CN104658765B - A kind of stainless steel nonwoven fabric base electrode material for super capacitor, preparation method and application - Google Patents
A kind of stainless steel nonwoven fabric base electrode material for super capacitor, preparation method and application Download PDFInfo
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- CN104658765B CN104658765B CN201510056357.6A CN201510056357A CN104658765B CN 104658765 B CN104658765 B CN 104658765B CN 201510056357 A CN201510056357 A CN 201510056357A CN 104658765 B CN104658765 B CN 104658765B
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Abstract
The invention discloses a kind of stainless steel nonwoven fabric base electrode material for super capacitor, preparation method and application, using stainless steel non-woven fabrics as base material, the nanostructure of one of growth in situ metal oxide, bimetallic oxide, bimetallic sulfide, metal hydroxides and conducting polymer on the base material obtains the stainless steel nonwoven fabric base Novel super capacitor electrode material of growth in situ nanostructure.In the selection of base material, compared with carbon cloth and nickel foam, stainless steel non-woven fabrics is as base material, with light, intensity is high, the features such as active material of unit area load is more are higher by other two kinds of base materials with the electrode material either specific discharge capacity of its preparation or area specific capacity.Stainless steel non-woven fabrics is the electrode material for super capacitor that substrate prepares, and the integral area that cyclic voltammetry curve surrounds is bigger than on carbon cloth and nickel foam, and the capacitance of the electrode material based on stainless steel nonwoven fabric base bottom wants some higher.
Description
Technical field
The present invention relates to the preparation of electrode material for super capacitor more particularly to a kind of stainless steel nonwoven fabric base are super
Capacitor electrode material, preparation method and application.
Background technology
Increasingly deficient and environment the deterioration increasingly of traditional fossil energy resource, effectively promotes solar energy and wind energy etc.
The development of regenerative resource.But solar energy, wind energy have fluctuation and intermittence, and effective energy storage device is needed to ensure that it can
The stable grid-connected work in power grid.Meanwhile that also there is an urgent need to development costs is low, environment is friendly for ev industry fast-developing
Energy storage device good, energy density is high.Ultracapacitor is also known as electrochemical capacitor, is between traditional capacitor and secondary cell
Between a kind of new type of energy storage device.Its charge storage be far above Typical physical capacitor, and charge-discharge velocity, efficiency and
Safety is much better than accumulator.
Ultracapacitor can be divided into double electric layers supercapacitor by energy storage mechnism and Faradic pseudo-capacitor (is called counterfeit electricity
Hold).But the process of either double layer capacitor or Faradic pseudo-capacitor, energy storage occurs mainly in the table of electrode
Face.Specific capacitance, electric conductivity, specific surface area and the structural stability of electrode material are super capacitor energy storage and conversion performance
Determinant.Therefore, in order to improve energy density and power density, either double electric layers supercapacitor, faraday is accurate electric
Container or the two hybrid super capacitor, electrode material must have large specific surface area, conductivity height and stable structure
Etc. characteristics.
The preparation method of electrode material mainly has coating and growth in situ two types.But coat the electrode material prepared not
The part specific surface area of its base material is only had lost, technique is cumbersome, and since the addition of binder makes in reaction process
Charge cannot transmit in time, electric conductivity decline.Meanwhile the active material of coating is easy to peel off under mechanicals efforts.And it is former
The electrode material of position growth type then can effectively avoid these problems, not only ensure that the good electric conductivity of situ contact, Er Qiejie
It closes securely, it is easy to operate.Meanwhile the nano structural material of growth largely increases the specific surface area of electrode material.
