CN109097788A - A kind of double carbon coupling transiting metal nickel based quantum dot elctro-catalyst and preparation method thereof - Google Patents
A kind of double carbon coupling transiting metal nickel based quantum dot elctro-catalyst and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to material, energy technology field, specially a kind of double carbon coupling transiting metal nickel based quantum dot elctro-catalysts and preparation method thereof.Presoma is used as using the Ni-based zeolite imidazole skeleton thin slice/graphene oxide of two dimension, by its converted in-situ is the porous carbon-coated transiting metal nickel based quantum dot/graphene heterogeneous material compound of two dimension N doping by a step low temperature pyrolyzer method.The composite material forms unique porous carbon and graphene " double carbon " coupling metal quantum point structure, has the characteristics that strong interface interaction, large specific surface area, electric conductivity height, N doping and defect is abundant and metal quantum point is evenly dispersed；Excellent electro catalytic activity and stability are shown when being used for evolving hydrogen reaction and oxygen evolution reaction as bifunctional electrocatalyst；It is a kind of novel total moisture solution elctro-catalyst efficiently, economic.Preparation process of the present invention is simple, low in cost, and large scale preparation may be implemented.
Description
Technical field
The invention belongs to materials, energy technology field, and in particular to a kind of double carbon coupling transiting metal nickel based quantum dot electricity
Catalyst and preparation method thereof.
Background technique
With the exhaustion of fossil energy and the aggravation of problem of environmental pollution, it is traditional to replace that people are seeking new energy
The stone energy.Hydrogen Energy has attracted the extensive concern of whole world researcher as a kind of cleaning, renewable energy.Pass through electrolysis water
Hydrogen manufacturing is a kind of practicability technology for meeting sustainable development, and institute's consuming electric power can be by wind-power electricity generation, and solar battery etc. is mentioned
For.The core of electrolysis water reaction relates generally to liberation of hydrogen (HER) and analysis oxygen (OER) two half-reactions, but due to being related to during it
And proton/electronics coupled transfer process to multistep, thermodynamics of reactions and dynamics are slower, cause in electrolysis water liberation of hydrogen and analysis
Higher overpotential is needed during oxygen.To solve this problem, elctro-catalyst is needed, urgently for reducing reaction energy barrier
With raising reaction rate.Currently, the catalyst as composed by the noble metals such as platinum, iridium and ruthenium is that electrolysis aquatic products hydrogen production oxygen is most effective
A kind of elctro-catalyst, but due to they in the deposit of nature limited, higher cost, it is difficult to meet industrialization answer on a large scale
With.Therefore, efficient stable is researched and developed, cheap, rich reserves elctro-catalysts are imperative to substitute noble metal catalyst.And
The difunctional water decomposition elctro-catalyst that can be effectively catalyzed to liberation of hydrogen and oxygen evolution reaction simultaneously may be implemented in same medium
In the reaction of full decomposition water, greatly reduce electrode preparation cost, simplify production process, thus with more wide application before
Scape.But high activity, stabilization, difunctional electrocatalysis material cheap and easy to get how are designed and prepare, it is still a challenge.
Summary of the invention
The purpose of the present invention is to provide a kind of double carbon coupling transiting metal nickel based quantum dot electro-catalysis efficiently, inexpensive
Agent and preparation method thereof.
