CN109913899A - A kind of preparation method of catalysis electrode, catalysis electrode and electrolysis wetting system - Google Patents
A kind of preparation method of catalysis electrode, catalysis electrode and electrolysis wetting system Download PDFInfo
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- CN109913899A CN109913899A CN201910265196.XA CN201910265196A CN109913899A CN 109913899 A CN109913899 A CN 109913899A CN 201910265196 A CN201910265196 A CN 201910265196A CN 109913899 A CN109913899 A CN 109913899A
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Abstract
One kind is inventor provided using conductive substrates as kernel, contains α-Fe2O3Compound with Co element is the preparation method of the catalysis electrode of outer layer, comprising the following steps: pretreatment, for the first time hydro-thermal, secondary hydro-thermal, calcining obtain the catalysis electrode.The technical solution is directly synthesized on electrically-conductive backing plate using hydro-thermal method, obtains catalysis electrode, simple for process, is obtained containing α-Fe2O3With the catalysis electrode of Co elements compounding object, this method makes α-Fe2O3It is effectively adulterated with Co element, which has stable hexagon 3-D nano, structure, while chemical property with higher, can effectively catalytic electrolysis water reaction.
Description
Technical field
The present invention relates to catalyst technical field, especially with regard to the preparation method of catalysis electrode a kind of, catalysis electrode with
And electrolysis wetting system.
Background technique
Recently as the fast development of nanosecond science and technology, the numerous studies of people, which concentrate on, has good crystal form and shape
The nano structural material of looks, superior physical properties and chemical characteristic, and it is applied to catalytic field.Compared to other materials, receive
Rice structure is with following advantage: (1) nanoscale particle has bigger specific surface area, to increase catalyst and reaction
The contact of substance and solution；(2) nano particle can expose more active sites, to improve the catalytic efficiency of catalyst；
(3) nanostructure can improve in electro-catalysis.Nano iron oxide as a kind of green functional material, have excellent photocatalysis,
Electro-catalysis and photoelectric conversion performance are widely used in photocatalysis, the fields such as photoelectrocatalysis and elctro-catalyst.Fe base catalyst has
Good chemical stability and electrochemical stability.One-dimensional nanostructure can be used as native catalytic material application electrolytic process
In, be conducive to the transmission separation process of electronics, to achieve the purpose that improve photoelectrolysis performance and efficiency.
And Fe base catalyst is as elctro-catalyst, since itself crystal morphology limitation and internal resistance are larger, need to its into
Row element doping improves its defect sturcture, to improve its chemical property.In the world today, majority research concentrates on two step systems
Standby doping or the ferric oxide nanometer particle supported.For directly synthesizing multistage three-dimensional three-dimensional manometer knot on electrically-conductive backing plate
Structure, and the research for preparing one-dimensional doping iron oxide simultaneously is less.
Summary of the invention
In order to solve the problems, such as background technique, it is desirable to provide one kind synthesizes the catalysis containing Fe base directly on electrically-conductive backing plate
Agent, the method for obtaining catalysis electrode, resulting catalysis electrode also have stronger electrochemical catalysis performance simultaneously.
The first aspect of the present invention provides a kind of preparation method of catalysis electrode, comprising the following steps:
Pretreatment: first conductive substrates are successively cleaned by ultrasonic with acetone, ethyl alcohol and deionized water；It again will be after cleaning
Conductive substrates are successively cleaned with hydrochloric acid, deionized water；
Hydro-thermal for the first time: pretreated conductive substrates being put into after the first precursor solution and carry out hydro-thermal reaction for the first time, institute
The temperature for stating hydro-thermal reaction for the first time is 50-200 DEG C, time 0.5-24h, contains 0.001-1M in first precursor solution
Co2+Ion；
Secondary hydro-thermal: the conductive substrates after hydro-thermal process for the first time are put into after the second precursor solution and carry out secondary water heat instead
It answers, the temperature of the secondary hydro-thermal reaction is 50-200 DEG C, time 0.5-24h, is contained in second precursor solution
The Fe of 0.001-1M3+Ion；
Calcining: after the conductive substrates after secondary hydro-thermal process are cleaned with deionization, 400-800 DEG C of calcining 0.5-
8h, cooled to room temperature obtain the catalysis electrode.
