CN110066000A - A kind of preparation method and applications of Ag doping lead dioxide electrode - Google Patents
A kind of preparation method and applications of Ag doping lead dioxide electrode Download PDFInfo
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- CN110066000A CN110066000A CN201910462255.2A CN201910462255A CN110066000A CN 110066000 A CN110066000 A CN 110066000A CN 201910462255 A CN201910462255 A CN 201910462255A CN 110066000 A CN110066000 A CN 110066000A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
- C02F2001/46138—Electrodes comprising a substrate and a coating
- C02F2001/46142—Catalytic coating
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/46—Apparatus for electrochemical processes
- C02F2201/461—Electrolysis apparatus
- C02F2201/46105—Details relating to the electrolytic devices
- C02F2201/4612—Controlling or monitoring
- C02F2201/46125—Electrical variables
- C02F2201/4614—Current
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/46—Apparatus for electrochemical processes
- C02F2201/461—Electrolysis apparatus
- C02F2201/46105—Details relating to the electrolytic devices
- C02F2201/4618—Supplying or removing reactants or electrolyte
Abstract
The present invention relates to a kind of preparation method and applications of simple substance Ag doping lead dioxide electrode, belong to electrode material application field.The method is as follows: after first titanium plate is cleared up and polished, titanium plate being impregnated into oxalic acid aqueous solution except oxide layer, finally titanium plate is cleaned and dried up with deionized water；Titanium plate is immersed into standing certain time in configured silver plating liquid and obtains silver coated titanium plate；Using copper sheet as cathode, to be coated with the titanium plate of elemental silver middle layer as anode, with Pb (NO3)2、Cu(NO3)2Mixed solution with NaF is electroplate liquid, carries out electro-deposition, obtains the lead dioxide electrode of simple substance Ag doping.The degradation effect of the organic pollutants such as energy consumption of the present invention is low, long service life, Pyrogentisinic Acid is significant.
Description
Technical field
The present invention relates to a kind of preparation method and applications of simple substance Ag doping lead dioxide electrode, and in particular to it is a kind of with
Titanium is Ag doping lead dioxide electrode (the abbreviation Ti/Ag-PbO of matrix2) and its application in Electrocatalysis Degradation pollutant, belong to
In electrode material application field.
Background technique
Electro-catalysis technology has many advantages, such as that equipment is simple, oxidability is strong, reaction rate is fast, without secondary pollution, is a kind of
It is suitble to toxic, difficult for biological degradation organic wastewater the water treatment technology of processing.Anode material is the core of the technology, brown lead oxide electricity
Pole because its catalytic oxidation activity is high, corrosion-resistant strong, preparation simply can be applicable to oxygen evolution reaction, chemicals production, prepare ozone with
And become one of electrocatalytic oxidation anode material most with prospects (Li X, Pletcher D, Walsh F in wastewater treatment
C.Electrodeposited lead dioxide coatings[J].Chemical Society Reviews,2011,40
(7):3879-3894.)。
But lead dioxide electrode there are still current efficiency in use it is low, power consumption is high the problems such as, and be catalyzed
Activity can continue to lift up.Therefore, scholars many in recent years is dedicated to modified lead dioxide electrode.Such as patent CN
10253465 A describe a kind of preparation method of titanium-based antimony doped tin lead dioxide electrode, lead dioxide electrode surface obtained
Uniformly, fine and close, electrode current efficiency is able to promote electrocatalytic oxidation activity with higher；103132076 A of patent CN is introduced
A kind of ti-supported lead dioxide electric preparation method of lanthanum, gadolinium codope, by the synergistic effect of lanthanum, gadolinium codope, electrode have compared with
Big specific surface area and more active site, are conducive to the adsorption and desorption of pollutant, can greatly improve the degradation to organic matter
Effect, and long service life；Patent CN 101054684 describes one kind and prepares Lead dioxide anode modifiedby fluorine resin on Titanium base
Method, lead dioxide electrode surface obtained uniformly, fine and close electrocatalytic oxidation activity with higher.Therefore reasonable member
Element doping can effectively improve the performances such as the current efficiency, catalysis oxidation ability and service life of lead dioxide electrode, but at present
Until never for solve energy consumption problem carried out research.
Due to PbO2Electrode is prepared by the method for anodic oxidation, is the oxidation reaction occurred in anode, if electricity is heavy
There are Ag in hydrops+It can only deposit, can not be generated on anode on cathode, therefore, the prior art does not use anodic oxygen
The method of change prepares the relevant report of Ag doping lead dioxide electrode.
