CN105321725B - A kind of ultracapacitor micro-nano structure electrode material and electrode piece preparation method - Google Patents
A kind of ultracapacitor micro-nano structure electrode material and electrode piece preparation method Download PDFInfo
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- CN105321725B CN105321725B CN201510718789.9A CN201510718789A CN105321725B CN 105321725 B CN105321725 B CN 105321725B CN 201510718789 A CN201510718789 A CN 201510718789A CN 105321725 B CN105321725 B CN 105321725B
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Abstract
The present invention provides a kind of ultracapacitor micro-nano structure electrode material and electrode piece preparation method.Electrode material includes the matrix being made up of collector and the amorphous alloy material being plated on matrix；The amorphous alloy material is one kind in amorphous ni-cu-p coating, amorphous nickel cobalt phosphorus or amorphous ferronickel phosphorus alloy.Micron order born of the same parents' shape amorphous ni-cu-p coating surface is uniformly distributed amorphous ni-cu-p coating nano particle.Electrode piece preparation method include alkaline degreasing, washing, pickling, washing, chemical plating, washing, burn into washing, dry or dry up step.The advantages that amorphous ni-cu-p coating electrode slice of preparation is conductive, mechanical property, corrosion resistance and heat-resist, and internal resistance is small, and specific capacitance is high and good cycling stability, and adhesion is high between electrode material and collector, and electrode material thickness is uniform.Preparation method provided by the invention have the characteristics that required equipment investment is few, process is few, technological operation is simple, it is easily controllable, reproducible, be adapted to industrialization production.
Description
Technical field
The invention belongs to supercapacitor technologies field, more particularly to a kind of ultracapacitor micro-nano structure electrode material
And electrode piece preparation method.
Background technology
Ultracapacitor has the advantages that high security, high power density, high current charge-discharge and long circulation life, too
The fields such as positive energy wind power generation, electric automobile, consumer electronics, electromagnetism high power weaponry have boundless application, are
The novel energy storage apparatus that various countries are competitively studied in recent years.
Electrode is the core component of ultracapacitor, and therefore, prepared by the design of new electrode materials and electrode is domestic and international
The study hotspot and emphasis of ultracapacitor research field.The electrode material for super capacitor reported mainly include carbon material,
Metal oxide and conducting polymer three major types.Compared with the double electric layers supercapacitor of carbon material manufacture, under equal area,
The ultracapacitor manufactured with the metal oxide with fake capacitance feature, its capacitance are tens of up to electric double layer capacitance value
Times；Compared with conductive polymer electrodes material, metal oxide electrode material has good heat resistance.
Metal oxide electrode material is divided to noble metal and the class of cheap metal oxide two.Noble metal oxide electrodes material is such as
Ruthenium-oxide is expensive, is restricted in civil area application.In contrast to this, cheap metal oxide such as nickel oxide, manganese oxide
Relatively low Deng electrode material price, cost advantage is obvious, is a kind of fake capacitance electrode material of great application potential.
Research shows that the deficiency that cheap metal oxide electrode material is primarily present includes：1）Prepared by electrode include metal
The techniques such as oxide powder preparation, metal oxide electrode material film preparation, electrode material membrane and collector connection, each work
Include some processes again in skill, not only total preparation technology long flow path, and the factor for influenceing electrode performance is more；2）Metal aoxidizes
Thing electric conductivity itself is very poor, is unfavorable for electric transmission in charge and discharge process, causes its power density not high；3）Metal oxide machine
Tool poor-performing, it is restricted in the application of complicated applied force occasion；4）High is required to the corrosion resistance of current collector material；5）Metal oxygen
Synthesized between compound electrode material membrane and collector matrix by suppressing, adhesion is poor, membrane thickness unevenness；6）Internal resistance is larger,
Anti-over-charging, which is crossed, to be put poor with short-circuit capability, and security is poor.
The content of the invention
The present invention is in order to solve drawbacks described above present in prior art and deficiency, there is provided a kind of ultracapacitor micro-nano
Structure electrode material and electrode piece preparation method, solves the existing oxidation of common metal oxide super capacitor electrode material
The technical barrier such as interface cohesion difference between thing poorly conductive, technology for preparing electrode complexity, electrode material and collector.
