CN105070531B - A kind of preparation method of the stretchable formula linear supercapacitor based on polyurethane carbon nano tube compound material - Google Patents
A kind of preparation method of the stretchable formula linear supercapacitor based on polyurethane carbon nano tube compound material Download PDFInfo
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- CN105070531B CN105070531B CN201510473280.2A CN201510473280A CN105070531B CN 105070531 B CN105070531 B CN 105070531B CN 201510473280 A CN201510473280 A CN 201510473280A CN 105070531 B CN105070531 B CN 105070531B
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Abstract
The invention provides a kind of preparation method of the stretchable formula linear supercapacitor based on polyurethane/multi-wall carbon nano-tube composite material, comprise the following steps:TPUE and multi-walled carbon nanotube are added into double screw extruder and carry out dispensing, internal layer TPU/CNT composites are obtained;TPUE, multi-walled carbon nanotube and calcium carbonate superfine powder are added into double screw extruder and carry out dispensing, outer layer TPU/CNT/ calcium carbonate superfine powder composites are obtained;By internal layer TPU/CNT composites and outer layer TPU/CNT/ calcium carbonate superfine powder composites, co-extrusion prepares composite fibre;By the composite fibre through diluted acid pore, surface precipitated nanocrystals MnO2, coated electrolyte and TPU/CNT solution, you can obtain stretchable formula linear supercapacitor.Ultracapacitor preparation method of the present invention, it is simple to operate, it is with low cost, it is very suitable for industrial applications.
Description
Technical field
The invention belongs to ultracapacitor preparation method technical field, more specifically, more particularly to a kind of be based on polyurethane
The preparation method of the stretchable formula linear supercapacitor of carbon nano tube compound material.
Background technology
Existing stretchable formula ultracapacitor prepares typically more complexity, and tensile property is poor, and electrolyte and electrode
The adhesiveness of material is poor, causes the electrochemistry of stretchable ultracapacitor and can reach related request.
CNT is common conductive material in ultracapacitor due to possessing preferable electric conductivity, but its specific volume
Value is low, limits the application of its capacitor prepared;Nanometer MnO2Due to high-energy-density, high-specific surface area, than
Capacity is high, is preferable electrode material, but because self-conductance rate is low, result in the MnO under large area2Poor electrochemistry
How performance, therefore, effectively combine both, and realizes that preparation technology is simple, stretchable base material and electrolyte and
The good adhesiveness of electrode material, is technical barrier urgently to be resolved hurrily in current stretchable formula ultracapacitor.
The content of the invention
It is an object of the invention to be based on polyurethane carbon nanotube composite there is provided one kind according to the deficiencies in the prior art
The preparation method of the stretchable formula linear supercapacitor of material.
The above-mentioned purpose of the present invention is achieved through the following technical solutions:
The invention provides a kind of stretchable formula linear supercapacitor based on polyurethane carbon nano tube compound material
Preparation method, comprises the following steps:
S1. TPUE and multi-walled carbon nanotube are added into double screw extruder to be blended, obtained
TPU/CNT composites;
S2. TPUE, multi-walled carbon nanotube and calcium carbonate superfine powder are added into double screw extruder to carry out
Blending, obtains TPU/CNT/ calcium carbonate superfine powder composites;
S3. gained TPU/CNT/ calcium carbonate superfine powders in gained TPU/CNT composites in S1 steps and S2 steps are combined
Material, is molded, the drawing and filament forming under 2 ~ 6 m/min speed through double-layer coextrusion equipment, obtains internal layer for TPU/CNT composite woods
Material, outer layer is the composite fibre of TPU/CNT/ calcium carbonate superfine powder composites;
S4. gained composite fibre in S3 steps, through diluted acid pore, is obtained into the composite fibre of porous surface;
S5. by the composite fibre of gained porous surface in S4, through chemical precipitation method surface precipitated nanocrystals MnO2, precipitated
Cheng Hou, surface coated electrolyte, after after fully contact certain time, coating TPU/CNT solution in surface obtains stretchable formula wire
Ultracapacitor.
TPU/CNT composites not only can be as composite fibre substrate in S1, and is coated in the second layer as super
The electrode of capacitor, the TPU/CNT/ nanometers MnO with internal layer2Material formation asymmetry electrode.