Summary of the invention
For the deficiencies in the prior art, the purpose of the present invention is to provide a kind of Ag doping lead dioxide electrodes
Preparation method is formed simple substance silver layer on Titanium base surface using chemical reduction method, is then formed on its surface using electrodeposition process
Doped with the PbO of elemental silver2Layer；Prepared electrode Pyrogentisinic Acid's class organic pollutant has good degradation.
The purpose of the present invention is what is be achieved through the following technical solutions.
A kind of preparation method of Ag doping lead dioxide electrode, specific step is as follows for the preparation method:
The pretreatment of step 1. titanium plate
First titanium plate is cleaned, is then polished, then titanium plate is impregnated into temperature is 95 DEG C and mass fraction is
2h in 15% oxalic acid solution；By titanium plate after being taken out in oxalic acid solution, then with deionized water is cleaned and dried up；
The preparation of step 2. elemental silver middle layer
Silver ammino solution is instilled in the reducing solution of sodium potassium tartrate tetrahydrate dropwise and obtains silver plating liquid；Pretreated titanium plate is put into
In silver plating liquid, simple substance silver layer is formed on Titanium base surface through electronation, obtains the titanium plate for being coated with silver-colored simple substance middle layer；
Step 3. electro-deposition PbO2
Using copper sheet as cathode, to be coated with the titanium plate of silver-colored simple substance middle layer as anode, with Pb (NO3)2、Cu(NO3)2With NaF's
Mixed solution is electrodeposit liquid, in 20mA/cm2Current density under electro-deposition 2h, obtain the electrode；
Wherein, in the electrodeposition process, the stirring rate of electrodeposit liquid is 80rpm, and electrodeposition temperature is 60 DEG C,
20mA/cm2Current density under electro-deposition 2h.
In step 1, the titanium plate material is the industrially pure titanium that purity is not less than 99.5%.
In step 2, silver plating liquid configuration process is as follows: ammonium hydroxide (80-100ml/L) is instilled silver nitrate solution (20-30g/L)
In obtain silver ammino solution after solution clarification, silver ammino solution is added in isometric potassium sodium tartrate solution (100g/L) and is obtained
Silver plating liquid.
Step 2 silver ammino solution instills in potassium sodium tartrate solution, and the temperature of silver plating liquid is maintained at 30 DEG C, a length of 1- when silver-plated
3h。
In the electrodeposit liquid of step 3, Pb (NO3)2Concentration be 0.5-0.7mol/L, Cu (NO3)2Concentration be 0.1-
The concentration of 0.2mol/L, NaF are 0.01-0.1mol/L, and the pH value of electrodeposit liquid is 1-2.
Elemental silver is entrained in titanium dioxide lead layer in Ag doping lead dioxide electrode made from the above method.
A kind of application of Ag doping lead dioxide electrode of the present invention, it is organic that the electrode is suitable for degradation of phenol class
Pollutant；
When degradation of phenol class organic pollutant, cathode is copper sheet, and anode is the electrode, current density 20mA/cm2,
The initial concentration of phenol organic pollutant to be degraded in the solution is 100mg/L, Na in solution2SO4Concentration
0.35mol/L, solution ph 5.
The physicochemical property of metal element A g is uniform and stable, thermally conductive, electric conductivity is fabulous, without secondary pollution and economy and storage
Amount is better than most of rare earth elements.The present invention uniformly prepares one layer of fine and close simple substance using chemical reduction method on Titanium base surface
Silver.Because the conductivity of silver is better than most metals, the conductivity of electrode entirety is greatly improved after doping, and reduce
The charge transfer resistance of electrode makes electrode obtain higher catalytic activity and lower energy consumption, and the silver layer of even compact exists
Protect titanium substrate not oxidized when electro-deposition brown lead oxide, to further improve electric conductivity and the catalysis work of electrode
Property.The knot of matrix and coating is enhanced since the thermal conductivity of silver well reduces thermal stress during preparing titanium dioxide lead layer
Resultant force is to improve the service life of electrode, and thermal conductivity is well anti-to reduce thermal stress under the use environment of high temperature in the future
Only the advantage of electrode chap is even more to emerge from.Then titanium dioxide is formed using electrodeposition process on its surface using silver-plated Titanium base
Lead active layer, elemental silver part remains in titanium-based bottom surface portion and is dispersed into brown lead oxide while forming titanium dioxide lead layer
The internal conductivity that electrode entirety is greatly improved of layer achievees the purpose that reduce energy consumption while improving catalytic capability.
