CN105244188A - Preparation method of carbon nano tube yarn flexible super capacitor composite electrode material - Google Patents
Preparation method of carbon nano tube yarn flexible super capacitor composite electrode material Download PDFInfo
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- CN105244188A CN105244188A CN201510687692.6A CN201510687692A CN105244188A CN 105244188 A CN105244188 A CN 105244188A CN 201510687692 A CN201510687692 A CN 201510687692A CN 105244188 A CN105244188 A CN 105244188A
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- 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
Abstract
The invention discloses a preparation method of a carbon nanotube yarn flexible super capacitor composite electrode material. The method comprises the steps of textile process preparation of carbon nanotube yarns, electroplating composite preparation of an electrode material raw product, and heating and purifying processing of an electrode material; and finally a carbon nano tube loaded transition-state metal oxide composite electrode material can be obtained; and transition-state metal oxides attached onto the cathode material include Co3O4 nanoparticles, NiO nanoparticles or MnO2 nanoparticles. The preparation method of the carbon nanotube yarn flexible super capacitor composite electrode material has the advantages of broad application prospect, excellent mechanical performance and green and environmentally-friendly process.
Description
Technical field
The present invention relates to electrode material for super capacitor technical field, be specially the pliable and tough composite electrode material for super capacitor preparation method of a kind of carbon nano-tube yarn.
Background technology
It is high that ultracapacitor has power density, and charge-discharge velocity is fast, the advantages such as cycle life reaches more than ten thousand times, and operating temperature range is wide.Be widely applied in consumer electronic product industries such as automobile, science and techniques of defence, Aero-Space and household electrical appliance, become the focus of countries in the world research.In the research and development of ultracapacitor, how improving the electric capacity content of ultracapacitor, energy density and power density is important research topic, and the exploitation of high performance electrode material is the key technology addressed this problem.
At present, material with carbon element, owing to having the many advantages such as good electric property, mechanical performance, corrosion resistance, chemistry and high-temperature stability, is one of desirable electrode material of ultracapacitor.The caliber of carbon nano-tube is generally a few nanometer to tens nanometers, and length is at several microns to tens microns, and its specific area is large, good conductivity, is the ideal electrode material of ultracapacitor.But the simple carbon nano-tube that uses is as electrode material for super capacitor, its capacitance and energy density limited, often carbon nano-tube and other hawk electric materials combination electrode material be need be prepared into as transiting state metal oxide compound, the ultracapacitor device capacitance of assembling, energy density and stability etc. improved.
Flexible super capacitor can have important using value in fields such as daily electronic product, national defence, the flexible super capacitor of processability excellence to remain in current research an important challenge, and flexible electrode material is the key factor the most of restriction flexible super capacitor.The general carbon paper of self-control support or the carbon cloth of adopting prepares flexible super capacitor as flexible electrode material, but these flexible super capacitors are often two dimension or three-dimensional, can not effectively weave in common wearable daily necessities.Carbon nano-tube yarn is morphologically one-dimensional linear, and mechanical performance, electric conductivity and chemical stability are fine, is to prepare the desirable electrode material of linear pliable and tough ultracapacitor.Regrettably, simple use carbon nano-tube thread material, due to the restriction of its Storage mechanism, its content stored is still not high.
Summary of the invention
The present invention is low for overcoming conventional linear pliable and tough ultracapacitor electric capacity capacity, energy density and the problem that power density is undesirable and mechanical stability is poor etc., the preparation method of the pliable and tough linear composite electrode material for super capacitor of a kind of carbon nano-tube yarn base is provided, have have a extensive future, the feature of the excellent and technique environmental protection of mechanical performance.
The present invention can be achieved through the following technical solutions:
The invention discloses the pliable and tough composite electrode material for super capacitor preparation method of a kind of carbon nano-tube yarn, comprise the following steps:
The weaving preparation of the first step, carbon nano-tube yarn: cross carbon nano pipe array prepared by chemical vapour deposition (CVD), adopting Weaving device to control rotating speed is under 1000 ~ 5000rpm condition, from array carbon nano tube, pull out carbon nano-tube by motor and after rotating twisting weaving to obtain diameter be 20 ~ 50 μm of carbon nano-tube yarns;
The galvanoplastic compound preparation of the thick product of second step, electrode material: adopt three electrode plating methods, using the carbon nano-tube yarn of first step gained as negative electrode, Ag/AgCl is reference electrode, metal platinum is comparison electrode, carries out electroplating the thick product obtaining electrode material in the electroplate liquid containing transiting state metal salt;
The heating purification processes of the 3rd step, electrode material: after prepared by the galvanoplastic compound of the thick product of second step electrode material, the thick product of second step electrode material of second step gained is heated 10 ~ 60min under 150 ~ 250 DEG C of conditions, final carbon nanotube loaded transiting state metal oxide combination electrode material can be obtained.