Preferably, TPUE and multi-walled carbon nanotube adding proportion in the S1, according to the mass fraction
For(6~8):(2~4), the screw speed of the double screw extruder is 100 r/min.
Preferably, TPUE, multi-walled carbon nanotube and calcium carbonate superfine powder adding proportion in the S2, are pressed
Mass fraction is calculated as 6:3:1.
Preferably, a diameter of 7 ~ 12 mm of the multi-walled carbon nanotube.
Preferably, a diameter of 1 μm of calcium carbonate superfine powder in the S2.
Preferably, the ultra-fine CaCO of internal layer TPU/CNT composites a diameter of 2 ~ 2.5mm, outer layer TPU/CNT/ in the S33
The thickness of composite is 0.5 ~ 1mm.
Preferably, pore step is under 150% stretching condition, to be passed through thread composite fibre with roller in the S4
In the reactive tank for filling 10% watery hydrochloric acid, roller slewing rate utilizes calcium carbonate and watery hydrochloric acid reaction generation gas in 1 m/min
Pore.
Preferably, chemical precipitation method surface precipitated nanocrystals MnO in the S52Method is that 0.1 is added in reactive tank
mol/L Mn(NO3)2Solution is as electrolyte, and composite fibre is passed through hydrogen and reacted as working electrode, control hydrogen speed
Rate, the nanometer MnO2A diameter of 5nm.
Preferably, use polyvinyl acidic hydrogel in coated electrolyte in the S5, wherein, polyvinyl alcohol with
The mass ratio of phosphoric acid is 1:1.5.
Preferably, the method that TPU/CNT solution is coated in the S5 is first by TPUE according to 10 g/
L ratio matches somebody with somebody generating polyurethane toluene solution, then according to mass ratio TPU:CNT is(6~8):(2~4)Ratio add many wall carbon
Nanotube is made into TPU/CNT solution and is coated, and coats 2 ~ 3 layers, the thickness of coating is 0.5 ~ 1mm.
Preferably, double screw extruder extrusion temperature is 185 ~ 225 DEG C in the S1 and S2, and forming temperature is in the S3
185~225℃。
The ultracapacitor prepared using above-mentioned preparation method is all fallen in the scope of protection of the present invention.
Further, application of the material prepared by preparation method of the present invention in stretchable energy-storage travelling wave tube is prepared
Also in the scope of the present invention.
TPUE has excellent elastic, good caking property.Multi-walled carbon nanotube has relatively low
Resistance, special nano-space structure and high-specific surface area, with good electric conductivity.This patent uses multi-wall carbon nano-tube
Pipe, caliber be about two kinds of materials of 7 ~ 12nm, TPU and CNT in specific proportions, with(6~8):(2~4)Ratio mixing, by double spiral shells
Rotation extruder is prepared in TPU/CNT composites, composite not only due to the dispersed formation of multi-walled carbon nanotube is led
Electric network, so that with good electric conductivity, and because TPU presence so that material has good tensility.
This patent prepares the ultra-fine CaCO of TPU/CNT and TPU/CNT/ by Twin screw extruder3Two kinds of composites, then
Prepare donble layer composite fibre through double-layer coextrusion, this method in actual applications can consecutive production, with good industry
Application value.
Nanometer MnO2Because with high-energy-density, high-specific surface area, abundance, price is cheap, theoretical specific capacity is high
Up to 1400Fg-1, become a kind of highly desirable environmentally friendly electrode material.But because self-conductance rate is low, it result in big
MnO under area2Poor chemical property, therefore, in order to improve electrical conductivity, preparing porous, film or composite is
MnO2One of path pursued.This patent dilute acid pretreatment under stretching condition falls causes composite fiber surface many after calcium carbonate superfine powder
Hole, then using electrochemical deposition method surface deposition nanometer MnO2, prepare TPU/CNT/ nanometers of MnO2Composite.Material because
For CNT and nanometer MnO2It is compound, enhance the electrical conductivity and specific capacity of material.During chemical precipitation, Mn(NO3)2For electricity
Liquid is solved, composite fibre is passed through hydrogen and reacted, by controlling Mn as working electrode(NO3)2Concentration, current density and electricity
Kinetic potential can prepare the MnO of high concentration2It is deposited on composite fiber surface, MnO2Diameter is about 5nm, because composite fiber surface
Pore, the MnO of precipitation2It can be distributed, be consolidated very much during stretching in hole.
