CN108447701A - High/low temperature flexible fiber shape ultracapacitor and its preparation method and application - Google Patents

High/low temperature flexible fiber shape ultracapacitor and its preparation method and application Download PDF

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Publication number
CN108447701A
CN108447701A CN201810186705.5A CN201810186705A CN108447701A CN 108447701 A CN108447701 A CN 108447701A CN 201810186705 A CN201810186705 A CN 201810186705A CN 108447701 A CN108447701 A CN 108447701A
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low temperature
fiber shape
flexible fiber
oxide
temperature flexible
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CN201810186705.5A
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王斌
程建丽
王转培
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Institute of Chemical Material of CAEP
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/46—Metal oxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/48—Conductive polymers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • 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
    • Y02E60/13—Energy storage using capacitors

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Electric Double-Layer Capacitors Or The Like (AREA)

Abstract

The present invention provides a kind of preparation methods of high/low temperature flexible fiber shape ultracapacitor, it is that two conducting polymer composite fibre electrodes are arranged in parallel with certain spacing, both ends are fixed on using conductive tape and conductive silver glue in PET film, surface coats water system gel electrolyte, obtains high/low temperature flexible fiber shape ultracapacitor integration device.The present invention also provides high/low temperature flexible fiber shape ultracapacitor and its applications.The present invention DEG C still maintains high-energy density in wide temperature range environment from 60 to 100, the security performance with superelevation, and be bent at any angle without influencing its performance.

