CN106563813B - A kind of Ag-CoSe2Nanobelt and its preparation method and application - Google Patents
A kind of Ag-CoSe2Nanobelt and its preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of Ag CoSe2Nanobelt and its preparation method and application.Ag CoSe of the present invention2Nanobelt structural integrity, electric conductivity is excellent, the simple CoSe of current density ratio when overpotential is 0.35V2Nanocatalyst promotes 8 times, is 10mA/cm in current density2When overpotential be only 0.32V, than simple CoSe2Nanocatalyst reduces 73mV, in addition, Ag CoSe of the present invention2During nanobelt can be used in electrolysis water oxygen evolution reaction directly as catalyst, and excellent catalytic activity in catalytic reaction process is shown, there is very big advantage.Ag CoSe of the present invention2The preparation method of nanobelt uses micro ion exchange process, compared with traditional nanocrystal synthetic method, the present invention reacts easy to be quick, mild condition, and the operating time is short, program is simple, synthesis cost is greatly lowered, and building-up process is more environmentally friendly, gained nanobelt size uniformity, good dispersion, to improve the catalytic activity to electrolysis water oxygen evolution reaction, has wide application prospect.
Description
Technical field
The invention belongs to two-dimension nano materials synthesis, the energy, catalysis correlative technology fields, relate in particular to a kind of Ag-
CoSe2Nanobelt and its preparation method and application.
Background technology
In face of the present situation of the increasingly reduction of traditional energy resource, energy problem more attracts attention.Hydrogen energy source is as a kind of
New cleaning fuel has huge development space in new energy field.Essential industry of the electrolysis water as current hydrogen source
Form, reaction process are but limited to the higher reaction barrier of anode of electrolytic water oxygen evolution reaction.To reduce the reaction wall of the reaction
It builds, all kinds of catalyst materials are widely used in oxygen evolution reaction process, to accelerate reaction rate.However, as at present most
Efficient oxygen evolution reaction catalysts, yttrium oxide and oxidation ruthenium nano-particle are expensive since its reserves is rare, lead to hydrogen energy source
Manufacturing cost is high, significantly limit this kind of catalyst electrolysis water field large-scale application.Therefore, it is designed for
The cost-efficiently nanocatalyst of anode of electrolytic water oxygen evolution reaction is of great significance.
In recent years, as using graphene as the discovery of the New Two Dimensional nano material of representative, two-dimension nano materials are in the energy
Catalytic field achieves great breakthrough.Two-dimension nano materials are realized with its high specific surface area during electrocatalytic reaction
High-efficient contact between catalytic media, to realize, quick charge transfer provides guarantee between interface, to be expected to as base
The electrolysis water oxygen evolution reaction catalysts that plinth is simple and efficient by specific structure design.
As a kind of typical two-dimension nano materials, dimensional Co Se2Nanobelt is with its unique metalline, a large amount of exposures
Active site and good structural stability causes the interest of more and more researchers in catalytic process.Meanwhile it urging
The electric conductivity of agent also has the function of particularly important during electrolysis water.Good electric conductivity can be eliminated anti-in electro-catalysis
It should be catalyzed the Schottky energy barrier that interface generates in the process, it is ensured that good energy conversion efficiency.And the property of nano material takes
Certainly in its structure, pattern and component, therefore, how probe by dimensional Co Se2Nanobelt structure regulating realizes its conduction
Property promotion for promoted catalytic activity have very important significance.
However, still having much urgently in terms of the structure design of two-dimension nano materials and electric conductivity regulation and control and Properties Control at present
Problem to be solved.For example,《ACS nanometers》(ACS Nano 8.3970-3978,2014) is reported on two-dimensional graphene surface
The two-dimentional two cobaltous selenide nanobelts of growth promote the electric conductivity of catalyst and then improve the method for catalytic activity, but in catalytic process
In, carbon material is highly prone to the etching for the oxygen atom that water power parses, and is unfavorable for being stabilized for catalyst structure, and prepares few
Layer graphene is also required to the time-consuming process of a series of complex, increases the time cost of experiment.《German applied chemistry》
(Angewandte Chemie International Edition 55.5733-5738,2016) is reported in lithium ion intercalation
Two dimension Cu is promoted under hydrolysis2WS4The method of nanoplate, although the self-conductive of two-dimensional material is due to interlayer lithium
The effect for the hydrogen that ion hydrolysis generates is significantly improved, however, being inserted into the time of two-dimensional material interlayer process for lithium ion
Cost is very high (for 24 hours), and the additive containing lithium use and the reaction condition of ice bath ultrasonic (3h) for a long time makes reaction cost
It is very high, it is unfavorable for preparing on a large scale.