Compared with prior art, the present invention has advantages below and beneficial effect:
The TPU/CNT that the present invention is provided and TPU/CNT/ nanometers of MnO2Composite formation asymmetry electrode, plays respective
Advantage, cover the shortage, produce cooperative effect, obtain with low cost, high performance combined electrode supercapacitor.
Strongly adherent between the gel electrolyte and flexible electrode of the stretchable ultracapacitor that the present invention is provided, can
Break away from the existing package technique of stretchable ultracapacitor need to by stretchable substrate constraint, simplify packaging technology.
The ultracapacitor prepared according to the present embodiment is when extensibility is up to 150%, and its specific capacitance is kept substantially
It is constant;It is 2 mA/cm in current density2When, after the ultracapacitor cycle charge-discharge 2000 times, its capacitance fade be less than or
Equal to 10%.
Ultracapacitor preparation method of the present invention, it is simple to operate, it is with low cost, it is very suitable for industrial applications.
Brief description of the drawings
Fig. 1 is the preparation method flow chart that the embodiment of the present invention 1 is provided.
Fig. 2 is to prepare TPU/CNT (70/30) composite through double screw extruder melt blending.
Fig. 3 is electrochemical process nanometer MnO on TPU/CNT billot area loads2Particle.
Fig. 4 is in TPU/CNT/ nanometers of MnO2Billot surface coats PVA/H3PO4Gel electrolyte.
Fig. 5 is in TPU/CNT/ nanometers of MnO2/ electrolyte billot surface coats TPU&CNT toluene solution.
Fig. 6 is the stretchable formula linear supercapacitor structure based on polyurethane & carbon nano tube compound materials.
Fig. 7 is the coextrusion operating diagram of embodiment 1.
Embodiment
This technology is further illustrated below in conjunction with specific embodiment, but embodiment does not do any type of to this technology
Limit.Unless stated otherwise, the reagent of the invention used, method and apparatus is the art conventional reagent, methods and apparatus.
Embodiment 1, is the preparation method flow chart of the present embodiment 1 as shown in Figure 1
The preparation of TPU/CNT composites:
As shown in Fig. 2 according to mass ratio being 7 by TPUE and multi-walled carbon nanotube:3 ratio is added
Ratcheting type double screw extruder carries out dispensing.Screw speed is about 100 r/min.From 7:3 ratio, is because CNT's contains
Amount at 0 to 20%, the electric conductivity of TPU/CNT composites is very small, CNT content between 20% to 30%, composite
Electric conductivity performance quickly increases, and CNT content is after 30%, and growth rate slows down, so CNT contents have between 30% to 40%
There is good electric conductivity.Secondly, with the increase of CNT contents, the Young's modulus and tensile strength of TPU/CNT composites are continuous
Increase, the elongation of composite constantly declines.EVA/10 wt%CNTT Young's modulus, tensile strength and elongation are respectively
18.5 MPa, 5.8 MPa and 436%, EVA/30 wt%CNT Young's modulus, tensile strength and elongation are respectively 372.9
MPa, 22.3 MPa and 55.3%.So, in the case that CNT contents are 30%, TPU/CNT composites have excellent property
Can, it is suitable as stretchable conductive material and uses.
The preparation of TPU/CNT/ calcium carbonate superfine powder composites:
By TPUE, multi-walled carbon nanotube and calcium carbonate superfine powder according to 6:3:1 ratio adds ratcheting
Type double screw extruder carries out dispensing.Screw speed is about 100 r/min.The calcium carbonate superfine powder mass fraction used is left 10%
In the case of the right side, calcium carbonate superfine powder can be uniformly dispersed in composite fiber surface, removed through watery hydrochloric acid and insert gap calcium carbonate pore,
Pore size distribution is uniform, and pore size meets follow-up with chemical precipitation method surface precipitated nanocrystals MnO2Technological requirement.Elastic polyurethane
Body, multi-walled carbon nanotube are according to 6:3 ratio, can also meet the requirement of composite fibre mechanical property and electric conductivity.
It is many used in TPU/CNT composites and TPU/CNT/ calcium carbonate superfine powder composites prepared by this patent
A diameter of 7 ~ 12 mm of wall carbon nano tube.