In order to solve the above technical problems, the present invention provides a kind of ultracapacitor micro-nano structure electrode material, including by collecting
The matrix that fluid is formed and the amorphous alloy material being plated on matrix；The amorphous alloy material be amorphous ni-cu-p coating,
One kind in amorphous nickel cobalt phosphorus or amorphous ferronickel phosphorus alloy.
Preferably, the collector is conductive metal material or electrically conductive, non-metallic material, the conductive metal material
Expect that for one kind in steel foil, metal nickel foil, nickel foam or copper foil, the electrically conductive, non-metallic material be carbon material.
A kind of ultracapacitor micro-nano structure electrode piece preparation method, comprises the following steps：
Step 1, the pretreatment of electrode slice, electrode slice is made as matrix using current collector material, then in turn through alkali
Property oil removing, washing, pickling, washing processing step electrode slice is handled；
Step 2, plating is carried out to electrode slice, using chemical plating or electric plating method by amorphous alloy material be plated on through
Cross on pretreated electrode slice, then washed；The amorphous alloy material is amorphous ni-cu-p coating, amorphous nickel cobalt phosphorus
Or one kind in amorphous ferronickel phosphorus alloy；
Step 3, corrosion, corrosion treatment is carried out to the electrode slice for being plated with amorphous alloy material that step 2 obtains so that
The amorphous alloy material on electrode slice surface possesses micro-nano structure；
Step 4, the post-processing of electrode slice, the electrode slice after excessive erosion is washed, dry or drying processing.
Wherein, in step 2, the amorphous alloy material is amorphous ni-cu-p coating, and the mass fraction of wherein copper is not less than
18%, the mass fraction of phosphorus is not less than 10%, and remaining is nickel.
In step 2, the concentration of each component is respectively in chemical plating fluid, 3.5 ~ 5.5 g/l of copper sulphate, nickel sulfate
20 g/l, 25 g/l of sodium hypophosphite, 40 g/l of sodium citrate, 40 g/l of sodium acetate, 2.6 g/l of sodium hydroxide, Potassiumiodate
1 mg/litre, chemical plating process temperature are 85 ± 1 DEG C, and electroless plating time is 30 ~ 120 minutes.
In step 3, the corrosion is acid corrosion.
Preferably, acid corrosion medium is sulfuric acid, and the volume fraction of sulfuric acid is 10-20%, and etching time is 10-40 hours.
Preferably, the etching time of 20% sulfuric acid solution at room temperature is used as 20-40 hours.
Preferably, the etching time of 20% sulfuric acid solution at 50 DEG C is used as 10-20 hours.
The advantageous effects that the present invention is reached：
1. amorphous ni-cu-p coating is deposited directly to by current collector material system by the present invention by chemical plating or electroplating technology
Into electrode slice surface, there is good adhesion between amorphous ni-cu-p coating and collector matrix；
2. electrode slice prepared by the present invention has good mechanical performance, available for complicated applied force occasion；
3. electrode slice of the present invention is respectively provided with excellent corrosion resistance in highly acid and strong basicity environment；
4. electrode slice prepared by the present invention has good electric conductivity, internal resistance is smaller；
5. electrode slice prepared by the present invention has good heat resistance and heat endurance, the occasion higher available for temperature；
6. the present invention super capacitor electrode slice preparation method there is technique to be simple and convenient to operate, equipment investment is few, into
The features such as this low, suitable industrialization production.
Brief description of the drawings
Electrode slice surface topography SEM figures prepared by Fig. 1 embodiment of the present invention 1；
Electrode slice surface XRD spectrum prepared by Fig. 2 embodiment of the present invention 1；
The cyclic voltammetry curve of electrode slice prepared by Fig. 3 embodiment of the present invention 2；
The circulation cyclic voltammetry curve and its specific capacitance of electrode slice prepared by Fig. 4 embodiment of the present invention 3 become with circulation cycle
Change curve；
The cyclic voltammetry curve of electrode prepared by Fig. 5 embodiment of the present invention 4.
Embodiment
In order to be better understood by technical characteristic, technology contents and its technique effect reached of the present invention, now this is sent out
Bright accompanying drawing is described in detail in conjunction with the embodiments.
Patent of the present invention is further illustrated with reference to the accompanying drawings and examples.
