CN109759066A - A kind of preparation method for the cobalt nickel bimetal oxide oxygen-separating catalyst that boron doping is graphene-supported - Google Patents
A kind of preparation method for the cobalt nickel bimetal oxide oxygen-separating catalyst that boron doping is graphene-supported Download PDFInfo
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- CN109759066A CN109759066A CN201910085743.6A CN201910085743A CN109759066A CN 109759066 A CN109759066 A CN 109759066A CN 201910085743 A CN201910085743 A CN 201910085743A CN 109759066 A CN109759066 A CN 109759066A
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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
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- 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 present invention provides a kind of preparation methods of cobalt nickel bimetal oxide oxygen-separating catalyst that boron doping is graphene-supported comprising following steps: S1, preparation contain Co2+And Ni2+Graphene oxide water solution presoma；S2, by NaBH4Aqueous solution is added drop-wise to above-mentioned containing Co2+And Ni2+Graphene oxide water solution presoma in, react at room temperature, obtain the graphene for being loaded with cobalt nickel compound；S3, by the graphene for being loaded with cobalt-nickel oxide in an inert atmosphere, be warming up to 300~600 DEG C with the rate of 2~10 DEG C/min, carry out calcination, obtain the graphene-supported cobalt nickel bimetal oxide oxygen-separating catalyst of the boron doping.The present invention is with following the utility model has the advantages that the graphene-supported cobalt-nickel oxide preparation cost of boron doping is cheap in the present invention, method is simple and easy, controllability is high.
Description
Technical field
The present invention relates to a kind of preparation method of cobalt nickel bimetal oxide oxygen-separating catalyst that boron doping is graphene-supported,
Belong to electrochemical catalysis technical field.
Background technique
Hydrogen-oxygen fuel cell becomes current energy field due to having the advantages that high-energy density and almost zero carbon emission
Research hotspot.Practical hydrogen-oxygen fuel cell is developed to have great significance to the energy and environmental problem of the world today.Reduce hydrogen
Gas preparation cost is the key link for promoting hydrogen-oxygen fuel cell.A kind of more environmentally friendly method for preparing hydrogen is exactly electrolysis water
Hydrogen manufacturing, water electrolysis hydrogen production reaction are divided into the hydrogen evolution reaction of the oxygen evolution reaction and cathode of anode.Wherein anodic oxygen air elutriation
Sluggish four electronic processes are one of the central factors for restricting electrolysis water application out, and finding suitable catalyst is to solve to ask
The important channel of topic.
Traditional oxygen evolution elctro-catalyst for having excellent performance is typically all the electro-catalysis based on yttrium oxide, ruthenium-oxide
Agent, expensive price and low earth reserves, limit further practical application.In recent years, researcher explores more
Kind is based on non-noble metal oxygen evolution elctro-catalyst, is based particularly on cobalt and/or nickel is the multiple compounds of component, such as
Oxide, hydroxide, phosphide, boride etc..It is very good that nearest research work shows that the oxide of nickel cobalt is shown
Oxygen evolution electrocatalysis characteristic (Angew.Chem.Int.Ed.2017,56,1-6；ChemSusChem,2018,11,2752-
2757), and preparation method is simple and easy, has the characteristics that dissolubility is low, catalytic activity is high, chemical property is stable, is a kind of
Very promising base metal oxygen evolution elctro-catalyst.But most reported values about nickel cobalt oxide are still at present
There is certain gap away from the elctro-catalyst based on noble metal, and also farther out from business application.
Summary of the invention
For the defects in the prior art, the object of the present invention is to provide a kind of double gold of the cobalt nickel that boron doping is graphene-supported
Belong to the preparation method of oxide oxygen-separating catalyst.
The present invention is achieved by the following technical solutions:
The present invention provides a kind of preparation sides of cobalt nickel bimetal oxide oxygen-separating catalyst that boron doping is graphene-supported
Method comprising following steps:
S1, preparation contain Co2+And Ni2+Graphene oxide water solution presoma；
S2, by NaBH4Aqueous solution is added drop-wise to above-mentioned containing Co2+And Ni2+Graphene oxide water solution presoma in, room temperature
Lower reaction obtains graphene-supported cobalt nickel compound；
S3, by the graphene-supported cobalt nickel compound of the boron doping in an inert atmosphere, with the rate of 2~10 DEG C/min
300~600 DEG C are warming up to, calcination is carried out, obtains the graphene-supported cobalt nickel bimetal oxide analysis oxygen catalysis of the boron doping
Agent.