The diameter that calcium carbonate is added in TPU/CNT/ calcium carbonate superfine powder composites prepared by this patent is about 1 μm.
It is that TPU/CNT composite outer layers are the ultra-fine CNTs of TPU/CNT/ that internal layer is prepared with double-layer coextrusion equipment
Composite fibre:
As shown in fig. 7, both the above composite is produced into internal layer TPU/CNT through double-layer coextrusion extruder extrusion die
The ultra-fine CaCO of composite a diameter of 2 ~ 2.5mm, outer layer TPU/CNT/3Thickness of composite material is 0.5 ~ 1mm composite fibre.So
After cool down, use crawler type pulling equipment, the drawing and filament forming under 2 ~ 6 m/min speed.
Composite fibre removes through watery hydrochloric acid and inserts gap calcium carbonate pore
Under 150% stretching condition, in the reactive tank with roller by thread composite fibre by filling 10% watery hydrochloric acid, rolling
Slewing rate is taken turns in 1 m/min, calcium carbonate and watery hydrochloric acid reaction generation gas pore is utilized.
The composite fibre of surface pore is through chemical precipitation method surface precipitated nanocrystals MnO2
As shown in figure 3, adding 0.1 mol/L Mn during chemical precipitation, in reactive tank(NO3)2Solution is used as electricity
Liquid is solved, composite fibre is passed through hydrogen and reacted as working electrode, control hydrogen gas rate, make obtained MnO2Diameter is about
5nm(The time of composite fibre intrusion reactive tank is 45s, the MnO of production2It is evenly distributed in hole, content is adapted to), because multiple
The pore of condensating fiber surface, the MnO of precipitation2It can be distributed, be consolidated very much during stretching in hole.
Composite fiber surface coated electrolyte
As shown in figure 4, using PVA Acidic hydrogels, PVA in ultracapacitor:Phosphoric acid quality ratio is 1:1.5, will
Electrolyte is coated in composite fibre electrode surface, electrolyte is fully contacted with electrode.
Surface coats TPU/CNT solution
As shown in figure 5, at normal temperatures, TPU matches somebody with somebody generating polyurethane toluene solution according to 10 g/L ratio, then according to TPU:
CNT is 7:3 ratio adds multi-walled carbon nanotube, and sonic oscillation is uniform, is made into TPU/CNT solution, TPU/CNT solution is coated
Formerly be coated with the composite fibre electrode surface of dielectric substrate, coat 2 ~ 3 layers, the thickness of coating is 0.5 ~ 1mm, both it is stretchable
Linear supercapacitor.
Fig. 6 is the structural representation for the ultracapacitor that the embodiment of the present invention 1 is obtained.
The ultracapacitor prepared according to the present embodiment is when extensibility is up to 150%, and its specific capacitance is kept substantially
It is constant;It is 2 mA/cm in current density2When, after the ultracapacitor cycle charge-discharge 2000 times, its capacitance fade be less than or
Equal to 10%.Strongly adherent between the gel electrolyte and flexible electrode of the ultracapacitor that the present invention is provided, can break away from
Can draw the existing package technique of flexible super capacitor need to by stretchable substrate constraint, simplify packaging technology, and pass through
Surface pore, the MnO of precipitation2Be evenly distributed in hole, during stretching very consolidate, reached simultaneously reinforcing material electrical conductivity and
The double effectses of specific capacity.
Claims (9)
1. a kind of preparation method of the stretchable formula linear supercapacitor based on polyurethane carbon nano tube compound material, its feature
It is, comprises the following steps:
S1. TPUE and multi-walled carbon nanotube are added into double screw extruder and carries out dispensing, obtain TPU/
CNT composites;
S2. TPUE, multi-walled carbon nanotube and calcium carbonate superfine powder are added into double screw extruder and carry out dispensing,
Obtain TPU/CNT/ calcium carbonate superfine powder composites;
S3. by gained TPU/CNT/ calcium carbonate superfine powder composite woods in gained TPU/CNT composites in S1 steps and S2 steps
Material, is molded through double-layer coextrusion equipment, and uses crawler type pulling equipment, and the drawing and filament forming under 2 ~ 6 m/min speed obtains interior
Layer is TPU/CNT composites, and outer layer is the composite fibre of TPU/CNT/ calcium carbonate superfine powder composites;
S4. gained composite fibre in S3 steps, through diluted acid pore, is obtained into the composite fibre of porous surface;
S5. by the composite fibre of gained porous surface in S4, through chemical precipitation method surface precipitated nanocrystals MnO2, after the completion of precipitation,
Surface coated electrolyte, after after fully contact certain time, coating TPU/CNT solution in surface obtains stretchable formula wire super
Capacitor.
