CN106884190A - A kind of preparation of classifying porous material and classifying porous material - Google Patents
A kind of preparation of classifying porous material and classifying porous material Download PDFInfo
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- CN106884190A CN106884190A CN201510934247.5A CN201510934247A CN106884190A CN 106884190 A CN106884190 A CN 106884190A CN 201510934247 A CN201510934247 A CN 201510934247A CN 106884190 A CN106884190 A CN 106884190A
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- porous material
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- classifying porous
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/10—Oxidising
- C23C8/12—Oxidising using elemental oxygen or ozone
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/80—After-treatment
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- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Electrochemistry (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Inert Electrodes (AREA)
Abstract
The present invention relates to a kind of preparation method of nano porous metal, refer in particular to it is a kind of the metals such as gold, copper, silver, zinc, iron, nickel are oxidized to oxide, then by the two-step method method for preparing nano porous metal of electrochemical reduction.Compared with prior art, the preparation method of porous material of the present invention has environmental protection, simplicity, easy to implement, low production cost；And the aperture of porous metals and porosity distribution are controllable in preparation process；And most of metal can form oxide, porous metals can be prepared by way of the removing oxonium ion of simple and fast afterwards, therefore the method has the advantages that to commonly use simultaneously.
Description
Technical field
The invention belongs to technical field of material, more particularly to a kind of preparation method of porous material.
Background technology
Nano porous metal is this year come the class novel nano structure material for growing up, because it has than table
Area is big, density is small, flexible structure is adjustable, good penetrability the features such as so that porous material by widely should
For separating, being catalyzed, sense, the field such as medicine, electrode, machinery.
A kind of common method for preparing porous metals is de- alloyage and template.De- alloy approach will typically be used
Used as raw material, alloy is generally prepared specialty alloys using metallurgical method, by two kinds of electrochemical potentialses difference compared with
Big metal is constituted.By relatively active in the method control dissolving raw material of electrolysis or chemical attack
Metallic element, so as to produce pore space structure in raw material.The final hole skeleton for remaining is by raw material
The metal of middle relative inertness is constituted.Template, technique is relative complex, high cost, it is difficult to realize industrial metaplasia
Produce, at the same it is single using silver-colored pore structure prepared by the above method, and be difficult to control to.
The content of the invention
The present invention is directed to problems of the prior art, invented it is a kind of it is simple be easily achieved prepare porous material
The method of material.
To realize foregoing invention content, the present invention is realized using following technical scheme：
A kind of preparation method of classifying porous material is comprised the following steps：
(1) oxidation processes in electrolyte are carried out to metal material using electrochemical oxidation method or uses thermal oxide
Method carries out oxidation processes in oxygen atmosphere to metal material；
(2) electrochemical reduction is carried out to the metal material after step (1) gained treatment；
Metal material described in step (1) be gold, silver, copper, zinc, iron, nickel, magnesium in one or two
Alloy above；Electrolyte described in step (1) be NaOH and KOH in one or two.
The electrochemical oxidation and the detailed process of electrochemical reduction treatment of being carried out to metal material is with the gold
Category material is working electrode, with the one kind in platinum, graphite rod, silver, gold be to electrode, silver/silver chlorate, mercury/
Mercury oxide or saturation calomel are reference electrode；The method of the electrochemical oxidation and electrochemical reduction is constant potential
Method.
Oxidate temperature described in step (1) is not less than 100 DEG C, and the thermal oxidation time is 1s~24h.
The oxidate temperature is preferably 200 DEG C~1000 DEG C, and the thermal oxidation time is preferably 30min~12
h。
Electrochemical oxidation current potential in the electrochemical oxidation process relative to reversible hydrogen electrode is not less than 0V, electricity
The chemical oxidation time is 1s~12h.
In the electrochemical oxidation process 0V~3V is preferably relative to reversible hydrogen electrode electrochemical oxidation current potential；
The electrochemical oxidation time is preferably 10min~3h.
During the electrochemical reduction relative to reversible hydrogen electrode electrochemical reduction current potential be -0.1V~-3V；
The electrochemical reduction time is 1s~12h.
Electrochemical reduction current potential during the electrochemical reduction relative to reversible hydrogen electrode is preferably -0.6
V~-1.2V；The electrochemical reduction time is preferably 10min~3h.
Classifying porous material obtained in the porous material preparation method, obtained classifying porous material, by gold
Category nanoparticle aggregation formed one-level hole aggregation assemble again formation second hole aggregation be connected with each other and
Formed；There is one-level hole, the aperture in one-level hole is 5~300nm on the aggregation of the one-level hole；Described two grades
There is second hole, the aperture of second hole is 0.5~5 μm on the aggregation of hole.
In the obtained classifying porous material, a diameter of 10~100nm of metal nanoparticle, the one-level
A diameter of 1~6 μm of hole aggregation.
Compared with prior art, the preparation method of porous material of the present invention have environmental protection, simplicity, easily
In implementation, low production cost；And the aperture of porous metals and porosity distribution are controllable in preparation process；And
Most of metal can form oxide, can be prepared by way of the removing oxonium ion of simple and fast afterwards
Porous metals are obtained, therefore the method has the advantages that to commonly use simultaneously.
