous solution of zinc iodide at 1 mol/l.
Fig. 10 shows the contact angle change curves for an untreated graphite plate (top) and a paraffin-treated graphite plate (bottom) in a 1-mole per liter aqueous solution of zinc bromide.
Detailed Description
The present invention will be further described with reference to the accompanying drawings, which will become apparent to those skilled in the art.
As shown in fig. 1, comprising a closed glass vessel containing molten paraffin in which graphite plates are immersed; the top of the glass container is provided with an air path leading to the mechanical pump, and the air path is provided with an air path switch.
Example 1: paraffin soaking infiltration of graphite plates
The method for heating and melting the organic matter to soak the graphite plate effectively realizes that the organic matter permeates into the pores of the conductive graphite rod or the graphite plate. And cleaning and drying the cut graphite plate, wherein the cleaning is ultrasonic cleaning in ethanol and deionized water, and then drying for 24 hours at 60 ℃. Paraffin is put into a specially designed quartz beaker (as shown in figure 1), the paraffin in the beaker is in a molten state by heating, the cleaned sample is put into the paraffin in the molten state, the graphite plate sample is taken out after different soaking times, and the organic part on the surface of the graphite plate is clearly visible after being scraped by a special tool (as shown in figure 2). The electrical conductivity of the graphite plate was measured to control the soaking time and the amount of paraffin penetration. It was found experimentally that the amount of paraffin infiltrated into the graphite plates did not increase monotonically over time (as shown in fig. 3), reaching a maximum at 20 minutes, and then the amount of paraffin infiltrated decreased inversely. In conjunction with the conductivity measurements (as shown in fig. 4), it was determined that a soaking time of about 10 minutes was most suitable, and the conductivity drop was not the greatest. In order to visually observe the leakage effect of a waterproof solution of a paraffin-treated graphite plate, the shape and stability of a water drop on the surface of a graphite plate electrode are observed by directly using a contact angle meter. The contact angle of the pure water solution on the surface of the untreated graphite plate was 47 degrees and rapidly decreased with time (as shown in fig. 5). After 60 minutes, the contact angle of the aqueous solution on the surface of the untreated graphite plate was only 20 degrees. And ten minutes after the graphite plate is treated by the paraffin, the contact angle of the aqueous solution on the surface of the treated graphite plate is 90 degrees, and the aqueous solution slowly decreases along with time (as shown in figure 6). After 60 minutes, the contact angle of the aqueous solution on the surface of the paraffin-treated graphite plate can be kept at 75 degrees. The organic matter is permeated into the pores of the conductive graphite rod or the graphite plate, and the leakage of the aqueous solution can be effectively prevented.
Example 2: paraffin soak infiltration under pressure of graphite plates
In order to more effectively realize the permeation of the organic matters into the pores of the conductive graphite rod or the graphite plate, the method for heating and melting the organic matters to soak the graphite plate under the pressurization condition is adopted, the pressurization effect of the sealed quartz container is realized through the mechanical pump, and the molten paraffin is convenient to permeate into the graphite plate. The high power optical microscope photograph shows that the paraffin portion of the surface of the graphite plate is still clearly visible (as shown in the upper panel of fig. 7). And ten minutes after the graphite plate is treated with paraffin under pressure, the contact angle of the aqueous solution on the surface of the treated graphite plate is 125 degrees (as shown in the lower graph of fig. 7), and the contact angle is reduced slowly along with the time. The contact angle of the aqueous solution on the surface of the graphite plate after the treatment is hardly reduced within 150 seconds (as shown in fig. 8).
Example 3
In order to better observe the anti-seepage effect of the paraffin-treated graphite plate obtained by the invention and effectively confirm that the graphite plate can be used for a specific aqueous solution battery, we observe the contact angle results of zinc iodide aqueous solutions with different concentrations. For high concentration zinc iodide aqueous solution (1 mol per liter), the contact angle at the surface of the untreated graphite plate was 28 degrees and rapidly decreased with time (as shown in the nine upper panels). After 120 minutes, the contact angle of the aqueous solution of zinc iodide on the surface of the untreated graphite plate was only 5 degrees. The initial contact angle of the aqueous solution of zinc iodide on the surface of the graphite plate after treatment was 100 degrees and decreased slowly with time (as shown in the lower graph of fig. 9). After 200 minutes, the contact angle of the aqueous solution on the surface of the paraffin-treated graphite plate can be kept at 90 degrees.
Example 4
In order to better observe the anti-seepage effect of the paraffin-treated graphite plate obtained by the invention and effectively confirm that the graphite plate can be used for a specific aqueous solution battery, we observe the contact angle results of zinc bromide aqueous solutions with different concentrations. For high concentrations of aqueous zinc bromide (1 mol per liter), the contact angle at the surface of the untreated graphite plate was 28 degrees and declined rapidly over time (as shown in the upper graph of fig. 10). After 100 minutes, the contact angle of the aqueous zinc bromide solution on the surface of the untreated graphite plate was only 15 degrees. The initial contact angle of the aqueous zinc bromide solution on the surface of the graphite plate after treatment was 90 degrees and declined relatively slowly over time (as shown in the lower graph of fig. 10). After 200 minutes, the contact angle of the aqueous solution on the surface of the paraffin-treated graphite plate can be kept at 80 degrees.
The present invention has been described in detail with reference to the embodiments, and it should be understood by those skilled in the art that various modifications and decorations, such as changes to carbon-based materials and changes to organic substances, etc., may be made without departing from the principle of the present invention, and such modifications and decorations should be regarded as the protection scope of the present invention.

