CN109261149A - The nano-porous silver of self-supporting and the preparation method of silver electrode - Google Patents
The nano-porous silver of self-supporting and the preparation method of silver electrode Download PDFInfo
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- CN109261149A CN109261149A CN201810853627.XA CN201810853627A CN109261149A CN 109261149 A CN109261149 A CN 109261149A CN 201810853627 A CN201810853627 A CN 201810853627A CN 109261149 A CN109261149 A CN 109261149A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 64
- 239000004332 silver Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 229910001428 transition metal ion Inorganic materials 0.000 claims abstract description 12
- SDLBJIZEEMKQKY-UHFFFAOYSA-M silver chlorate Chemical compound [Ag+].[O-]Cl(=O)=O SDLBJIZEEMKQKY-UHFFFAOYSA-M 0.000 claims abstract description 10
- 239000011343 solid material Substances 0.000 claims abstract description 9
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 229910021381 transition metal chloride Inorganic materials 0.000 claims abstract description 7
- 239000011244 liquid electrolyte Substances 0.000 claims abstract description 6
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 6
- -1 transition-metal cation Chemical class 0.000 claims abstract description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 239000001103 potassium chloride Substances 0.000 claims description 4
- 235000011164 potassium chloride Nutrition 0.000 claims description 4
- 238000007654 immersion Methods 0.000 claims description 3
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 3
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 2
- 229910001510 metal chloride Inorganic materials 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 22
- 238000005265 energy consumption Methods 0.000 abstract description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 7
- 239000001301 oxygen Substances 0.000 abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 5
- 230000010757 Reduction Activity Effects 0.000 abstract description 3
- 230000036647 reaction Effects 0.000 abstract description 3
- 229910021607 Silver chloride Inorganic materials 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
- 238000006722 reduction reaction Methods 0.000 description 17
- 239000003792 electrolyte Substances 0.000 description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 16
- 230000009467 reduction Effects 0.000 description 13
- 239000008367 deionised water Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- 210000004027 cell Anatomy 0.000 description 7
- 230000005611 electricity Effects 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 238000002484 cyclic voltammetry Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 210000003850 cellular structure Anatomy 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010408 sweeping Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 229910017944 Ag—Cu Inorganic materials 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 238000007578 melt-quenching technique Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920005597 polymer membrane Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/50—Silver
-
- B01J35/61—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention provides a kind of preparation method of nano-porous silver, using the solid material of at least surface argentiferous as precursor, it immerses in the liquid electrolyte containing transition metal ions and metal chloride, promote silver surface to spontaneously form silver chlorate by transition-metal cation by micro cell reaction, forms nano-porous silver after electroreduction.The present invention also provides a kind of preparation methods of the nanoporous silver electrode of self-supporting, are prepared using silver electrode as precursor using the above method.Compared with prior art, nano-porous silver is prepared using the method for the invention, promotes silver surface to spontaneously form silver chlorate by transition-metal cation by micro cell reaction；Nano-porous silver is formed after electroreduction, compared with original silver electrode, oxygen reduction activity is significantly improved；Compared with prior art, it eliminates to silver electrode and applies voltage formation this energy consumption process of AgCl, reduce energy consumption；This method has many advantages, such as that simple, operation controllability is strong.
Description
Technical field
The invention belongs to field of nano material preparation, more particularly to the nano-porous silver and self-supporting of a kind of self-supporting
Nanoporous silver electrode preparation method.
Background technique
Silver-colored (Ag) is enriched compared to noble metals such as Pt, Pd with stock number, the advantages such as cheap, for Ag is as catalyst
To multiple reactions, such as: oxygen reduction reaction (ORR), carbon dioxide electro-reduction reaction (CO2RR), hydrogenation reaction etc. all has good
Catalytic activity.Research of the Ag as ORR elctro-catalyst, has there is more than 60 years history.Since the 1980s, alkaline
Many realistic problems such as the cost of fuel cell Yin Qigao and its carbonation being difficult to avoid that in practical application are difficult to solve
Certainly, the research work temperature of alkaline fuel cell is caused to reduce, so that the research of Ag base ORR elctro-catalyst be made also to substantially reduce.