The three-dimensional conductive base material generally used at present is nickel foam and carbon cloth/paper.Although nickel foam has good
Electric conductivity and higher specific surface area, but it is not corrosion-resistant, and without flexibility, kinking repeatedly is easily broken off.Although carbon cloth/paper tool
Have the advantages that acid and alkali-resistance, good conductivity, flexibility are good, but needed before growth activity substance on carbon cloth/paper with strong oxidizer into
Row hydrophilic treated, bad mechanical strength, in air non-refractory, cause it incompatible with many synthetic methods in addition.Therefore, it seeks
Look for it is a kind of it is new be produced on a large scale corrosion-resistant, flexibility is good, and generally applicable conductive substrates are particularly necessary.
Invention content
Another object of the present invention is to provide that a kind of specific capacity is big, and service life is long, flexible super applied widely electricity
Container.
Technical scheme is as follows：
This law provides a kind of preparation method of stainless steel nonwoven fabric base electrode material for super capacitor first, using stainless steel
Non-woven fabrics is as base material, growth in situ metal oxide, bimetallic oxide, bimetallic vulcanization on the base material
The nanostructure of one of object, metal hydroxides and conducting polymer obtains the stainless steel non-woven fabrics of growth in situ nanostructure
Base novel electrode material for super capacitor.
The preparation method, specifically includes following steps：
A1, stainless steel non-woven fabrics is cleaned, removes organic and inorganic impurity；
A2, prepare corresponding growth metal oxide, bimetallic oxide, bimetallic sulfide, metal hydroxides and
The nanostructure reaction solution of one of conducting polymer；
A3, the stainless steel non-woven fabrics cleaned up is immersed in corresponding reaction solution；
A4, using hydrothermal growth process, in 90-200 DEG C of baking oven, keep the temperature 1-10h；Or electrochemical deposition method is used,
On the working electrode (s by the stainless steel non-woven fabrics folder after cleaning, saturated calomel electrode is reference electrode, and Pt pieces are to electrode, in phase
Potentiostatic electrodeposition 1-60min under the sedimentation potential answered；
A5, treated stainless steel non-woven fabrics is taken out, rinsed dry to get to the stainless of growth in situ multidimensional nanostructure
Steel nonwoven fabric base Novel super capacitor electrode material.
In the preparation method, the metal oxide is MnO2、Fe2O3、Fe3O4、Co3O4, one of CoO；Bimetallic
Oxide is NiCo2O4、ZnCo2O4、NiMo2O4、ZnMn2O4One of；Bimetallic sulfide is NiCo2S4、ZnCo2S4、NiMo2S4、
ZnMn2S4One of；Metal hydroxides Ni (OH)2、Co(OH)2、Fe(OH)3、NixCo(1-x)(OH)6xOne of；Conducting polymer is
One of polyaniline (PAN), polypyrrole (PPY), poly- 3,4-ethylene dioxythiophene (PEDOT).
In the preparation method, obtained electrode material is the nanometer material that growth has different-shape in the step A4
Material, the nano material of the different-shape including piece, stick, line, needle and flower-shape.
In the preparation method, in the step A5, for growth in situ metal oxide, double gold on base material
The stainless steel non-woven fabrics for belonging to oxide will be also heat-treated after rinsing drying：By the stainless steel nonwoven after the reaction of drying
Cloth is placed on Al2O3In crucible, 1-10h is kept the temperature in 200-600 DEG C of air, presoma is pyrolyzed.
The present invention also provides the stainless steel nonwoven fabric base electrode of super capacitor that any of the above-described preparation method obtains
Material.
The present invention also provides stainless steel nonwoven cloth materials to prepare stainless steel nonwoven fabric base electrode material for super capacitor
In application, using stainless steel non-woven fabrics as base material, in base material growth in situ metal oxide, the bimetallic oxygen
The nanostructure of one of compound, bimetallic sulfide, metal hydroxides and conducting polymer, obtains growth in situ nanostructure
Stainless steel nonwoven fabric base Novel super capacitor electrode material.
The present invention is prepared with high-specific surface area, and suppleness is good, and growth has the stainless steel nonwoven fabric base of nanostructure
Electrode material can be applied in energy storage, electric vehicle and various flexible electronic devices.
