CN110075890A - A kind of bimetallic layered hydroxide chelating Ti3C2Compound and its preparation method and application - Google Patents
A kind of bimetallic layered hydroxide chelating Ti3C2Compound and its preparation method and application Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 229910009819 Ti3C2 Inorganic materials 0.000 claims abstract description 37
- 239000003054 catalyst Substances 0.000 claims abstract description 34
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000001257 hydrogen Substances 0.000 claims abstract description 19
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 19
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 8
- 238000005119 centrifugation Methods 0.000 claims abstract description 8
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims abstract description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 28
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 14
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 12
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 229910052697 platinum Inorganic materials 0.000 claims description 7
- 229910009818 Ti3AlC2 Inorganic materials 0.000 claims description 5
- 229940011182 cobalt acetate Drugs 0.000 claims description 5
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 5
- 239000013049 sediment Substances 0.000 claims description 5
- 229920000557 Nafion® Polymers 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- 206010013786 Dry skin Diseases 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 241000040710 Chela Species 0.000 claims 1
- 230000005611 electricity Effects 0.000 claims 1
- 238000012986 modification Methods 0.000 claims 1
- 230000004048 modification Effects 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 229910052742 iron Inorganic materials 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 239000010941 cobalt Substances 0.000 abstract 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 9
- 238000004502 linear sweep voltammetry Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- QVYYOKWPCQYKEY-UHFFFAOYSA-N [Fe].[Co] Chemical compound [Fe].[Co] QVYYOKWPCQYKEY-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 description 1
- 229910002546 FeCo Inorganic materials 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- 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
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- Chemical Kinetics & Catalysis (AREA)
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- Inorganic Chemistry (AREA)
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Abstract
The present invention discloses a kind of bimetallic layered hydroxide chelating Ti3C2- MXene catalyst and its preparation method and application, is related to electrochemical technology field.A kind of bimetallic layered hydroxide chelating Ti3C2The preparation method of-MXene catalyst includes the following steps: with Ti3AlC2- MAX is raw material, with LiF+HCl stripping method, obtains Ti3C2-MXene.By the hydroxide and Ti of iron and cobalt3C2- MXene mixing, under Ar gas shielded, heats 120 DEG C of holding 3h, obtains FeCo-LDH/Ti by centrifugation and 60 DEG C of vacuum drying3C2-MXene.The present invention prepares bimetallic stratiform hydroxide composite safety easy to operate, to load FeCo-LDH/Ti3C2The glass-carbon electrode of-MXene compound is working electrode, studies electro-catalysis cathode water oxygen liberation of hydrogen process, take-off potential is lower, and hydrogen generating quantity is larger.
Description
Technical field
The invention belongs to electro-catalysis fields, and specially iron cobalt layered hydroxide chelating is in two-dimensional layer Ti3C2On-MXene
Obtain FeCo-LDH/Ti3C2Electro-catalysis cathode hydrogen evolution effect can be improved in-MXene material.
Background technique
Become a hot topic and important problem in the Efficient Conversion of the contemporary society that the energy is increasingly in short supply, the energy.Hydrogen quilt
It is considered a kind of clean energy resource of important substitute fossil fuels, can be made by electro-catalysis water-splitting.Pass through electro-catalysis
Mode electro-catalysis obtains hydrogen energy source, plays important facilitation to energy crisis is nowadays slowed down.However electro-catalysis obtains Hydrogen Energy
The process in source can face many problems, such as how to reach lower overpotential and higher electro-catalysis rate and how to overcome
Slow dynamics etc..Platinum is most effective catalyst in evolving hydrogen reaction.However the scarcity of platinum and high cost seriously hinder platinum
Extensive use in electrolytic cell hydrogen manufacturing.
MXene is a kind of novel two-dimentional early stage transition metal carbide/nitride, has excellent electrochemical energy storage
Energy, electronegativity and high electrical conductivity.In removing MAX (Ti3AlC2) during, Mn+1XnA atom between layer is by various functional groups
Replace, generating has hydroxyl, and oxygen or fluorin radical terminate the MXene nanometer sheet on surface in traditional two-dimensional atomic crystal such as graphite
This advantage is difficult to realize in alkene, stratiform transition metal dichalcogenide (LTMD) and double-metal hydroxide (LDH).Therefore,
MXene may be the excellent substitute of chemistry functional graphene, in conjunction with bimetallic layered hydroxide, rapid electric charge be added to turn
It moves, is coupled between strong interface, promote the catalysis course of electro-catalysis.
