CN110286148A - The method of electronic transport mechanism in nano wire film electrochemical device and in-situ study nano wire charge and discharge process - Google Patents

The method of electronic transport mechanism in nano wire film electrochemical device and in-situ study nano wire charge and discharge process Download PDF

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CN110286148A
CN110286148A CN201910300792.7A CN201910300792A CN110286148A CN 110286148 A CN110286148 A CN 110286148A CN 201910300792 A CN201910300792 A CN 201910300792A CN 110286148 A CN110286148 A CN 110286148A
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nano wire
electronic transport
situ
charge
transport mechanism
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CN110286148B (en
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徐林
刘琴
麦立强
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Wuhan University of Technology WUT
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R27/00—Arrangements for measuring resistance, reactance, impedance, or electric characteristics derived therefrom
    • G01R27/02—Measuring real or complex resistance, reactance, impedance, or other two-pole characteristics derived therefrom, e.g. time constant
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
    • 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
    • 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
    • H01M10/058—Construction or manufacture
    • 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

Abstract

The present invention relates to a kind of methods of electronic transport mechanism in in-situ study nano wire charge and discharge process, it is characterised in that includes the following steps: 1) to make miniature interdigital collector in substrate surface using ultraviolet photolithographic and high temperature pyrolysis/thermal evaporation method；2) nano wire uniformly and is in an orderly manner covered on above-mentioned miniature interdigital collector as positive electrode using cosolvent evaporation；3) by aqueous electrolyte drop coating in substrate surface, and it is inserted into the assembling that zinc electrode completes nano wire film electrochemical device, then it is tested for the property and is characterized.The beneficial effects of the present invention are: pre- addition manganese ion can be explained as Zn-MnO2When battery electrolyte, the essential reason of electrochemical performance, and the correlative study for nanowire electrochemical device material structure and electrochemistry, electronic transport performance provides a kind of diagnostic platform.

