CN106563813A - Ag-CoSe2 nanoribbon and preparation method and purpose thereof - Google Patents
Ag-CoSe2 nanoribbon and preparation method and purpose thereof Download PDFInfo
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Abstract
The invention discloses an Ag-CoSe2 nanoribbon and a preparation method and a purpose thereof. The Ag-CoSe2 nanoribbon is complete in structure and excellent in electric conductivity; when the overpotential is 0.35 V, the current density is increased by 8 times compared with pure CoSe2 nanocatalyst; when the current density is 10 mA/cm2, the overpotential is only 0.32 V, and is reduced by 73 mV compared with the pure CoSe2 nanocatalyst; and in addition, the Ag-CoSe2 nanoribbon can directly serve as a catalyst for the electrolysed water oxygen evolution reaction process, shows excellent catalysis activity in the catalysis reaction process, and achieves more advantages. The preparation method of the Ag-CoSe2 nanoribbon uses a micro ion exchange method; compared with a traditional nanometer crystal synthesis method, the preparation method of the Ag-CoSe2 nanoribbon is simple and fast in reaction, mild in conditions, short in operation time and simple in procedures, largely reduces the synthesis cost, and is more environment-friendly in synthesis process; and the obtained nanoribbon is uniform in size and excellent in dispersibility, so that the catalysis activity of the electrolysed water oxygen evolution reaction is improved, and the application prospect is broad.
Description
Technical field
The invention belongs to two-dimension nano materials synthesis, the energy, catalysis correlative technology field, relate in particular to a kind of Ag-
CoSe2Nano belt and its production and use.
Background technology
In the face of the present situation for increasingly reducing of traditional energy resource, energy problem more receives publicity.Hydrogen energy source is used as a class
New cleaning fuel, has huge development space in new energy field.Essential industry of the electrolysis water as current hydrogen source
Form, its 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
Build, all kinds of catalyst materials are widely used in oxygen evolution reaction process, to accelerating reaction rate.However, as at present most
Efficient oxygen evolution reaction catalysts, yttrium oxide and oxidation ruthenium nano-particle are rare due to its reserves, expensive, cause hydrogen energy source
Preparation cost remains high, and significantly limit large-scale application of this kind of catalyst in electrolysis water field.Therefore, it is designed for
The cost-efficiently nanocatalyst of anode of electrolytic water oxygen evolution reaction is significant.
In recent years, with the discovery of the New Two Dimensional nano material with Graphene as representative, two-dimension nano materials are in the energy
Catalytic field achieves greatly breakthrough.During two-dimension nano materials realize electrocatalytic reaction with its high specific surface area
High-efficient contact between catalytic media, to realize that quick charge transfer provides guarantee between interface, so as to be expected to as base
Plinth obtains simple efficient electrolysis water oxygen evolution reaction catalysts by specific structure design.
As the two-dimension nano materials of a quasi-representative, dimensional Co Se2Nano belt is with its unique metalline, a large amount of to expose
Avtive spot and good structural stability in catalytic process cause the interest of more and more researcheres.Meanwhile, urge
The electric conductivity of agent also has particularly important effect during electrolysis water.Good electric conductivity can eliminate anti-in electro-catalysis
The Schottky energy barrier that interface produces is catalyzed during answering, it is ensured that good energy conversion efficiency.And the property of nano material takes
Structure certainly in it, pattern and component, therefore, how probe into by dimensional Co Se2Nano belt structure regulating realizes which is conductive
Property lifting for lifted catalysis activity have very important significance.
However, still having much urgently in terms of the structure design and electric conductivity regulation and control of two-dimension nano materials 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 method that two-dimentional two cobaltous selenides nano belt lifts the electric conductivity of catalyst and then improves catalysis activity is grown, but in catalytic process
In, material with carbon element is highly prone to the etching of the oxygen atom that water power is parsed, and is unfavorable for the stable existence of catalyst structure, and prepares few
Layer graphene is also required to the time-consuming process of 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 lifted under hydrolysis2WS4The method of nanoplate, although the self-conductive of two-dimensional material is due to interlayer lithium
The effect of the hydrogen that ion hydrolysis is produced is significantly improved, however, the time of two-dimensional material interlayer process is inserted for lithium ion
Cost very high (24h), and the reaction condition of using containing lithium additive and ice bath long-time ultrasonic (3h) causes reaction cost
It is very high, it is unfavorable for extensive preparation.