But in recent years, Ag base ORR elctro-catalyst becomes research by the rise of alkaline polymer membrane cell once again
Hot spot.
Self-supporting nano porous metal is because of its own good cellular structure, high specific surface area, good electric conductivity etc.
Design feature has special advantage in electro-catalysis field.Especially to metal-air battery, chemical sensor, fuel electricity
For the device and device of the electrochemical reactions such as pond, electrochemical reaction occurs on gas liquid solid three phase boundary, there is gas,
Liquid, the transmission of electricity and transition process, so the nano porous metal material with self supporting structure is because good possessed by its own
Good cellular structure has splendid application prospect.The method for commonly preparing self supporting structure porous metals includes de- alloy
Method, template etc..The method using Ag base noncrystal alloy as precursor preparation nano-porous silver has been invented by Liu Xiong army et al.
(CN103255441B), a series of Ag-Mg-Ca amorphous alloy ribbons are prepared using the method for fast melt-quenching first, then selected
Selecting suitable electrolyte progress electrochemistry goes alloying component to corrode, and removes Mg and Ca element, obtains nano-porous silver.This method
Although avoiding caustic alkali and high-temperature burning process in the de- alloyage of tradition, alloy precursor preparation process is complicated, and energy consumption is high,
Atom utilization is low.Therefore develop that preparation process is simple, nano porous metal preparation method of atom economy is of great significance.
Publication No. is that the patent of CN105689733A discloses the method that electrochemical method prepares nano-porous silver, and silver is carried out electricity first
Chemical oxidation generates silver chlorate, then by silver chlorate electrochemical reduction to be silver-colored, forms nano-porous silver after chloride ion removing.It is this
Method preparation process is simple, however the oxidation and reduction of silver are both needed to apply voltage, and process energy consumption is high, needs the system of invention low energy consumption
The method of standby nano porous metal.
Summary of the invention
The present invention for the deficiency of self-supporting nanoporous silvery Preparation Method in the prior art, provide it is a kind of it is simple and easy to do,
The method of the nano-porous silver for the preparation self-supporting that low energy consumption.This method utilize micro cell principle, by transition metal ions with
Silver-colored spontaneous reaction generates silver chlorate, eliminates this energy consumption step of electrochemical oxidation, after through electrochemical reduction to generate nanometer more
Kong Yin.It can make electrode surface nanosizing, porous using this method, to improve the oxygen reduction activity of electrode.
To achieve the above object, the present invention is realized using scheme in detail below:
A kind of preparation method of the nano-porous silver of self-supporting, using the solid material of at least surface argentiferous as precursor, leaching
Enter in the liquid electrolyte containing transition metal ions and metal chloride, is reacted by micro cell by transition-metal cation
Promote silver surface to spontaneously form silver chlorate, forms nano-porous silver after electroreduction.
Further, the transition metal ions is Cu2+Or Fe3+。
Further, the Cu2+Or Fe3+Concentration be 0.005-1M.
Further, the metal chloride is any one in copper chloride, iron chloride, sodium chloride or potassium chloride.
Further, the solid material of at least surface argentiferous is in the liquid containing transition metal ions and metal chloride
Dip time is 0.01-3600s in body electrolyte.
Further, content 0.01-99.9% silver-colored in the solid material of at least surface argentiferous.
Further, the solid material of at least surface argentiferous is filamentary silver, silver strip or silver bullion.
The present invention also provides a kind of preparation methods of the nanoporous silver electrode of self-supporting, using silver electrode as precursor, leaching
Enter in the liquid electrolyte containing transition metal ions and metal chloride, is reacted by micro cell by transition-metal cation
Promote silver surface to spontaneously form silver chlorate, the nanoporous silver electrode of self-supporting is made after electroreduction.