Preferably, carbon nano-pipe array described in the first step is classified as the multi-walled carbon nano-tubes of chemical vapour deposition (CVD), and in described carbon nano pipe array, Single Carbon Nanotubes length is 250 ~ 400 μm, and diameter is 10 ~ 30nm.
Preferably, three electrode plating methods described in second step are constant potential plating, and the voltage of plating is ~ 0.5 ~ 2.0V; Electroplating time is 5 ~ 500s; Electroplate liquid is the aqueous solution of containing metal sodium salt and transiting state metal salt.
Preferably, the metal sodium salt contained by described electroplate liquid is NaNO
3, Na
2sO
4, one or more in NaCl etc.
Preferably, in described electroplate liquid, contained transiting state metal salt is Co (NO
3)
2, CoSO
4, Co (CH
3cOO)
2and one or more in their hydrate, the load transitions state metal oxide being now attached to carbon nanotube loaded transiting state metal oxide combination electrode material is Co
3o
4nano particle.
Preferably, contained in described electroplate liquid transiting state metal salt is Ni (NO
3)
2, NiSO
4, Ni (CH
3cOO)
2and one or more in their hydrate, the load transitions state metal oxide being now attached to carbon nanotube loaded transiting state metal oxide combination electrode material is NiO nano particle.
Preferably, in described electroplate liquid, contained transiting state metal salt is Mn (NO3)
2, Mn (SO
4)
2, Mn (CH
3cOO)
2and one or more in their hydrate, the load transitions state metal oxide being now attached to carbon nanotube loaded transiting state metal oxide combination electrode material is MnO
2nano particle.
Preferably, the concentration of described metal sodium salt is 0.05 ~ 0.5mol/L, and the concentration of transiting state metal salt is 0.01 ~ 1.0mol/L.The solvent of the described aqueous solution is redistilled water.
The pliable and tough composite electrode material for super capacitor preparation method of a kind of carbon nano-tube yarn of the present invention, has following beneficial effect:
The first, have a extensive future, the carbon nano-tube yarn based super capacitor combination electrode material prepared by the present invention is first by simple and mechanical spinning weaving carbon nano-tube yarn, then by a step galvanoplastic load transitions state metal oxide.Do not need complicated process equipment, preparation process is simple, has good using value.
The second, stable mechanical property, carbon nano-tube yarn based composites prepared by the present invention can be used as pliable and tough linear electrode material for super capacitor, have good mechanical stability, pliability excellent and the performance such as arbitrarily can to bend, such ultracapacitor is woven in daily life furnishings by Weaving method.
Three, technique environmental protection, the present invention adopts step constant potential galvanoplastic at carbon nano-tube yarn linear load transiting state metal oxide, and electroplating bath components used is simple, environmentally friendly.Electroplating technology is simply controlled, and not containing corrosive gas, plating normal temperature carries out, and electroplating process is without discharge of steam.
Embodiment
In order to make those skilled in the art person understand technical scheme of the present invention better, below in conjunction with embodiment, product of the present invention is described in further detail.
Embodiment 1
The pliable and tough composite electrode material for super capacitor preparation method of a kind of carbon nano-tube yarn of the present invention, is specifically carried out: weaved under rotating speed is 2000rpm condition by self-control spinning equipment and prepare the carbon nano-tube yarn that diameter is about 30 μm according to the following steps; Adopt step constant potential galvanoplastic, using this carbon nano-tube yarn as negative electrode, Ag/AgCl is reference electrode, and metal platinum is comparison electrode, containing 1.0mol/LCo (NO
3)
2, the NaNO of 0.1mol/L
3distilled water electroplate liquid in electroplate, under-1.0V constant voltage condition, electroplate 5min, after having electroplated by this carbon nano-tube complex yarn 200
oheat 10min in an oven under C condition, obtain this carbon nano-tube yarn linear load Co
3o
4combination electrode material.
Embodiment 2
The pliable and tough composite electrode material for super capacitor preparation method of a kind of carbon nano-tube yarn of the present invention, is specifically carried out: weaved under rotating speed is 2000rpm condition by self-control spinning equipment and prepare the carbon nano-tube yarn that diameter is about 31 μm according to the following steps; Adopt step constant potential galvanoplastic using this carbon nano-tube yarn as negative electrode, Ag/AgCl is reference electrode, and metal platinum is comparison electrode, containing 1.0mol/LNi (NO
3)
2, the NaNO of 0.1mol/L
3distilled water electroplate liquid in electroplate, under-1.0V constant voltage condition, electroplate 6min, after having electroplated by this carbon nano-tube complex yarn 170
oheat 30min in an oven under C condition, obtain this carbon nano-tube yarn linear load NiO combination electrode material.