Further, the material of the conductive substrates is foam metal, including nickel foam, foamed aluminium and foam copper.Foam
Material is cheap and easy to get, easy to operate, chemical stability is good.
Further, in the hydro-thermal for the first time and secondary hydrothermal step, the reaction carries out in water heating kettle, hydro-thermal reaction
After the completion, water heating kettle is cooled to room temperature in 10min.
Further, in the hydrothermal step for the first time, first precursor solution contains the Co of 0.001-1M2+Ion,
The ammonium fluoride of 0.001-0.1M urea and 0.01-0.5M.It wherein can be used but be not limited only to Co (NO3)2、CoCl2Co is provided2+From
Son.
Further, in the secondary hydrothermal step, second precursor solution contains the Fe of 0.001-1M3+Ion,
The ammonium fluoride of 0.001-0.1M urea and 0.01-0.5M.It wherein can be used but be not limited only to Fe (NO3)3、FeCl3Fe is provided3+From
Son.
Further, in the calcining step, the atmosphere that when calcining uses includes air and nitrogen.Atmosphere can also include
The mixed gas of hydrogen and argon gas；Wherein the volume percent content of argon gas is 95%, and the volume percent content of hydrogen is
5%.
The second aspect of the present invention provides a kind of catalysis electrode, and the catalysis electrode is by any of the above-described preparation side
Method preparation.
Further, the catalysis electrode is to contain α-Fe using conductive substrates as kernel2O3Compound with Co element is
Outer layer.
Further, the catalysis electrode is used for electrolysis water.
The third aspect of the present invention provides a kind of electrolysis wetting system, and the electrolysis wetting system uses above-mentioned catalysis electrode
For anode.
It is different from the prior art, Co-OH-CO is deposited in electrically-conductive backing plate upper surface using hydro-thermal method in above-mentioned technical proposal3
And FeOOH, then calcined；After calcining, FeOOH is converted to α-Fe2O3It obtains surface and contains α-Fe2O3With Co elements compounding object
Catalysis electrode, this method makes α-Fe2O3It is effectively adulterated with Co element, which has stable hexagon three
Dimension nanometer construction has biggish specific surface area, while chemical property with higher, can effectively catalytic electrolysis water reaction.
Detailed description of the invention
Fig. 1 is the picture of the electrically-conductive backing plate of the sealing of insulating tape described in embodiment 1, and wherein meshing is that insulating tape is close
Envelope part (20 × 5mm2), blank is conducting surface (10 × 10mm of exposure2)；
Fig. 2 is the structural schematic diagram of water heating kettle, and left side is the water heating kettle liner equipped with precursor solution, and right side is that hydro-thermal is anti-
Answer kettle external structure；
Fig. 3 is that the battery that electrode prepared by embodiment 1 is anode carries out the full battery performance map of electrolysis water；
Fig. 4 is 50 times of scanning electron microscope (SEM) photographs of electrode surface prepared by embodiment 3；
Fig. 5 is 15000 times of scanning electron microscope (SEM) photographs of electrode surface prepared by embodiment 3；
Fig. 6 is the XRD spectrum of electrode prepared by embodiment 3, specifically with the sweep speed of 5 °/min from 20 ° to 80 °, H
Represent the XRD characteristic peak of iron oxide；
Fig. 7 is the XRF spectrogram of electrode prepared by embodiment 3.
Specific embodiment
Technology contents, construction feature, the objects and the effects for detailed description technical solution, below in conjunction with specific reality
It applies example and attached drawing is cooperated to be explained in detail.
A kind of preparation of the catalysis electrode of embodiment 1
Use nickel foam as electrically-conductive backing plate, which is pre-processed.Successively with acetone, ethyl alcohol and deionized water into
Row ultrasonic cleaning；The conductive substrates after cleaning are successively cleaned with hydrochloric acid, deionized water again；Electrically-conductive backing plate is set in conduction
The depositional area on surface is 1 × 1cm2, rest part seals with insulating tape；It is specifically shown in Fig. 1.