The present invention compared with prior art have following advantages and effects
(1) using the nano-porous silver of the method for the invention preparation self-supporting, by micro cell reaction by transition gold
Belonging to cation promotes silver surface to spontaneously form silver chlorate, the nano-porous silver of self-supporting is formed after electroreduction, with prior art phase
Than eliminating to silver electrode and applying voltage formation this energy consumption process of AgCl, reduce energy consumption；Self-supporting is formed after electroreduction
Nano-porous silver, compared with original silver electrode, oxygen reduction activity is significantly improved.
(2) this method has many advantages, such as that simple, operation controllability is strong.
Detailed description of the invention
Fig. 1 is the SEM electron microscopic picture for the nano-porous silver being prepared according to embodiment 1；
Fig. 2 be the nano-porous silver for preparing of comparative example 1 and embodiment 1,2 as oxygen reduction reaction elctro-catalyst when oxygen also
Former performance curve.
Specific embodiment
Combined with specific embodiments below and attached drawing is described in further details the present invention.
Embodiment 1:
By diameter be 5mm Ag electrode with 50nm aluminium oxide polished material polish electrode to mirror surface after, be washed with deionized water
Electrode surface, then the ultrasound 15s in ethyl alcohol and ultrapure water respectively.The Ag electrode polished is put into containing 10mM Cu2+Chlorine
Change in sodium electrolyte, is rinsed with water completely after impregnating 10min.Using the Ag electrode after impregnating as working electrode, Pt conducts pair
Electrode, Hg/HgO is as reference electrode, and electrolyte is the NaOH of 0.1M, with 10mV s in -0.8~0.3V potential region-1's
It sweeps speed and carries out cyclic voltammetry scan (20 circle), electrochemical reduction is carried out to electrode, generates nano-porous silver, to the Ag electricity after reduction
Pole carries out electron-microscope scanning, as a result as shown in Figure 1.
ORR polarization curve is tested in the case where electrode revolving speed is 1600rpm, ORR half wave potential is 0.672V, compared to initial
Ag electrode improves 20mV, as shown in Figure 2.
Embodiment 2:
By diameter be 5mm Ag electrode with 50nm aluminium oxide polished material polish electrode to mirror surface after, be washed with deionized water
Electrode surface, then the ultrasound 15s in ethyl alcohol and ultrapure water respectively.The Ag electrode polished is put into containing 0.1M Fe3+Chlorine
Change in sodium electrolyte, is rinsed with water completely after impregnating 10min.Using the Ag electrode after impregnating as working electrode, Pt conducts pair
Electrode, Hg/HgO is as reference electrode, and electrolyte is the NaOH of 0.1M, with 10mV s in -0.8~0.3V potential region-1's
It sweeps speed and carries out cyclic voltammetry scan (20 circle), electrochemical reduction is carried out to electrode, generates nano-porous silver.
ORR polarization curve is tested in the case where electrode revolving speed is 1600rpm, ORR half wave potential is 0.732V, compared to initial
Ag electrode improves 60mV, as shown in Figure 2.
Embodiment 3:
The Ag silk that diameter is 0.5mm is respectively placed in deionized water, is cleaned by ultrasonic 30min in acetone, after, use deionized water
Clean Ag silk table face.The Ag being ultrasonically treated silk is put into 0.1M Cu2+Potassium chloride electrolyte in, impregnate 10min after rushed with water
Wash clean.Using the Ag silk after impregnating as working electrode, Pt are used as to electrode, and Hg/HgO is as reference electrode, electrolyte
The NaOH of 0.1M, with 10mV s in -0.8~0.3V potential region-1Speed of sweeping carry out cyclic voltammetry scan (20 circle), to electrode
It carries out electrochemical reduction and generates nano-porous silver.
Embodiment 4:
The Ag silk that diameter is 0.5mm is respectively placed in deionized water, is cleaned by ultrasonic 30min in acetone, after, use deionized water
Clean Ag silk table face.The Ag being ultrasonically treated silk is put into 0.1M Fe3+Potassium chloride electrolyte in, impregnate 10min after, will soak
After Ag silk after bubble is rinsed with water completely, using the Ag silk after impregnating as working electrode, Pt as to electrode, Hg/HgO conduct
Reference electrode, electrolyte is the NaOH of 0.1M, in -0.8~0.3V potential region with 10mV s-1Sweep speed carry out cyclic voltammetric sweep
(20 circle) is retouched, electrochemical reduction is carried out to electrode, generates nano-porous silver.