Preferably, described to contain Co2+And Ni2+Graphene oxide water solution presoma in, Co2+And Ni2+Object
The ratio between amount of matter is (1~4): (4~1).
Preferably, described to contain Co2+And Ni2+Graphene oxide water solution presoma the preparation method comprises the following steps:
Cobalt salt and nickel salt are dissolved in deionized water, mixed solution is obtained；
Single-layer graphene oxide is added into the mixed solution, and is ultrasonically treated 30min at room temperature, obtains containing oxidation
The mixed solution of the presoma of graphene.
Preferably, the NaBH4The concentration of aqueous solution is 0.1~1mol/L.
Preferably, the NaBH4The drop rate of aqueous solution is 50 μ L/s.
Preferably, the time of the calcination is 1~5h.
Compared with prior art, the present invention have it is following the utility model has the advantages that
1, the graphene-supported cobalt-nickel oxide preparation cost of boron doping is cheap in the present invention, method is simple and easy, controllable
Property it is high；
2, the graphene-supported cobalt-nickel oxide of boron doping shows high oxygen evolution electro-catalysis in alkaline medium
Activity and higher long-play stability；
3, it by the adjusting of cobalt salt in precursor solution and nickel salt ratio, realizes product oxygen and the excellent of electrocatalysis characteristic is precipitated
Change.
4, by carrying out the annealing under different temperatures to the product after sodium borohydride reduction, regulate and control the crystal form knot of product
Electrocatalysis characteristic is precipitated in structure, the oxygen for further improving product；
5, boron doping graphite is promoted by the interaction cooperateed between cobalt nickel binary oxide and boron doping graphene the two
The cobalt-nickel oxide composite material oxygen evolution electrocatalysis characteristic of alkene load greatly improves.
Detailed description of the invention
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon:
Fig. 1 is the process schematic of the graphene-supported cobalt-nickel oxide of synthesis boron doping of the invention；
Fig. 2 is the scanning electron microscope (SEM) photograph of the graphene-supported cobalt-nickel oxide of boron doping obtained in embodiment 1 in the present invention；
Fig. 3 is the transmission electron microscope picture of the graphene-supported cobalt-nickel oxide of boron doping obtained in embodiment 1 in the present invention；
Fig. 4 is the XRD spectrum of the graphene-supported cobalt-nickel oxide of boron doping obtained in embodiment 1 in the present invention；
Fig. 5 is cobalt nickel compound graphene-supported obtained in embodiment 1 in the present invention in 1.0M KOH electrolyte
LSV figure；
Fig. 6 is that the cobalt-nickel oxide that the obtained boron doping of embodiment 1 is graphene-supported in the present invention is electrolysed in 1.0M KOH
LSV figure in matter；
Fig. 7 is the cobalt-nickel oxide and other contrast materials that the obtained boron doping of embodiment 1 is graphene-supported in the present invention
The LSV figure of oxygen evolution reaction in 1.0M KOH electrolyte；
Fig. 8 is the corresponding Tafel curve obtained by LSV curve in Fig. 7；
Fig. 9 is the graphene-supported cobalt-nickel oxide of boron doping 10mA/cm in 1.0mol/LKOH electrolyte2Electric current
Long-play stability diagram under density.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
Embodiment 1
The present embodiment is prepared for a kind of cobalt nickel bimetal oxide oxygen-separating catalyst that boron doping is graphene-supported, such as Fig. 1
It is shown, the specific steps are as follows:
By 0.5mmol Co (NO3)2·6H2O and 0.5mmol Ni (NO3)2·6H2O is dissolved into the deionization of 100mL together
In water, sufficiently dissolution is stirred；The single-layer graphene oxide of 15mg is added in above-mentioned solution, and is stirred at room temperature 30 minutes
Dissolve it sufficiently, solution colour at this time is brownish black, is obtained containing Co2+And Ni2+Graphene oxide water solution forerunner
Body；
By 0.5mol/LNaBH4Aqueous solution contains Co described in being added dropwise under stiring2+And Ni2+Graphene oxide it is water-soluble
Liquid presoma can generate a small amount of bubble during the addition process, be stirred at room temperature after dropwise addition 40 minutes, grow on the surface of graphene
Cobalt-nickel oxide out, it is washed, be dried to obtain graphene-supported cobalt nickel compound；
There is the graphene of cobalt-nickel oxide to be transferred in porcelain boat the load, is placed in the middle part of tube furnace, in logical argon gas
After air-discharging half an hour, 400 DEG C are warming up to from 25 DEG C with the rate of 5 DEG C/min, and in 400 DEG C of holding 2h, be down to naturally later
Room temperature obtains the graphene-supported cobalt nickel bimetal oxide composite of boron doping.
