CN109706475A - A kind of heterojunction nanometer material elctro-catalyst and its CO2Reduction application - Google Patents
A kind of heterojunction nanometer material elctro-catalyst and its CO2Reduction application Download PDFInfo
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 34
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- 238000006243 chemical reaction Methods 0.000 abstract description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 2
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- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 17
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- 238000006555 catalytic reaction Methods 0.000 description 5
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
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- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
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Abstract
The invention belongs to CO2Reduction and technique for fixing field, disclose with a kind of heterojunction nanometer material Au-Ag/Ag2S is as catalyst, by applying voltage in response matrix liquid for CO2The method for being reduced to carbon compound.The present invention restrained effectively evolving hydrogen reaction, improve CO2To the efficiency of alcohol product orientation conversion, the faradic efficiency of ethyl alcohol can reach 70%, in CO2Green conversion field is with a wide range of applications.
Description
Technical field
The invention belongs to CO2Reduction field, and in particular to a kind of heterojunction nanometer material Au-Ag/Ag2S is catalyzed CO2Also
It originally was the new method of carbon compound.
Background technique
Since the industrial revolution, atmospheric greenhouse gas CO caused by fossil fuel largely burns2Concentration persistently increases
21 century mankind environmental problem urgently to be solved.And utilize electro-catalysis technology by CO2It is reduced into the organic liquor with high added value
Physical efficiency source (such as HCOOH, CH3OH and C2H5OH etc.), it on the one hand solves the problems, such as carbon source loss, on the other hand alleviates greenhouse
Climate change caused by effect is to realize CO2One of the desirable route of green conversion.
Electro-catalysis restores CO2Gaseous state and liquid product numerous types (such as CO, CH4、HCOOH、CH3OH、C2H5OH and
CH3COOH etc.), and catalyst activity and selectivity how is improved by CO2It is efficiently converted into the liquid that can be convenient storage and utilize
Physical efficiency source is current field critical issue urgently to be resolved.Metal/semiconductor nano heterojunction passes through metal and semiconductor two
Kind material of different nature is formed by connecting by hetero-junctions, and special heterojunction structure imparts the unique ohm of this material and connects
Characteristic and/or high Schottky (Schottky) contact berrier are touched, the biography of electronics, hole and various excitons can be effectively accelerated
It is defeated, it shows compared with its base metal or semiconductor more preferably catalytic performance, in CO2Before green conversion field has wide application
Scape.Therefore, developing one kind has the nano heterogeneous junction structure elctro-catalyst of metal/semiconductor for CO2Reduction has important meaning
Justice.
Currently, the monometallics such as Au, Ag material or Ag2S nanocatalyst surface electroreduction CO2Primary product be CO gas,
The report of liquid product is also very rare.Therefore, it is heterogeneous to prepare and screen highly selective Au/Ag Base Metal/semiconductor nano
Elctro-catalyst is tied, by CO2The alcohol product that being efficiently converted into can be convenient storage and utilize has important practical significance.
Summary of the invention
It has been surprisingly found that CO2In heterojunction nanometer material Au-Ag/Ag2The electricity at this metal/semiconductor interface S is urged
Changing reduzate is mainly methanol and ethyl alcohol, moreover, by reasonable regulating and controlling voltage, the faradic efficiency of ethyl alcohol be can achieve
70%.The present invention can efficiently solve CO at this stage2It is bad and low to alcohols orientation conversion ratio to restore the universal activity of elctro-catalyst
The problems such as, in highly selective CO2There are great potential and bright prospects in green conversion.
Technical scheme is as follows:
A kind of Au-Ag/Ag2S hetero-junctions nanometer electrical catalyst grows Ag in its surface extension using Au nanoparticle as core
Nanoshells, using Au-Ag nano material as skeleton, loaded Ag2S nanostructure, the Au-Ag/Ag2S hetero-junctions nano electro-catalytic
Agent at least some dimension is within the scope of 0.1~999.9nm.
In one embodiment, the Au-Ag/Ag2S hetero-junctions nanometer electrical catalyst nanorod length is 90-110nm.