Double carbon provided by the invention couple transiting metal nickel based quantum dot elctro-catalyst, prepare the raw material being related to and include:
Graphene oxide, nickel salt, cobalt salt, molysite, methylimidazole, methanol etc..Its preparation process includes: to utilize combined oxidation graphene
The Ni-based zeolite imidazole skeleton thin slice of two-dimensional ultrathin (2D Ni-ZIF@GO) be used as presoma, under inert atmosphere protection, pass through one
Thermal reduction and the carbonisation of 2D Ni-ZIF@G that low temperature pyrolyzer method carries out GO are walked, two-dimentional N doping porous carbon packet is prepared in situ
Transiting metal nickel based quantum dot/graphene the heterogeneous material compound covered.The composite material forms unique porous carbon and graphene
" double carbon " couples metal quantum point structure, has strong interface interaction, large specific surface area, electric conductivity height, N doping and defect abundant
And metal quantum point it is evenly dispersed the features such as, the composite material as bifunctional electrocatalyst be used for liberation of hydrogen and oxygen evolution reaction
When, it shows excellent electric catalyticing characteristic, in the KOH solution of 1.0 M, for HER and OER, generates 10 milliamperes and often put down
It is 133 and 265 mV that square centimetre of current density, which only needs overpotential,；When as total moisture solution, 10 milliamperes every square li is generated
The current density of rice only needs 1.475 volts of voltage.It is a kind of novel total moisture solution elctro-catalyst efficiently, economic.This is compound
Material elctro-catalyst prepares raw materials used at low cost, and simple process, energy consumption of reaction is low, and large scale preparation may be implemented.
The preparation method of above-mentioned double carbon coupling transiting metal nickel based quantum dot elctro-catalysts, specific steps are as follows:
(1) the Ni-based zeolite imidazole skeleton thin slice presoma (2D of two-dimensional ultrathin of combined oxidation graphene is prepared using coprecipitation
Ni-ZIF@GO): the Nickelous nitrate hexahydrate for weighing 200 ~ 400 mg is dissolved in the methanol solution of 5 ~ 10 mL, by above-mentioned solution
It is sufficiently mixed with the graphene oxide suspension of 10 ~ 20 mL, stirs 10 ~ 20 min；The 2- first of 300 ~ 400 mg will further be contained
Base imidazolemethanol solution is slowly added into above-mentioned mixed liquor, and 8 ~ 15 min are stirred at room temperature；Then mixed liquor is transferred to
It in the autoclave of 50 mL, is placed in 170 ~ 200 DEG C of insulating box, reacts 4 ~ 8 h, room temperature is cooling, by product
Centrifuge separation, is cleaned 3 ~ 4 times with deionized water；Finally place the product in 45 ~ 65 DEG C of freeze drier, freeze
Dry 40 ~ 50 h, products therefrom are denoted as 2D Ni-ZIF@GO；
(2) preparation (Ni@NC@NG) of double carbon coupling transiting metal nickel based quantum dot composite materials: the 2D Ni- that will be prepared
ZIF@G presoma, weighs and is placed in porcelain boat in right amount, porcelain boat is put into tube furnace, argon gas is passed through, with the speed of 2 ~ 4 DEG C/min
Degree is heated to 300 ~ 600 DEG C, keeps the temperature 1.5 ~ 3h at this temperature to get target product is arrived, is denoted as Ni@NC@NG.
Composite material Ni@NC@NG prepared by the present invention, can be used as bifunctional electrocatalyst, be used for liberation of hydrogen and oxygen evolution reaction,
And it is used for total moisture solution.When being used for evolving hydrogen reaction and oxygen evolution reaction, excellent electro catalytic activity and stability are all shown；
When for total moisture solution, the voltage that 10 milliamperes of current densities every square centimeter only need 1.475 volts is generated, better than business
Noble metal electrolysis water catalyst.
When for evolving hydrogen reaction and oxygen evolution reaction, specific steps are as follows: the Ni NC NG composite material of preparation is loaded into glass
On carbon electrode, as working electrode, using calomel electrode as reference electrode, carbon-point is used as to electrode；It is saturated in argon gas, oxygen
Its polarization curve is tested in 1.0 M KOH solutions.When for total moisture solution, respectively with Ni@NC@NG composite material directly as yin
Pole and anode test its total moisture solution performance in 1.0 M KOH solutions of saturation.
Present invention has an advantage that
(1) in the Ni@NC@NG composite material prepared, transiting metal nickel quantum dot is uniformly dispersed, and forms with double carbon of N doping
Very strong interface coupling effect, sufficiently exposes active site；
(2) Ni@NC@NG composite material has double carbon coupled structures and biggish specific surface area, in terms of so that it is applied to electro-catalysis
When, it is able to maintain higher catalytic activity, excellent stability and excellent electric conductivity；
(3) it prepares raw material and relates only to the common reagent such as Nickelous nitrate hexahydrate, methylimidazole, graphene and methanol, ethyl alcohol,
At low cost, product purity is high, and preparation process is simple, easy to industrialized production；And preparation process of the invention can be also extended to
The preparation of other magnesium-yttrium-transition metals/carbon nano tube/graphene three-dimensional hierarchical composite material elctro-catalyst.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph (SEM) of Ni@NC@NG composite material prepared by the embodiment of the present invention 1.