The graphene-supported cobalt-nickel oxide composite material of the boron doping that the present embodiment obtains is scanned electron microscope analysis,
As a result as shown in Fig. 2, it can clearly be seen that the graphene of the pleated structure of big lamella in sample after high-temperature process.It is transmitted
After electron microscope analysis, as a result as shown in figure 3, the laminated structure of small area is distributed on the surface of graphene, tested in conjunction with XRD, such as Fig. 4
It is shown, it can be deduced that small laminated structure is the structure of cobalt nickel binary oxide.
The activity for carrying out electrochemistry production oxygen reaction to the material obtained before and after calcination in embodiment 1 respectively detects, and has
Body method are as follows: measured under three electrode conditions, rotating disk electrode (r.d.e) supported catalyst is as working electrode, and wherein catalyst is negative
Carrying capacity is 0.45mg/cm2, as to electrode, saturated calomel electrode is carbon-point as reference electrode, the electrolyte of electrochemical reaction
The KOH solution of 1mol/L is scanned in the state of revolving speed 1600rmp.The sweep speed of LSV test is 5mV/s.As a result such as
Shown in Fig. 5 and Fig. 6, Co:Ni ratio is 1:1 and in 400 DEG C of CoNiO that treated obtainsx/ B- graphene sample is shown most
Good oxygen evolution electro catalytic activity, in 10mA/cm2Current density under, it is only necessary to the overpotential of 310mV.It is real better than comparison
Other materials (such as graphene, cobalt-nickel oxide) in testing are even better than the business RuO for generally acknowledging have excellent performance at present2Material
(Fig. 7).Resulting Tafel curve (Fig. 8) is calculated from LSV curve, it can be deduced that this CoNiOx/ B- graphene also has most
Small Tafel slope, Tafel slope value are 54.8mV/dec, and it is very fast to illustrate that this CoNiOx/B- grapheme material has
Dynamics.In addition, the catalyst is in 10mA/cm2Current density under (Fig. 9), by the test of 20h, potential change is very
It is small, illustrate its long-play stability with higher.
Embodiment 2
The present embodiment is prepared for a kind of cobalt nickel bimetal oxide oxygen-separating catalyst that boron doping is graphene-supported, such as Fig. 1
It is shown, the specific steps are as follows:
By 0.33mmol Co (NO3)2·6H2O and 0.66mmol Ni (NO3)2·6H2O be dissolved into together 100mL go from
In sub- water, sufficiently dissolution is stirred；The single-layer graphene oxide of 15mg is added in above-mentioned solution, and is stirred at room temperature 30 points
Clock dissolves it sufficiently, and solution colour at this time is brownish black, obtains containing Co2+And Ni2+Graphene oxide water solution forerunner
Body；
By 0.5mol/LNaBH4Aqueous solution contains Co described in being added dropwise under stiring2+And Ni2+Graphene oxide it is water-soluble
Liquid presoma can generate a small amount of bubble during the addition process, be stirred at room temperature after dropwise addition 40 minutes, grow on the surface of graphene
Cobalt-nickel oxide out, it is washed, be dried to obtain graphene-supported cobalt nickel compound；
The graphene of the graphene-supported cobalt nickel compound of the boron doping is transferred in porcelain boat, is placed in tube furnace
Portion is warming up to 400 DEG C from 25 DEG C after logical argon gas air-discharging half an hour with the rate of 5 DEG C/min, and in 400 DEG C of heat preservation 2h, certainly
It so is down to room temperature, obtains the graphene-supported cobalt nickel bimetal oxide composite of boron doping.