Description of the drawings
Fig. 1 is to grow NiCo on carbon cloth, nickel foam and stainless steel nonwoven fabric base bottom respectively2O4It is measured after nanostructure
Cyclic voltammetry curve, voltage range are -0.1-0.5V, and sweep speed is 5mV s-1；
Fig. 2 is to grow NiCo on carbon cloth, nickel foam and stainless steel nonwoven fabric base bottom respectively2O4It is measured after nanostructure
Constant current charge-discharge curve, voltage range are -0.15-0.35V, and current density is 1A g-1。
Specific implementation mode
Below in conjunction with specific embodiment, the present invention is described in detail.
The stainless steel nonwoven cloth material that the present invention uses is by a diameter of micro- for the development and production of Bell Ka Te companies of Belgium
The stainless steel fibre of meter level is paved through nonwoven, it is folded match and high temperature sintering forms, be chiefly used in filtration system, micro-structure and carbon cloth phase
Seemingly, have that three-dimensional netted, porous structure, porosity are high, surface area is big, even aperture distribution, flexibility are good, high mechanical strength,
It is a kind of ideal high temperature resistant, corrosion-resistant flexible 3 D base material.
Stainless steel non-woven fabrics is the stainless steel fibre felt (stainless steel is also made to be sintered felt) for being used for filtration system in recent years in fact
Predecessor, stainless steel non-woven fabrics is repressed, after heat treatment is stainless steel fibre felt currently on the market.Currently, domestic Xinxiang
Positive source purifies Science and Technology Ltd. (http：//www.xxzyjh.com/cpzx/jssj/20140217338.html) just have not
Become rusty steel fibre felt product.But stainless steel fibre felt is excessively closely knit, and intensity is excessive, loses flexible and big porosity advantage, real
Border is used for flexible energy storage substrate, can bulk purchase the said firm is repressed, stainless steel non-woven fabrics of heat treatment.
Specific implementation mode one：The stainless steel nonwoven fabric base electrode material system of present embodiment Hydrothermal Growth nanostructure
Preparation Method follows these steps to implement：
One, stainless steel non-woven fabrics is cut into 1 × 3cm2100mL beakers are put into, then add acetone to no mistake non-woven fabrics, ultrasound
7min or so is handled, then 7min is ultrasonically treated with dilute hydrochloric acid.Deionized water is rinsed repeatedly, then with absolute ethyl alcohol ultrasound 7min.It puts
Enter 80 DEG C of air dry oven drying.
Two, hydrothermal growth nano-structured solution is prepared：0.65gNi(NO3)2, 1.3gCo (NO3)2, 1.62g urea, 45mL
Deionized water, 45mL absolute ethyl alcohols.
Three, reaction solution is put into the reaction kettle of polytetrafluoroethyllining lining, dried stainless steel non-woven fabrics is submerged
In solution.
Four, reaction kettle is tightened, is put into 90 DEG C of -200 DEG C of thermostatic drying chambers, hydro-thermal 1-10h.
Five, it after water heating kettle cooling completely, takes out the non-woven fabrics after reaction and is rinsed with deionized water, be put into air dry oven 80
DEG C drying, the stainless steel non-woven fabrics after the reaction of drying is placed on Al2O3In crucible, 1-10h is kept the temperature in 200-600 DEG C of air, it will
Presoma is pyrolyzed into NiCo2O4There is NiCo to get to growth2O4The stainless steel nonwoven fabric base electrode material of nanostructure.
Specific implementation mode two：The present embodiment is different from the first embodiment in that the hydrothermal growth that step 2 is prepared
Solution (5mmol Co (the NO of nanostructure3)2, 10mmol NH4F, 25mmol Co (NH2)2, 70mL H2O).Other steps and
Parameter is same as the specific embodiment one.Obtaining growth has Co3O4The stainless steel nonwoven fabric base electrode material of nanostructure.