Pretreated electrically-conductive backing plate is placed in water heating kettle liner, conducting surface is towards hydrothermal reaction kettle liner center and with absolutely
Edge adhesive tape fixes upper semisection.It is added into water heating kettle liner and contains 0.01mol/L Co (NO3)2, 0.1mol/L ammonium fluoride and
0.1mol/L urea is stirred evenly as presoma；100 DEG C of heating 4h in baking oven will be put into after the completion of water heating kettle sealing；Instead
Water heating kettle should be cooled to room temperature in 10min with furnace after the completion；
The electrically-conductive backing plate of taking-up is placed in water heating kettle liner, conducting surface towards hydrothermal reaction kettle liner center and with insulation
Adhesive tape fixes upper semisection.It is added into water heating kettle liner and contains 0.01mol/L Fe (NO3)3, 0.01mol/L ammonium fluoride and
0.01mol/L urea is stirred evenly as presoma；100 DEG C of heating 8h in baking oven will be put into after the completion of water heating kettle sealing；Instead
Should after the completion of by water heating kettle with being cooled to room temperature in furnace 10min；
Sample is taken out from water heating kettle, and insulating tape is removed after deionized water is cleaned, then sample is put into air
Calcining, from room temperature with the heating rate of 10 DEG C/min to calcining 4 hours after 500 DEG C, cooled to room temperature obtains α-Fe2O3With
The catalysis electrode of Co element progress Effective Doping.
For the catalysis electrode obtained using embodiment 1 as cathode, Pt/C is anode, electrolyte: 1M KOH, test temperature to electrode
80 DEG C, carry out electricity hydrolysis test.Test results are shown in figure 3, shows that the catalyst of preparation is applied to tool when electrolysis water process
There is higher full battery performance.The catalysis electrode chemical property with higher for illustrating embodiment preparation, can effectively be catalyzed electricity
Xie Shui reaction.
A kind of preparation of the catalysis electrode of embodiment 2
Use foamed aluminium as electrically-conductive backing plate, and above-mentioned pretreatment is carried out to the substrate.Successively with acetone, ethyl alcohol and go from
Sub- water is cleaned by ultrasonic；The conductive substrates after cleaning are successively cleaned with hydrochloric acid, deionized water again；Setting sample is being led
The depositional area in ammeter face is 1 × 1cm2, rest part seals with insulating tape；
Pretreated electrically-conductive backing plate is placed in water heating kettle liner, conducting surface is towards hydrothermal reaction kettle liner center and with absolutely
Edge adhesive tape fixes upper semisection.It is added into water heating kettle liner and contains 0.1mol/LCo (NO3)2, 0.05mol/L ammonium fluoride and
0.01mol/L urea is stirred evenly as presoma；200 DEG C of heating 0.5h in baking oven will be put into after the completion of water heating kettle sealing；
Water heating kettle is cooled to the furnace room temperature in 10min after the reaction was completed；The electrically-conductive backing plate of taking-up is placed in water heating kettle liner, is led
Electricity facing towards hydrothermal reaction kettle liner center and fixes upper semisection with insulating tape.It is added and contains into water heating kettle liner
0.05mol/L Fe(NO3)3, 0.5mol/L ammonium fluoride and 0.08mol/L urea stirs evenly as presoma；By water heating kettle
It is put into baking oven and heats for 24 hours after the completion of sealing for 50 DEG C；Water heating kettle is cooled to the furnace room temperature in 10min after the reaction was completed；From
Sample is taken out in water heating kettle, and insulating tape is removed after deionized water is cleaned, then sample is put into air and is calcined, from
For room temperature with the heating rate of 10 DEG C/min to calcining 8 hours after 400 DEG C, cooled to room temperature obtains α-Fe2O3With Co element
Carry out the catalysis electrode of Effective Doping.