Up to the present, there has been no document reports under the conditions of water phase it is simple and quick prepare structural integrity, have it is good
The dimensional Co Se of electric conductivity and excellent catalytic activity2The method of nanometer band structure.
Invention content
Technical problem to be solved by the invention is to provide a kind of structural integrities, and there is satisfactory electrical conductivity to live with excellent catalysis
The nanobelt and preparation method thereof of property.
In order to solve the above-mentioned technical problem, the present invention adopts the following technical scheme that：A kind of Ag-CoSe2Nanobelt.
Further, the Ag-CoSe2The surface of nanobelt is smooth (210) crystal face.
Further, the Ag-CoSe2Nanobelt is two-dimensional layered structure, interlamellar spacing 0.63nm.Layer structure is advantageous
Reaction medium and catalyst come into full contact in catalytic electrolysis elutriation oxygen reaction process, are carried out with accelerating reaction.
Further, the Ag-CoSe2The width of nanobelt is 300~500nm.The width of 300~500nm ensure that
Co active sites are conducive to the promotion of reactivity in the abundant exposure on surface in nanobelt.
The present invention also provides above-mentioned Ag-CoSe2The preparation method of nanobelt, includes the following steps：
(1) dimensional Co Se2The preparation of-DETA nanobelts
Cobalt acetate and sodium selenite are taken, is added in the mixed solution of deionized water and diethylenetriamine, stirs evenly, so
It is heated 16 hours under conditions of being placed on 175~185 DEG C, obtains the dimensional Co Se that mean breadth is 300~500nm2-DETA
The solution of nanobelt obtains dimensional Co Se finally by centrifugation, washing, drying process2- DETA nanobelts；
(2)Ag-CoSe2The preparation of nanobelt
By dimensional Co Se made from step (1)2- DETA nanobelts are dissolved in deionized water, mixed liquor A are obtained, to mixing
Silver nitrate is added in liquid A, stirs evenly, is reacted 6 hours under conditions of being subsequently placed in 155~165 DEG C, obtains Ag-CoSe2Nanometer
The solution of band obtains the Ag-CoSe finally by centrifugation, washing, drying process2Nanobelt.
Further, in step (1), the molar ratio of cobalt acetate and sodium selenite is 1:2.
Further, in step (1), the volume ratio of deionized water and diethylenetriamine is 1:2.The volume ratio ensures institute
CoSe obtained2- DETA is uniform nanometer band structure.
Further, in step (2), dimensional Co Se2The molar ratio of-DETA nanobelts and silver nitrate is 1:0.01.This matches
Than may insure CoSe2The integrality of two-dimensional structure.
Further, the silver nitrate is to be added in form of an aqueous solutions.It is added in form of an aqueous solutions and is conducive to nitric acid
Silver in the reaction system evenly dispersed, to prepare pattern and the uniform Ag-CoSe of component2Nanobelt.
The present invention also provides above-mentioned Ag-CoSe2Application of nanobelt during electrolysis water oxygen evolution reaction as catalyst.
Beneficial effects of the present invention are：
1. Ag-CoSe of the present invention2Nanobelt structural integrity, electric conductivity is excellent, current density when overpotential is 0.35V
Than simple CoSe2Nanocatalyst promotes 8 times, is 10mA/cm in current density2When overpotential be only 0.32V, than simple
CoSe2Nanocatalyst reduces 73mV, in addition, Ag-CoSe of the present invention2Nanobelt can be used in electrolysis water directly as catalyst
During oxygen evolution reaction, and excellent catalytic activity in catalytic reaction process is shown, there is very big advantage.
2. Ag-CoSe of the present invention2The preparation method of nanobelt uses micro ion exchange process, obtains two-dimensional layered structure
Ag-CoSe2Nanobelt, and directly obtain Ag-CoSe2High conductivity nanocatalyst, with traditional nanocrystal synthetic method phase
Than the present invention reacts easy to be quick, and mild condition, the operating time is short, and program is simple, and synthesis cost is greatly lowered, and synthesizes
Process is more environmentally friendly, gained nanobelt size uniformity, good dispersion, to improve the catalytic activity to electrolysis water oxygen evolution reaction,
Has wide application prospect.