Specific implementation mode three：Argon gas is added when present embodiment is heat-treated unlike specific implementation mode two to protect
Shield.Other steps and parameter are identical with embodiment two.Obtaining growth has the stainless steel nonwoven fabric base electricity of CoO nanostructures
Pole material.The effect that present embodiment adds argon gas protection is to keep Co2+It is not oxidized by oxygen at high temperature.
Specific implementation mode four：The present embodiment is different from the first embodiment in that the hydrothermal growth that step 2 is prepared
Solution (the 48mg NiCl of nanostructure2·6H2O, 75mg urea, 30mL H2O) and without the subsequent heat treatment of step 5.Its
Its step and parameter are same as the specific embodiment one.Obtaining growth has Ni (OH)2The stainless steel nonwoven fabric base of nanostructure
Electrode material.
Specific implementation mode five：Have the present embodiment is different from the first embodiment in that step 5 obtains growth
NiCo2O4After the stainless steel nonwoven fabric base electrode material of nanostructure, the Na of 160mmol/L is placed it in2In S solution, 90-200
Hydro-thermal 1-10h at DEG C takes out the non-woven fabrics after reaction and is rinsed with deionized water, be put into forced air drying after water heating kettle cooling completely
80 DEG C of drying of case, obtaining growth has NiCo2S4The stainless steel nonwoven fabric base electrode material of nanostructure.
Specific implementation mode six：Present embodiment electrochemical deposition method grows the stainless steel nonwoven fabric base electrode of nanostructure
Material preparation method follows these steps to implement：
One, electrochemical deposition solution (5mmol Ni (NO are prepared3)2, 10mmol Co (NO3)2, 100mLH2O)；
Two, on the working electrode (s by the stainless steel non-woven fabrics folder by the processing of one step 1 of specific implementation mode, it is heavy to immerse
Product solution.Use Pt pieces for electrode, saturated calomel electrode is reference electrode.
Three, it is deposited with potentiostatic method, chooses deposition voltage -1V, deposit 1-10min.
Four, post-depositional stainless steel non-woven fabrics is taken out, is first rinsed with deionized water, then use washes of absolute alcohol.
Five, the sample after cleaning 60 DEG C of air dry ovens are put into dry.
Present embodiment, which obtains growth, NixCo(1-x)(OH)6xThe stainless steel nonwoven fabric base electrode material of nanostructure.
Specific implementation mode seven：Present embodiment uses cyclic voltammetry from step 3 unlike specific implementation mode six
It is deposited, take-off potential is -1.1V, and termination current potential is -0.5V, sweep speed 5-10mV/s, sedimentation time 20-
60min.Other steps and parameter are identical as specific implementation mode six.
Present embodiment, which obtains growth, NixCo(1-x)(OH)6xThe stainless steel nonwoven fabric base electrode material of nanostructure.
Specific implementation mode eight：The electro-deposition that present embodiment is prepared from step 1 unlike specific implementation mode six is molten
Liquid (10.05g HClO4, 4.65g aniline monomers AN, 100mL H2O).Other steps and parameter are identical as specific implementation mode six.
Present embodiment, which obtains growth, the stainless steel nonwoven fabric base electrode material of polyaniline (PAN) nanostructure.
Specific implementation mode nine：Present embodiment chemical deposition grows the stainless steel nonwoven fabric base electrode material of nanostructure
Preparation method for material follows these steps to implement：
One, chemical deposition solution (0.493g HCl, 0.1g aniline monomer AN, 0.265g (NH is prepared4)2S2O8, 10mL
H2O)；
Two, in the solution by the submergence of stainless steel non-woven fabrics, low-temp reaction 1-10h.
Three, sample is taken out, is rinsed with deionized water, 80 DEG C of air dry oven drying are put into.
Present embodiment, which obtains growth, the stainless steel nonwoven fabric base electrode material of PAN nanostructures.