Summary of the invention
In order to solve the above-mentioned technical problem, an object of the present invention be by make the layered hydroxide of iron cobalt with
MXene is combined, and obtains FeCo-LDH/Ti3C2- MXene material.
The second object of the present invention is to by FeCo-LDH/Ti3C2- MXene material is led applied to electro-catalysis water dissociation technology
Domain has lower take-off potential and biggish hydrogen amount of precipitation in electro-catalysis cathode hydrogen evolution process, shows preferably to be catalyzed
Effect.
To achieve the goals above, the technical solution adopted by the present invention is that: a kind of bimetallic layered hydroxide chelating
Ti3C2- MXene catalyst, the bimetallic layered hydroxide chelate Ti3C2- MXene catalyst is FeCo-LDH/
Ti3C2-MXene。
A kind of above-mentioned bimetallic layered hydroxide chelates Ti3C2The preparation method of-MXene catalyst, including walk as follows
Suddenly,
1)Ti3C2The preparation of-MXene: by Ti3AlC2- MAX and LiF, mixed in hydrochloric acid, after 72-80h is stirred at room temperature, add
Ionized water, centrifugation, washes off impurity, takes lower sediment, deionized water is added into lower sediment, shake up, ultrasonic disperse, centrifugation,
Upper liquid is collected, is filtered, vacuum drying obtains Ti3C2- MXene powder；
2)FeCo-LDH/Ti3C2The preparation of-MXene: by Ti3C2- MXene powder is added in bimetallic aqueous slkali,
Ultrasonic disperse, the heating stirring 3h under Ar gas shielded, gained suspension obtain FeCo-LDH/Ti by centrifugation, vacuum drying3C2-
MXene compound.
Preferably, a kind of above-mentioned bimetallic layered hydroxide chelates Ti3C2The preparation method of-MXene catalyst, step
It is rapid 1) in, the ternary layered material MAX phase is Ti3AlC2。
A kind of bimetallic layered hydroxide chelating Ti stated3C2The preparation method of-MXene catalyst in step 1), is pressed
Matter liquor ratio, Ti3AlC2- MAX:LiF:HCl is 1g:1-5g:5-15mL.
Preferably, a kind of above-mentioned bimetallic layered hydroxide chelates Ti3C2The preparation method of-MXene catalyst, step
It is rapid 2) in, the bimetallic hydroxide solution is the potassium hydroxide solution for having iron chloride and cobalt acetate.
Preferably, a kind of above-mentioned bimetallic layered hydroxide chelates Ti3C2The preparation method of-MXene catalyst, step
It is rapid 2) in, by the mass ratio of the material, Fe:Co:KOH=0.5-1:1-5:5-10.
Preferably, a kind of above-mentioned bimetallic layered hydroxide chelates Ti3C2The preparation method of-MXene catalyst, step
It is rapid 2) in, by the mass ratio of the material, Fe:Co:KOH=0.5:2:6.
Preferably, a kind of above-mentioned bimetallic layered hydroxide chelates Ti3C2The preparation method of-MXene catalyst, step
It is rapid 2) in, the heating temperature be 120 DEG C.
A kind of above-mentioned bimetallic layered hydroxide chelates Ti3C2- MXene catalyst is in electro-catalysis cathode hydrogen evolution process
In application.
Above-mentioned application, the method is as follows:
1)FeCo-LDH/Ti3C2The preparation of-MXene modified electrode: by bimetallic stratiform hydroxide described in claim 1
Object chelates Ti3C2Catalyst is dispersed in the mixed liquor of dehydrated alcohol and Nafion, after ultrasonic disperse, is stirred to react 1- at room temperature
2h obtains suspension；By in suspended drop-coated to glass-carbon electrode, after 40 DEG C of dryings of baking oven, FeCo-LDH/Ti is obtained3C2- MXene is repaired
Adorn electrode；
2) with FeCo-LDH/Ti3C2- MXene modified electrode is working electrode, using platinum filament or platinum guaze as to electrode, with
Ag/AgCl is reference electrode, constitutes three-electrode system, electro-catalysis cathode hydrogen evolution.