Description of the drawings
Fig. 1 is the dimensional Co Se prepared by the embodiment of the present invention 12The scanning electron microscope diagram of-DETA nanobelts；
Fig. 2 is the Ag-CoSe prepared by the embodiment of the present invention 12The transmission electron microscope figure of nanobelt, (a) Ag-CoSe2
The low power transmission electron microscope figure of nanobelt, illustration are the side view for reflecting layer structure；(b) high-resolution of single nanobelt
Transmission electron microscope figure；
Fig. 3 is the single Ag-CoSe prepared by the embodiment of the present invention 12Scanning transmission electron microscope-element of nanobelt
Analysis chart, wherein including (a) angle of elevation annular dark, (b, c, d) element distribution analysis；
Fig. 4 is the two-dimentional Ag-CoSe prepared by the embodiment of the present invention 12Nanobelt and CoSe simple before ion exchange2It receives
Rice band Raman spectrogram；
Fig. 5 is the two-dimentional Ag-CoSe prepared by the embodiment of the present invention 12Nanobelt and CoSe simple before ion exchange2It receives
Rice strip resistance rate variation with temperature curve；
Fig. 6 is the two-dimentional Ag-CoSe prepared by the embodiment of the present invention 12Nanobelt and CoSe simple before ion exchange2It receives
Electro-catalysis linear scan curve of the rice band in catalytic electrolysis elutriation oxygen reaction process.
Specific implementation mode
With reference to embodiment, the invention will be further described：
Embodiment 1
Ag-CoSe2The preparation method of nanobelt, includes the following steps：
(1) dimensional Co Se2The preparation of-DETA nanobelts
At normal temperatures, successively to 50 of the mixed solution equipped with 13.333mL deionized waters and 26.666mL diethylenetriamines
249mg cobalt acetates and 173mg sodium selenites are added in the glass beaker of mL, magnetic agitation 30 is divided at room temperature by the mixed solution
Clock is then transferred into the water heating kettle that volume is 50mL, after continuation is heated 16 hours at 180 DEG C, is just obtained as shown in Figure 1
, mean breadth is the dimensional Co Se of 300-500nm2The solution of-DETA nanobelts, finally by dimensional Co Se2- DETA nanobelts
Solution by centrifugation, mixed liquor washing, the drying of deionized water and ethyl alcohol, obtain dimensional Co Se2- DETA nanobelts；
(2)Ag-CoSe2The preparation of nanobelt
At normal temperatures, 21mg dimensional Cos Se is added into the glass reaction bottle of 20mL successively2- DETA nanobelts and 15mL
After dissolving, the aqueous solution that 1mL contains 0.17mg silver nitrates is injected into glass reaction bottle for deionized water, and magnetic force stirs at room temperature
It mixes 30 minutes, is transferred in the water heating kettle that volume is 20mL, continuation is reacted 6 hours at 160 DEG C, just obtains product Ag-CoSe2It receives
Rice band has unique layer structure, single nanometer as shown in Fig. 2, as can be seen from the figure products therefrom two-dimensional structure is complete
The width of band shows as (210) crystal face of two cobaltous selenides between 300-500nm, in layer, and the Elemental redistribution of whole region can
It is learnt by Fig. 3, Co, Se is evenly distributed on Ag elements in whole region.Silver ion be successfully entered also can as shown in Figure 4, with
The progress of ion exchange, Raman spectrum is in 670cm-1Locate peak and widthization occur, shows silver ion and led into two cobaltous selenide lattices
Its crystal structure is caused local dip occur.
Embodiment 2
Ag-CoSe2The preparation method of nanobelt, includes the following steps：
(1) dimensional Co Se2The preparation of-DETA nanobelts
At normal temperatures, successively to 50 of the mixed solution equipped with 13.333mL deionized waters and 26.666mL diethylenetriamines
249mg cobalt acetates and 173mg sodium selenites are added in the glass beaker of mL, magnetic agitation 30 is divided at room temperature by the mixed solution
Clock is then transferred into the water heating kettle that volume is 50mL, and after continuation is heated 16 hours at 175 DEG C, obtaining mean breadth is
The dimensional Co Se of 300-500nm2The solution of-DETA nanobelts, finally by dimensional Co Se2The solution of-DETA nanobelts pass through from
Mixed liquor washing, the drying of the heart, deionized water and ethyl alcohol, obtain dimensional Co Se2- DETA nanobelts；
(2)Ag-CoSe2The preparation of nanobelt
At normal temperatures, 21mg dimensional Cos Se is added into the glass reaction bottle of 20mL successively2- DETA nanobelts and 15mL
After dissolving, the aqueous solution that 1mL contains 0.17mg silver nitrates is injected into glass reaction bottle for deionized water, and magnetic force stirs at room temperature
It mixes 30 minutes, is transferred in the water heating kettle that volume is 20mL, continuation is reacted 6 hours at 165 DEG C, just obtains product Ag-CoSe2It receives
Rice band, products therefrom two-dimensional structure is complete, have unique layer structure, the width of single nanobelt between 300-500nm,
(210) crystal face of two cobaltous selenides is shown as in layer, Co, Se are evenly distributed on Ag elements in whole region, with ion exchange
Progress, Raman spectrum is in 670cm-1Locate peak and widthization occur, show silver ion leads to its crystal knot into two cobaltous selenide lattices
There is local dip in structure.
