CN109913893A - A kind of ferriferous oxide micron chip self-supporting electrode and its synthetic method - Google Patents
A kind of ferriferous oxide micron chip self-supporting electrode and its synthetic method Download PDFInfo
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- CN109913893A CN109913893A CN201910325043.XA CN201910325043A CN109913893A CN 109913893 A CN109913893 A CN 109913893A CN 201910325043 A CN201910325043 A CN 201910325043A CN 109913893 A CN109913893 A CN 109913893A
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- iron
- supporting electrode
- ferriferous oxide
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- micron chip
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a kind of ferriferous oxide micron chip self-supporting electrode and its synthetic methods, belong to self-supporting electrode fabrication field.The self-supporting electrode is foamed iron, and the surface homoepitaxial of foamed iron has the oxide of the iron of micron chip pattern.The synthetic method of ferriferous oxide micron chip self-supporting electrode, foamed iron is immersed in aqueous solution of urea, and hydro-thermal reaction obtains the ferriferous oxide micron chip self-supporting electrode.The present invention reacts at a certain temperature using foamed iron as reactant and urea liquid, synthesize homoepitaxial in foam iron surface on the surface of self-supporting electrode foam iron, the oxide catalyst of iron with micron chip architecture, and the oxide catalyst electro-chemical activity of the iron is good.Foamed iron in the present invention both participated in reacting as support electrode, while as reactant, reduces the cost of support electrode, saves material utilization amount, simplifies experimental procedure.
Description
Technical field
The present invention relates to self-supporting electrode fabrication fields, and in particular to a kind of ferriferous oxide micron chip self-supporting electrode
And its synthetic method.
Background technique
In recent years, in renewable energy, since the water resource in the whole world is abundant, so water-splitting produces hydrogen and becomes renewable energy
The first choice in source, and determine water-splitting efficiency rate be electrode material selection, at this stage the highest electrode material of efficiency be it is expensive
Metal, but due to noble metal selling at exorbitant prices, it is difficult to which large area is universal, so needing a kind of new electrode material at this stage to expire
Compound is attached to support electrode surface using hydro-thermal method by a wide range of production hydrogen of foot, the prior art, that is to say, that existing
For the preparation of self-supporting electrode in technology, while reactant and support electrode are needed, causes preparation process complicated, cost of material
It is higher.
Summary of the invention
The purpose of the invention is to overcome the problems of the prior art, a kind of ferriferous oxide micron chip self-supporting electricity is provided
Pole and its synthetic method.
One of the objects of the present invention is to provide a kind of ferriferous oxide micron chip self-supporting electrode, which is iron
The electrode or electrode surface part of substrate matter are the electrode of iron-based material, and the surface homoepitaxial of the iron-based material has micron
The oxide of the iron of piece pattern.
Preferably, iron-based material is foamed iron.
Preferably, the oxide of iron is Fe3O4。
The second object of the present invention is to provide a kind of synthetic method of ferriferous oxide micron chip self-supporting electrode, will be described
Foamed iron is immersed in the aqueous solution of urea that concentration is 0.188-0.313mol/L, and it is micro- that hydro-thermal reaction obtains the ferriferous oxide
Rice piece self-supporting electrode.
Preferably, the time of hydro-thermal reaction is 12-14 hours, temperature is 120-140 DEG C.
Preferably, specifically includes the following steps:
S1, removal of impurities pretreatment is carried out to foamed iron；
S2, it weighs urea and is dissolved in ultrapure water, the aqueous solution of urea of clear homogeneous is obtained after stirring；
S3, it pretreated foamed iron is put into the aqueous solution of urea being stirred carries out hydro-thermal reaction；
S4, to after reaction, foamed iron be taken out and is cooled to room temperature, obtains product, by products therefrom ethyl alcohol and super
Then pure water alternate treatment carries out vacuum drying treatment, obtain the ferriferous oxide micron chip self-supporting electrode.