Description

High/low temperature flexible fiber shape ultracapacitor and its preparation method and application
Technical field
The present invention relates to a kind of capacitors, and in particular to a kind of preparation method of water system high/low temperature capacitor and its extreme ring Application in border.
Background technology
Wearable electronic device and electronic fabric are fast-developing in mancarried electronic aid and have good application prospect. Fibrous ultracapacitor has small, and flexibility is high, the characteristics of convenient for being designed to various structure, therefore is acknowledged as It is most potential energy storage electronic material.Compared with the ultracapacitor of traditional two-dimensional structure and battery, one-dimensional threadiness Ultracapacitor than energy lower limit its application.Although having in terms of improving fibrous capacitor energy density prodigious Progress, such as high specific capacitance is designed, the carbon material of high conductivity, the metal oxide of some embedded fake capacitances, by being assembled into Asymmetrical capacitor increases its voltage window using ionic liquid or organic electrolyte.But it is still deposited in extreme environment It is greatly challenging, including low energy densities, significantly capacity attenuation, expensive electrolyte (ionic liquid) and liquid The leakage safety problem of electrolyte.
The fibrous ultracapacitor studied at present be largely based on high toxicity and inflammable organic electrolyte (acetonitrile, With high volatile and low burning point) or highly viscous costliness il electrolyte or concentrated acid (H2SO4,H3PO4) and alkali Property (NaOH) solvent these all have prodigious security risk.Especially being flexible wearable electronic device is affixed directly to people Skin on, in practical applications, this kind of electronic device inevitably bends or distorts, once leak, this A little potential safety problems will be more serious.However, so far, the research of fibrous capacitor most of at present is also It is especially to exist to thermal equator region (being higher than 40 DEG C) these capacitors in the winter of severe cold (being less than -20 DEG C) in room temperature environment It may not work in extreme environment and cannot meet the needs of people.The performance of capacitor can deteriorate in extreme environment, example Such as capacitance fade, internal resistance increases, cycle life increase and due to internal heat increase so as to cause explosion, these Problem can seriously limit its practical application.
As far as we know, the high-energy density threadiness at present from less than -30 DEG C to higher than 50 DEG C in extreme environment can The flexible water system capacitor of wearing is not yet reported that.Therefore, we devise a new class of fibrous ultracapacitor combination water Be the nanometer crystal fiber of gel electrolyte and nucleocapsid, in wide temperature range environment from -60 to 100 DEG C to still maintain high-energy close Degree, and the security performance with superelevation.Design for related electronic devices and its high/low temperature device provides new thinking.
Invention content
Present invention aim to address above-mentioned technical problems, provide a kind of preparation and its application of water system high/low temperature capacitor Method.The preparation method of the present invention is not necessarily to special installation, large-scale production easy to implement；And in the environment of high/low temperature not Influence its chemical property.
In order to reach above-mentioned technique effect, the present invention takes following technical scheme：
A kind of preparation method of high/low temperature flexible fiber shape ultracapacitor
Two conducting polymer composite fibre electrodes are arranged in parallel with certain spacing, and both ends use conductive tape and conduction Elargol is fixed in PET film, and surface coats water system gel electrolyte, obtains high/low temperature flexible fiber shape ultracapacitor one Body device.
In the present invention, used water system gel electrolyte, component includes water, electrolyte and PVA, and mass ratio is water：Electricity Xie Zhi：PVA=10：1.5：1, electrolyte includes lithium chloride, sodium chloride, potassium chloride, lithium sulfate, sodium sulphate, potassium sulfate, perchloric acid Lithium, sodium perchlorate, potassium hyperchlorate, carboxymethyl cellulose lithium, sodium carboxymethylcellulose and potassium carboxymethylcellulose.
In the present invention, the high/low temperature, it is characterised in that high temperature is more than or equal to 100 DEG C, and low temperature is less than or equal to -60 DEG C, This research provides possibility for the development of wearable device under extreme condition, not only can be adapted for the environment to make a clear distinction between the four seasons, And efficient performance is still maintained in the larger desert of the temperature difference, in addition to this, still have in snow-coated plateau area very stable Performance.
The present invention also provides a kind of preparation methods of conducting polymer composite fibre electrode, it includes the following steps：
It is prepared using the conducting polymer and metal and oxide mixture of different proportion by the method for wet spinning flexible Polymer composite fibrous 0.01~10h of processing in inorganic solution that is polymer composite fibrous, will obtaining, is cleaned with distilled water, Dry 0.01~1h in 50~150 DEG C of baking oven.By obtain it is polymer composite fibrous coat one layer of polymeric again, inorganic 0.01~10h is handled in solution, obtaining high working voltage window (be not less than 1V) and superelevation conductivity, (conductivity is not less than The conducting polymer composite fibre electrode of nucleocapsid 500S/cm).
In the present invention, the metal and oxide of the conducting polymer composite fibre, including iron, copper, cobalt, manganese, ruthenium, Molybdenum, zinc, tungsten, tin, aluminium, magnesium, silver, gold, platinum, cobalt oxide, iron oxide, manganese oxide, ruthenium-oxide, molybdenum oxide, zinc oxide, tungsten oxide, Tin oxide, copper oxide and aluminium oxide；
In the present invention, the metal of the conducting polymer composite fibre and the ratio of oxide, it is characterised in that described Ratio be 0.01~99.0wt%.
It is super by aforementioned high/low temperature flexible fiber shape the present invention also provides high/low temperature flexible fiber shape ultracapacitor What the preparation method of grade capacitor was prepared.
The present invention also provides the application of high/low temperature flexible fiber shape ultracapacitor, be apply it is close in wearable high-energy Spend ultracapacitor field.
Compared with prior art, the present invention having advantageous effect below：
Compared with prior art, the present invention provides a kind of preparation and its application of water system ultralow temperature capacitor, has operation Simply, flexility is good, and it is strong to weave ability, the characteristics of high-performance high security still can be kept in high and low temperature environment, Without special installation, large-scale production easy to implement.It can be applied in wearable high-energy density super capacitor field.
Description of the drawings
Fig. 1 is the polymer composite fibrous SEM figures of the high conductivity of nucleocapsid of the present invention.
Fig. 2 is the CV figures of the polymer composite fibrous multivoltage window of high conductivity of nucleocapsid of the present invention.
Fig. 3 is the CV figures of the polymer composite fibrous different scanning rates of high conductivity of nucleocapsid of the present invention.