In one embodiment, the Au-Ag/Ag2Its transmission electron microscope picture of S hetero-junctions nanometer electrical catalyst such as 1 institute of attached drawing
Show.
In one embodiment, the Au-Ag/Ag2Its High-Resolution Map of S hetero-junctions nanometer electrical catalyst is as shown in Fig. 2.
In one embodiment, the Au-Ag/Ag2S hetero-junctions nanometer electrical catalyst at least some dimension 0.1~
Within the scope of 999.9nm, refer to the Au-Ag/Ag in transmission electron microscope picture2S hetero-junctions nanometer electrical catalyst length and width or height (or
Thickness) it is 0.1~999.9nm.
Another method of the present invention provides Au-Ag/Ag2S hetero-junctions nanometer electrical catalyst restores CO2Method, toward response matrix
Solution is passed through CO2, with heterojunction nanometer material Au-Ag/Ag2S is catalyst, and the following voltage of application -1.0V is in response matrix liquid
Restore CO2For carbon compound.
In some embodiments, the solute of the response matrix solution is KOH, NaOH, KHCO3、NaHCO3、K2CO3Or
Na2CO3At least one of, the solvent of response matrix liquid is water, acetonitrile or its mixture.
Further, the voltage value is using standard hydrogen electrode as reference.
Methanol and ethanol content are 90% or more in the carbon compound.
The faradic efficiency of ethyl alcohol is up to 70% in the carbon compound.
In some embodiments, CO is carried out using the catalyst2Specific step is as follows for electrochemical reduction:
Step 1) is by Au-Ag/Ag2S heterojunction nanometer material is assembled in different substrate surfaces and constitutes working electrode；
Response matrix solution is added in step 2) electrolytic cell, is put into load Au-Ag/Ag2S working electrode and suitable reference
Electrode and to electrode, connects electrochemical workstation；
Step 3) is passed through CO into response matrix solution2Gas；
Step 4) applies voltage and promotes CO2Reduction reaction occurs in catalyst surface
In some embodiments, described to be passed through CO into response matrix solution2Gas leads to CO2The rate of gas be 10~
60mL/min；The voltage is -0.4V~-1.0V.
The present invention utilizes above-mentioned Au-Ag/Ag2S material is as CO2Elctro-catalyst is restored, is big based on possessing in such material
Metal/semiconductor interfacial activity site is measured, can be effectively facilitated between reaction molecular and nanocatalyst during the reaction
Electron-transport efficiency reduces CO2The reaction energy barrier converted to alcohol product, and then improve the activity and selectivity of catalyst.
Compared with prior art, the invention has the advantages that and the utility model has the advantages that
1) in the present invention, hetero-junctions nanocatalyst Au-Ag/Ag2Promote CO to the metal/semiconductor interface selective of S2
It is converted to alcohol product, wherein methanol and ethanol content are 90% or more, and the faradic efficiency of ethyl alcohol can reach 70% or more.
2) reaction condition of the invention is mild, easy to operate, favorable reproducibility, has good economic benefit and Environmental Effect
Benefit.
Figure of description
Fig. 1 is Au-Ag/Ag made from embodiment 12The transmission electron microscope picture of S hetero-junctions nanocatalyst；
Fig. 2 is Au-Ag/Ag made from embodiment 12The High-Resolution Map of S hetero-junctions nanocatalyst；
Fig. 3 is that Au-Ag/Ag is made in embodiment 12The Elemental redistribution scanning figure of S；
Fig. 4 is the Au-Ag/Ag assembled with 1cm*1cm FTO conductive glass surface2S hetero-junctions nanocatalyst is work
Electrode carries out scan round voltammogram in -0.8V~-0.4V range with the speed of sweeping of 50mV/s, and curve A expression is passed through argon gas
Scan round volt；Curve B indicates the scan round volt for being passed through argon gas；
Fig. 5 be using 1cm*1cm FTO conductive glass surface assemble using different catalysts as working electrode, -0.9V~-
Linear scan voltammogram within the scope of 0.4V.