Up to the present, not yet have document report it is simple and quick under the conditions of water phase prepare structural integrity, with good
Dimensional Co Se of electric conductivity and excellent catalytic activity2The method of nanometer band structure.
The content of the invention
The technical problem to be solved is to provide a kind of structural integrity, lives with excellent catalysis with satisfactory electrical conductivity
Nano belt of property and preparation method thereof.
In order to solve above-mentioned technical problem, the present invention is adopted the following technical scheme that：A kind of Ag-CoSe2Nano belt.
Further, the Ag-CoSe2The surface of nano belt is smooth (210) crystal face.
Further, the Ag-CoSe2Nano belt is two-dimensional layered structure, and interlamellar spacing is 0.63nm.Layer structure is favourable
In catalytic electrolysis elutriation oxygen course of reaction, reaction medium and catalyst are fully contacted, and are carried out with accelerating reaction.
Further, the Ag-CoSe2The width of nano belt is 300～500nm.The width of 300～500nm ensure that
In nano belt, Co avtive spots are conducive to the lifting of reactivity in the abundant exposure on surface.
The present invention also provides above-mentioned Ag-CoSe2The preparation method of nano belt, comprises the following steps：
(1) dimensional Co Se2The preparation of-DETA nano belt
Cobalt acetate and sodium selenite are taken, is added in the mixed solution of deionized water and diethylenetriamine, is stirred, so
After be placed in 175～185 DEG C under conditions of heat 16 hours, obtain mean breadth be 300～500nm dimensional Co Se2- DETA receives
The solution of rice band, eventually passes centrifugation, washing, dried, obtains dimensional Co Se2- DETA nano belt；
(2)Ag-CoSe2The preparation of nano belt
By dimensional Co Se obtained in step (1)2- DETA nano belt is dissolved in deionized water, obtains mixed liquor A, to mixing
Silver nitrate is added in liquid A, is stirred, reacted 6 hours under conditions of being subsequently placed in 155～165 DEG C, obtain Ag-CoSe2Nanometer
The solution of band, eventually passes centrifugation, washing, dried, obtains the Ag-CoSe2Nano belt.
Further, in step (1), the mol 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 ensure that institute
Obtained CoSe2- DETA is homogeneous nanometer band structure.
Further, in step (2), dimensional Co Se2The mol ratio of-DETA nano belt and silver nitrate is 1:0.01.This matches somebody with somebody
Than may insure CoSe2The integrity of two-dimensional structure.
Further, the silver nitrate is to add in form of an aqueous solutions.Add in form of an aqueous solutions and be conducive to nitric acid
Dispersed in reaction system, homogeneous so as to the prepare pattern and component Ag-CoSe of silver2Nano belt.
The present invention also provides above-mentioned Ag-CoSe2Application of the nano belt during electrolysis water oxygen evolution reaction as catalyst.
Beneficial effects of the present invention are：
1. Ag-CoSe of the present invention2Nano belt structural integrity, electric conductivity are excellent, electric current density when overpotential is 0.35V
Than simple CoSe2Nanocatalyst lifts 8 times, is 10mA/cm in electric current density2When overpotential be only 0.32V, than simple
CoSe2Nanocatalyst reduces 73mV, in addition, Ag-CoSe of the present invention2Nano belt can be used in electrolysis water directly as catalyst
During oxygen evolution reaction, and excellent catalysis activity in catalytic reaction process is shown, with very big advantage.
2. Ag-CoSe of the present invention2The preparation method of nano belt uses micro ion exchange process, obtains two-dimensional layered structure
Ag-CoSe2Nano belt, and directly obtain Ag-CoSe2High conductivity nanocatalyst, with traditional nanocrystal synthetic method phase
Than present invention reaction is easy to be quick, and mild condition, operating time are short, and program is simple, and synthesis cost is greatly lowered, and synthesizes
Process is more environmentally friendly, gained nano belt size uniformity, good dispersion, so as to improve the catalysis activity to electrolysis water oxygen evolution reaction,
Possesses wide application prospect.