Fig. 4 is the concatenated CV curves of the polymer composite fibrous capacitor of high conductivity of nucleocapsid of the present invention.
Fig. 5 is the CV curves of the polymer composite fibrous capacitor parallel connection of high conductivity of nucleocapsid of the present invention.
Fig. 6 is CV curve of the polymer composite fibrous capacitor of high conductivity in high-temperature-range of nucleocapsid of the present invention.
Fig. 7 is CV curve of the polymer composite fibrous capacitor of high conductivity in low temperature region of nucleocapsid of the present invention.
Fig. 8 is that the polymer composite fibrous capacitor of high conductivity of nucleocapsid of the present invention is bent different angle at 75 DEG C CV curves.
Fig. 9 is that the polymer composite fibrous capacitor of high conductivity of nucleocapsid of the present invention is bent different angle at -60 DEG C CV curves.
Figure 10 is that the polymer composite fibrous capacitor of high conductivity of nucleocapsid of the present invention lights 1 green at 75 DEG C The picture of LED light.
Figure 11 is that the polymer composite fibrous capacitor of high conductivity of nucleocapsid of the present invention lights 1 green at -60 DEG C The picture of LED light.
Figure 12 is the structural schematic diagram of high/low temperature flexible fiber shape ultracapacitor of the present invention.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to Limit the present invention.
Embodiment 1
As shown in Fig. 12, the conducting polymer composite fibre 1 of two nucleocapsids is arranged in parallel with the spacing of 1mm, and two End is fixed on using conductive tape and conductive silver glue 3 in PET film 2, and surface coats lithium chloride-PVA gel electrolytes 4, that is, makes Obtain high/low temperature flexible fiber shape ultracapacitor integration device.
Embodiment 2
The conducting polymer composite fibre of two nucleocapsids is arranged in parallel with the spacing of 1mm, and both ends use conductive tape And conductive silver glue is fixed in PET film, surface coats potassium sulfate-PVA gel electrolytes, obtains high/low temperature flexible fiber shape Ultracapacitor integration device.
Embodiment 3
The conducting polymer composite fibre of two nucleocapsids is arranged in parallel with the spacing of 1mm, and both ends use conductive tape And conductive silver glue is fixed in PET film, surface coats sodium sulphate-PVA gel electrolytes, obtains high/low temperature flexible fiber shape Ultracapacitor integration device.
Embodiment 4
The conducting polymer composite fibre of two nucleocapsids is arranged in parallel with the spacing of 1mm, and both ends use conductive tape And conductive silver glue is fixed in PET film, surface coats sodium carboxymethylcellulose-PVA gel electrolytes, and it is gentle to obtain height Property threadiness ultracapacitor integration device.
Embodiment 5
The conducting polymer composite fibre of two nucleocapsids is arranged in parallel with the spacing of 1mm, and both ends use conductive tape And conductive silver glue is fixed in PET film, surface coats potassium chloride-PVA gel electrolytes, obtains high/low temperature flexible fiber shape Ultracapacitor integration device.
Embodiment 6
The polypyrrole of 99.0wt.% and ferric oxide nanometer particle mixture are prepared into polymerization flexible by the method for wet spinning Object composite fibre, the polymer composite fibrous immersion treatment 0.1h in inorganic solution that will be obtained are cleaned with distilled water, at 80 DEG C Baking oven in dry 0.1h.By obtain it is polymer composite fibrous coat a strata pyrroles again, 0.1h is handled in inorganic solution, The conducting polymer for obtaining high working voltage window (1.0V) and the nucleocapsid of superelevation conductivity (conductivity 500S/cm) is compound Fiber electrode.Wherein, inorganic solvent can be N-Methyl pyrrolidone, N, N- dimethylpropionamides, n,N-dimethylacetamide, One in the tert-butyl alcohol, n-butanol, isobutanol, isopropanol, chloroform, dichloromethane, tetrahydrofuran ethylene glycol, methanol and ethyl alcohol Kind is a variety of
Embodiment 7
The polypyrrole of 60.0wt.% and cobalt oxide mixture of nanoparticles are prepared into polymerization flexible by the method for wet spinning Object composite fibre, the polymer composite fibrous immersion treatment 0.2h in inorganic solution that will be obtained are cleaned with distilled water, 100 DEG C baking oven in dry 0.1h.By obtain it is polymer composite fibrous coat a strata pyrroles again, handled in inorganic solution 0.2h obtains the conducting polymer of high working voltage window (1.3V) and the nucleocapsid of superelevation conductivity (conductivity 600S/cm) Object composite fibre electrode.
Embodiment 8
The polythiophene of 40.0wt.% and ruthenium-oxide mixture of nanoparticles are prepared into polymerization flexible by the method for wet spinning Object composite fibre, the polymer composite fibrous immersion treatment 0.05h in inorganic solution that will be obtained are cleaned with distilled water, 120 DEG C baking oven in dry 0.2h.By obtain it is polymer composite fibrous coat a strata thiophene again, handled in inorganic solution 0.05h obtains the conducting polymer of high working voltage window (1.5V) and the nucleocapsid of superelevation conductivity (conductivity 700S/cm) Object composite fibre electrode.
Embodiment 9
The polyaniline of 20.0wt.% and cupric oxide nano line mixture are prepared into polymer flexible by the method for wet spinning Composite fibre, the polymer composite fibrous immersion treatment 0.3h in inorganic solution that will be obtained are cleaned with distilled water, at 150 DEG C Baking oven in dry 0.01h.By obtain it is polymer composite fibrous coat a strata aniline again, handled in inorganic solution 0.3h obtains the conducting polymer of high working voltage window (1.6V) and the nucleocapsid of superelevation conductivity (conductivity 700S/cm) Object composite fibre electrode.
Embodiment 10
The polypyrrole of 5.0wt.% and silver nano-grain mixture polymer flexible is prepared by the method for wet spinning to answer Condensating fiber, the polymer composite fibrous immersion treatment 0.5h in inorganic solution that will be obtained are cleaned with distilled water, at 100 DEG C Dry 0.5h in baking oven.By obtain it is polymer composite fibrous coat a strata pyrroles again, 0.5h is handled in inorganic solution, is obtained It is multiple to the conducting polymer of high working voltage window (1.6V) and the nucleocapsid of superelevation conductivity (the not low 700S/cm of conductivity) Condensating fiber electrode.
Embodiment 11
The poly- furans of 0.01wt.% and gold nano grain mixture polymer flexible is prepared by the method for wet spinning to answer Condensating fiber, the polymer composite fibrous immersion treatment 0.3h in inorganic solution that will be obtained are cleaned with distilled water, at 120 DEG C Dry 0.1h in baking oven.By obtain it is polymer composite fibrous coat a strata furans again, 0.3h is handled in inorganic solution, is obtained It is multiple to the conducting polymer of high working voltage window (1.3V) and the nucleocapsid of superelevation conductivity (the not low 400S/cm of conductivity) Condensating fiber electrode.
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair Bright preferable embodiment, embodiment of the present invention are not limited by the above embodiments, it should be appreciated that people in the art Member can be designed that a lot of other modification and implementations, these modifications and implementations will be fallen in principle disclosed in the present application Within scope and spirit.