Specific embodiment
Below by embodiment, the present invention will be further described.
The hetero-junctions nanocatalyst that laboratory independently synthesizes is assembled in 1cm*1cm FTO conductive glass surface by embodiment
As working electrode, respectively using Ag/AgCl electrode and carbon-point as reference electrode and to electrode, carried out in response matrix solution
Electro-chemical test is to evaluate catalyst performance.
Embodiment 1 prepares Au-Ag/Ag2S hetero-junctions nanocatalyst
(1) 90mg polyvinylpyrrolidone (K30), 620mg cetyl trimethyl are added in polytetrafluoroethyllining lining
The silver nitrate and 8.6mL water that gold chloride that 450 μ L of ammonium chloride, concentration are 48.56mM, 1000 μ L concentration are 102mM stir 4min
It is uniformly mixed it and obtains mixed solution；
(2) mixed solution that step (1) obtains is placed in water heating kettle, after water heating kettle and liner sealing, is filled with gas
It is 0.8Mpa by initial pressure set, by the reaction temperature control of water heating kettle at 200 DEG C, the hydro-thermal reaction time is controlled in 20h, is obtained
To the preferable Ag-Au-Ag hetero-junctions nanometer rods of dispersion degree；
(3) it is cooled to room temperature after reaction to step (2), Ag-Au-Ag hetero-junctions nanometer rods is taken out, through centrifuge washing 3
It is scattered in after secondary in 6mL water and obtains Ag-Au-Ag hetero-junctions nanometer rods dispersion liquid；
(4) take step (3) Ag-Au-Ag hetero-junctions nanometer rods dispersion liquid 6mL that the 0.02M Na of 16 μ L is added2S aqueous solution pair
Its surface is vulcanized, and shaggy Au-Ag/Ag is obtained2S hetero-junctions nanocatalyst (Fig. 1)；It is available by Fig. 1,
Au-Ag/Ag2S hetero-junctions nanocatalyst length is in 90~110nm, and monodispersity is good, and particle size distribution is uniform.Wherein, Au
Nano particle diameter is 20nm-30nm, Ag nanoshells with a thickness of 90-110nm, and the Ag of molecular level2S is dispersed in
The surface Ag.
2 Au-Ag/Ag of embodiment2S hetero-junctions nano electro-catalytic CO2The method of reduction
(1) in 0.5M KHCO3CO is led to uninterruptedly with the rate of 10~60mL/min in solution2Gas, with 1cm*1cm FTO
The Au-Ag/Ag of conductive glass surface assembling2S hetero-junctions nanocatalyst be working electrode, in -0.3V~-1.0V range with
The speed of sweeping of 50mV/s carries out linear sweep voltammetry test；
(2) experiment shows Au-Ag/Ag2S has superior electro-catalysis CO2Reduction activation, the current density at -0.95V
Reach -310mA/mg；
(3) amount of ethyl alcohol and methanol is respectively 300 in the carbonaceous products that application -0.95V potential electrolysis is collected into after 1 hour
μm ol/ (h*mg) and 520 μm of ol/ (h*mg), wherein the faradic efficiency of ethyl alcohol is about 70%
3 Au-Ag/Ag of embodiment2S hetero-junctions nano electro-catalytic CO2The method of reduction
(1) in 0.5M NaHCO3CO is led to uninterruptedly with the rate of 10~60mL/min in solution2Gas, with 1cm*1cm
The Au-Ag/Ag of FTO conductive glass surface assembling2S hetero-junctions nanocatalyst is working electrode, in -0.3V~-1.0V range
It is interior that linear sweep voltammetry test is carried out with the speed of sweeping of 50mV/s；
(2) amount of ethyl alcohol and methanol is respectively 180 in the carbonaceous products that application -0.75V potential electrolysis is collected into after 1 hour
μm ol/ (h*mg) and 670 μm of ol/ (h*mg), wherein the faradic efficiency of ethyl alcohol is about 50%.