Description of the drawings
Fig. 1 is dimensional Co Se prepared by the embodiment of the present invention 12The scanning electron microscope diagram of-DETA nano belt；
Fig. 2 is the Ag-CoSe prepared by the embodiment of the present invention 12The transmission electron microscope figure of nano belt, (a) Ag-CoSe2
The low power transmission electron microscope figure of nano belt, illustration are the side view for reflecting layer structure；The high-resolution of (b) single nano belt
Transmission electron microscope figure；
Fig. 3 is the single Ag-CoSe prepared by the embodiment of the present invention 12Scanning transmission electron microscope-the element of nano belt
Analysis chart, wherein comprising (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 12Simple CoSe before nano belt and ion exchange2Receive
Rice band Raman spectrogram；
Fig. 5 is the two-dimentional Ag-CoSe prepared by the embodiment of the present invention 12Simple CoSe before nano belt and ion exchange2Receive
Rice strip resistance rate variation with temperature curve；
Fig. 6 is the two-dimentional Ag-CoSe prepared by the embodiment of the present invention 12Simple CoSe before nano belt and ion exchange2Receive
Rice electro-catalysis linear scanning curve of the band in catalytic electrolysis elutriation oxygen course of reaction.
Specific embodiment
With reference to embodiment, the invention will be further described：
Embodiment 1
Ag-CoSe2The preparation method of nano belt, comprises the following steps：
(1) dimensional Co Se2The preparation of-DETA nano belt
At normal temperatures, successively to the mixed solution equipped with 13.333mL deionized waters and 26.666mL diethylenetriamines
249mg cobalt acetates and 173mg sodium selenite are added in the glass beaker of 50mL, by mixed solution magnetic agitation 30 at room temperature
Minute, it is then transferred in the water heating kettle that volume is 50mL, after continuing to heat 16 hours at 180 DEG C, just obtains as shown in Figure 1
, dimensional Co Se of the mean breadth for 300-500nm2The solution of-DETA nano belt, finally by dimensional Co Se2- DETA nano belt
Solution through centrifugation, the mixed liquor washing of deionized water and ethanol, drying, obtain dimensional Co Se2- DETA nano belt；
(2)Ag-CoSe2The preparation of nano belt
At normal temperatures, successively in the glass reaction bottle of 20mL add 21mg dimensional Cos Se2- DETA nano belt and 15mL go
Ionized water, after dissolving, injects the aqueous solution that 1mL contains 0.17mg silver nitrate, at room temperature magnetic agitation in glass reaction bottle
30 minutes, proceed in the water heating kettle that volume is 20mL, continue to react 6 hours at 160 DEG C, just obtain product Ag-CoSe2Nanometer
Band, as shown in Fig. 2 as can be seen from the figure products therefrom two-dimensional structure is complete, with unique layer structure, single nano belt
Width between 300-500nm, show as (210) crystal face of two cobaltous selenides in layer, the Elemental redistribution of its whole region can be by
Fig. 3 learns that Co, Se and Ag element is evenly distributed in whole region.Silver ion be successfully entered also can as shown in Figure 4, with
The carrying out of ion exchange, Raman spectrum is in 670cm-1There is widthization in place peak, and showing silver ion causes into two cobaltous selenide lattices
There is local dip in its crystal structure.
Embodiment 2
Ag-CoSe2The preparation method of nano belt, comprises the following steps：
(1) dimensional Co Se2The preparation of-DETA nano belt
At normal temperatures, successively to the mixed solution equipped with 13.333mL deionized waters and 26.666mL diethylenetriamines
249mg cobalt acetates and 173mg sodium selenite are added in the glass beaker of 50mL, by mixed solution magnetic agitation 30 at room temperature
Minute, it is then transferred in the water heating kettle that volume is 50mL, after continuing to heat 16 hours at 175 DEG C, obtaining mean breadth is
Dimensional Co Se of 300-500nm2The solution of-DETA nano belt, finally by dimensional Co Se2The solution of-DETA nano belt through from
The mixed liquor washing of the heart, deionized water and ethanol, drying, obtain dimensional Co Se2- DETA nano belt；
(2)Ag-CoSe2The preparation of nano belt
At normal temperatures, successively in the glass reaction bottle of 20mL add 21mg dimensional Cos Se2- DETA nano belt and 15mL go
Ionized water, after dissolving, injects the aqueous solution that 1mL contains 0.17mg silver nitrate, at room temperature magnetic agitation in glass reaction bottle
30 minutes, proceed in the water heating kettle that volume is 20mL, continue to react 6 hours at 165 DEG C, just obtain product Ag-CoSe2Nanometer
Band, products therefrom two-dimensional structure are complete, with unique layer structure, the width of single nano belt between 300-500nm, layer
(210) crystal face of two cobaltous selenides is shown as inside, Co, Se and Ag element is evenly distributed in whole region, with ion exchange
Carry out, Raman spectrum is in 670cm-1There is widthization in place peak, and showing silver ion causes its crystal structure into two cobaltous selenide lattices
There is local dip.