Beneficial effect
The method of the present invention uses chemical reduction method to form simple substance silver layer on Titanium base surface first, i.e., is coated on anode plate
Elemental silver, during electro-deposition, the elemental silver plated on anode plate under strongly acidic solution can dissolve, and the method for the present invention exists
During elemental silver dissolution falls off, PbO that the simple substance Ag of part was deposited later2It is wrapped in PbO2Inside, can not further with acid
Reaction, to remain the silver-colored simple substance of part.And elemental silver package in part increases the conductive capability of electrode, improves catalysis and lives
Property.
Electrode of the present invention is suitable for degradation of phenol class waste water, and removal rate is up to 98% or more, final product of degrading
It is environmental-friendly for carbon dioxide and water；Technology for preparing electrode of the present invention is simple, easy to operate, and overall cost is low, Pyrogentisinic Acid
Degradation effect it is significant.
Detailed description of the invention
Fig. 1 is scanning electron microscope (SEM) figure of Ag doping lead dioxide electrode.
Fig. 2 is the scanning electron microscope diagram of pure lead dioxide electrode.
Fig. 3 is X-ray electron spectrum (XPS) figure of Ag doping lead dioxide electrode.
Fig. 4 is X-ray fluorescence spectra (XRF) figure of Ag doping lead dioxide electrode.
Fig. 5 is the AC impedance figure of different doping Ag doping lead dioxide electrodes and pure lead dioxide electrode.
Fig. 6 be the phenol removal rate of different doping Ag doping lead dioxide electrodes and pure lead dioxide electrode at any time
Change comparison diagram.
Specific embodiment
The present invention will be further described With reference to embodiment.
In following embodiment:
Titanium plate: the industrially pure titanium of titaniferous 99.5%；
Silver plating liquid is prepared: 30ml ammonium hydroxide (80ml/L) is instilled in 20ml silver nitrate solution (20g/L) after solution clarification
Silver ammino solution is added in 50ml potassium sodium tartrate solution (100g/L) and obtains silver plating liquid by obtained silver ammino solution.
AC impedance test: exchange resistance is carried out using CHI660D electrochemical workstation (Shanghai Chen Hua Instrument Ltd.)
Anti- test, simulation obtain charge transfer resistance；Test carries out at normal temperature, and supporting electrolyte sodium sulfate concentration is 0.1M.
Embodiment 1
A kind of preparing for Ag doping lead dioxide electrode is as follows:
The pretreatment of step 1. titanium plate
First polished titanium plate with the sand paper of 240 mesh, 600 mesh respectively, after titanium plate impregnated into ultrasonic oil removing 15min in acetone,
Titanium plate is impregnated into the oxalic acid aqueous solution that temperature is 95 DEG C and mass fraction is 15% 2h except oxide layer again；By titanium plate from
After being taken out in oxalic acid solution, then with deionized water is cleaned and dried up；
The preparation of step 2. simple substance silver layer
It is molten that 30ml ammonium hydroxide (80ml/L) is instilled to the silver-colored ammonia obtained after solution clarification in 20ml silver nitrate solution (20g/L)
Liquid, will silver ammino solution be added 50ml potassium sodium tartrate solution (100g/L) in obtain silver plating liquid, by titanium plate be immersed 1-3h with
Obtain the substrate of different Ag doping amounts.
Step 3. is by 16.56gPbO2、0.042gNaF、0.1gHNO3It is dissolved in 100ml deionized water, obtained solution is i.e.
For electrodeposit liquid；Using copper sheet as cathode, using middle layer titanium plate obtained in step 2 as anode, by electrodeposition temperature and stirring speed
Rate is respectively set to 65 DEG C and 100rpm, then 20mA/cm again2Electro-deposition current density under electro-deposition 2h, obtain Ag doping
Lead dioxide electrode.
Fig. 1 is scanning electron microscope (SEM) figure of Ag doping lead dioxide electrode, and Fig. 2 is pure lead dioxide electrode
Scanning electron microscope diagram, by Fig. 1 and Fig. 2 it is found that the doping of elemental silver and having not been changed the surface topography of electrode.
Fig. 3 is X-ray electron spectrum (XPS) figure of Ag doping lead dioxide electrode, as seen from the figure silver Ag3d3And Ag3d5Point
There is not apparent peak at 369eV and 375eV, the two peaks are the characteristic peak of zero-valent silver, it was demonstrated that doping in brown lead oxide coating
Silver exist with simple substance form.