The present invention provides a kind of ultracapacitor micro-nano structure electrode material, including the matrix and plating being made up of collector
Amorphous alloy material on matrix；The amorphous alloy material is amorphous ni-cu-p coating, amorphous nickel cobalt phosphorus or amorphous ferronickel
One kind in phosphorus alloy；The collector is conductive metal material or electrically conductive, non-metallic material, the conductive metal material
Expect that for one kind in steel foil, metal nickel foil, nickel foam or copper foil, the electrically conductive, non-metallic material be carbon material.
A kind of ultracapacitor micro-nano structure electrode piece preparation method, comprises the following steps：
Step 1, the pretreatment of electrode slice, electrode slice is made as matrix using current collector material, then in turn through alkali
Property oil removing, washing, pickling, washing processing step electrode slice is handled；
Step 2, plating is carried out to electrode slice, using chemical plating or electric plating method by amorphous alloy material be plated on through
Cross on pretreated electrode slice, then washed；The amorphous alloy material is amorphous ni-cu-p coating, amorphous nickel cobalt phosphorus
Or one kind in amorphous ferronickel phosphorus alloy；Preferably, the amorphous alloy material is the quality of amorphous ni-cu-p coating, wherein copper
Fraction is not less than 18%, and the mass fraction of phosphorus is not less than 10%, and remaining is nickel.When using chemical plating, respectively formed in chemical plating fluid
The concentration of material is respectively 3.5 ~ 5.5 g/l of copper sulphate, 20 g/l of nickel sulfate, 25 g/l of sodium hypophosphite, sodium citrate
40 g/l, 40 g/l of sodium acetate, 2.6 g/l of sodium hydroxide, the mg/litre of Potassiumiodate 1, chemical plating process temperature is 85 ± 1
DEG C, electroless plating time is 30 ~ 120 minutes.
Step 3, corrosion, corrosion treatment is carried out to the electrode slice for being plated with amorphous alloy material that step 2 obtains so that
The amorphous alloy material on electrode slice surface possesses micro-nano structure；The corrosion is acid corrosion.Acid corrosion medium is sulfuric acid, sulfuric acid
Volume fraction is 10-20%, and etching time is 10-40 hours.After sulfuric acid concentration adjusts in the corrosive medium of preparation, accordingly
Etching time also needs to adjust, and generally, as sulfuric acid concentration declines, need to extend etching time；And in the timing of sulfuric acid concentration one, raising
Corrosive medium temperature, etching time need to be shortened.Corrode at room temperature according to 20% sulfuric acid solution, then etching time is 20-40
Hour；Corrode according to 20% sulfuric acid solution at 50 DEG C, then etching time is 10-20 hours.
Step 4, the post-processing of electrode slice, the electrode slice after excessive erosion is washed, dry or drying processing.
Embodiment 1
The electrode sheet matrix being made up of collector uses steel foil, and the size of matrix is 20mm × 10mm × 0.21mm, actual
In production, the size of matrix material and matrix can be designed adjustment according to being actually needed for electrode slice, and electrode slice is entered first
Row oil removing, washing, pickling and washing, electroless plating technology plating amorphous ni-cu-p coating is then used on electrode slice, then will
The electrode slice of plating amorphous ni-cu-p coating is put into room temperature in the sulfuric acid solution that volumetric concentration is 20% and corroded 25 hours, corrosion knot
Shu Hou, washing is taken out, dries or dries up, produces required electrode slice.
As shown in Figure 1, using SEM（SEM）Morphology characterization is carried out to electrode slice surface, can from Fig. 1
To find out, there is micro-nano structure feature, cellular structure size is about 4 microns, uniform on cellular structure surface on electrode slice surface
The amorphous ni-cu-p coating nanoparticle size of distribution is about 250 nanometers.
Fig. 2 is electrode slice surfacing X-ray diffraction（XRD）Collection of illustrative plates, electrode slice material is amorphous ambrose alloy as can be known from Fig. 2
Phosphorus alloy.
Embodiment 2
The electrode sheet matrix being made up of collector uses steel foil, and the size of matrix is 20mm × 10mm × 0.21mm, actual
In production, the size of matrix material and matrix can be designed adjustment according to being actually needed for electrode slice, and electrode slice is entered first
Row oil removing, washing, pickling and washing, electroless plating technology plating amorphous ni-cu-p coating is then used on electrode slice, then will
The electrode slice of plating amorphous ni-cu-p coating is put into volumetric concentration and corroded 14 hours for 50 DEG C in 20% sulfuric acid solution, corrosion knot
Shu Hou, washing is taken out, dries or dries up, produces required electrode slice.
