CN109461596A - A kind of preparation method and application of the flexible ultra-thin all-solid-state supercapacitor based on titanium carbide - Google Patents
A kind of preparation method and application of the flexible ultra-thin all-solid-state supercapacitor based on titanium carbide Download PDFInfo
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- CN109461596A CN109461596A CN201811328352.4A CN201811328352A CN109461596A CN 109461596 A CN109461596 A CN 109461596A CN 201811328352 A CN201811328352 A CN 201811328352A CN 109461596 A CN109461596 A CN 109461596A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 239000010936 titanium Substances 0.000 claims abstract description 13
- 238000004146 energy storage Methods 0.000 claims abstract description 8
- 238000005516 engineering process Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000003828 vacuum filtration Methods 0.000 claims abstract description 5
- 239000006185 dispersion Substances 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 229910009819 Ti3C2 Inorganic materials 0.000 claims description 19
- 230000005611 electricity Effects 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 239000000725 suspension Substances 0.000 claims description 2
- 239000006227 byproduct Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 8
- 238000012983 electrochemical energy storage Methods 0.000 abstract description 5
- 238000011017 operating method Methods 0.000 abstract 1
- 239000003990 capacitor Substances 0.000 description 6
- 238000011161 development Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 210000004209 hair Anatomy 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910009818 Ti3AlC2 Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011245 gel electrolyte Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- H01G11/54—Electrolytes
- H01G11/56—Solid electrolytes, e.g. gels; Additives therein
-
- 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)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Manufacturing & Machinery (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention discloses the preparation method and application of the flexible ultra-thin all-solid-state supercapacitor based on titanium carbide, it is by titanium carbide (Ti which, which is sandwich structure,3C2) dispersion liquid of ultrathin nanometer piece is made up after flexible electrode of vacuum filtration technology and coats H between two panels flexible electrode2SO4/ PVA gel composition, operating method is simple, can be completed under normal temperature and pressure conditions；Flexible ultra-thin all-solid-state supercapacitor using published method of the present invention preparation has excellent electrochemical energy storage property and good mechanical performance, and thickness is only 190-210 μm, belongs to ultrathin energy storage device, can provide energy for minitype portable electronic equipment.
Description
Technical field
The present invention relates to capacitance technology fields, are specifically related to a kind of all solid state super electricity of the flexible ultra-thin based on titanium carbide
The preparation method of container and its electrochemical energy storage field application.
Background technique
With the fast development of electronic technology, the wearable electronics such as electronic sensor, flexible display, health monitoring apparatus
Equipment by all circles extensive concern and achieve development at full speed.Wearable electronic device has flexible, intelligent, frivolous spy
Point, traditional rigidity, large volume bulk battery are obviously difficult to meet the energy storage demand of such device, in order to match wearable electronic
Equipment, it is necessary to develop energy storage device lighter, thin, flexible that can be compatible.
Flexible all-solid-state supercapacitor is made of fexible film electrode and solid gel electrolyte, can quickly be filled because having
Electric discharge, high specific capacitance, high power density, the cycle life of overlength, safety and environmental protection and excellent mechanical property and wide make
It is the key equipment of flexible electronic device of new generation with extensive concern the advantages that temperature range by scientific circles and industrial circle.
Different from traditional capacitor, in flexible super capacitor, base, electrode and electrolyte are flexible, and can assign electricity
The various shapes of container can provide form and function more abundant, can satisfy the growth requirement of electronic equipment.
Two-dimensional electrode material can be used for preparing flexible all-solid-state supercapacitor, and the property of itself helps to increase material
Surface area and active site utilization rate, while the diffusion length of ion is reduced, to increase the capacitance and multiplying power of material
Characteristic.Based on two-dimentional Ti3C2The development of the flexible ultra-thin supercapacitor of ultrathin nanometer piece, can not only promote new electrode material
Development, it can also effectively promote flexible ultra-thin energy storage device development and its answering as portable electronic device function
With.