Embodiment 3
Ag-CoSe2The preparation method of nano belt, comprises the following steps：
(1) dimensional Co Se2The preparation of-DETA nano belt
At normal temperatures, successively to the mixed solution equipped with 13.333mL deionized waters and 26.666mL diethylenetriamines
249mg cobalt acetates and 173mg sodium selenite are added in the glass beaker of 50mL, by mixed solution magnetic agitation 30 at room temperature
Minute, it is then transferred in the water heating kettle that volume is 50mL, after continuing to heat 16 hours at 185 DEG C, obtaining mean breadth is
Dimensional Co Se of 300-500nm2The solution of-DETA nano belt, finally by dimensional Co Se2The solution of-DETA nano belt through from
The mixed liquor washing of the heart, deionized water and ethanol, drying, obtain dimensional Co Se2- DETA nano belt；
(2)Ag-CoSe2The preparation of nano belt
At normal temperatures, successively in the glass reaction bottle of 20mL add 21mg dimensional Cos Se2- DETA nano belt and 15mL go
Ionized water, after dissolving, injects the aqueous solution that 1mL contains 0.17mg silver nitrate, at room temperature magnetic agitation in glass reaction bottle
30 minutes, proceed in the water heating kettle that volume is 20mL, continue to react 6 hours at 155 DEG C, just obtain product Ag-CoSe2Nanometer
Band, products therefrom two-dimensional structure are complete, with unique layer structure, the width of single nano belt between 300-500nm, layer
(210) crystal face of two cobaltous selenides is shown as inside, Co, Se and Ag element is evenly distributed in whole region, with ion exchange
Carry out, Raman spectrum is in 670cm-1There is widthization in place peak, and showing silver ion causes its crystal structure into two cobaltous selenide lattices
There is local dip.
Embodiment 4
To Ag-CoSe2The test of nano belt electric conductivity with compare
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, bonding silver wire make electrode, and test its resistivity variation with temperature rule, and curve obtained is as shown in Figure 5.
Being continuously increased with temperature, the resistivity of material gradually increase with temperature, show two-dimensional layer Ag-CoSe2Nano belt is unique
Metallic character；Under room temperature (300K), Ag-CoSe2The resistivity of nano belt is only 7.48 × 10-6Ω m, and it is simple
CoSe2The resistivity of nano belt has but reached 1.05 × 10-4Ω m, show Ag-CoSe after ion exchange2Nano belt electric conductivity
Significant increase.
Embodiment 5
To Ag-CoSe2Nano belt is electrolysed the test of the electrocatalysis characteristic of elutriation oxygen reaction and compares
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 is 5%), ultrasound are added to form paste in 1 hour
After shape thing, take it is a certain amount of be added drop-wise to glassy carbon electrode surface, survey as working electrode and in 0.1M potassium hydroxide solutions after being dried
Fixed its catalysis activity to electrolysis water oxygen evolution reaction.Oxygen is passed through in potassium hydroxide solution constantly, scanning speed is 5mV/s,
Electrode rotating speed is 1600rpm, and gained linear scanning curve is as shown in Figure 6.Electric current density when overpotential is 0.35V reaches
22.36mA/cm2, and simple CoSe2The electric current density of nanocatalyst is only 2.72mA/cm2, the two-dimensional nano catalyst ratio
Simple CoSe2Nanocatalyst lifts 8 times.In addition, being 10mA/cm in electric current density2When overpotential be only 0.32V, than list
Pure CoSe2Nanocatalyst reduces 73mV, shows the excellent catalysis activity in catalytic reaction process of the structure.