4 Au-Ag/Ag of embodiment2S hetero-junctions nano electro-catalytic CO2The method of reduction
(1) in 0.5M KHCO3CO is led to uninterruptedly with the rate of 10~60mL/min in solution2Gas, with 1cm*1cmFTO
It is working electrode that the Ag nano wire of conductive glass surface assembling, which is catalyst, the sweeping with 50mV/s in -0.3V~-1.0V range
Speed carries out linear sweep voltammetry test；
(2) experiment shows that Ag nano wire has electro-catalysis CO2Reduction activation, current density at -0.95V is -
120mA/mg；
(3) in the liquid carbonaceous products being collected into after application -0.4V~0.95V free voltage range Inner electrolysis 1 hour
Ethyl alcohol is not detected, illustrates Au-Ag/Ag2S electro-catalysis CO2The generation of ethyl alcohol is due to caused by metal/semiconductor interface in reduction.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (9)
1. a kind of Au-Ag/Ag2S hetero-junctions nanometer electrical catalyst grows Ag nanometers in its surface extension using Au nanoparticle as core
Shell, using Au-Ag nano material as skeleton, loaded Ag2S nanostructure, the Au-Ag/Ag2S hetero-junctions nanometer electrical catalyst is extremely
Some few dimension is within the scope of 0.1~999.9nm.
2. Au-Ag/Ag described in claim 12S hetero-junctions nanometer electrical catalyst, it is characterised in that the Au-Ag/Ag2S hetero-junctions
Nanometer electrical catalyst nanorod length is 90-110nm.
3. Au-Ag/Ag described in claim 12S hetero-junctions nanometer electrical catalyst, it is characterised in that the Au nano particle diameter is
20nm-30nm, Ag nanoshells with a thickness of 90-110nm.
4. Au-Ag/Ag described in claim 12S hetero-junctions nanometer electrical catalyst, it is characterised in that its transmission electron microscope picture such as attached drawing 1
It is shown.
5. Au-Ag/Ag described in claim 12S hetero-junctions nanometer electrical catalyst, it is characterised in that its High-Resolution Map such as 2 institute of attached drawing
Show.
6. any Au-Ag/Ag of claim 1-52S hetero-junctions nanometer electrical catalyst restores CO2Method, it is characterised in that
CO is passed through toward response matrix solution2, with heterojunction nanometer material Au-Ag/Ag2S is catalyst, application -0.4V to -1.0V voltage
CO is restored in response matrix liquid2For carbon compound.
7. method as claimed in claim 6, which is characterized in that the solute of the response matrix liquid is KOH, NaOH, KHCO3、
NaHCO3、K2CO3Or Na2CO3At least one of, the solvent of response matrix liquid is water, acetonitrile or its mixture.
8. method as claimed in claim 6, the specific steps are that:
1) by Au-Ag/Ag2S heterojunction nanometer material is assembled in different substrate surfaces and constitutes working electrode；
2) response matrix solution is added in electrolytic cell, is put into load Au-Ag/Ag2S working electrode and reference electrode and to electrode, even
Connect electrochemical workstation；
3) CO is passed through into response matrix solution2Gas；
4) apply voltage and promote CO2Reduction reaction occurs in catalyst surface.
9. method according to claim 8, step 3) is described to be passed through CO into response matrix solution2Gas leads to CO2The speed of gas
Rate is 10~60mL/min；The voltage is -0.4V to -1.0V.
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| US11717809B2 (en) | 2020-08-24 | 2023-08-08 | Honda Motor Co., Ltd. | Metal-semiconductor hybrid structures, syntheses thereof, and uses thereof |
| US12083505B2 (en) | 2020-08-24 | 2024-09-10 | Hondan Motor Co., Ltd. | Metal-semiconductor hybrid structures, syntheses thereof, and uses thereof |
| CN113106472A (en) * | 2021-04-01 | 2021-07-13 | 南京理工大学 | For photoelectrocatalysis of CO2Super-structure plane photoelectrode for reduction reaction mechanism research |
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