Electrode slice characterizes, using PARSTAT2273 electrochemical workstations, using Hg/HgO electrodes as reference electrode, platinum electrode
For auxiliary electrode, 2 mol/L KOH solutions are electrolyte solution, and sweep speed is 50 mV/s, potential window 0.25-0.65
V, electrode slice are working electrode, its bare area 0.95 cm2, respectively obtain the electrode in room temperature and 50 DEG C of electrolyte solution
The cyclic voltammetry curve of piece, as shown in figure 3, measurement result shows, redox peaks be present on the cyclic voltammetry curve of electrode slice,
It is a kind of fake capacitance electrode material to illustrate amorphous ni-cu-p coating.Calculating shows, amorphous ni-cu-p coating prepared by the above method
Specific capacitance of the electrode slice in room temperature is 0.138 F/cm2, specific capacitance at 50 DEG C is 0.197 F/cm2。
Embodiment 3
The electrode sheet matrix being made up of collector uses steel foil, and the size of matrix is 20mm × 10mm × 0.21mm, actual
In production, the size of matrix material and matrix can be designed adjustment according to being actually needed for electrode slice, and electrode slice is entered first
Row oil removing, washing, pickling and washing, electroless plating technology plating amorphous ni-cu-p coating is then used on electrode slice, then will
The electrode slice of plating amorphous ni-cu-p coating is put into volumetric concentration and corroded 12 hours for 50 DEG C in 20% sulfuric acid solution, corrosion knot
Shu Hou, washing is taken out, dries or dries up, produces required electrode slice.
Electrode slice characterizes, and with CHI660E electrochemical workstations, using Hg/HgO electrodes as reference electrode, platinum electrode is auxiliary
Electrode, 2 mol/L KOH solutions are electrolyte solution, and sweep speed is 50 mV/s, and potential window is 0.25-0.65 V, electrode
Piece is working electrode, its bare area 0.80 cm2, measure electric during 2000 cycles of measurement circulation in room temperature electrolyte solution
The cyclic voltammetry curve of pole piece is with the change of circulation cycle, and as shown in fig. 4 a, measurement result shows, the cyclic voltammetric of electrode slice is bent
Redox peaks on line be present, it is a kind of fake capacitance electrode material to illustrate amorphous ni-cu-p coating；By the way that electrode slice is calculated
Specific capacitance with the change curve of circulation cycle, as shown in Figure 4 b, result of calculation shows, the specific capacitance of electrode slice is at circulation initial stage
Increase with the increase of circulation cycle, tended towards stability after about circulating 200 cycles.
Embodiment 4
The electrode sheet matrix being made up of collector uses steel foil, and the size of matrix is 20mm × 10mm × 0.21mm, actual
In production, the size of matrix material and matrix can be designed adjustment according to being actually needed for electrode slice, and electrode slice is entered first
Row oil removing, washing, pickling and washing, electroless plating technology plating amorphous ni-cu-p coating is then used on electrode slice, then will
The electrode slice of plating amorphous ni-cu-p coating is put into volumetric concentration and corroded 12 hours for 50 DEG C in 20% sulfuric acid solution, corrosion knot
Shu Hou, washing is taken out, dries or dries up, produces required electrode slice.
Electrode slice characterizes, using PARSTAT2273 electrochemical workstations, using Hg/HgO electrodes as reference electrode, platinum electrode
For auxiliary electrode, 2 mol/L KOH solutions are electrolyte solution, and sweep speed is 150 mV/s, potential window 0.25-0.65
V, electrode slice are working electrode, its bare area 0.80 cm2, obtain the cyclic voltammetric of electrode slice in electrolyte solution at room temperature
Curve, as shown in figure 5, by calculating, the specific capacitance of amorphous ni-cu-p coating electrode slice is 0.063 F/cm2。
The present invention is disclosed with preferred embodiment above, so it is not intended to limiting the invention, all to take equivalent substitution
Or the technical scheme that the scheme of equivalent transformation is obtained, all fall within protection scope of the present invention.