The beneficial effects of the present invention are:
1, present invention preparation Ti3C2The method of-MXene, safety easy to operate, with Ti3AlC2- MAX is raw material, passes through stripping
From Al, washing centrifugation repeatedly, obtain upper liquid be in few layer of Ti3C2- MXene, method simple and effective.
2, FeCo-LDH/Ti prepared by the present invention3C2- MXene compound, Fe and Co bimetallic is with layered hydroxide
Form is carried on few layer of Ti3C2On-MXene, the bimetallic used is at low cost for iron chloride and cobalt acetate.
3, in the present invention, to load FeCo-LDH/Ti3C2The glass-carbon electrode of-MXene material is working electrode, in electro-catalysis
Cathode hydrogen evolution process has lower take-off potential and biggish hydrogen amount of precipitation, shows preferable catalytic effect.
Detailed description of the invention
Fig. 1 is the Ti prepared in example example 13C2The raw material Ti of-MXene3AlC2The scanning electron microscope (SEM) photograph (SEM) of-MAX.
Fig. 2 is the Ti prepared in embodiment 13C2The transmission electron microscope picture (TEM) of-MXene material.
Fig. 3 is the FeCo-LDH/Ti prepared in embodiment 13C2The scanning electron microscope (SEM) photograph (SEM) of-MXene composite material.
Fig. 4 is bimetallic layered hydroxide, Ti in embodiment 23C2- MXene, FeCo-LDH and FeCo-LDH/
Ti3C2The linear sweep voltammetry comparison diagram of-MXene compound.
Fig. 5 is FeCo-LDH/Ti in embodiment 23C2The I-t relational graph of-MXene and FeCo-LDH.
Specific embodiment
Below with reference to appended implementation legend detailed description of the present invention embodiment, this embodiment is in order to more clearly
Understand the present invention, but the present invention is not limited thereto embodiment.
Embodiment 1
(1) FeCo-LDH/Ti3C2The preparation of-MXene
Include the following steps:
1、Ti3C2The preparation of-MXene:
1) 0.2g Ti is weighed in 50mL centrifuge tube3AlC2- MAX is slowly added to 0.2g LiF and 98% hydrochloric acid 2ml, room
After temperature stirring 72h, deionized water is added, the reaction solution of acquisition is centrifuged (10000rpm, 10min) 6 times, abandons supernatant.
2) 40mL deionized water is added in the sediment into centrifuge tube, shakes up, is uniformly mixed precipitating with deionized water,
Centrifuge tube is put into ultrasonic disperse (750W, 10min) in large power supersonic machine, taking-up continues to be centrifuged (3500rpm, 10min) receipts
Collect upper liquid, filters vacuum drying, obtain few layer of Ti3C2-MXene。
2、FeCo-LDH/Ti3C2The preparation of-MXene
1) 0.0811g iron chloride, 0.531g cobalt acetate and 0.336g potassium hydroxide are weighed, 2mL deionization, ultrasound is added
Dissolution, obtains dispersion liquid.
2) it weighs 5mg and lacks layer Ti3C2- MXene powder is added in the resulting dispersion liquid of step 1).
3) the resulting solution of step 2) is uniformly mixed, pours into Shleck bottles, under Ar gas shielded, is stirred in 120 DEG C of heating
3h；Gained reactant is put into centrifuge tube, and centrifugation (9000 turns, 5min) is three times.Be put into vacuum oven, 60 DEG C of dryings for 24 hours,
Obtain powdered substance, as FeCo-LDH/Ti3C2- MXene catalyst.
(2) it detects
1, Fig. 1 Ti3AlC2The scanning electron microscope (SEM) photograph of-MAX, as seen from Figure 1 Ti3AlC2The visible layer structure in the section-MAX.
2, Fig. 2 is the Ti of few layer3C2The transmission electron microscope picture of-MXene, from Figure 2 it can be seen that the Ti prepared in the present invention3C2-
MXene is very thin single layer flaky substance.
3, Fig. 3 is the FeCo-LDH/Ti of preparation3C2The scanning electron microscope (SEM) photograph of-MXene material, as seen from Figure 3, few layer
Ti3C2The area load of-MXene sheet FeCo bimetallic layered hydroxide.