Embodiment 3
The pliable and tough composite electrode material for super capacitor preparation method of a kind of carbon nano-tube yarn of the present invention, is specifically carried out: weaved under rotating speed is 5000rpm condition by self-control spinning equipment and prepare the carbon nano-tube yarn that diameter is about 36 μm according to the following steps; Adopt step constant potential galvanoplastic, using this carbon nano-tube yarn as negative electrode, Ag/AgCl is reference electrode, and metal platinum is comparison electrode, containing 0.2mol/LMnSO
4, the Na of 0.1mol/L
2sO
4distilled water electroplate liquid in electroplate, under-1.5V constant voltage condition, electroplate 1min, after having electroplated by this carbon nano-tube complex yarn 170
oheat 30min in an oven under C condition, obtain this carbon nano-tube yarn linear load MnO
2combination electrode material.
Embodiment 4
The pliable and tough composite electrode material for super capacitor preparation method of a kind of carbon nano-tube yarn of the present invention, is specifically carried out: weaved under rotating speed is 3000rpm condition by self-control spinning equipment and prepare the carbon nano-tube yarn that diameter is about 20 μm according to the following steps; Adopt step constant potential galvanoplastic, using this carbon nano-tube yarn as negative electrode, Ag/AgCl is reference electrode, and metal platinum is comparison electrode, containing 0.2mol/LCo (CH
3cOO)
2, electroplate in the distilled water electroplate liquid of the NaCl of 0.5mol/L, under-0.8V constant voltage condition, electroplate 3min, after having electroplated by this carbon nano-tube complex yarn at baking oven 200
oheat 2min in an oven under C condition, obtain this carbon nano-tube yarn linear load Co
3o
4combination electrode material.
Embodiment 5
The pliable and tough composite electrode material for super capacitor preparation method of a kind of carbon nano-tube yarn of the present invention, is specifically carried out: weaved under rotating speed is 2000rpm condition by self-control spinning equipment and prepare the carbon nano-tube yarn that diameter is about 25 μm according to the following steps; Adopt step constant potential galvanoplastic, using this carbon nano-tube yarn as negative electrode, Ag/AgCl is reference electrode, and metal platinum is comparison electrode, containing 0.3mol/LNiSO
4, electroplate in the distilled water electroplate liquid of the NaCl of 0.2mol/L, under-1.0V constant voltage condition, electroplate 2min, after having electroplated by this carbon nano-tube complex yarn thing 150
oin Muffle furnace, heat 60min under C condition, obtain this carbon nano-tube yarn linear load NiO combination electrode material.
In order to verify that the present invention prepares the performance of gained combination electrode material, carry out electric performance test and measuring mechanical property to the combination electrode material of embodiment 1 ~ 5 gained respectively, concrete outcome is as follows:
1) measuring mechanical property method is: the capacitance conservation rate after this electrode material is assembled into symmetrical ultracapacitor after 180o bends 100 times repeatedly.Concrete data are as shown in table 1:
Table 1 electrode material assembling ultracapacitor bends the capacitance conservation rate of 100 times at 180o repeatedly
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
| Capacitance conservation rate/% | 95 | 92 | 94 | 93 | 93 |
2) electrical performance test method is: using previously prepared good carbon nano-tube yarn composite material as pliable and tough electrode, using PVA-H2SO4 gel (it is in 1molL-1H2SO4 that 5gPVA is dissolved in 50mL molar concentration) as electrolyte and barrier film, adopt CHI660E electrochemical workstation, according to gained cyclic curve under 0.1Vs-1 sweep speed, calculate specific capacitance and energy density.Concrete data are as shown in table 2:
The capacitance of table 2 electrode material assembling ultracapacitor and energy density data table
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
| Capacitance (mF/cm 2） | 43 | 24 | 37 | 40 | 26 |
| Energy density (uWh/ cm 2） | 1.06 | 0.47 | 0.82 | 1.02 | 0.51 |
The above, be only preferred embodiment of the present invention, not does any pro forma restriction to the present invention; The those of ordinary skill of all industry all can shown in by specification and the above and implement the present invention swimmingly; But all those skilled in the art are not departing within the scope of technical solution of the present invention, disclosed above technology contents can be utilized and make a little change, modify with differentiation equivalent variations, be Equivalent embodiments of the present invention; Meanwhile, all according to substantial technological of the present invention to the change of any equivalent variations that above embodiment is done, modify and differentiation etc., within the protection range all still belonging to technical scheme of the present invention.