Electro-chemical test is carried out according to method in the same manner as in Example 1.As shown in fig. 6, products therefrom is in 10mAcm-2Electricity
Overpotential and embodiment 1 under current density is close, but its Tafel slope is 76.5mV dec-1, chemical property is compared with embodiment 1
It is slightly poor.
Embodiment 3
The present embodiment is prepared for a kind of cobalt nickel bimetal oxide oxygen-separating catalyst that boron doping is graphene-supported, such as Fig. 1
It is shown, the specific steps are as follows:
By 0.66mmol Co (NO3)2·6H2O and 0.33mmol Ni (NO3)2·6H2O be dissolved into together 100mL go from
In sub- water, sufficiently dissolution is stirred；The single-layer graphene oxide of 15mg is added in above-mentioned solution, and is stirred at room temperature 30 points
Clock dissolves it sufficiently, and solution colour at this time is brownish black, obtains containing Co2+And Ni2+Graphene oxide water solution forerunner
Body；
By 0.5mol/LNaBH4Aqueous solution contains Co described in being added dropwise under stiring2+And Ni2+Graphene oxide it is water-soluble
Liquid presoma can generate a small amount of bubble during the addition process, be stirred at room temperature after dropwise addition 40 minutes, grow on the surface of graphene
Cobalt-nickel oxide out, it is washed, be dried to obtain graphene-supported cobalt nickel compound；
The graphene of the graphene-supported cobalt nickel compound of the boron doping is transferred in porcelain boat, is placed in tube furnace
Portion is warming up to 400 DEG C from 25 DEG C after logical argon gas air-discharging half an hour with the rate of 5 DEG C/min, and in 400 DEG C of heat preservation 2h, certainly
It so is down to room temperature, obtains the graphene-supported cobalt nickel bimetal oxide composite of boron doping.
The graphene-supported cobalt-nickel oxide composite material of the boron doping that the present embodiment obtains is scanned electron microscope analysis,
As a result as shown in Fig. 2, it can clearly be seen that the graphene of the pleated structure of big lamella in sample after high-temperature process.It is transmitted
After electron microscope analysis, as a result as shown in figure 3, the laminated structure of small area is distributed on the surface of graphene, tested in conjunction with XRD, such as Fig. 4
It is shown, it can be deduced that small laminated structure is the structure of cobalt nickel binary oxide.
Electro-chemical test is carried out according to method in the same manner as in Example 1.As shown in fig. 6, products therefrom is in 10mA cm-2
Overpotential and embodiment 1 under current density is close, but its Tafel slope is 76.6mV dec-1, chemical property is compared with embodiment
1 is slightly poor.
Embodiment 4
The present embodiment is prepared for a kind of cobalt nickel bimetal oxide oxygen-separating catalyst that boron doping is graphene-supported, such as Fig. 1
It is shown, the specific steps are as follows:
By 0.5mmol Co (NO3)2·6H2O and 0.5mmol Ni (NO3)2·6H2O is dissolved into the deionization of 100mL together
In water, sufficiently dissolution is stirred；The single-layer graphene oxide of 15mg is added in above-mentioned solution, and is stirred at room temperature 30 minutes
Dissolve it sufficiently, solution colour at this time is brownish black, is obtained containing Co2+And Ni2+Graphene oxide water solution forerunner
Body；
By 0.5mol/LNaBH4Aqueous solution contains Co described in being added dropwise under stiring2+And Ni2+Graphene oxide it is water-soluble
Liquid presoma can generate a small amount of bubble during the addition process, be stirred at room temperature after dropwise addition 40 minutes, grow on the surface of graphene
Cobalt-nickel oxide out, it is washed, be dried to obtain graphene-supported cobalt nickel compound；Products therefrom is not heated, is directly used as
Elctro-catalyst.
Electro-chemical test is carried out according to method in the same manner as in Example 1.As shown in figure 5, products therefrom is in 10mA cm-2
Overpotential under current density is 285mV, and Tafel slope is 157.3mV dec-1, chemical property compared with 1 gap of embodiment compared with
Greatly.
Comparative example 1
The difference of this comparative example and embodiment 1 is only that the molar ratio of Co ion and Ni ion is 1:5.
Comparative example 2
The difference of this comparative example and embodiment 1 is only that the molar ratio of Co ion and Ni ion is 5:1.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring substantive content of the invention.