Preferably, including cleaning step to the foamed iron pre- step that clean in step S1, the cleaning step is as follows: first
It with acetone soak ultrasound 10-20min, is then impregnated with the dilute hydrochloric acid of 3moL/L, then alternately rinses 2-5 with ultrapure water and ethyl alcohol
Time, it then impregnates stand-by in deionized water.
Preferably, in S5 the vacuum drying treatment time be 3-5h, treatment temperature be 20-30 DEG C.
Compared with prior art, the beneficial effects of the present invention are: the application is using foamed iron as reactant and 0.188-
The urea liquid of 0.313mol/L carries out hydro-thermal reaction at a certain temperature, synthesizes on the surface of self-supporting electrode foam iron
It is even to be grown in foam iron surface, the oxide of the iron with micron chip architecture, and the electro-chemical activity of the oxide of the iron is good.This
Foamed iron both participates in reacting as support electrode, while as reactant in invention, reduces the cost of support electrode, saves material
Dosage simplifies experimental procedure.
Detailed description of the invention
Fig. 1 is Fe manufactured in the present embodiment3O4XRD spectrum.
Fig. 2 is that the ferriferous oxide manufactured in the present embodiment for being grown in self-supporting electrode surface shines at 3K scanning electron microscope (SEM)
Piece.
Fig. 3 is the LSV H2-producing capacity curve of the ferriferous oxide manufactured in the present embodiment for being grown in self-supporting electrode surface.
Fig. 4 is that the LSV of the ferriferous oxide manufactured in the present embodiment for being grown in self-supporting electrode surface produces oxygen performance curve.
Specific embodiment
With reference to the accompanying drawing and embodiment specific embodiments of the present invention will be described in detail, it is to be understood that this
The protection scope of invention is not limited by the specific implementation.Based on the embodiments of the present invention, ordinary skill people
Member's every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention,
The test method of actual conditions is not specified in the following example, usually according to normal condition, or according to proposed by each manufacturer
Condition.
Embodiment 1
S1, foamed iron is cut, cut size is 1 × 5cm；Then the foamed iron cut is cleaned, first
With acetone soak ultrasound 10 minutes, is then impregnated 20 seconds with the dilute hydrochloric acid of 3moL/L, is alternately rinsed three times with ultrapure water and ethyl alcohol,
It is then placed in deionized water stand-by.
S2, it weighs urea 0.282g and is dissolved in ultrapure water 25ml, the aqueous solution of urea of clear homogeneous is obtained after stirring.
S3, the aqueous solution of urea being stirred is poured into the high temperature water heating kettle with polytetrafluoroethyllining lining, by step S1
In pretreated foamed iron be put into polytetrafluoroethyllining lining and seal, be put into baking oven and reacted.Reaction time is 12 hours,
Temperature is 120 DEG C.
S4, to after the reaction was completed, reaction kettle is cooled to room temperature, products therefrom ethyl alcohol and ultrapure water cross processing are gone forward side by side
Row vacuum drying treatment, vacuum drying treatment time are 3h, and treatment temperature is 20 DEG C, obtain the ferriferous oxide micron chip certainly
Support electrode.
Embodiment 2
S1, foamed iron is cut, cuts out having a size of 1 × 5cm, then cleans the foamed iron cut, it is first
First with acetone soak ultrasound 10 minutes, is then impregnated 30 seconds with the dilute hydrochloric acid of 3moL/L, alternately rinse three with ultrapure water and ethyl alcohol
Time, it is then placed in deionized water stand-by.
S2, it weighs urea 0.47g and is dissolved in ultrapure water 25ml, the aqueous solution of urea of clear homogeneous is obtained after stirring.
S3, the aqueous solution of urea being stirred is poured into the high temperature water heating kettle with polytetrafluoroethyllining lining, by step S1
In pretreated foamed iron be put into polytetrafluoroethyllining lining and seal, be put into baking oven and reacted, the reaction time is 14 hours,
Temperature is 140 DEG C.