X-ray fluorescence spectra (XRF) figure of the Ag doping lead dioxide electrode prepared by the present embodiment, Fig. 4 is it is found that logical
Cross the doping for changing the changeable silver of silver-plated duration.Specifically it is shown in Table 1.
Table 1
Fig. 5 is the AC impedance figure of different doping Ag doping lead dioxide electrodes and pure lead dioxide electrode, Cong Tuke
Know, as the electrode that the increase of simple substance silver content is prepared shows smaller semicircle radius and lower Rct, illustrates elemental silver
Doping can significantly promote the conductive capability of electrode and as the increase conductive capability of doping continues to lift up.
Embodiment 2
A kind of preparing for Ag doping lead dioxide electrode is as follows:
The pretreatment of step 1. titanium plate
First polished titanium plate with the sand paper of 240 mesh, 600 mesh respectively, after titanium plate impregnated into ultrasonic oil removing 15min in acetone,
Titanium plate is impregnated into the oxalic acid aqueous solution that temperature is 95 DEG C and mass fraction is 15% 2h except oxide layer again；By titanium plate from
After being taken out in oxalic acid solution, then with deionized water is cleaned and dried up；
The preparation of step 2. simple substance silver layer
It is molten that 35ml ammonium hydroxide (90ml/L) is instilled to the silver-colored ammonia obtained after solution clarification in 25ml silver nitrate solution (30g/L)
Liquid, will silver ammino solution be added 60ml potassium sodium tartrate solution (100g/L) in obtain silver plating liquid, by titanium plate be immersed 1-3h with
Obtain the substrate of different Ag doping amounts.
Step 3. is by 16.56gPbO2、0.042gNaF、0.1gHNO3It is dissolved in 100ml deionized water, obtained solution is i.e.
For electrodeposit liquid；Using copper sheet as cathode, using middle layer titanium plate obtained in step 2 as anode, by electrodeposition temperature and stirring speed
Rate is respectively set to 65 DEG C and 100rpm, then 20mA/cm again2Electro-deposition current density under electro-deposition 2h, obtain Ag doping
Lead dioxide electrode.
The electrode obtained is used for degradation of phenol class waste water, and removal rate is up to 98% or more.
Embodiment 3
A kind of preparing for Ag doping lead dioxide electrode is as follows:
The pretreatment of step 1. titanium plate
First polished titanium plate with the sand paper of 240 mesh, 600 mesh respectively, after titanium plate impregnated into ultrasonic oil removing 15min in acetone,
Titanium plate is impregnated into the oxalic acid aqueous solution that temperature is 95 DEG C and mass fraction is 15% 2h except oxide layer again；By titanium plate from
After being taken out in oxalic acid solution, then with deionized water is cleaned and dried up；
The preparation of step 2. simple substance silver layer
It is molten that 30ml ammonium hydroxide (80ml/L) is instilled to the silver-colored ammonia obtained after solution clarification in 20ml silver nitrate solution (20g/L)
Liquid, will silver ammino solution be added 50ml potassium sodium tartrate solution (100g/L) in obtain silver plating liquid, by titanium plate be immersed 1-3h with
Obtain the substrate of different Ag doping amounts.
Step 3. is by 18.5g PbO2、0.1g NaF、0.2g HNO3It is dissolved in 100ml deionized water, obtained solution is i.e.
For electrodeposit liquid；Using copper sheet as cathode, using middle layer titanium plate obtained in step 2 as anode, by electrodeposition temperature and stirring speed
Rate is respectively set to 65 DEG C and 100rpm, then 20mA/cm again2Electro-deposition current density under electro-deposition 2h, obtain Ag doping
Lead dioxide electrode.
The electrode obtained is used for degradation of phenol class waste water, and removal rate is up to 98% or more.
Comparative example 1
Step 1. titanium plate is pre-processed with embodiment 1；
Step 2 uses Titanium board as anode, and pure titanium dioxide is prepared with the step 3 of embodiment 1 in other step parameters
Lead electrode.
The pure lead dioxide electrode Pyrogentisinic Acid's of Ag doping lead dioxide electrode and comparative example 1 described in embodiment 1
Degradation property test is as follows:
Preparation initial phenol concentration is 100mg/L and Na2SO4The solution of the concentration 0.45M of electrolyte, and by pH value tune
It is 5；Using copper sheet as cathode, using Ag doping lead dioxide electrode or pure lead dioxide electrode as anode, then 20mA/cm again2's
It degrades under current density；Degradation process removes a sample every 30min, obtains curve shown in fig. 6.