Embodiment 5:
It will be respectively placed in deionized water for 50% Ag-Cu alloy sheet with a thickness of the silver content of 1mm, is cleaned by ultrasonic in acetone
30min, after, it is washed with deionized water Ag piece surface.The Ag piece being ultrasonically treated is put into 0.1M chlorination copper electrolyte, is impregnated
After 5min, after the Ag piece after immersion is rinsed with water completely, using the Ag piece after impregnating as working electrode, Pt as to electricity
Pole, Hg/HgO is as reference electrode, and electrolyte is the NaOH of 0.1M, with 10mV s in -0.8~0.3V potential region-1Sweep
Speed carries out cyclic voltammetry scan (20 circle), carries out electrochemical reduction to electrode, generates nano-porous silver.
Embodiment 6:
It is washed with deionized water deionized water is respectively placed in a thickness of the Ag piece of 1mm after being cleaned by ultrasonic 30min in acetone
Net Ag piece surface.The Ag piece being ultrasonically treated is put into 0.1M iron chloride electrolyte, after impregnating 0.01s, by the Ag after immersion
After piece is rinsed with water completely, using the Ag piece after impregnating as working electrode, Pt are used as to electrode, and Hg/HgO is as reference electricity
Pole, electrolyte is the NaOH of 0.1M, with 10mV s in -0.8~0.3V potential region-1Sweep speed carry out cyclic voltammetry scan
(20 circle), carries out electrochemical reduction to electrode, generates nano-porous silver.
Comparative example 1:
Ag rotating disc electrode (round, diameter 5mm) (Tianjin Aidahengsheng Technology Development Co., Ltd) is as work electricity
Pole, Pt are used as to electrode, and Hg/HgO carries out ORR test as reference electrode in the NaOH electrolyte of 0.1M.- 0.8~
With 10mV s in 0.3V potential region-1Speed of sweeping carry out cyclic voltammetry scan (20 circle), electrode revolving speed is 1600rpm, ORR polarization
The half wave potential of curve is 0.652V, as shown in Figure 2.
Interpretation of result:
(1) as shown in Figure 1, the finally obtained porous silver of embodiment 1 has porous structure, by having a size of 100 rans
Aggregation of silver particles formed, duct is formed between particle；The gap of Nano silver grain aggregation forms up to a hundred nanometers of duct.
(2) Fig. 2 is the nano-porous silver for preparing of comparative example 1 and embodiment 1, embodiment 2 as oxygen reduction reaction electro-catalysis
Hydrogen reduction performance curve when agent.As shown in Figure 2, the hydrogen reduction performance of the nano-porous silver of Examples 1 and 2 preparation is better than comparison
Example 1, the reason is that since nano-porous silver has bigger specific surface area and is conducive to the pore structure of mass transfer.Prepared by embodiment 2
The hydrogen reduction performance of nano-porous silver is better than embodiment 1, because of the transition metal ions Fe in the electrolyte of embodiment 23+Oxidation
Performance ratio Cu2+By force, and concentration is high, high concentration, high oxidative transition metal ions be conducive to the system of nanoporous ag material
It is standby.
Embodiment described above is only that preferred embodiments of the present invention will be described, not to the scope of the present invention
It is defined, without departing from the spirit of the design of the present invention, those of ordinary skill in the art are to technical solution of the present invention
The various changes and improvements made should all be fallen into the protection scope that claims of the present invention determines.
Claims (8)
1. a kind of preparation method of the nano-porous silver of self-supporting, it is characterised in that: make the solid material of at least surface argentiferous
It for precursor, immerses in the liquid electrolyte containing transition metal ions and metal chloride, is reacted by micro cell by transition
Metal cation promotes silver surface to spontaneously form silver chlorate, forms nano-porous silver after electroreduction.