The present invention provides one kind to be based on Ti by the preparation of vacuum filtration technology3C2The flexible electrode of nanometer sheet, and at two
H is coated between flexible electrode2SO4For/PVA gel as solid electrolyte, the titanium carbide flexibility for being finally assembling to sandwich structure is super
The method of thin all-solid-state supercapacitor.The capacitor not only has the mechanical properties such as good flexible, ultra-thin property, also has excellent
Different electrochemical energy storage performance.
Summary of the invention
It is an object of the invention to solve deficiency in the prior art, develop a kind of low cost, low energy consumption, preparation process letter
The flexible ultra-thin all-solid-state supercapacitor based on titanium carbide of list, energy storage excellent, satisfactory mechanical property.
The technical solution of the present invention is as follows: a kind of preparation side of the flexible ultra-thin all-solid-state supercapacitor based on titanium carbide
Method, concrete operation step are as follows: by Ti3C2Ultrathin nanometer piece dispersion liquid filters film forming using vacuum filtration technology, dries at room temperature
6h forms fexible film electrode, coats H one piece of fexible film electrode side2SO4/ PVA gel, the electrode for coating gel is set
The dry 15min in 40 DEG C of baking ovens, is placed after gel side covers upper another dried fexible film electrode after taking-up
Dry 5h, is assembled into the flexible ultra-thin all-solid-state supercapacitor of sandwich structure in 40 DEG C of baking ovens.
Further, the flexible ultra-thin all-solid-state supercapacitor based on titanium carbide with a thickness of 190-210 μm.
Further, the Ti3C2The preparation step of nanometer sheet are as follows:
1) LiF is mixed with 9M HCl, and magnetic agitation to LiF is completely dissolved, and is slowly added to the Ti with quality such as LiF3AlC2,
Mixture is placed in reaction kettle, reacts 72h under the conditions of 60 DEG C；
2) product is carried out to centrifugal treating under conditions of 3500rpm, 5min, is washed product in step 1 with deionized water
To pH > 6, and it is dried in vacuo；
3) substance obtained in step 2 is dispersed by the concentration of 10g/L in deionized water, in the frequency of 600 W after drying
Ultrasound 4h under rate；
4) solution after ultrasound is centrifuged under the conditions of 3500rpm, 1h, upper layer suspension liquid is Ti3C2Ultrathin nanometer
Piece.
Further, the flexible ultra-thin all-solid-state supercapacitor based on titanium carbide can be applicable to electrochemical energy storage
In.
The invention has the benefit that
(1) preparation method of the flexible ultra-thin all-solid-state supercapacitor of the present invention based on titanium carbide is simple, often
It can be completed under the conditions of normal temperature and pressure；
It (2) is only 190- using titanium carbide flexible ultra-thin all-solid-state supercapacitor thickness prepared by published method of the present invention
210 μm, belong to ultrathin energy storage device, energy can be provided for minitype portable electronic equipment；
(3) there is good machine using the titanium carbide flexible ultra-thin all-solid-state supercapacitor of published method of the present invention preparation
Tool performance can be bent under different angle, which is convenient for providing energy for flexible portable's electronic equipment；
(4) there is excellent electricity using the titanium carbide flexible ultra-thin all-solid-state supercapacitor of published method of the present invention preparation
Chemical energy storage property.
Detailed description of the invention
Fig. 1 is the Ti that the embodiment of the present invention 1 obtains3C2The SEM photograph of ultrathin nanometer piece；
Fig. 2 is the Ti that the embodiment of the present invention 1 obtains3C2The TEM photo of ultrathin nanometer piece；
Fig. 3 is the Ti that the embodiment of the present invention 11 obtains3C2The AFM photo of ultrathin nanometer piece；
Fig. 4 is the Ti that the embodiment of the present invention 1 obtains3C2The top view SEM photograph of membrane electrode；
Fig. 5 is the Ti that the embodiment of the present invention 1 obtains3C2The side view SEM photograph of membrane electrode；
Fig. 6 is the Ti that the embodiment of the present invention 1 obtains3C2The top view optical photograph of flexible ultra-thin all-solid-state supercapacitor；
Fig. 7 is the Ti that the embodiment of the present invention 1 obtains3C2The bending figure of flexible ultra-thin all-solid-state supercapacitor；
Fig. 8 is the Ti that the embodiment of the present invention 2 obtains3C2The CV of flexible ultra-thin all-solid-state supercapacitor schemes；
Fig. 9 is the Ti that the embodiment of the present invention 3 obtains3C2The GCD of flexible ultra-thin all-solid-state supercapacitor schemes.