Claims (6)

1. A preparation and calibration method of an impermeable conductive graphite plate for an aqueous solution battery is characterized by comprising the following steps:
(1) cutting a graphite plate into small pieces of 1cm multiplied by 1cm as a base material, ultrasonically cleaning the small pieces in ethanol and deionized water, and then drying the small pieces for 24 hours at the temperature of 60 ℃;
(2) the preparation of the organic matter by high-temperature melting (60-90 ℃) can be realized in the atmospheric environment, and the high-temperature melting (60-90 ℃) of the organic matter can also be realized in the pressurized environment;
(3) soaking the graphite plate cleaned in the step (1) in the organic matter prepared in the step (2) for 4-60min to form an organic matter infiltration layer on the surface of the graphite plate, and then drying at room temperature;
(4) cutting off redundant organic matters on the surface by using a scraper, and judging the surface treatment process of the organic matters by taking the conductivity of the measured graphite plate as a standard;
(5) cleaning the conductive graphite plate composite material infiltrated by the organic matters obtained in the step (4), and drying at 60 ℃ for 24 h;
(6) the effect of liquid permeation prevention was observed with a contact angle measuring instrument. And measuring the contact angles of different solutions and the graphite plate and the change process along with time to judge the liquid seepage prevention effect of the graphite plate.
2. The method for preparing and calibrating the impermeable conductive graphite sheet for the aqueous solution battery according to claim 1, wherein in the step (2), the organic substance can be a polymer organic material such as PVDF, paraffin, PVA, and the like.
3. The method for preparing and calibrating the impermeable conductive graphite sheet for the aqueous solution battery according to claim 1, wherein in the step (2) and the step (3), the graphite sheet is treated by a high-temperature molten organic matter, which can be in an atmospheric environment or a pressurized environment, and the soaking time is 4 to 60 minutes.
4. The method for preparing and calibrating a seepage-proofing conductive graphite plate for an aqueous solution battery as claimed in claim 1, wherein in the step (2) and the step (3), the graphite plate is treated by high-temperature molten organic matter, and the soaking time is 4 to 60 minutes.
5. The method for preparing and calibrating the impermeable conductive graphite sheet for the aqueous solution battery according to claim 1, wherein in the step (5), the impermeable conductive graphite sheet is dried at 60 ℃ for 24 hours in a cleaning process.
6. In the step (6), the contact angle measuring instrument is used for observing the liquid seepage prevention effect, and the seepage prevention function of the conductive graphite plate is quantified through the change slope of the contact angle and the change slope of the contact angle along with time.
CN202111176291.6A 2021-10-09 2021-10-09 Preparation and calibration method of anti-seepage conductive graphite plate for aqueous solution battery Pending CN113921825A (en)

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Publication number Priority date Publication date Assignee Title
CN1366356A (en) * 2001-10-30 2002-08-28 华南理工大学 Liquid leakage prevention method of zinc-air battery
CN101359745A (en) * 2007-08-02 2009-02-04 原子能委员会 Method of manufacturing a fuel cell on a porous medium
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WO2018136975A1 (en) * 2017-01-23 2018-07-26 eChemion, Inc. Manufacturing impervious bipolar materials from porous graphite
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CN108666594A (en) * 2018-04-03 2018-10-16 华东师范大学 A kind of bipolar plates manufacture craft
CN108666595A (en) * 2018-05-18 2018-10-16 深圳市晶特智造科技有限公司 A kind of graphite bi-polar plate surface texture optimization method
CN111718205A (en) * 2019-03-20 2020-09-29 山东工业陶瓷研究设计院有限公司 Porous wave-transparent material super-hydrophobic hole sealing layer and preparation method thereof

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Application publication date: 20220111