Fig. 2 is the transmission electron microscope picture (TEM) of Ni@NC@NG composite material prepared by the embodiment of the present invention 1.
Fig. 3 is the X-ray diffraction energy spectrum analysis figure (XRD) of Ni@NC@NG composite material prepared by the embodiment of the present invention 1
Fig. 4 is Ni@NC@NG composite material prepared by the embodiment of the present invention 1, with 5 millivolts of sweep speeds per second at 1.0 moles
HER linear sweep voltammetry curve graph in every liter of potassium hydroxide electrolyte.
Fig. 5 is Ni@NC@NG composite material prepared by the embodiment of the present invention 1, with 5 millivolts of sweep speeds per second 1.0
OER linear sweep voltammetry curve graph in mole every liter of potassium hydroxide electrolyte.
Fig. 6 is Ni@NC@NG composite material prepared by the embodiment of the present invention 1, with 5 millivolts of sweep speeds per second 1.0
All-hydrolytic test in mole every liter of potassium hydroxide electrolyte.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples, but protection scope of the present invention is not limited only to
These embodiments.For a further understanding of the present invention, below with reference to example and attached drawing, the present invention is further described.
Embodiment 1, the preparation method and application (Ni NC NG) of double carbon coupling transition metal nickel cobalt quantum dot composite materials,
The following steps are included:
(1) the Ni-based zeolite imidazole skeleton thin slice presoma (2D of two-dimensional ultrathin of combined oxidation graphene is prepared using coprecipitation
Ni-ZIF@GO): the Nickelous nitrate hexahydrate for weighing 300 mg is dissolved in the methanol solution of 5 mL, by above-mentioned solution and 10 mL
Graphene oxide suspension is sufficiently mixed, and stirs 20 min.Further by 5 mL, the 2-methylimidazole solution of 300 mg slowly adds
Enter into above-mentioned mixed liquor, 10 min are stirred at room temperature；Then mixed liquor is transferred in the autoclave of 50 mL, is put
It is placed in 180 DEG C of insulating box, reacts 4 h, room temperature is cooling, and product is centrifugated, is cleaned 3 times with deionized water.Finally will
Product is placed in 50 DEG C of freeze drier, is freeze-dried 48 h, products therefrom is 2D Ni-ZIF@G；
(2) preparation (Ni@NC@NG) of double carbon coupling transiting metal nickel based quantum dot composite materials: the 2D Ni- that will be prepared
ZIF@G presoma, is weighed and is placed in porcelain boat in right amount, porcelain boat is put into tube furnace, argon gas is passed through, added with the speed of 2 DEG C/min
Heat keeps the temperature 2 h at this temperature to 450 DEG C to get Ni@NC@NG composite material is arrived.
Ni NC NG composite material prepared by the present invention, when being used for bifunctional catalyst, specific steps are as follows: by preparation
Ni@NC@NG composite material loads on glass-carbon electrode as working electrode, using calomel electrode as reference electrode, carbon-point conduct
To electrode.The chemical property of its HER and OER are tested in the 1.0 M KOH solutions that argon gas, oxygen are saturated.As total moisture
It is complete to test it respectively with Ni NC NG composite material directly as cathode and anode in 1.0 M KOH solutions of saturation by Xie Shi
Water dispersible energy.