Correspondingly, on the basis of the preparation method based on above-mentioned stainless steel nonwoven fabric base super capacitance electrode material, this hair
It is bright to additionally provide stainless steel nonwoven fabric base super capacitance electrode material.In the nature of things, the stainless steel nonwoven fabric base super capacitor
Electrode material can be prepared by the above method, if preparing the stainless steel nonwoven fabric base super capacitor electricity with other methods
Pole material, then also in the range of the disclosure of the embodiment of the present invention and protection.
Embodiment one：The stainless steel nonwoven fabric base electrode material preparation method of present embodiment Hydrothermal Growth nanostructure
It follows these steps to implement：
One, stainless steel non-woven fabrics is cut into 1 × 3cm2100mL beakers are put into, then add acetone to no mistake non-woven fabrics, ultrasound
7min or so is handled, then 7min is ultrasonically treated with dilute hydrochloric acid.Deionized water is rinsed repeatedly, then with 7~8min of absolute ethyl alcohol ultrasound.
It is put into 80 DEG C of air dry oven drying.
Two, hydrothermal growth nano-structured solution is prepared：0.65g Ni(NO3)2, 1.3g Co (NO3)2, 1.62g urea,
45mL deionized waters, 45mL absolute ethyl alcohols.
Three, reaction solution is put into the reaction kettle of polytetrafluoroethyllining lining, dried stainless steel non-woven fabrics is submerged
In solution.
Four, reaction kettle is tightened, is put into 100 DEG C of thermostatic drying chambers, hydro-thermal 8h.
Five, it after water heating kettle cooling completely, takes out the non-woven fabrics after reaction and is rinsed with deionized water, be put into air dry oven 80
DEG C drying, the stainless steel non-woven fabrics after the reaction of drying is placed on Al2O3In crucible, 3h is kept the temperature in 250 DEG C of air, by presoma
It is pyrolyzed into NiCo2O4There is NiCo to get to growth2O4The stainless steel nonwoven fabric base electrode material of nanostructure.
Embodiment two：Present embodiment electrochemical deposition method grows the stainless steel nonwoven fabric base electrode material system of nanostructure
Preparation Method follows these steps to implement：
One, electrochemical deposition solution (5mmol Ni (NO are prepared3)2, 10mmol Co (NO3)2, 100mLH2O)
Two, on the working electrode (s by the stainless steel non-woven fabrics folder by the processing of one step 1 of specific implementation mode, it is heavy to immerse
Product solution.Use Pt pieces for electrode, saturated calomel electrode is reference electrode.
Three, it is deposited with potentiostatic method, chooses deposition voltage -1V, deposit 5min.
Four, post-depositional stainless steel non-woven fabrics is taken out, is first rinsed with deionized water, then use washes of absolute alcohol.
Five, the sample after cleaning 60 DEG C of air dry ovens are put into dry.
The present embodiment, which obtains growth, NixCo(1-x)(OH)6xThe stainless steel nonwoven fabric base electrode material of nanostructure.
Using the method for embodiment one, NiCo is grown on different substrates2O4Nanostructure, to the electrode material of different base
The mechanical property and chemical property of material are tested, as a result as follows：
Density, tensile strength and the load NiCo of 1 different base of table2O4The comparison of amount and its specific capacity
Table 1 can be seen that：Compared with carbon cloth and nickel foam, stainless steel non-woven fabrics is light, and intensity is high, unit area load
Active material is more, and other two kinds of substrates are higher by with the electrode material either specific discharge capacity of its preparation or area specific capacity
Material.