Specific embodiment
Following embodiment further illustrates the contents of the present invention, but should not be construed as limiting the invention.Without departing substantially from
In the case where essence of the present invention, to modification made by the method for the present invention, step or condition and replaces, belong to model of the invention
It encloses.
Embodiment 1: the flexible ultra-thin all-solid-state supercapacitor based on titanium carbide
Step 1: Ti3C2Preparation
(1) 1g LiF is dispersed in 20mL 9M HCl, magnetic agitation to LiF is completely dissolved；
(2) to prevent hot-spot, it is slowly added to 1g Ti3AlC2；
(3) mixture is placed in reaction kettle, reacts 72h under the conditions of 60 DEG C；
(4) product is subjected to centrifugal treating (3500rpm/5min), be washed with deionized 6 times, with ethanol washing 2 times,
Vacuum drying；
(5) product after drying 0.1g is weighed to be scattered in 10mL deionized water, under the conditions of 600W, ultrasonic 4h；
(6) product after ultrasound is subjected to centrifugal treating (3500rpm, 1h), supernatant is required substance.
Step 2: Ti3C2The preparation of flexible electrode
Using vacuum filtration technology, by 10mL 0.01g/mL Ti3C2Dispersion liquid filters film forming, dries 6h at room temperature.
Step 3: Ti3C2The preparation of flexible ultra-thin all-solid-state supercapacitor
H is coated in the side of flexible electrode2SO4/ PVA gel, gel gross mass are 0.022g, will coat the electrode of gel
After being placed in 40 DEG C of baking ovens dry 15min, upper another plate electrode is covered in gel side and is placed in 40 DEG C of baking ovens dry 5h
Form the flexible ultra-thin all-solid-state supercapacitor of sandwich structure.
After tested, the thickness of the flexible ultra-thin all-solid-state supercapacitor is only 0.191mm, belongs to ultrathin accumulator
Part can provide energy for minitype portable electronic equipment, have excellent electrochemical energy storage property.
By attached drawing 1,2,3 it can be seen that Ti3C2The size of ultrathin nanometer piece is about 200nm, and average thickness is about 1.3nm.By
Attached drawing 5 is it can be seen that Ti3C2Membrane electrode thickness is only 10 μm, and has layer structure, and duct is conducive to ion transmission.
Fig. 7 is the bending figure of the flexible ultra-thin all-solid-state supercapacitor, and what is be as can be seen from the figure prepared is super
Capacitor has excellent mechanical performance, and buckle resistance is strong, and electrode structure is stablized.
Embodiment 2:Ti3C2The cyclic voltammetry of flexible ultra-thin all-solid-state supercapacitor
Capacitor sizes: 1.5cm × 0.6cm；Positive and negative anodes: Ti3C2Flexible electrode；Electrolyte: H2SO4/ PVA gel；Electricity
Press range: -0.3V~0.3V；Sweep speed: 1mV/s, 2mV/s, 5mV/s, 10mV/s, 20mV/s, 30mV/s, 50mV/s.
As shown in figure 8, Ti3C2Flexible ultra-thin all-solid-state supercapacitor 1mV/s sweep speed under specific capacitance value reach
0.328F cm-2, electrochemical performance.
Embodiment 3:Ti3C2The constant current charge-discharge test of flexible ultra-thin all-solid-state supercapacitor
Capacitor sizes: 1.5cm × 0.6cm；Positive and negative anodes: Ti3C2Flexible electrode；Electrolyte: H2SO4/ PVA gel；Electricity
Press range: -0.3V~0.3V；Current density: 3mA cm-2, 5mA cm-2, 10mA cm-2, 20mA cm-2, 30mA cm-2。
As shown in figure 9, Ti3C2Flexible ultra-thin all-solid-state supercapacitor is in 3mA cm-2Current density under, area ratio electricity
Capacitance reaches 1F cm-2。
Basic principles and main features and advantage of the invention have been shown and described above.But the foregoing is merely this hairs
Bright specific embodiment, technical characteristic of the invention are not limited thereto, and any those skilled in the art is not departing from this hair
The other embodiments obtained under bright technical solution should all cover within the scope of the patent of the present invention.