Comparative example 1
(1) preparation of FeCo-LDH catalyst
0.0811g iron chloride, 0.531g cobalt acetate and 0.3361g potassium hydroxide are weighed, 2mL deionized water, Ar gas is added
120 DEG C are heated in atmosphere, keep 3h；Gained reactant is put into centrifuge tube, is centrifuged (9000 turns, 5min) three times, repeatedly with water
Washing.It is put into freeze drier freezing, obtains powdered substance FeCo-LDH.
The influence that 2 different modifying electrode of embodiment aoxidizes electro-catalysis anode water
(1) prepared by electrode
The FeCo-LDH/Ti for taking 4mg embodiment 1 to prepare respectively3C2- MXene powder, Ti3C2- MXene powder and comparative example
The FeCo-LDH and Co (OH) of 1 preparation2Catalyst is separately added into 995 μ l dehydrated alcohols and 5 μ l Nafion, ultrasonic disperse
5min stirs 1h.Gained mixed liquor is shifted on 5 μ l to glass-carbon electrode with liquid-transfering gun respectively, dry under room temperature, is evaporated completely solvent
Entirely, the glass-carbon electrode of coating different materials is obtained.
(2) chemical property detects
All tests of this experiment are all made of the CHI660E electrochemical workstation of Shanghai Chen Hua company.
The speed of rotation for detecting linear sweep voltammetry (LSV) is 1600rpm, and sweep speed is 10mV s-1.To coat difference
The glass-carbon electrode of catalyst is working electrode, and Pt are used as to electrode, and Ag/AgCl is that reference electrode is constituted in H-type electrolytic cell
Three-electrode system.Electro-chemical test is carried out, test results are shown in figure 4.It is all in the present invention to measure on Ag/AgCl electrode
Current potential, according to Evs RHE=Evs Ag/AgCl+ 0.059pH+0.198 is converted to the current potential relative to RHE.
Fig. 4 is Evs Ag/AgClLinear sweep voltammetry figure between -1.0V--1.8V, it is different at four kinds as seen from the figure
Catalyst Fe Co-LDH/Ti3C2-MXene,FeCo-LDH,Co(OH)2,Ti3C2The take-off potential E of-MXenevs Ag/AgClRespectively
Are as follows: -0.24V, -0.40V, -0.52V, -0.53V, FeCo-LDH/Ti3C2The take-off potential of-MXene is minimum, is Evs Ag/AgCl
=-0.24V, FeCo-LDH/Ti in four kinds of catalyst3C2The E of-MXeneJ=10mA cm-2Minimum-the 0.35V of voltage.Identical
Under voltage, FeCo-LDH/Ti3C2The highest current density of-MXene, hydrogen generating quantity is maximum, therefore best performance is got over.
3 FeCo-LDH/Ti of embodiment3C2- MXene is tested as the catalytic stability of catalytic hydrogen evolution material
(1) preparation of electrode
The FeCo-LDH/Ti for taking 4mg embodiment 1 to prepare respectively3C2FeCo-LDH prepared by-MXene powder and comparative example 1,
995 μ l dehydrated alcohols and 5 μ l Nafion, ultrasonic disperse 5min are separately added into, 1h is stirred.Gained mixed liquor uses liquid-transfering gun respectively
It shifts on 5 μ l to glass-carbon electrode, it is dry under room temperature, make solvent volatilization completely, obtains FeCo-LDH/Ti3C2- MXene modified electrode
With FeCo-LDH modified electrode.
(3) electrochemical property test
Respectively to obtain FeCo-LDH/Ti3C2- MXene modified electrode and FeCo-LDH modified electrode are as working electrode, Pt
Silk is as to electrode, and Ag/AgCl is that reference electrode constitutes three-electrode system, using the KOH solution of 1M as electrolyte, in CHI
On 760D electrochemical workstation using standard three electrode system in H-type electrolytic cell, elctro-catalyst is assessed in 1M KOH to yin
Pole Hydrogen Evolution Performance effect.As a result as shown in figure 5, the speed of rotation, sweep speed of the linear sweep voltammetry (LSV) in 1600rpm are
10mV s-1It is measured.All current potentials measured on Ag/AgCl electrode in the present invention, according to Evs RHE=Evs Ag/AgCl+
0.059pH+0.198 is converted to the current potential relative to RHE.