2. preparation method according to claim 1, which is characterized in that the transition metal ions is Cu2+Or Fe3+。
3. preparation method according to claim 2, which is characterized in that the Cu2+Or Fe3+Concentration be 0.005-1M.
4. preparation method according to claim 1-3, which is characterized in that the metal chloride be copper chloride,
Any one in iron chloride, sodium chloride or potassium chloride.
5. preparation method according to claim 1, which is characterized in that the solid material of at least surface argentiferous is containing
Dip time is 0.01-3600s in the liquid electrolyte of transition metal ions and metal chloride.
6. preparation method according to claim 1, which is characterized in that silver-colored in the solid material of at least surface argentiferous
Content 0.01-99.9%.
7. preparation method according to claim 1, which is characterized in that the solid material of at least surface argentiferous is silver
Silk, silver strip or silver bullion.
8. a kind of preparation method of the nanoporous silver electrode of self-supporting, which is characterized in that using silver electrode as precursor, immersion contains
In the liquid electrolyte for having transition metal ions and metal chloride, is reacted by micro cell and promoted by transition-metal cation
Silver surface spontaneously forms silver chlorate, and the nanoporous silver electrode of self-supporting is made after electroreduction.
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| CN201810853627.XA CN109261149A (en) | 2018-07-30 | 2018-07-30 | The nano-porous silver of self-supporting and the preparation method of silver electrode |
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| CN201810853627.XA CN109261149A (en) | 2018-07-30 | 2018-07-30 | The nano-porous silver of self-supporting and the preparation method of silver electrode |
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| CN109261149A true CN109261149A (en) | 2019-01-25 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112853400A (en) * | 2021-01-05 | 2021-05-28 | 昆明理工大学 | Preparation method of nano-porous silver-based substrate with surface having Raman signal enhancing function |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20030038000A (en) * | 2001-11-08 | 2003-05-16 | 진준형 | Process for producing standard electrode coated with silver/silver chloride thin layer using a porous |
| CN104925750A (en) * | 2015-05-07 | 2015-09-23 | 南京文钧医疗科技有限公司 | Preparation method for TiO2 nanowire-Ag/AgCl-Fe3O4 composite material with Yolk-Shell structures |
| CN106884190A (en) * | 2015-12-15 | 2017-06-23 | 中国科学院大连化学物理研究所 | A kind of preparation of classifying porous material and classifying porous material |
| CN106881087A (en) * | 2015-12-16 | 2017-06-23 | 中国科学院大连化学物理研究所 | A kind of cube skeletal porous silver and preparation method thereof |
-
2018
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20030038000A (en) * | 2001-11-08 | 2003-05-16 | 진준형 | Process for producing standard electrode coated with silver/silver chloride thin layer using a porous |
| CN104925750A (en) * | 2015-05-07 | 2015-09-23 | 南京文钧医疗科技有限公司 | Preparation method for TiO2 nanowire-Ag/AgCl-Fe3O4 composite material with Yolk-Shell structures |
| CN106884190A (en) * | 2015-12-15 | 2017-06-23 | 中国科学院大连化学物理研究所 | A kind of preparation of classifying porous material and classifying porous material |
| CN106881087A (en) * | 2015-12-16 | 2017-06-23 | 中国科学院大连化学物理研究所 | A kind of cube skeletal porous silver and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| LIZHI YUAN ET AL.: "Electrochemically sythesized freestanding 3D nanoporous silver electrode with high electrocatalytic activity", 《CATALYSIS SCIENCE & TECHNOLOGY》 * |
| MIKI KANNA ET AL.: "Preparation of an Economic Home-Made Ag/AgCl Electrode from Silver Recovered from Laboratory Wastes", 《CHIANG MAI JOURNAL OF SCIENCE》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112853400A (en) * | 2021-01-05 | 2021-05-28 | 昆明理工大学 | Preparation method of nano-porous silver-based substrate with surface having Raman signal enhancing function |
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Application publication date: 20190125 |