Description

Electricity is defeated in nano wire film electrochemical device and in-situ study nano wire charge and discharge process The method of transport mechanism
Technical field
The invention belongs to nanometer material and electrochemical technology fields, and in particular to a kind of in-situ study nano wire charge and discharge The method of electronic transport mechanism in journey.
Background technique
Energy consumption have stimulated to the increasing demand of energy storage device, wherein Zinc ion battery due to its high element it is rich Degree, cheap price and it is environmental-friendly many advantages, such as receive significant attention.However Zinc ion battery is due to its cycle performance Difference keeps its extensive use seriously hampered, therefore the cycle performance for improving water system Zinc ion battery is put into a large amount of research , but the intrinsic mechanism of water system Zinc ion battery capacity attenuation is still smudgy at present.
Monodimension nanometer material is because of its special physical and chemical performance and the potential advantages that can be used as quantum device, it is considered to be Connect microcosmic and macroscopical tie.In research before, there is work to be prepared for single nano-wire device, in-situ monitoring Li+From Sub- Na+The ion transmission path of ion.However this technology can also be further improved.First, single nano-wire and collector Between exist very big contact resistance, there are very big differences with conventional batteries for its electrochemical process；Second, single nano-wire device Part preparation process is complicated, has certain selectivity to material.And nano wire film electrochemical device can optimize its limitation, To the in-situ study of nano line electrode charge and discharge ion transport mechanism have deeper into exploration.
Summary of the invention
This paper presents a kind of methods of electronic transport mechanism in in-situ study nano wire charge and discharge process, receive for in-situ study The essence of rice noodles capacity attenuation provides a platform.
The technical proposal adopted by the invention to solve the above technical problems is that: it is electric in in-situ study nano wire charge and discharge process The method of transport mechanism, it is characterised in that include the following steps:
1) miniature interdigital collector is made in substrate surface using ultraviolet photolithographic and high temperature pyrolysis/thermal evaporation method；
2) nano wire uniformly and is in an orderly manner covered on by conduct on above-mentioned miniature interdigital collector using cosolvent evaporation Positive electrode；
3) it by aqueous electrolyte drop coating in substrate surface, and is inserted into zinc electrode and completes nano wire film electrochemical device Assembling, is then tested for the property and characterizes to it.
According to the above scheme, the nano wire is barium oxide nano wire or Mn oxide nano wire.
According to the above scheme, the Mn oxide nano wire is manganese dioxide nanowire, zinc-manganese oxide nano thread or sodium Mn oxide nano wire, the barium oxide nano wire are vanadium pentoxide nanowires or vanadium dioxide nanowire.
According to the above scheme, the zinc electrode is ultra-fine zinc bar or plating zinc metal sheet.
According to the above scheme, the aqueous electrolyte be following electrolyte one kind or their mixing: zinc salt, manganese salt and Sodium salt.
According to the above scheme, the aqueous electrolyte is one kind of following electrolyte: Na2SO4、ZnSO4Or ZnSO4With Na2SO4、MnSO4Mixed electrolytic solution.
According to the above scheme, the performance test and characterizing method include the following steps:
1) charge-discharge test is carried out to electrochemical device, stands battery under different charging and discharging states, then Electronic transport performance test in situ is carried out to the nano wire of the ordered arrangement on the substrate；
2) structural characterization in situ is carried out to the nano wire of ordered arrangement under different charging and discharging states；
3) according to the nano wire of ordered arrangement, electronic transport performance compares and structure change under different charging and discharging states, i.e., It can obtain the essence that ion pair nano wire capacity attenuation influences.
According to the above scheme, the structural characterization in situ includes raman microspectroscopy spectrum analysis.
A kind of nano wire film electrochemical device, to comprise the following steps that using obtained by following preparation methods
1) miniature interdigital collector is made in substrate surface using ultraviolet photolithographic and high temperature pyrolysis/thermal evaporation method；
2) nano wire uniformly and is in an orderly manner covered on by conduct on above-mentioned miniature interdigital collector using cosolvent evaporation Positive electrode；
3) it by aqueous electrolyte drop coating in substrate surface, and is inserted into zinc electrode and completes nano wire film electrochemical device.
The beneficial effects of the present invention are: pre- addition manganese ion can be explained as Zn-MnO2When battery electrolyte, electrochemistry The essential reason haveing excellent performance, and be the correlative study of nanowire electrochemical device material structure and electrochemistry, electronic transport performance Provide a kind of diagnostic platform；The assembling of nano wire film electrochemical device is not needed using conductive agent and bonding in the present invention Agent, have between the nano wire and electrolyte of proper alignment it is good contact, be the biggish zinc metal sheet of area to electrode, therefore measure Electrochemistry can preferably reflect the intrinsic electrochemical behavior of nano wire；Electronic transport and structural characterization to nano wire are all It is carried out under state in situ, can reflect the intrinsic variation of nano wire conductivity and structure in battery charge and discharge process, disclose material The essential reason of material deterioration capacity attenuation.
Detailed description of the invention
Fig. 1 is nano wire film electrochemical device schematic diagram；
Fig. 2 is the miniature interdigital pyrolytic carbon production flow diagram of embodiment 1；
Fig. 3 is that total solution-deposition method prepares nano wire film schematic diagram；
Fig. 4 is ordered into the scanning figure of arranging nano-wire；
Fig. 5 be embodiment 1 nano wire film under different charging and discharging states electronic transport performance curve；
Fig. 6 be embodiment 1 nano wire film under first circle charging and discharging state in-situ Raman curve.
Specific embodiment
In order to better understand the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention Content is not only limited to the following examples.
Embodiment 1:
The technical solution of nano wire film electrochemical device assembling (as shown in Figure 1) includes the following steps, successively carries out:
1) coating photoresist SU8-2000.5 is on the silica silicon chip that there is one layer of 600nm thickness on surface, by ultraviolet Photoetching and high temperature pyrolysis technology prepare the pyrolytic carbon collector (as shown in Figure 2) of 100nm thickness；
2) it by the manganese dioxide nanowire prepared with hydro-thermal method anode, is dispersed in by the way that cosolvent evaporation is uniform sequential (as shown in Figure 3) is stated on the pyrolytic carbon collector of preparation, and high resolution scanning is as shown in Figure 4；
3) configuration concentration is the zinc sulfate of 2M and the manganese sulfate aqueous electrolyte of 0.1M, and drop coating is inserted into substrate surface Ultra-fine zinc bar is the assembling for completing nano wire film electrochemical device.