S4, to after the reaction was completed, reaction kettle is cooled to room temperature, products therefrom ethyl alcohol and ultrapure water cross processing are gone forward side by side
Row vacuum drying treatment, vacuum drying treatment time are 3h, and treatment temperature is 30 DEG C, obtain described obtaining ferriferous oxide micron
Piece self-supporting electrode.
Embodiment 3
S1, foamed iron is cut, cut size is 1 × 5cm, the foamed iron cut is cleaned, first with third
Ketone impregnates ultrasound 10 minutes, is then impregnated 30 seconds with the dilute hydrochloric acid of 3moL/L, alternately rinses three times with ultrapure water and ethyl alcohol, then
It puts into stand-by in deionized water.
S2, it weighs urea 0.376g and is dissolved in ultrapure water 25ml, the aqueous solution of urea of clear homogeneous is obtained after stirring.
S3, the aqueous solution of urea being stirred is poured into the high temperature water heating kettle with polytetrafluoroethyllining lining, by step S1
In pretreated foamed iron be put into polytetrafluoroethyllining lining and seal, be put into baking oven and reacted.Reaction time is 12 hours,
Temperature is 120 DEG C.
S4, to after the reaction was completed, reaction kettle is cooled to room temperature, products therefrom ethyl alcohol and ultrapure water cross processing are gone forward side by side
Row vacuum drying treatment, vacuum drying treatment time are 3h, and treatment temperature is 30 DEG C, obtain described obtaining ferriferous oxide micron
Piece self-supporting electrode.
It should be noted that we have carried out XRD diagram to the ferriferous oxide of above-described embodiment 1-3 self-supporting electrode surface
Spectrum, SEM photograph, LSV H2-producing capacity curve and LSV produce oxygen performance curve.The results show that the iron that the various embodiments described above are prepared
The surface of oxide micron chip self-supporting electrode synthesizes homoepitaxial in foam iron surface, the oxygen of the iron with micron chip architecture
Compound, the ferriferous oxide are Fe3O4, and electro-chemical activity is good.Wherein the testing result of the embodiment of the present invention 1 is as follows:
Fig. 1 is Fe prepared by the present embodiment 13O4XRD spectrum, as can be seen from Figure 1 X-ray powder diffraction peak
Index is Fe3O4。
Fig. 2 is that the ferriferous oxide for being grown in self-supporting electrode surface prepared by the present embodiment 1 shines at 3K scanning electron microscope (SEM)
Piece.As can be seen from Figure 2 it can be seen that micron chip is uniformly grown in self-supporting electrode foam iron surface.
Fig. 3 is the LSV H2-producing capacity curve of the ferriferous oxide for being grown in self-supporting electrode surface prepared by the present embodiment 1.
Fig. 4 is that the LSV of the ferriferous oxide for being grown in self-supporting electrode surface prepared by the present embodiment 1 produces oxygen performance curve；
It can be found out respectively in 100mA/cm by Fig. 3 and Fig. 4-2Current density under, produce Hydrogen over potential be about
368mV, in 100mA/cm-2Current density under, produce oxygen overpotential be about 448mV.Electro-chemical activity is preferable.
Involved in claims of the present invention when numberical range, it is thus understood that two endpoints of each numberical range and two
Any one numerical value can be selected between a endpoint, since the step method of use is identical as embodiment, repeat in order to prevent, this
Invention describes preferred embodiment and its effect.Once a person skilled in the art knows basic creative concepts, then
Additional changes and modifications may be made to these embodiments.So it includes preferred embodiment that the following claims are intended to be interpreted as
And fall into all change and modification of the scope of the invention.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (8)
1. a kind of ferriferous oxide micron chip self-supporting electrode, which is characterized in that self-supporting electrode is the electrode or electricity of iron-based material
Pole surface part is the electrode of iron-based material, and the surface homoepitaxial of the iron-based material has the oxidation of the iron of micron chip pattern
Object.