Embodiment 3
Ag-CoSe2The preparation method of nanobelt, includes the following steps：
(1) dimensional Co Se2The preparation of-DETA nanobelts
At normal temperatures, successively to 50 of the mixed solution equipped with 13.333mL deionized waters and 26.666mL diethylenetriamines
249mg cobalt acetates and 173mg sodium selenites are added in the glass beaker of mL, magnetic agitation 30 is divided at room temperature by the mixed solution
Clock is then transferred into the water heating kettle that volume is 50mL, and after continuation is heated 16 hours at 185 DEG C, obtaining mean breadth is
The dimensional Co Se of 300-500nm2The solution of-DETA nanobelts, finally by dimensional Co Se2The solution of-DETA nanobelts pass through from
Mixed liquor washing, the drying of the heart, deionized water and ethyl alcohol, obtain dimensional Co Se2- DETA nanobelts；
(2)Ag-CoSe2The preparation of nanobelt
At normal temperatures, 21mg dimensional Cos Se is added into the glass reaction bottle of 20mL successively2- DETA nanobelts and 15mL
After dissolving, the aqueous solution that 1mL contains 0.17mg silver nitrates is injected into glass reaction bottle for deionized water, and magnetic force stirs at room temperature
It mixes 30 minutes, is transferred in the water heating kettle that volume is 20mL, continuation is reacted 6 hours at 155 DEG C, just obtains product Ag-CoSe2It receives
Rice band, products therefrom two-dimensional structure is complete, have unique layer structure, the width of single nanobelt between 300-500nm,
(210) crystal face of two cobaltous selenides is shown as in layer, Co, Se are evenly distributed on Ag elements in whole region, with ion exchange
Progress, Raman spectrum is in 670cm-1Locate peak and widthization occur, show silver ion leads to its crystal knot into two cobaltous selenide lattices
There is local dip in structure.
Embodiment 4
To Ag-CoSe2The test of nanobelt electric conductivity is compared with
Ag-CoSe prepared by embodiment 12Tabletting after nanometer belt grinding, is cut into after being pressed into the uniform sheet of specific thicknesses
Regular oblong bonds silver wire and makes electrode, and tests its resistivity variation with temperature rule, and curve obtained is as shown in Figure 5.
With being continuously increased for temperature, the resistivity of material is gradually increased with temperature, shows two-dimensional layer Ag-CoSe2Nanobelt is unique
Metallic character；Under room temperature (300K), Ag-CoSe2The resistivity of nanobelt is only 7.48 × 10-6Ω m, and simple
CoSe2The resistivity of nanobelt has but reached 1.05 × 10-4Ω m show Ag-CoSe after ion exchange2Nanobelt electric conductivity
Significant increase.
Embodiment 5
To Ag-CoSe2Nanobelt is electrolysed the test of the electrocatalysis characteristic of elutriation oxygen reaction compared with
Two-dimensional layer Ag-CoSe prepared by embodiment 12Nanocatalyst is dissolved in 1mL water and isopropyl alcohol mixture (water
Volume ratio with isopropanol is 3：1) in, 40 microlitres of Nafion solutions (mass fraction 5%) are added, ultrasound forms paste in 1 hour
After shape object, take it is a certain amount of be added drop-wise to glassy carbon electrode surface, surveyed as working electrode and in 0.1M potassium hydroxide solutions after dry
Determine its catalytic activity to electrolysis water oxygen evolution reaction.Constantly it is passed through oxygen in potassium hydroxide solution, sweep speed 5mV/s,
Electrode rotating speed is 1600rpm, and gained linear scan curve is as shown in Figure 6.Current density when overpotential is 0.35V reaches
22.36mA/cm2, and simple CoSe2The current density of nanocatalyst is only 2.72mA/cm2, the two-dimensional nano catalyst ratio
Simple CoSe2Nanocatalyst promotes 8 times.In addition, being 10mA/cm in current density2When overpotential be only 0.32V, than list
Pure CoSe2Nanocatalyst reduces 73mV, shows structure catalytic activity excellent in catalytic reaction process.