Technical solution used by nano wire film electrochemical device in-situ characterization includes the following steps, successively carries out:
1) cyclic voltammetry and constant current charge-discharge test are carried out to battery, keeps battery quiet under different charging and discharging states It sets 5 minutes, electronic transport performance test (as shown in Figure 5) in situ is then carried out to manganese dioxide nanowire film on substrate.Its In, the equipment of electrochemical property test is as follows: Keithley6220 characteristic of semiconductor analyzer provides constant-current source.Test result is aobvious Show, by constant-current discharge process, apparent downward trend is presented in conductivity, and by constant-current charge process, conductivity presents obvious Downward trend, disclose reversible deintercalation process of the zinc ion in nano wire；
2) test of micro-zone in situ Raman is carried out (such as Fig. 6 institute to the manganese dioxide nanowire film under different charging and discharging states Show).Raman test result shows that reversible transition has occurred in manganese dioxide during discharge, is changed into MnOOH and Mn3O4。
Embodiment 2:
The technical solution of nano wire film electrochemical device assembling includes the following steps, successively carries out:
1) coating photoresist SU8-2000.5 is on the silica silicon chip that there is one layer of 600nm thickness on surface, by ultraviolet Photoetching and thermal evaporation technology prepare the titanium collector of 100nm thickness；
2) it by the manganese dioxide nanowire prepared with hydro-thermal method anode, is uniformly dispersed in by cosolvent evaporation above-mentioned On the titanium collector of preparation；
3) configuration concentration is the zinc sulfate aqueous electrolyte of 2M, and drop coating is inserted into ultra-fine zinc bar and is completed in substrate surface The assembling of nano wire film electrochemical device.
Technical solution used by nano wire film electrochemical device in-situ characterization includes the following steps, successively carries out:
1) cyclic voltammetry and constant current charge-discharge test are carried out to battery, keeps battery quiet under different charging and discharging states It sets 5 minutes, electronic transport performance test in situ is then carried out to manganese dioxide nanowire film on substrate.Wherein, electrochemistry The equipment that can be tested is as follows: Keithley6220 characteristic of semiconductor analyzer provides constant-current source；
2) test of micro-zone in situ Raman is carried out to the manganese dioxide nanowire film under different charging and discharging states.Raman test The results show that reversible transition has occurred in manganese dioxide during discharge, it is changed into MnOOH and Mn3O4。
Embodiment 3:
The technical solution of nano wire film electrochemical device assembling includes the following steps, successively carries out:
1) coating photoresist SU8-2000.5 is on the silica silicon chip that there is one layer of 600nm thickness on surface, by ultraviolet Photoetching and thermal evaporation technology prepare the golden collector of 100nm thickness；
2) it by the manganese dioxide nanowire prepared with hydro-thermal method anode, is uniformly dispersed in by cosolvent evaporation above-mentioned On the golden collector of preparation；
3) configuration concentration is the zinc sulfate aqueous electrolyte of 2M, and drop coating is inserted into ultra-fine zinc bar and is completed in substrate surface The assembling of nano wire film electrochemical device.
Technical solution used by nano wire film electrochemical device in-situ characterization includes the following steps, successively carries out:
1) cyclic voltammetry and constant current charge-discharge test are carried out to battery, keeps battery quiet under different charging and discharging states It sets 5 minutes, electronic transport performance test in situ is then carried out to manganese dioxide nanowire film on substrate.Wherein, electrochemistry The equipment that can be tested is as follows: Keithley6220 characteristic of semiconductor analyzer provides constant-current source；
2) test of micro-zone in situ Raman is carried out to the manganese dioxide nanowire film under different charging and discharging states.Raman test The results show that reversible transition has occurred in manganese dioxide during discharge, it is changed into MnOOH and Mn3O4。
Embodiment 4:
The technical solution of nano wire film electrochemical device assembling includes the following steps, successively carries out:
1) coating photoresist SU8-2000.5 is on the silica silicon chip that there is one layer of 600nm thickness on surface, by ultraviolet Photoetching and high temperature pyrolysis technology prepare the pyrolytic carbon collector of 100nm thickness；
2) zinc-manganese oxide nano thread anode will be prepared with hydro-thermal method, be uniformly dispersed in by cosolvent evaporation above-mentioned On the pyrolytic carbon collector of preparation；
3) configuration concentration is the zinc sulfate aqueous electrolyte of 2M, and drop coating is inserted into ultra-fine zinc bar and is completed in substrate surface The assembling of nano wire film electrochemical device.
Technical solution used by nano wire film electrochemical device in-situ characterization includes the following steps, successively carries out:
1) cyclic voltammetry and constant current charge-discharge test are carried out to battery, keeps battery quiet under different charging and discharging states It sets 5 minutes, electronic transport performance test in situ is then carried out to manganese dioxide nanowire film on substrate.Wherein, electrochemistry The equipment that can be tested is as follows: Keithley6220 characteristic of semiconductor analyzer provides constant-current source；
2) test of micro-zone in situ Raman is carried out to the manganese dioxide nanowire film under different charging and discharging states.Raman test The results show that reversible transition has occurred in manganese dioxide during discharge, it is changed into MnOOH and Mn3O4。
Embodiment 5:
The technical solution of nano wire film electrochemical device assembling includes the following steps, successively carries out:
1) coating photoresist SU8-2000.5 is on the silica silicon chip that there is one layer of 600nm thickness on surface, by ultraviolet Photoetching and high temperature pyrolysis technology prepare the pyrolytic carbon collector of 100nm thickness；
2) sodium manganese oxide nanowire positive electrode will be prepared with hydro-thermal method, be uniformly dispersed in by cosolvent evaporation above-mentioned On the pyrolytic carbon collector of preparation；
3) configuration concentration is the zinc sulfate of 2M and the sodium sulphate aqueous electrolyte of 0.2M, and drop coating is inserted into substrate surface Ultra-fine zinc bar is the assembling for completing nano wire film electrochemical device.
Technical solution used by nano wire film electrochemical device in-situ characterization includes the following steps, successively carries out:
1) cyclic voltammetry and constant current charge-discharge test are carried out to battery, keeps battery quiet under different charging and discharging states It sets 5 minutes, electronic transport performance test in situ is then carried out to manganese dioxide nanowire film on substrate.Wherein, electrochemistry The equipment that can be tested is as follows: Keithley6220 characteristic of semiconductor analyzer provides constant-current source；
2) test of micro-zone in situ Raman is carried out to the manganese dioxide nanowire film under different charging and discharging states.Raman test The results show that reversible transition has occurred in manganese dioxide during discharge, it is changed into MnOOH and Mn3O4。