Claims (4)
1. a kind of preparation method of the flexible ultra-thin all-solid-state supercapacitor based on titanium carbide, which is characterized in that specific preparation
Step are as follows: first by Ti3C2Ultrathin nanometer piece dispersion liquid filters film forming using vacuum filtration technology, and dry 6h is formed soft at room temperature
Property membrane electrode, coat H one piece of fexible film electrode side2SO4The electrode for coating gel is placed in 40 DEG C of bakings by/PVA gel
Dry 15min in case, is placed in 40 DEG C of bakings after gel side covers upper another dried fexible film electrode after taking-up
Dry 5h, is assembled into the flexible ultra-thin all-solid-state supercapacitor of sandwich structure in case.
2. a kind of preparation method of the flexible ultra-thin all-solid-state supercapacitor based on titanium carbide as described in claim 1,
Be characterized in that, the flexible ultra-thin all-solid-state supercapacitor prepared with a thickness of 190-210 μm.
3. a kind of preparation method of the flexible ultra-thin all-solid-state supercapacitor based on titanium carbide as claimed in claim 2,
It is characterized in that, the Ti3C2The preparation step of nanometer sheet are as follows:
1) LiF is mixed with 9M HCl, and magnetic agitation to LiF is completely dissolved, and is slowly added to the Ti with quality such as LiF3AlC2, will mix
It closes object to be placed in reaction kettle, reacts 72h under the conditions of 60 DEG C；
2) product is carried out to centrifugal treating under conditions of 3500rpm, 5min, with deionized water by product in step 1 be washed till pH >
6, and be dried in vacuo；
3) substance obtained in step 2 is dispersed in deionized water, to surpass under the frequency of 600W by the concentration of 10g/L after drying
Sound 4h；
4) solution after ultrasound is centrifuged under the conditions of 3500rpm, 1h, upper layer suspension liquid is Ti3C2Ultrathin nanometer piece.
4. a kind of flexible ultra-thin all-solid-state supercapacitor based on titanium carbide as claimed in any one of claims 1-3 is in electricity
Application in chemical energy storage.
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| CN201811328352.4A CN109461596A (en) | 2018-11-09 | 2018-11-09 | A kind of preparation method and application of the flexible ultra-thin all-solid-state supercapacitor based on titanium carbide |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109809481A (en) * | 2019-04-10 | 2019-05-28 | 南京邮电大学 | A kind of polyhedral method of titanium dioxide using the preparation of titanium carbide ultrathin nanometer piece with hollow structure |
| CN109887758A (en) * | 2019-03-18 | 2019-06-14 | 南京邮电大学 | A kind of preparation method of the oversize titanium carbide nanometer sheet with pleated structure and its application on electrochemical energy storage |
| CN113563079A (en) * | 2021-07-02 | 2021-10-29 | 东北大学 | Preparation method of series of novel tungsten-rare earth-based MAX phases and derivative two-dimensional tungsten-based layered carbide thereof |
| CN114773858A (en) * | 2022-03-30 | 2022-07-22 | 华南理工大学 | Flame-retardant tracking-resistant silicone rubber composition and preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109887758A (en) * | 2019-03-18 | 2019-06-14 | 南京邮电大学 | A kind of preparation method of the oversize titanium carbide nanometer sheet with pleated structure and its application on electrochemical energy storage |
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| CN113563079A (en) * | 2021-07-02 | 2021-10-29 | 东北大学 | Preparation method of series of novel tungsten-rare earth-based MAX phases and derivative two-dimensional tungsten-based layered carbide thereof |
| CN114773858A (en) * | 2022-03-30 | 2022-07-22 | 华南理工大学 | Flame-retardant tracking-resistant silicone rubber composition and preparation method and application thereof |
| CN114773858B (en) * | 2022-03-30 | 2023-05-23 | 华南理工大学 | Flame-retardant tracking-resistant silicone rubber composition and preparation method and application thereof |
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Application publication date: 20190312 |