2. a kind of ferriferous oxide micron chip self-supporting electrode as described in claim 1, which is characterized in that the iron-based material is
Foamed iron.
3. a kind of ferriferous oxide micron chip self-supporting electrode as described in claim 1, which is characterized in that the oxide of the iron
For Fe3O4。
4. a kind of synthetic method of ferriferous oxide micron chip self-supporting electrode as claimed in claim 2, which is characterized in that by institute
It states foamed iron to be immersed in the aqueous solution of urea that concentration is 0.188-0.313mol/L, hydro-thermal reaction obtains the ferriferous oxide
Micron chip self-supporting electrode.
5. the synthetic method of ferriferous oxide micron chip self-supporting electrode as claimed in claim 4, which is characterized in that the hydro-thermal
The time of reaction is 12-14 hours, and temperature is 120-140 DEG C.
6. the synthetic method of ferriferous oxide micron chip self-supporting electrode as claimed in claim 4, which is characterized in that specifically include
Following steps:
S1, removal of impurities pretreatment is carried out to foamed iron；
S2, it weighs urea and is dissolved in ultrapure water, the aqueous solution of urea of clear homogeneous is obtained after stirring；
S3, it pretreated foamed iron is put into the aqueous solution of urea being stirred carries out hydro-thermal reaction；
S4, to after reaction, foamed iron be taken out and is cooled to room temperature, obtains product, by products therefrom ethyl alcohol and ultrapure water
Then alternate treatment carries out vacuum drying treatment, obtain the ferriferous oxide micron chip self-supporting electrode.
7. the synthetic method of ferriferous oxide micron chip self-supporting electrode as claimed in claim 6, which is characterized in that the step
Carrying out removal of impurities pre-treatment step to foamed iron in S1 includes cleaning step, and the cleaning step is as follows: first with acetone soak ultrasound
Then 10-20min is impregnated with the dilute hydrochloric acid of 3moL/L, then alternately rinsed 2-5 times with ultrapure water and ethyl alcohol, is then immersed in
It is stand-by in ionized water.
8. the synthetic method of ferriferous oxide micron chip self-supporting electrode as claimed in claim 6, which is characterized in that the step
The vacuum drying treatment time is 3-5h in S5, and treatment temperature is 20-30 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110711583A (en) * | 2019-10-24 | 2020-01-21 | 山东大学 | Efficient electrocatalyst material with three-dimensional structure and preparation method and application thereof |
| CN113529133A (en) * | 2021-07-30 | 2021-10-22 | 清华大学 | Preparation method of self-supporting type bifunctional catalytic electrode |
| CN114843530A (en) * | 2022-03-29 | 2022-08-02 | 中北大学南通智能光机电研究院 | Preparation method of cobalt-iron/foam iron |
| CN115026121A (en) * | 2022-06-13 | 2022-09-09 | 中南大学 | Method and device for electrokinetic remediation of heavy metal contaminated soil by using nanostructure foam iron-based sulfide three-dimensional electrode |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110711583A (en) * | 2019-10-24 | 2020-01-21 | 山东大学 | Efficient electrocatalyst material with three-dimensional structure and preparation method and application thereof |
| CN113529133A (en) * | 2021-07-30 | 2021-10-22 | 清华大学 | Preparation method of self-supporting type bifunctional catalytic electrode |
| CN114843530A (en) * | 2022-03-29 | 2022-08-02 | 中北大学南通智能光机电研究院 | Preparation method of cobalt-iron/foam iron |
| CN115026121A (en) * | 2022-06-13 | 2022-09-09 | 中南大学 | Method and device for electrokinetic remediation of heavy metal contaminated soil by using nanostructure foam iron-based sulfide three-dimensional electrode |
| CN115026121B (en) * | 2022-06-13 | 2023-11-03 | 中南大学 | Method and device for electrically repairing heavy metal contaminated soil by using nano-structure foam iron-based sulfide three-dimensional electrode |
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