Claims (8)
1. the pliable and tough composite electrode material for super capacitor preparation method of carbon nano-tube yarn, is characterized in that comprising the following steps:
The weaving preparation of the first step, carbon nano-tube yarn: cross carbon nano pipe array prepared by chemical vapour deposition (CVD), adopting Weaving device to control rotating speed is under 1000 ~ 5000rpm condition, from array carbon nano tube, pull out carbon nano-tube by motor and after rotating twisting weaving to obtain diameter be 20 ~ 50 μm of carbon nano-tube yarns;
The galvanoplastic compound preparation of the thick product of second step, electrode material: adopt three electrode plating methods, using the carbon nano-tube yarn of first step gained as negative electrode, Ag/AgCl is reference electrode, metal platinum is comparison electrode, carries out electroplating the thick product obtaining electrode material in the electroplate liquid containing transiting state metal salt;
The heating purification processes of the 3rd step, electrode material: after prepared by the galvanoplastic compound of the thick product of second step electrode material, the thick product of second step electrode material of second step gained is heated 10 ~ 60min under 150 ~ 250 DEG C of conditions, final carbon nanotube loaded transiting state metal oxide combination electrode material can be obtained.
2. the pliable and tough composite electrode material for super capacitor preparation method of carbon nano-tube yarn according to claim 1, it is characterized in that: carbon nano-pipe array described in the first step is classified as the multi-walled carbon nano-tubes of chemical vapour deposition (CVD), in described carbon nano pipe array, Single Carbon Nanotubes length is 250 ~ 400 μm, and diameter is 10 ~ 30nm.
3. the pliable and tough composite electrode material for super capacitor preparation method of carbon nano-tube yarn according to claim 2, is characterized in that: three electrode plating methods described in second step are constant potential plating, and the voltage of plating is ~ 0.5 ~ 2.0V; Electroplating time is 5 ~ 500s; Electroplate liquid is the aqueous solution of containing metal sodium salt and transiting state metal salt.
4. the pliable and tough composite electrode material for super capacitor preparation method of carbon nano-tube yarn according to claim 3, is characterized in that: the metal sodium salt contained by described electroplate liquid is NaNO
3, Na
2sO
4, one or more in NaCl etc.
5. the pliable and tough composite electrode material for super capacitor preparation method of carbon nano-tube yarn according to claim 3, is characterized in that: in described electroplate liquid, contained transiting state metal salt is Co (NO
3)
2, CoSO
4, Co (CH
3cOO)
2and one or more in their hydrate.
6. the pliable and tough composite electrode material for super capacitor preparation method of carbon nano-tube yarn according to claim 4, is characterized in that: transiting state metal salt contained in described electroplate liquid is Ni (NO
3)
2, NiSO
4, Ni (CH
3cOO)
2and one or more in their hydrate.
7. the pliable and tough composite electrode material for super capacitor preparation method of carbon nano-tube yarn according to claim 4, is characterized in that: in described electroplate liquid, contained transiting state metal salt is Mn (NO3)
2, Mn (SO
4)
2, Mn (CH
3cOO)
2and one or more in their hydrate.
8. the pliable and tough composite electrode material for super capacitor preparation method of the carbon nano-tube yarn according to any one of claim 5 ~ 7 claim, it is characterized in that: the concentration of described metal sodium salt is 0.05 ~ 0.5mol/L, the concentration of transiting state metal salt is 0.01 ~ 1.0mol/L.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105780242A (en) * | 2016-05-04 | 2016-07-20 | 东华大学 | Carbon nanotube fabric with multi-scale pore structure and preparation method thereof |
| CN106206053A (en) * | 2016-08-09 | 2016-12-07 | 东华大学 | There is the fabric of multistage conductive channel and utilize its method preparing ultracapacitor |
| CN107248456A (en) * | 2017-04-26 | 2017-10-13 | 东莞市鸿愃实业有限公司 | The preparation method of CNT yarn based flexible super capacitor combination electrode material |
| CN108109855A (en) * | 2017-12-15 | 2018-06-01 | 中南民族大学 | A kind of preparation method of the flexible super capacitor based on wire/cotton thread/polymer complex yarn |
| CN109390549A (en) * | 2018-10-17 | 2019-02-26 | 南通南京大学材料工程技术研究院 | A kind of new preparation process of foldable lithium ion cell positive |
| CN110752095A (en) * | 2019-11-15 | 2020-02-04 | 重庆大学 | Method for synthesizing metal oxide array on conductive fiber, fiber structure metal/oxide composite electrode and application |
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