Present invention has an advantage that the dispersion of transiting metal nickel quantum dot is equal in the Ni@NC@NG composite material of (1) preparation
It is even, very strong interface coupling is formd with double carbon of N doping and is acted on, and active site is sufficiently exposed；(2) Ni@NC@NG composite wood
Material has double carbon coupled structures and biggish specific surface area, excellent electric conductivity, protect its application in terms of electro-catalysis can
Hold higher catalytic activity；(3) it prepares raw material and relates only to Nickelous nitrate hexahydrate, methylimidazole, graphene and methanol etc. often
Reagent, at low cost, product purity is high, and preparation process is simple, and preparation process easy to industrialized production and of the invention may be used also
It is extended to the preparation of pair other of carbon coupling or polynary magnesium-yttrium-transition metal quantum dot composite material elctro-catalyst.
Embodiment 2, preparation method and application (the NiCo@of double carbon coupling binary transition metal nickel cobalt quantum dot composite materials
NC@NG), comprising the following steps:
(1) the two-dimensional ultrathin nickel cobalt base zeolite imidazole skeleton thin slice presoma of combined oxidation graphene is prepared using coprecipitation
(2D Ni-ZIF@GO): the cabaltous nitrate hexahydrate of the Nickelous nitrate hexahydrate and 50 mg that weigh 250 mg respectively is dissolved in 10 mL's
In methanol solution, the graphene oxide suspension of above-mentioned solution and 20 mL is sufficiently mixed, stirs 20 min.Further by 5
The 2-methylimidazole solution of mL, 400 mg are slowly added into above-mentioned mixed liquor, and 10 min are stirred at room temperature；It then will mixing
Liquid is transferred in the autoclave of 50 mL, is placed in 190 DEG C of insulating box, and 6 h are reacted, and room temperature is cooling, by product from
Heart separation, is cleaned 4 times with deionized water.Finally place the product in 50 DEG C of freeze drier, it is freeze-dried 48 h, gained
Product is 2D NiCo-ZIF@G；
(2) preparation (NiCo@NC@NG) of double carbon coupling binary transition metal nickel cobalt quantum dot composite materials: the 2D that will be prepared
NiCo-ZIF@G presoma, weighs and is placed in porcelain boat in right amount, porcelain boat is put into tube furnace, argon gas is passed through, with 2 DEG C/min's
Speed is heated to 500 DEG C, keeps the temperature 2 h at this temperature to get NiCo@NC@NG composite material is arrived.
NiCo@NC@NG composite material prepared by the present invention, when being used for bifunctional catalyst, described in test method and example 1
Equally.
Present invention has an advantage that in the NiCo NC NG composite material of (1) preparation, the dispersion of transition metal nickel cobalt quantum dot
Uniformly, very strong interface coupling effect is formd with double carbon of N doping, sufficiently exposes active site；(2) NiCo@NC@NG is multiple
Condensation material has double carbon coupled structures and biggish specific surface area, excellent electric conductivity, while NiCo quantum dot contains largely
Defect can expose more active sites, higher catalytic activity is possessed in electrocatalytic hydrogen evolution and oxygen evolution reaction；(3) it prepares
Raw material relates only to Nickelous nitrate hexahydrate, cabaltous nitrate hexahydrate, methylimidazole, graphene and methanol, ethyl alcohol etc. and commonly tries
Agent, at low cost, product purity is high, and preparation process is simple, and preparation process easy to industrialized production and of the invention can be also extended to
The preparation of other or polynary magnesium-yttrium-transition metal quantum dot composite material elctro-catalyst of the coupling of double carbon.