Brief description of the drawings
Fig. 1 is the stereoscan photograph of porous zinc prepared by embodiment 1.
Fig. 2 is the carbon dioxide Electrochemical Properties curve of nanoporous zinc prepared by comparative example 1 and embodiment 1.
Specific embodiment
The present invention is described in detail with reference to embodiment.It is specific that certain present invention is not limited in these
Embodiment.
Comparative example 1：Zinc metal sheet (traditional Chinese medicines).
Embodiment 1：Prepare the solution of the NaOH containing 0.1M and as electrolyte, zinc metal sheet is used as work
Electrode, platinized platinum is that, to electrode, mercury/mercuric oxide electrode is reference electrode, first in 3V (relative to reversible hydrogen electricity
Pole) under carry out electrochemicial oxidation 30min, carry out electricity under -3V (relative to reversible hydrogen electrode) afterwards
Electronation 10min obtains porous zinc.
Embodiment 2：Prepare the solution of the KOH containing 0.2M and as electrolyte, copper wire is used as work electricity
Pole, platinized platinum is that, to electrode, silver/silver chloride electrode is reference electrode, first at 0V (relative to reversible hydrogen electrode)
Under carry out electrochemicial oxidation 1s, carry out electrochemistry also under -2V (relative to reversible hydrogen electrode) afterwards
Former 1s obtains Porous Cu.
Embodiment 3：Prepare the solution of the NaOH containing 0.3M and as electrolyte, nickel foil is used as work
Electrode, platinized platinum is that, to electrode, saturated calomel electrode is reference electrode, first in 2.0V (relative to reversible hydrogen electricity
Pole) under carry out electrochemicial oxidation 12h, carry out electricity under -1.2V (relative to reversible hydrogen electrode) again afterwards
Electronation obtains nickel porous 3h.
Embodiment 4：By 1cm2Copper Foil 24h is heat-treated in 1000 DEG C of air atmosphere, made afterwards
It is working electrode, used as electrolyte, platinized platinum is that, to electrode, mercury/mercuric oxide electrode is reference electricity to 0.2M KOH
Electrochemical reduction 12h is carried out under pole, then -1.2V (relative to reversible hydrogen electrode) obtain Porous Cu.
Embodiment 5：By 1cm2Iron foil 12h is heat-treated in 200 DEG C of air atmosphere, afterwards as
Working electrode, used as electrolyte, platinized platinum is that, to electrode, mercury/mercuric oxide electrode is reference electrode to 0.1M NaOH,
Electrochemical reduction 6h is carried out under -1.7V (relative to reversible hydrogen electrode) obtain porous iron again.
Embodiment 6：Prepare the solution of the KOH containing 0.5M and as electrolyte, filamentary silver is used as work
Electrode, platinized platinum is that, to electrode, silver/silver chloride electrode is reference electrode, first in 1.2V (relative to reversible hydrogen electricity
Pole) under carry out electrochemicial oxidation 3h, carry out electrification under -0.1V (relative to reversible hydrogen electrode) again afterwards
Learn reduction and obtain the porous silver of 3h.
Embodiment 7：By 1cm2Goldleaf 30min is heat-treated in 500 DEG C of oxygen atmosphere, made afterwards
It is working electrode, used as electrolyte, platinized platinum is that, to electrode, mercury/mercuric oxide electrode is reference electricity to 0.1M NaOH
Electrochemical reduction 10min is carried out under pole, then -0.6V (relative to reversible hydrogen electrode) obtain porous gold.
Embodiment 8：By 1cm2Magnesium paper tinsel 8h is heat-treated in 600 DEG C of oxygen atmosphere, afterwards as work
Make electrode, used as electrolyte, platinized platinum is that, to electrode, mercury/mercuric oxide electrode is reference electrode to 0.1M NaOH,
Electrochemical reduction 2h is carried out under -1.85V (relative to reversible hydrogen electrode) obtain porous magnesium again.
Fig. 1 is the stereoscan photograph of the nanoporous zinc prepared according to embodiment 1, and the material is received as shown in the figure
A diameter of 10-100nm of rice corpuscles, the size of the aggregation that nanoparticle aggregation is formed is 1-6 μm.
Fig. 2 is the carbon dioxide Electrochemical Properties curve of nanoporous zinc prepared by comparative example 1 and embodiment 1.
Compare and understand, the carbon dioxide activity of nanoporous zinc is higher than zinc metal sheet.
Claims (10)
1. a kind of preparation method of classifying porous material, it is characterised in that：Comprise the following steps,
(1) oxidation processes or use heat are carried out to metal material in electrolyte using electrochemical oxidation method
Method for oxidation carries out oxidation processes in oxygen atmosphere to metal material；
(2) electrochemical reduction is carried out to the metal material after step (1) gained treatment；
Metal material described in step (1) be gold, silver, copper, zinc, iron, nickel, magnesium in one or two
Alloy above；Electrolyte described in step (1) be NaOH and KOH in one or two.