Claims (9)

1. the method for electronic transport mechanism in in-situ study nano wire charge and discharge process, it is characterised in that include the following steps:
1) miniature interdigital collector is made in substrate surface using ultraviolet photolithographic and high temperature pyrolysis/thermal evaporation method；
2) nano wire uniformly and is in an orderly manner covered on above-mentioned miniature interdigital collector as anode using cosolvent evaporation Material；
3) by aqueous electrolyte drop coating in substrate surface, and it is inserted into the group that zinc electrode completes nano wire film electrochemical device Dress, is then tested for the property and characterizes to it.
2. the method for electronic transport mechanism, feature exist in in-situ study nano wire charge and discharge process according to claim 1 In the nano wire be barium oxide nano wire or Mn oxide nano wire.
3. the method for electronic transport mechanism, feature exist in in-situ study nano wire charge and discharge process according to claim 2 In the Mn oxide nano wire be manganese dioxide nanowire, zinc-manganese oxide nano thread or sodium manganese oxide nano wire, institute The barium oxide nano wire stated is vanadium pentoxide nanowires or vanadium dioxide nanowire.
4. the method for electronic transport mechanism, feature exist in in-situ study nano wire charge and discharge process according to claim 1 For ultra-fine zinc bar or zinc metal sheet is electroplated in the zinc electrode.
5. the method for electronic transport mechanism, feature exist in in-situ study nano wire charge and discharge process according to claim 1 In one kind or their mixing that the aqueous electrolyte is following electrolyte: zinc salt, manganese salt and sodium salt.
6. the method for electronic transport mechanism, feature exist in in-situ study nano wire charge and discharge process according to claim 5 In one kind that the aqueous electrolyte is following electrolyte: Na2SO4、ZnSO4Or ZnSO4With Na2SO4、MnSO4Mixing electricity Solve liquid.
7. the method for electronic transport mechanism, feature exist in in-situ study nano wire charge and discharge process according to claim 1 Include the following steps: in the performance test and characterizing method
1) charge-discharge test is carried out to electrochemical device, stands battery under different charging and discharging states, then to institute The nano wire for the ordered arrangement on substrate stated carries out electronic transport performance test in situ；
2) structural characterization in situ is carried out to the nano wire of ordered arrangement under different charging and discharging states；
3) according to the nano wire of ordered arrangement, electronic transport performance compares and structure change under different charging and discharging states, can obtain The essence that ion pair nano wire capacity attenuation influences out.
8. the method for electronic transport mechanism, feature exist in in-situ study nano wire charge and discharge process according to claim 7 In the structural characterization in situ include raman microspectroscopy spectrum analysis.
9. a kind of nano wire film electrochemical device, to comprise the following steps that using obtained by following preparation methods
1) miniature interdigital collector is made in substrate surface using ultraviolet photolithographic and high temperature pyrolysis/thermal evaporation method；
2) nano wire uniformly and is in an orderly manner covered on above-mentioned miniature interdigital collector as anode using cosolvent evaporation Material；
3) it by aqueous electrolyte drop coating in substrate surface, and is inserted into zinc electrode and completes nano wire film electrochemical device.
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