Embodiment 3, the preparation method and application of double carbon coupling ternary transition metal nickel cobalt quantum dot composite materials
(NiCoFe@NC@NG), comprising the following steps:
(1) two-dimensional ultrathin nickel cobalt iron nanometer sheet presoma (the 2D NiCoFe-ZIF@of composite graphite alkene is prepared using coprecipitation
G): weighing the Ni (NO of 200 mg respectively3)2•6H2O, 30 mg Co (NO3)2•6H2O and 30 mg Fe (NO3)2•6H2O is dissolved in 5
In the methanol solution of mL, above-mentioned solution and 17 mL graphene oxide suspensions are sufficiently mixed, stir 20 min.Further by 5
The 2-methylimidazole solution of mL, 328 mg are slowly added into above-mentioned mixed liquor, and 10 min are stirred at room temperature；It then will mixing
Liquid is transferred in the autoclave of 50 mL, is placed in 180 DEG C of insulating box, and 8 h are reacted, and room temperature is cooling, by product from
Heart separation, is cleaned 4 times with deionized water.Finally place the product in 50 DEG C of freeze drier, it is freeze-dried 48 h, gained
Product is 2D NiCoFe-ZIF@G；
(2) preparation (NiCoFe@NC@NG) of double carbon coupling ternary transition metal nickel cobalt quantum dot composite materials: by what is prepared
2D NiCoFe-ZIF@G presoma, weighs and is placed in porcelain boat in right amount, porcelain boat is put into tube furnace, argon gas is passed through, with 2 DEG C/
The speed of min is heated to 450 DEG C, keeps the temperature 2 h at this temperature to get NiCoFe@NC@NG composite material is arrived.
NiCoFe@NC@NG composite material prepared by the present invention, when being used for bifunctional catalyst, test method and 1 institute of example
It states the same.
Present invention has an advantage that the dispersion of transition metal quantum dot is equal in the NiCoFe@NC@NG composite material of (1) preparation
It is even, very strong interface coupling is formd with double carbon of N doping and is acted on, and active site is sufficiently exposed；(2) NiCoFe@NC@NG is multiple
Condensation material has double carbon coupled structures and biggish specific surface area, its application in terms of electro-catalysis is made to be able to maintain higher urge
Change activity, excellent stability and excellent electric conductivity；(3) it prepares raw material and relates only to Nickelous nitrate hexahydrate, six hydration nitre
The common reagents such as sour cobalt, six nitric hydrate iron, methylimidazole, graphene and methanol, at low cost, product purity is high, preparation
Simple process, preparation process easy to industrialized production and of the invention can also be extended to pair other of carbon coupling or polynary transition
The preparation of race's metal quantum point composite material elctro-catalyst.
Claims (3)
1. a kind of preparation method of double carbon coupling transiting metal nickel based quantum dot composite materials, which is characterized in that specific steps are as follows:
(1) the Ni-based zeolite imidazole skeleton thin slice presoma of two-dimensional ultrathin of combined oxidation graphene is prepared using coprecipitation: being claimed
The Nickelous nitrate hexahydrate of 200 ~ 400 mg is taken to be dissolved in the methanol solution of 5 ~ 15 mL, by above-mentioned solution and 10 ~ 20 mL
Graphene oxide suspension is sufficiently mixed, and stirs 15 ~ 25 min；The 2-methylimidazole methanol solution of 300 ~ 400 mg will be contained
It is added in above-mentioned mixed liquor, 8 ~ 15 min is stirred at room temperature；Then mixed liquor is transferred in autoclave, is placed
In 170 ~ 190 DEG C of insulating box, 4 ~ 8 h are reacted, room temperature is cooling, and product is centrifugated, 3 are cleaned with deionized water ~
4 times；Finally place the product in 55 ~ 65 DEG C of freeze drier, 40 ~ 50 h are freeze-dried, products therefrom is denoted as 2D
Ni-ZIF@GO；
(2) preparation of double carbon coupling transiting metal nickel based quantum dot composite materials: appropriate 2D Ni-ZIF@G presoma is weighed, is set
In porcelain boat, porcelain boat is put into tube furnace, is passed through argon gas, is heated to 300 ~ 600 DEG C with the speed of 2 ~ 4 DEG C/min,
1.5 ~ 3.0 h are kept the temperature at a temperature of this to get target product is arrived, and are denoted as Ni@NC@NG.
2. a kind of double carbon that the preparation method as described in claim 1 obtains couple transiting metal nickel based quantum dot composite material.
3. double carbon as claimed in claim 2 couple transiting metal nickel based quantum dot composite material, as bifunctional electrocatalyst
Application in evolving hydrogen reaction, oxygen evolution reaction and total moisture solution.
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| WO2022021946A1 (en) * | 2020-07-29 | 2022-02-03 | 天津大学 | Composite electrode material for oxygen reduction reaction, preparation method and use thereof |
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