Fig. 1 is to grow NiCo on carbon cloth, nickel foam and stainless steel nonwoven fabric base bottom respectively2O4It is measured after nanostructure
Cyclic voltammetry curve, voltage range are -0.1 0.5V, and sweep speed is 5mV s-1.Fig. 1 can be seen that：In stainless steel non-woven fabrics
NiCo is grown in substrate2O4After nanostructure, the integral area that cyclic voltammetry curve surrounds is bigger than on carbon cloth and nickel foam,
It can be seen that the capacitance of the electrode material based on stainless steel nonwoven fabric base bottom wants some higher.In addition, being based on stainless steel non-woven fabrics
NiCo2O4The redox peaks of nanostructure are more obvious, also fully demonstrate three-dimensional stainless steel non-woven fabrics high conductivity,
High porosity, high-specific surface area are very beneficial for the transmission of electronics, ion.
Fig. 2 is to grow NiCo on carbon cloth, nickel foam and stainless steel nonwoven fabric base bottom respectively2O4It is measured after nanostructure
Constant current charge-discharge curve, voltage range are -0.15-0.35V, and current density is 1A g-1.Fig. 2 can be seen that raw in three kinds of substrates
Long NiCo2O4The charging and discharging curve of the electrode material of preparation is not straight line, illustrates the presence of Faraday pseudo-capacitance.Meanwhile
Under identical current density, the NiCo based on stainless steel non-woven fabrics2O4The discharge platform of nanostructure, time are longer, therefore,
Also higher is consistent with cyclic voltammetry curve acquired results for its capacitance.
It should be understood that for those of ordinary skills, it can be modified or changed according to the above description,
And all these modifications and variations should all belong to the protection domain of appended claims of the present invention.
Claims (2)
1. a kind of preparation method of stainless steel nonwoven fabric base electrode material for super capacitor, which is characterized in that using stainless steel without
Woven fabric as base material, on the base material growth in situ metal oxide, bimetallic oxide, bimetallic sulfide,
The nanostructure of one of metal hydroxides and conducting polymer, the stainless steel nonwoven fabric base for obtaining growth in situ nanostructure are super
Grade capacitor electrode material；Include the following steps：
A1, stainless steel non-woven fabrics is cleaned, removes organic and inorganic impurity；
A2, corresponding growth metal oxide, bimetallic oxide, bimetallic sulfide, metal hydroxides and conduction are prepared
The nanostructure reaction solution of one of polymer；
A3, the stainless steel non-woven fabrics cleaned up is immersed in corresponding reaction solution；
A4, using hydrothermal growth process, in 90-200 DEG C of baking oven, keep the temperature 1-10h；Or electrochemical deposition method is used, it will be clear
On the working electrode (s, saturated calomel electrode is reference electrode to stainless steel non-woven fabrics folder after washing, and Pt pieces are to electrode, corresponding
Potentiostatic electrodeposition 1-60min under sedimentation potential；
Obtained electrode material is the different-shape for growing and having including piece, stick, line, needle and flower-shape in the step A4
Nano material；
A5, take out treated stainless steel non-woven fabrics, rinse it is dry to get to the stainless steel of growth in situ multidimensional nanostructure without
Woven fabric base novel electrode material for super capacitor；In the step A5, on base material growth in situ metal oxide,
The stainless steel non-woven fabrics of bimetallic oxide will be also heat-treated after rinsing drying：By the stainless steel after the reaction of drying
Non-woven fabrics is placed on Al2O3In crucible, 1-10h is kept the temperature in 200-600 DEG C of air, presoma is pyrolyzed；
The metal oxide is MnO2、Fe2O3、Fe3O4、Co3O4, one of CoO；Bimetallic oxide is NiCo2O4、ZnCo2O4、
NiMo2O4、ZnMn2O4One of；Bimetallic sulfide is NiCo2S4、ZnCo2S4、NiMo2S4、ZnMn2S4One of；Metal hydroxide
Object Ni (OH)2、Co(OH)2、Fe(OH)3、NixCo(1-x)(OH)6xOne of；Conducting polymer is polyaniline (PAN), polypyrrole
(PPY), one of poly- 3,4-ethylene dioxythiophene (PEDOT).
2. the stainless steel nonwoven fabric base electrode material for super capacitor that preparation method obtains according to claim 1.
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