A kind of preparation of the catalysis electrode of embodiment 3
Use nickel foam as electrically-conductive backing plate, and above-mentioned pretreatment is carried out to the substrate.Successively with acetone, ethyl alcohol and go from
Sub- water is cleaned by ultrasonic；The conductive substrates after cleaning are successively cleaned with hydrochloric acid, deionized water again；Fixed sample is being led
Depositional area (1 × the 1cm on electric substrate surface2), rest part is sealed with insulating tape；Pretreated electrically-conductive backing plate is placed in water
In hot kettle liner, conducting surface towards hydrothermal reaction kettle liner center and fixes upper semisection with insulating tape.Into water heating kettle liner
It is added and contains 0.2mol/L Co (NO3)2, 0.1mol/L ammonium fluoride and 0.01mol/L urea stirs evenly as presoma；
100 DEG C of heating 10h in baking oven will be put into after the completion of water heating kettle sealing；After the reaction was completed by water heating kettle furnace cooling in 10min
To room temperature；The electrically-conductive backing plate of taking-up is placed in water heating kettle liner, conducting surface towards hydrothermal reaction kettle liner center and with insulation
Adhesive tape fixes upper semisection.It is added into water heating kettle liner and contains 0.1mol/L Fe (NO3)3, 0.05mol/L ammonium fluoride and
0.02mol/L urea is stirred evenly as presoma；100 DEG C of heating 12h in baking oven will be put into after the completion of water heating kettle sealing；
Water heating kettle is cooled to the furnace room temperature in 10min after the reaction was completed；Sample is taken out from water heating kettle, after deionized water is cleaned
Insulating tape is removed, then sample is put into air and is calcined, from room temperature with the heating rate of 10 DEG C/min to heating after 550 DEG C
4 hours, cooled to room temperature obtained α-Fe2O3The catalysis electrode of Effective Doping is carried out with Co element.
The catalysis electrode that embodiment 3 is obtained carries out Shape measure, specific as shown in Figure 4-Figure 7.
Fig. 4 is 50 times of scanning electron microscope (SEM) photographs of electrode surface prepared by embodiment 3；Fig. 5 is electrode prepared by embodiment 3
15000 times of scanning electron microscope (SEM) photographs on surface.By Fig. 4-5 as it can be seen that the compound has stable hexagon 3-D nano, structure, have
Biggish specific surface area can provide good electronics conduction pathway as photoelectric and electrochemical catalyst, therefore aobvious
Good application prospect is shown.
Fig. 6 is the XRD spectrum of electrode prepared by embodiment 3, specifically with the sweep speed of 5 °/min from 20 ° to 80 °, H generation
The XRD characteristic peak of table iron oxide；Fig. 7 is the XRF spectrogram of electrode prepared by embodiment 3.It can be seen that by Fig. 6-Fig. 7, embodiment
Contain Fe element, Co element and Ni element in prepared electrode.
A kind of preparation of the catalysis electrode of embodiment 4
Use foamed aluminium as electrically-conductive backing plate, and above-mentioned pretreatment is carried out to the substrate.Successively with acetone, ethyl alcohol and go from
Sub- water is cleaned by ultrasonic；The conductive substrates after cleaning are successively cleaned with hydrochloric acid, deionized water again；Setting sample is being led
The depositional area in ammeter face is 1 × 1cm2, rest part seals with insulating tape；
Pretreated electrically-conductive backing plate is placed in water heating kettle liner, conducting surface is towards hydrothermal reaction kettle liner center and with absolutely
Edge adhesive tape fixes upper semisection.It is added into water heating kettle liner and contains 1mol/LCo (NO3)2, 0.5mol/L ammonium fluoride and 0.1mol/L
Urea is stirred evenly as presoma；Water heating kettle sealing is put into after the completion in baking oven and is heated for 24 hours for 50 DEG C；After the reaction was completed
Water heating kettle is cooled to the furnace room temperature in 10min；The electrically-conductive backing plate of taking-up is placed in water heating kettle liner, conducting surface is towards water
Upper semisection is simultaneously fixed with insulating tape in thermal response kettle liner center.It is added into water heating kettle liner and contains 1mol/L Fe (NO3)3、
0.5mol/L ammonium fluoride and 0.1mol/L urea are stirred evenly as presoma；Baking oven will be put into after the completion of water heating kettle sealing
In 200 DEG C of heating 0.5h；Water heating kettle is cooled to the furnace room temperature in 10min after the reaction was completed；Sample is taken out from water heating kettle,
Insulating tape is removed after deionized water is cleaned, then sample is put into air and is calcined, from room temperature with 10 DEG C/min's
For heating rate to calcining 0.5 hour after 800 DEG C, cooled to room temperature obtains α-Fe2O3Effective Doping is carried out with Co element
Catalysis electrode.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or the terminal device that include a series of elements not only include those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or end
The intrinsic element of end equipment.In the absence of more restrictions, being limited by sentence " including ... " or " including ... "
Element, it is not excluded that there is also other elements in process, method, article or the terminal device for including the element.This
Outside, herein, " being greater than ", " being less than ", " being more than " etc. are interpreted as not including this number；" more than ", " following ", " within " etc. understand
Being includes this number.