Due to dimensional Co Se2Nano belt with its special two-dimensional nanostructure and a large amount of exposed Co atoms, in catalytic water
There is unique advantage in terms of electrolysis analysis oxygen.The present invention is with dimensional Co Se2Nano belt as basic structure, while by it is micro from
Minimal amount of Ag ions are incorporated into CoSe by the method that son is exchanged2Crystal structure in, can both maintain two-dimensional nano band itself
Structural intergrity, again can utilize introduce silver ion to CoSe2The impact of electric conductivity so that with superior electrical conductivity two
Dimension stratiform Ag-CoSe2Nano belt is expected to play remarkable effect in catalytic field.
It should be understood that example as herein described and embodiment are not limited to the present invention, this area only for explanation
Technical staff can make various modifications or change according to it, all any modifications within the spirit and principles in the present invention, made,
Equivalent, improvement etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of Ag-CoSe2Nano belt.
2. Ag-CoSe as claimed in claim 12Nano belt, it is characterised in that：The Ag-CoSe2The surface of nano belt is flat
Whole (210) crystal face.
3. Ag-CoSe as claimed in claim 1 or 22Nano belt, it is characterised in that：The Ag-CoSe2Nano belt is two-dimensional layer
Shape structure, interlamellar spacing are 0.63nm.
4. Ag-CoSe as claimed in claim 1 or 22Nano belt, it is characterised in that：The Ag-CoSe2The width of nano belt is
300～500nm.
5. the Ag-CoSe as any one of Claims 1-42The preparation method of nano belt, it is characterised in that including following
Step：
(1) dimensional Co Se2The preparation of-DETA nano belt
Cobalt acetate and sodium selenite are taken, is added in the mixed solution of deionized water and diethylenetriamine, is stirred, then put
Heat 16 hours under conditions of 175～185 DEG C, obtain dimensional Co Se that mean breadth is 300～500nm2- DETA nano belt
Solution, eventually pass centrifugation, washing, dried, obtain dimensional Co Se2- DETA nano belt；
(2)Ag-CoSe2The preparation of nano belt
By dimensional Co Se obtained in step (1)2- DETA nano belt is dissolved in deionized water, obtains mixed liquor A, in mixed liquor A
Silver nitrate is added, is stirred, reacted 6 hours under conditions of being subsequently placed in 155～165 DEG C, obtain Ag-CoSe2Nano belt
Solution, eventually passes centrifugation, washing, dried, obtains the Ag-CoSe2Nano belt.
6. Ag-CoSe as claimed in claim 52The preparation method of nano belt, it is characterised in that：In step (1), cobalt acetate and
The mol ratio of sodium selenite is 1:2.
7. the Ag-CoSe as described in claim 5 or 62The preparation method of nano belt, it is characterised in that：In step (1), deionization
The volume ratio of water and diethylenetriamine is 1:2.
8. the Ag-CoSe as described in claim 5 or 62The preparation method of nano belt, it is characterised in that：In step (2), two dimension
CoSe2The mol ratio of-DETA nano belt and silver nitrate is 1:0.01.
9. the Ag-CoSe as described in claim 5 or 62The preparation method of nano belt, it is characterised in that：The silver nitrate is with water
The form of solution is added.
10. the Ag-CoSe as any one of Claims 1-42Nano belt conduct during electrolysis water oxygen evolution reaction is urged
The application of agent.
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| CN111346651A (en) * | 2020-04-08 | 2020-06-30 | 中国科学技术大学 | Silver selenide-cobalt diselenide composite material with Tuoling structure, and preparation method and application thereof |
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| CN109225301A (en) * | 2018-10-16 | 2019-01-18 | 中国科学技术大学先进技术研究院 | A kind of Ir/Co0.8Fe0.2Se2Monatomic catalyst of-NF and preparation method thereof, application |
| 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 |
| CN111346651A (en) * | 2020-04-08 | 2020-06-30 | 中国科学技术大学 | Silver selenide-cobalt diselenide composite material with Tuoling structure, and preparation method and application thereof |
| CN112850662A (en) * | 2021-02-10 | 2021-05-28 | 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 |
| 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 |
| CN113084185A (en) * | 2021-03-26 | 2021-07-09 | 华中科技大学 | Pd1-CoSe2Nanobelt and preparation method and application thereof |
| WO2023045336A1 (en) * | 2021-09-23 | 2023-03-30 | 广东邦普循环科技有限公司 | Hollow nano-selenide, preparation method therefor and application thereof |
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