Fig. 5 is that voltage is set as Evs Ag/AgClWhen for -1.4V, FeCo-LDH and FeCo-LDH/Ti3C2The time of-MXene
(t) with the relationship image of electric current (i), as seen from Figure 5, under identical voltage, with FeCo-LDH/Ti3C2- MXene is catalyst
Electric current is larger, and electric current is more stable, illustrates that the durability of catalyst is relatively good.
Claims (10)
1. a kind of bimetallic layered hydroxide chelates Ti3C2- MXene catalyst, which is characterized in that the bimetallic stratiform
Hydroxide chelates Ti3C2- MXene catalyst is FeCo-LDH/Ti3C2-MXene。
2. a kind of bimetallic layered hydroxide described in claim 1 chelates Ti3C2The preparation method of-MXene catalyst,
It is characterized in that, includes the following steps,
1)Ti3C2The preparation of-MXene: by MAX phase and LiF, mixed in hydrochloric acid, after 72-80h is stirred at room temperature, adding deionized water, from
The heart washes off impurity, takes lower sediment, and deionized water is added into lower sediment, shakes up, ultrasonic disperse, and upper layer is collected in centrifugation
Liquid filters, and vacuum drying obtains Ti3C2- MXene powder；
2)FeCo-LDH/Ti3C2The preparation of-MXene: by Ti3C2- MXene powder is added in bimetallic aqueous slkali, ultrasound point
It dissipates, the heating stirring 3h under Ar gas shielded, gained suspension obtains FeCo-LDH/Ti by centrifugation, vacuum drying3C2- MXene is multiple
Close object.
3. a kind of bimetallic layered hydroxide according to claim 2 chelates Ti3C2The preparation side of-MXene catalyst
Method, which is characterized in that in step 1), the ternary layered material MAX phase is Ti3AlC2-MAX。
4. a kind of bimetallic layered hydroxide according to claim 3 chelates Ti3C2The preparation side of-MXene catalyst
Method, which is characterized in that in step 1), by matter liquor ratio, Ti3AlC2The HCl of-MAX:LiF:98% is 1g:1-5g:5-15mL.
5. a kind of bimetallic layered hydroxide according to claim 2 chelates Ti3C2The preparation side of-MXene catalyst
Method, which is characterized in that in step 2), the bimetallic hydroxide solution is that have the potassium hydroxide of iron chloride and cobalt acetate molten
Liquid.
6. a kind of bimetallic layered hydroxide according to claim 5 chelates Ti3C2The preparation side of-MXene catalyst
Method, which is characterized in that in step 2), by the mass ratio of the material, Fe:Co:KOH=0.5-1:1-5:5-10.
7. a kind of bimetallic layered hydroxide according to claim 6 chelates Ti3C2The preparation side of-MXene catalyst
Method, which is characterized in that in step 2), by the mass ratio of the material, Fe:Co:KOH=0.5:2:6.
8. a kind of bimetallic layered hydroxide according to claim 2 chelates Ti3C2The preparation side of-MXene catalyst
Method, which is characterized in that in step 2), the heating temperature is 120 DEG C.
9. a kind of bimetallic layered hydroxide described in claim 1 chelates Ti3C2- MXene catalyst is analysed in electro-catalysis cathode
Application during hydrogen.
10. application according to claim 9, which is characterized in that method is as follows:
1)FeCo-LDH/Ti3C2The preparation of-MXene modified electrode: by bimetallic layered hydroxide chela described in claim 1
Close Ti3C2Catalyst is dispersed in the mixed liquor of dehydrated alcohol and Nafion, after ultrasonic disperse, is stirred to react 1-2h at room temperature, is obtained
Suspension；By in suspended drop-coated to glass-carbon electrode, after 40 DEG C of dryings of baking oven, FeCo-LDH/Ti is obtained3C2- MXene modification electricity
Pole；
2) with FeCo-LDH/Ti3C2- MXene modified electrode is working electrode, using platinum filament or platinum guaze as to electrode, with Ag/
AgCl is reference electrode, constitutes three-electrode system, electro-catalysis cathode hydrogen evolution.
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