It should be noted that being not intended to limit although the various embodiments described above have been described herein
Scope of patent protection of the invention.Therefore, it based on innovative idea of the invention, change that embodiment described herein is carried out and is repaired
Change, or using equivalent structure or equivalent flow shift made by description of the invention and accompanying drawing content, it directly or indirectly will be with
Upper technical solution is used in other related technical areas, is included within scope of patent protection of the invention.
Claims (10)
1. a kind of preparation method of catalysis electrode, which comprises the following steps:
Pretreatment: first conductive substrates are successively cleaned by ultrasonic with acetone, ethyl alcohol and deionized water；Again by the conduction after cleaning
Substrate is successively cleaned with hydrochloric acid, deionized water；
Hydro-thermal for the first time: pretreated conductive substrates being put into after the first precursor solution and carry out hydro-thermal reaction for the first time, the head
The temperature of secondary hydro-thermal reaction is 50-200 DEG C, time 0.5-24h, contains 0.001-1mol/L in first precursor solution
Co2+Ion；
Secondary hydro-thermal: carrying out secondary water thermal response after the conductive substrates after hydro-thermal process for the first time are put into the second precursor solution,
The temperature of the secondary hydro-thermal reaction is 50-200 DEG C, time 0.5-24h, contains 0.001- in second precursor solution
The Fe of 1mol/L3+Ion；
Calcining: after the conductive substrates after secondary hydro-thermal process are cleaned with deionization, 400-800 DEG C of calcining 0.5-8h, from
It is so cooled to room temperature, obtains the catalysis electrode.
2. preparation method according to claim 1, which is characterized in that the material of the conductive substrates is foam metal.
3. preparation method according to claim 1, which is characterized in that in the hydro-thermal for the first time and secondary hydrothermal step, institute
It states reaction to carry out in water heating kettle, after the completion of hydro-thermal reaction, water heating kettle is cooled to room temperature in 10min.
4. preparation method according to claim 1, which is characterized in that in the hydrothermal step for the first time, first forerunner
Liquid solution contains the Co of 0.001-1mol/L2+The ammonium fluoride of ion, 0.001-0.1mol/L urea and 0.01-0.5mol/L.
5. preparation method according to claim 1, which is characterized in that in the secondary hydrothermal step, second forerunner
Liquid solution contains the Fe of 0.001-1mol/L3+The ammonium fluoride of ion, 0.001-0.1mol/L urea and 0.01-0.5mol/L.
6. preparation method according to claim 1, which is characterized in that in the calcining step, atmosphere that when calcining uses
Including air and nitrogen.
7. a kind of catalysis electrode, which is characterized in that the catalysis electrode is prepared by any preparation method of claim 1-6.
8. catalysis electrode according to claim 7, which is characterized in that the catalysis electrode be using conductive substrates as kernel,
Contain α-Fe2O3Compound with Co element is the structure of outer layer.
9. catalysis electrode according to claim 7, which is characterized in that the catalysis electrode is used for electrolysis water.
10. a kind of electrolysis wetting system, which is characterized in that the electrolysis wetting system is using any catalysis of claim 7-9
Electrode is anode.
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Cited By (1)
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