Claims (6)
1. a kind of preparation method for the cobalt nickel bimetal oxide oxygen-separating catalyst that boron doping is graphene-supported, which is characterized in that
Include the following steps:
S1, preparation contain Co2+And Ni2+Graphene oxide water solution presoma；
S2, by NaBH4Aqueous solution is added drop-wise to above-mentioned containing Co2+And Ni2+Graphene oxide water solution presoma in, at room temperature instead
It answers, obtains graphene-supported cobalt nickel compound；
S3, by the graphene-supported cobalt nickel compound in an inert atmosphere, be warming up to 300 with the rate of 2~10 DEG C/min
~600 DEG C, calcination is carried out, the graphene-supported cobalt nickel bimetal oxide oxygen-separating catalyst of the boron doping is obtained.
2. the preparation side of the graphene-supported cobalt nickel bimetal oxide oxygen-separating catalyst of boron doping as described in claim 1
Method, which is characterized in that described to contain Co2+And Ni2+Graphene oxide water solution presoma in, Co2+And Ni2+Substance amount
The ratio between be (1~4): (4~1).
3. the preparation of the graphene-supported cobalt nickel bimetal oxide oxygen-separating catalyst of boron doping as claimed in claim 1 or 2
Method, which is characterized in that described to contain Co2+And Ni2+Graphene oxide water solution presoma the preparation method comprises the following steps:
Cobalt salt and nickel salt are dissolved in deionized water, mixed solution is obtained；
Single-layer graphene oxide is added into the mixed solution, and is ultrasonically treated 30min at room temperature, obtains containing graphite oxide
The mixed solution of the presoma of alkene.
4. the preparation side of the graphene-supported cobalt nickel bimetal oxide oxygen-separating catalyst of boron doping as described in claim 1
Method, which is characterized in that the NaBH4The concentration of aqueous solution is 0.1~1mol/L.
5. the preparation of the graphene-supported cobalt nickel bimetal oxide oxygen-separating catalyst of boron doping as described in claim 1 or 4
Method, which is characterized in that the NaBH4The drop rate of aqueous solution is 50 μ L/s.
6. the preparation side of the graphene-supported cobalt nickel bimetal oxide oxygen-separating catalyst of boron doping as described in claim 1
Method, which is characterized in that the time of the calcination is 1~5h.
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| CN111111731A (en) * | 2019-12-20 | 2020-05-08 | 济南大学 | Preparation method of graphene-loaded nitrogen-boron-doped nickel phosphide electrolyzed water catalyst |
| CN111111721A (en) * | 2020-01-19 | 2020-05-08 | 西北师范大学 | Preparation and application of boron-doped carbon shell-coated CoNi nanoparticle composite material |
| CN111961217A (en) * | 2020-08-26 | 2020-11-20 | 合肥工业大学 | Preparation method and application of amorphous metal oxide induced NiCo-BTC nanosheet |
| CN112853372A (en) * | 2021-01-05 | 2021-05-28 | 辽宁大学 | Preparation method and application of electrocatalyst B-MnO/CNT |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111111731A (en) * | 2019-12-20 | 2020-05-08 | 济南大学 | Preparation method of graphene-loaded nitrogen-boron-doped nickel phosphide electrolyzed water catalyst |
| CN111111721A (en) * | 2020-01-19 | 2020-05-08 | 西北师范大学 | Preparation and application of boron-doped carbon shell-coated CoNi nanoparticle composite material |
| CN111111721B (en) * | 2020-01-19 | 2022-04-26 | 西北师范大学 | Preparation and application of boron-doped carbon shell-coated CoNi nanoparticle composite material |
| CN111961217A (en) * | 2020-08-26 | 2020-11-20 | 合肥工业大学 | Preparation method and application of amorphous metal oxide induced NiCo-BTC nanosheet |
| CN111961217B (en) * | 2020-08-26 | 2022-04-22 | 合肥工业大学 | Preparation method and application of amorphous metal oxide induced NiCo-BTC nanosheet |
| CN112853372A (en) * | 2021-01-05 | 2021-05-28 | 辽宁大学 | Preparation method and application of electrocatalyst B-MnO/CNT |
| CN112853372B (en) * | 2021-01-05 | 2024-03-22 | 辽宁大学 | Preparation method and application of electrocatalyst B-MnO/CNT |
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