Claims (5)
1. a kind of ultracapacitor micro-nano structure electrode piece preparation method, the electrode material of use includes the base being made up of collector
Body and the amorphous alloy material being plated on matrix；The amorphous alloy material be amorphous ni-cu-p coating, amorphous nickel cobalt phosphorus or
One kind in amorphous ferronickel phosphorus alloy；The collector is conductive metal material or electrically conductive, non-metallic material, the conduction
Property metal material be steel foil, metal nickel foil, nickel foam or copper foil in one kind, the electrically conductive, non-metallic material is carbon material,
It is characterised in that it includes following steps：
Step 1, the pretreatment of electrode slice, electrode slice is made as matrix using current collector material, removed then in turn through alkalescence
Oil, washing, pickling, the processing step of washing are handled electrode slice；
Step 2, plating is carried out to electrode slice, amorphous alloy material is plated on by pre- using chemical plating or electric plating method
On electrode slice after processing, then washed；When the amorphous alloy material is amorphous ni-cu-p coating, the wherein quality of copper
Fraction is not less than 18%, and the mass fraction of phosphorus is not less than 10%, and remaining is nickel；The concentration difference of each component in chemical plating fluid
For, 3.5~5.5 g/l of copper sulphate, 20 g/l of nickel sulfate, 25 g/l of sodium hypophosphite, 40 g/l of sodium citrate, sodium acetate 40
G/l, 2.6 g/l of sodium hydroxide, the mg/litre of Potassiumiodate 1, chemical plating process temperature is 85 ± 1 DEG C, electroless plating time 30
~120 minutes；
Step 3, corrosion, corrosion treatment is carried out to the electrode slice for being plated with amorphous alloy material that step 2 obtains so that electrode
The amorphous alloy material on piece surface possesses micro-nano structure；
Step 4, the post-processing of electrode slice, the electrode slice after excessive erosion is washed, dry or drying processing.
2. ultracapacitor micro-nano structure electrode piece preparation method according to claim 1, it is characterised in that：Step 3
In, the corrosion is acid corrosion.
3. ultracapacitor micro-nano structure electrode piece preparation method according to claim 2, it is characterised in that：Acid corrosion is situated between
Matter is sulfuric acid, and the volume fraction of sulfuric acid is 10-20%, and etching time is 10-40 hours.
4. ultracapacitor micro-nano structure electrode piece preparation method according to claim 3, it is characterised in that：Using 20%
Sulfuric acid solution etching time at room temperature be 20-40 hours.
5. ultracapacitor micro-nano structure electrode piece preparation method according to claim 3, it is characterised in that：Using 20%
Etching time of the sulfuric acid solution at 50 DEG C be 10-20 hours.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105931861B (en) * | 2016-06-14 | 2018-04-03 | 南京工程学院 | A kind of preparation method for the electrode of super capacitor for being covered with active electrode film |
| CN108220825A (en) * | 2016-12-14 | 2018-06-29 | 刘志红 | A kind of Ni based amorphous alloy powders and its preparation process |
| CN107256807B (en) * | 2017-06-12 | 2018-10-30 | 南京工程学院 | A method of preparing sulphur, the oxygen compound composite film electrode of ambrose alloy |
| CN107275108B (en) * | 2017-06-12 | 2018-09-11 | 南京工程学院 | A method of preparing oxygen, the sulphur compound composite film electrode of nickel cobalt |
| CN112259383B (en) * | 2020-10-19 | 2022-02-22 | 南京工程学院 | In-situ preparation method of electrode coated with nickel molybdate copper composite film |
| CN114318398A (en) * | 2022-01-20 | 2022-04-12 | 青岛科技大学 | Water electrolysis hydrogen production electrode and preparation method thereof |
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| CN101373667A (en) * | 2008-09-17 | 2009-02-25 | 四川大学 | High potential super capacitor electrode material and preparing method thereof |
| CN104600272A (en) * | 2014-12-19 | 2015-05-06 | 华侨大学 | Mesh-shaped nickel-copper-phosphorus amorphous alloy electrode material and preparation method thereof |
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| CN101373667A (en) * | 2008-09-17 | 2009-02-25 | 四川大学 | High potential super capacitor electrode material and preparing method thereof |
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