Due to dimensional Co Se2The Co atoms that nanobelt is exposed with its special two-dimensional nanostructure and largely, in catalytic water
There is unique advantage in terms of electrolysis analysis oxygen.The present invention is with dimensional Co Se2Nanobelt as basic structure, while by it is micro from
Minimal amount of Ag ions are introduced into CoSe by the method that son exchanges2Crystal structure in, can both maintain two-dimensional nano band itself
Structural intergrity, and can utilize introduce silver ion to CoSe2The influence of electric conductivity so that two with superior electrical conductivity
Tie up stratiform Ag-CoSe2Nanobelt is expected to play remarkable effect in catalytic field.
It should be understood that example as described herein and embodiment are not intended to restrict the invention, this field only for explanation
Technical staff can make various modifications or variation according to it, all within the spirits and principles of the present invention, made by it is any modification,
Equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of Ag-CoSe2Nanobelt, it is characterised in that：By the way that Ag ions are introduced into CoSe2The CoSe of nanobelt2Crystal
It is formed in structure.
2. Ag-CoSe as described in claim 12Nanobelt, it is characterised in that：The Ag-CoSe2The surface of nanobelt is flat
Whole（210）Crystal face.
3. Ag-CoSe as claimed in claim 1 or 22Nanobelt, it is characterised in that：The Ag-CoSe2Nanobelt is two-dimensional layer
Shape structure, interlamellar spacing 0.63nm.
4. Ag-CoSe as claimed in claim 1 or 22Nanobelt, it is characterised in that：The Ag-CoSe2The width of nanobelt is
300~500nm.
5. Ag-CoSe according to any one of claims 1 to 42The preparation method of nanobelt, which is characterized in that including following
Step：
（1）Dimensional Co Se2The preparation of-DETA nanobelts
Cobalt acetate and sodium selenite are taken, is added in the mixed solution of deionized water and diethylenetriamine, stirs evenly, then set
In 175~185oIt is heated 16 hours under conditions of C, obtains the dimensional Co Se that mean breadth is 300~500nm2- DETA nanobelts
Solution, finally by centrifugation, washing, be dried, obtain dimensional Co Se2- DETA nanobelts；
（2）Ag-CoSe2The preparation of nanobelt
By step（1）Dimensional Co Se obtained2- DETA nanobelts are dissolved in deionized water, mixed liquor A are obtained, into mixed liquor A
Silver nitrate is added, stirs evenly, is subsequently placed in 155~165oIt is reacted 6 hours under conditions of C, obtains Ag-CoSe2Nanobelt it is molten
Liquid obtains the Ag-CoSe finally by centrifugation, washing, drying process2Nanobelt.
6. Ag-CoSe as claimed in claim 52The preparation method of nanobelt, it is characterised in that：Step（1）In, cobalt acetate and
The molar ratio of sodium selenite is 1:2.
7. such as Ag-CoSe described in claim 5 or 62The preparation method of nanobelt, it is characterised in that：Step（1）In, deionization
The volume ratio of water and diethylenetriamine is 1:2.
8. such as Ag-CoSe described in claim 5 or 62The preparation method of nanobelt, it is characterised in that：Step（2）In, two dimension
CoSe2The molar ratio of-DETA nanobelts and silver nitrate is 1:0.01.
9. such as Ag-CoSe described in claim 5 or 62The preparation method of nanobelt, it is characterised in that：The silver nitrate is with water
The form of solution is added.
10. Ag-CoSe according to any one of claims 1 to 42Nanobelt is used as during electrolysis water oxygen evolution reaction and urges
The application of agent.
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| CN109225301B (en) * | 2018-10-16 | 2021-04-23 | 中国科学技术大学先进技术研究院 | Ir/Co0.8Fe0.2Se2-NF single-atom catalyst, preparation method and application thereof |
| CN111346651B (en) * | 2020-04-08 | 2022-09-30 | 中国科学技术大学 | Silver selenide-cobalt diselenide composite material with Tuoling structure, and preparation method and application thereof |
| CN112850662B (en) * | 2021-02-10 | 2024-02-09 | 中国科学技术大学 | Strong-coupling layered cobalt diselenide, preparation method thereof and application thereof in preparation of hydrogen peroxide through electrocatalytic oxygen reduction reaction |
| CN113084185B (en) * | 2021-03-26 | 2022-05-20 | 华中科技大学 | Pd1-CoSe2Nanobelt and preparation method and application thereof |
| CN113964317A (en) * | 2021-09-23 | 2022-01-21 | 广东邦普循环科技有限公司 | Hollow nano selenide and preparation method and application thereof |
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