Fig. 6 is the phenol of different doping Ag doping lead dioxide electrodes and pure lead dioxide electrode that embodiment 1 obtains
Removal rate changes with time comparison diagram.Electrode after Ag doping is obviously improved the efficiency of degradation of phenol, because the doping of silver increases
The strong conductive capability of electrode, improves the delivery rate of electronics in reaction, reduces the voltage of reaction, improve the electric current of degradation
Efficiency.
Claims (8)
1. a kind of preparation method of Ag doping lead dioxide electrode, which is characterized in that specific step is as follows for the preparation method:
The pretreatment of step 1. titanium plate
First titanium plate is cleaned, is then polished, then titanium plate is impregnated into temperature is 95 DEG C and mass fraction is 15%
2h in oxalic acid solution；By titanium plate after being taken out in oxalic acid solution, then with deionized water is cleaned and dried up；
The preparation of step 2. simple substance silver layer
Silver ammino solution is instilled in the reducing solution of sodium potassium tartrate tetrahydrate dropwise and obtains silver plating liquid；Pretreated titanium plate is put into silver-plated
It carries out silver-plated in liquid, obtains the titanium plate for being coated with elemental silver middle layer；
Step 3. electro-deposition PbO2
Using copper sheet as cathode, to be coated with the titanium plate of elemental silver middle layer as anode, with Pb (NO3)2、Cu(NO3)2With the mixing of NaF
Solution is electrodeposit liquid, carries out electro-deposition, obtains the electrode.
2. the preparation method of Ag doping lead dioxide electrode according to claim 1, which is characterized in that silver-plated in step 2
The configuration process of liquid is as follows: the ammonium hydroxide of 80-100ml/L instilled in the silver nitrate solution of 20-30g/L, after solution clarification
To silver ammino solution, silver ammino solution is added in the potassium sodium tartrate solution of isometric 100g/L and obtains silver plating liquid.
3. the preparation method of Ag doping lead dioxide electrode according to claim 1, which is characterized in that silver-plated in step 2
The silver-plated temperature of liquid is maintained at 30 DEG C, a length of 1-3h when silver-plated.
4. the preparation method of Ag doping lead dioxide electrode according to claim 1, which is characterized in that the electricity of step 3 is heavy
In hydrops, Pb (NO3)2Concentration be 0.5-0.7mol/L, Cu (NO3)2Concentration be 0.1-0.2mol/L, the concentration of NaF is
0.01-0.1mol/L, the pH value of electrodeposit liquid are 1-2.
5. the preparation method of Ag doping lead dioxide electrode according to claim 1, which is characterized in that step 3 electro-deposition
Condition are as follows: the stirring rate of electrodeposit liquid be 80rpm, electrodeposition temperature be 60 DEG C, in 20mA/cm2Current density under electricity
Deposit 2h.
6. a kind of according to claim 1 to Ag doping lead dioxide electrode made from any one of 5 the methods, which is characterized in that
Elemental silver is entrained in titanium dioxide lead layer in the doping lead dioxide electrode.
7. a kind of according to claim 1 to the application of Ag doping lead dioxide electrode made from any one of 5 the methods, feature
It is, the electrode is used for degradation of phenol class organic pollutant.
8. the application of Ag doping lead dioxide electrode according to claim 7, which is characterized in that the organic dirt of degradation of phenol class
When contaminating object, cathode is copper sheet, and anode is according to electrode as claimed in claim 6, current density 20mA/cm2, benzene to be degraded
The initial concentration of phenol organic matter pollutant in the solution is 100mg/L, Na in solution2SO4Concentration 0.35mol/L, pH value of solution
Value is 5.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20170316891A1 (en) * | 2015-08-24 | 2017-11-02 | Nanotek Instruments, Inc. | Supercapacitor Having a High Volumetric Energy Density |
| CN108060451A (en) * | 2017-12-20 | 2018-05-22 | 陕西科技大学 | A kind of preparation method of hydrophobic natural fiber dioxide composite lead anode |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170316891A1 (en) * | 2015-08-24 | 2017-11-02 | Nanotek Instruments, Inc. | Supercapacitor Having a High Volumetric Energy Density |
| CN108060451A (en) * | 2017-12-20 | 2018-05-22 | 陕西科技大学 | A kind of preparation method of hydrophobic natural fiber dioxide composite lead anode |
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Application publication date: 20190730 |