2. as claimed in claim 1 classifying porous material preparation method, it is characterised in that：It is described to metal material
Material carry out electrochemical oxidation and electrochemical reduction treatment detailed process be with the metal material as working electrode,
It is that, to electrode, silver/silver chlorate, mercury/mercury oxide or saturation calomel are with the one kind in platinum, graphite rod, silver, gold
Reference electrode；The method of the electrochemical oxidation and electrochemical reduction is potentiostatic method.
3. as claimed in claim 1 classifying porous material preparation method, it is characterised in that：In step (1)
The oxidate temperature is not less than 100 DEG C, and the thermal oxidation time is 1s~24h.
4. as claimed in claim 3 classifying porous material method, it is characterised in that the oxidate temperature is preferred
It it is 200 DEG C~1000 DEG C, the thermal oxidation time is preferably 30min~12h.
5. as claimed in claim 1 or 2 classifying porous material preparation method, it is characterised in that：The electrification
In oxidizing process 0V, electrochemical oxidation time are not less than relative to the electrochemical oxidation current potential of reversible hydrogen electrode
It is 1s~12h.
6. as claimed in claim 5, it is characterised in that：Relative to reversible hydrogen electricity in the electrochemical oxidation process
The electrochemical oxidation current potential of pole is preferably 0V~3V；The electrochemical oxidation time is preferably 10min~3h.
7. as claimed in claim 1 or 2 classifying porous material preparation method, it is characterised in that：The electrification
Learn reduction during relative to reversible hydrogen electrode electrochemical reduction current potential be -0.1V~-3V；Electrochemical reduction
Time is 1s~12h.
8. as claimed in claim 7, it is characterised in that：Relative to reversible hydrogen during the electrochemical reduction
The electrochemical reduction current potential of electrode is preferably -0.6V~-1.2V；The electrochemical reduction time is preferably 10
Min~3h.
9., according to classifying porous material obtained in any porous material preparation methods of claim 1-8, it is special
Levy and be：Obtained classifying porous material, the one-level hole aggregation for being formed is assembled by metal nanoparticle again
The second hole aggregation that secondary aggregation is formed is interconnected to form；There is one-level hole on the aggregation of the one-level hole,
The aperture in one-level hole is 5~300nm；There is second hole, the aperture of second hole is on the second hole aggregation
0.5~5 μm.
10. as claimed in claim 9 classifying porous material, it is characterised in that：The obtained classifying porous material
In material, a diameter of 10~100nm of metal nanoparticle, a diameter of 1~6 μm of one-level hole aggregation.
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| CN201510934247.5A CN106884190A (en) | 2015-12-15 | 2015-12-15 | A kind of preparation of classifying porous material and classifying porous material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107723769A (en) * | 2017-10-24 | 2018-02-23 | 宝鸡市铭坤有色金属有限公司 | A kind of preparation method of nano-crystal nickel material |
| CN107904644A (en) * | 2017-10-19 | 2018-04-13 | 天津大学 | A kind of method for preparing tungsten nano surface porous active layer |
| CN107904645A (en) * | 2017-10-19 | 2018-04-13 | 天津大学 | A kind of anodized surface processing method for improving metal molybdenum foil surface-active |
| CN108570703A (en) * | 2018-04-08 | 2018-09-25 | 天津大学 | Preparation method of tungsten/copper laminated composite material based on tungsten sheet surface nanocrystallization |
| CN109261149A (en) * | 2018-07-30 | 2019-01-25 | 青岛科技大学 | The nano-porous silver of self-supporting and the preparation method of silver electrode |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107904644A (en) * | 2017-10-19 | 2018-04-13 | 天津大学 | A kind of method for preparing tungsten nano surface porous active layer |
| CN107904645A (en) * | 2017-10-19 | 2018-04-13 | 天津大学 | A kind of anodized surface processing method for improving metal molybdenum foil surface-active |
| CN107904644B (en) * | 2017-10-19 | 2019-10-01 | 天津大学 | A method of preparing tungsten nano surface porous active layer |
| CN107904645B (en) * | 2017-10-19 | 2019-10-11 | 天津大学 | A kind of anodized surface processing method improving metal molybdenum foil surface-active |
| CN107723769A (en) * | 2017-10-24 | 2018-02-23 | 宝鸡市铭坤有色金属有限公司 | A kind of preparation method of nano-crystal nickel material |
| CN108570703A (en) * | 2018-04-08 | 2018-09-25 | 天津大学 | Preparation method of tungsten/copper laminated composite material based on tungsten sheet surface nanocrystallization |
| CN108570703B (en) * | 2018-04-08 | 2019-12-20 | 天津大学 | Preparation method of tungsten/copper laminated composite material based on tungsten sheet surface nanocrystallization |
| CN109261149A (en) * | 2018-07-30 | 2019-01-25 | 青岛科技大学 | The nano-porous silver of self-supporting and the preparation method of silver electrode |
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