2. the stretchable formula linear supercapacitor according to claim 1 based on polyurethane carbon nano tube compound material
Preparation method, it is characterised in that TPUE and multi-walled carbon nanotube adding proportion in the S1, by quality
Number is calculated as 7:3, the screw speed of the double screw extruder is 100 r/min.
3. the stretchable formula linear supercapacitor according to claim 1 based on polyurethane carbon nano tube compound material
Preparation method, it is characterised in that TPUE, multi-walled carbon nanotube and calcium carbonate superfine powder addition ratio in the S2
Example, is according to the mass fraction 6:3:1.
4. the stretchable formula wire super capacitor based on polyurethane carbon nano tube compound material according to claim 1 or 3
The preparation method of device, it is characterised in that a diameter of 1 μm of calcium carbonate superfine powder in the S2.
5. the stretchable formula linear supercapacitor according to claim 1 based on polyurethane carbon nano tube compound material
Preparation method, it is characterised in that internal layer TPU/CNT composites a diameter of 2 ~ 2.5mm, outer layer TPU/CNT/ are ultra-fine in the S3
CaCO3The thickness of composite is 0.5 ~ 1mm.
6. the stretchable formula linear supercapacitor according to claim 1 based on polyurethane carbon nano tube compound material
Preparation method, it is characterised in that pore step is under 200% stretching condition, with roller by thread compound fibre in the S4
In reactive tank of the dimension by filling 10% watery hydrochloric acid, roller slewing rate is given birth in 1 m/min using calcium carbonate and watery hydrochloric acid reaction
Into gas pore.
7. the stretchable formula linear supercapacitor according to claim 1 based on polyurethane carbon nano tube compound material
Preparation method, it is characterised in that chemical precipitation method surface precipitated nanocrystals MnO in the S52Method is to be added in reactive tank
0.1 mol/L Mn(NO3)2Solution is as electrolyte, and composite fibre is passed through hydrogen and reacted as working electrode, controls hydrogen
Gas velocity rate, the nanometer MnO2A diameter of 5nm.
8. the stretchable formula linear supercapacitor according to claim 1 based on polyurethane carbon nano tube compound material
Preparation method, it is characterised in that use polyvinyl acidic hydrogel in the S5 in coated electrolyte, wherein, poly- second
The mass ratio of enol and phosphoric acid is 1:1.5.
9. the stretchable formula linear supercapacitor according to claim 1 based on polyurethane carbon nano tube compound material
Preparation method, it is characterised in that the method for TPU/CNT solution is coated in the S5 first to press TPUE
Ratio according to 10 g/L is made into polyurethane solutions, then according to mass ratio TPU:CNT is 7:3 ratio adds multi-walled carbon nanotube
TPU/CNT solution is made into be coated.
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CN105428082B (en) * | 2015-12-27 | 2018-02-27 | 复旦大学 | Stretchable ultracapacitor based on nitrogen-doped carbon nanometer pipe array/polyurethane combination electrode and preparation method thereof |
CN110379642B (en) * | 2019-07-31 | 2021-02-26 | 河北科技大学 | Stretchable nanofiber, application thereof, stretchable capacitor electrode comprising stretchable nanofiber and preparation method |
CN111029169B (en) * | 2019-12-31 | 2021-12-17 | 西安工业大学 | Nanoparticle sandwich composite material and preparation method thereof |
CN113916416B (en) * | 2021-09-23 | 2023-05-16 | 北京科技大学 | High-permeability strain non-sensitive electronic skin and preparation method thereof |
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CN103194858A (en) * | 2013-04-23 | 2013-07-10 | 北京化工大学 | Elastomer composite with high dielectric constant and low dielectric loss and preparation method thereof |
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CN103194858A (en) * | 2013-04-23 | 2013-07-10 | 北京化工大学 | Elastomer composite with high dielectric constant and low dielectric loss and preparation method thereof |
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