Claims (9)

1. the preparation method of high/low temperature flexible fiber shape ultracapacitor, it is characterised in that：
Two conducting polymer composite fibre electrodes are arranged in parallel with certain spacing, and both ends use conductive tape and conductive silver glue It is fixed in PET film, surface coats water system gel electrolyte, obtains the ultracapacitor integration of high/low temperature flexible fiber shape Device.
2. the preparation method of high/low temperature flexible fiber shape ultracapacitor according to claim 1, it is characterised in that：The water It is gel electrolyte, electrolyte includes lithium chloride, sodium chloride, potassium chloride, lithium sulfate, sodium sulphate, potassium sulfate, lithium perchlorate, height Sodium chlorate, potassium hyperchlorate, carboxymethyl cellulose lithium, sodium carboxymethylcellulose and potassium carboxymethylcellulose.
3. the preparation method of high/low temperature flexible fiber shape ultracapacitor according to claim 1, it is characterised in that：Described High/low temperature, high temperature are more than or equal to 100 DEG C, and low temperature is less than or equal to -60 DEG C.
4. the preparation method of high/low temperature flexible fiber shape ultracapacitor according to claim 1, it is characterised in that described to lead Electric polymer composite fibre electrode is prepared via a method which：
By the method for wet spinning polymerization flexible is prepared using the conducting polymer and metal and oxide mixture of different proportion Object composite fibre, the polymer composite fibrous 0.01~10h of processing in inorganic solution that will be obtained, is cleaned with distilled water, 50 Dry 0.01~1h in~150 DEG C of baking oven；By obtain it is polymer composite fibrous coat one layer of conducting polymer again, inorganic 0.01~10h is handled in solution, obtains the high working voltage window not less than 1V and superelevation conductivity not less than 500S/cm The conducting polymer composite fibre electrode of nucleocapsid.
5. the preparation method of high/low temperature flexible fiber shape ultracapacitor according to claim 4, it is characterised in that：
The conducting polymer includes polypyrrole and its derivative, Polyaniline and its derivative, polythiophene and its derivative, poly- furan It mutters and its derivative and polyacetylene and its derivative.
6. the preparation method of high/low temperature flexible fiber shape ultracapacitor according to claim 4, it is characterised in that：
The metal and oxide include iron, copper, cobalt, manganese, ruthenium, molybdenum, zinc, tungsten, tin, aluminium, magnesium, silver, gold, platinum, cobalt oxide, oxidation Iron, manganese oxide, ruthenium-oxide, molybdenum oxide, zinc oxide, tungsten oxide, tin oxide, copper oxide and aluminium oxide.
7. the preparation method of high/low temperature flexible fiber shape ultracapacitor according to claim 4, it is characterised in that：Described Ratio is 0.01~99.00wt%.
8. the preparation method of high/low temperature flexible fiber shape ultracapacitor described in claim 1 to 7 any claim is prepared into The high/low temperature flexible fiber shape ultracapacitor arrived.
9. the application of high/low temperature flexible fiber shape ultracapacitor described in claim 8, it is characterised in that applied wearable High-energy density super capacitor field.
CN201810186705.5A 2018-03-07 2018-03-07 High/low temperature flexible fiber shape ultracapacitor and its preparation method and application Pending CN108447701A (en)

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CN111599608A (en) * 2020-04-05 2020-08-28 上海理工大学 Molybdenum oxide/molybdenum core-sheath structure composite wire energy storage electrode material and preparation method of fibrous supercapacitor

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