CN110474062A - A kind of preparation and application of efficient MXene titanium carbide cell catalyst - Google Patents
A kind of preparation and application of efficient MXene titanium carbide cell catalyst Download PDFInfo
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/96—Carbon-based electrodes
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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
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- 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
- Y02E60/50—Fuel cells
Abstract
The invention reside in the cell catalyst for preparing a kind of efficient MXene titanium carbide, the present invention is used for zinc-air battery electrode catalyst.The catalyst use titanizing carbon (MXene), ZIF-67 and hexachlorocyclotriph,sphazene and to hydroxyl diphenyl sulphone (DPS) synthesis PZS for raw material, preparation method is first by Ti3AlC2The MXene of class grapheme material is generated in hydrochloric acid and lithium fluoride solution, cabaltous nitrate hexahydrate and methylimidazole is successively added in MXene solution later, ZIF-67 is generated in MXene surface in situ, and then doping PZS microballoon, a kind of high performance catalyst of Heteroatom doping is generated after final high temperature carbonization, the method of the present invention is simple, the catalyst of preparation has good electric conductivity, and large specific surface area has important value and meaning in the carbon-based oxygen reduction electro-catalyst field of Heteroatom doping.
Description
Technical field
The invention belongs to fuel cell electro-catalysis fields, and in particular to preparing a kind of modified two-dimensional material MXenes carbonization
The cell catalyst of titanium.
Background technique
Fuel cell is the 4th kind of new-generation technology after hydroelectric generation, heat energy power-generating and nuclear electric power generation,
It is middle application and research field it is most commonly used be hydrogen-oxygen fuel cell.Oxidation reaction and reduction reaction are respectively in hydrogen-oxygen fuel cell
Anode and cathode occur, for the hydrogen reduction of the hydroxide and cathode of accelerating anode, be equipped with contain in anode and cathode respectively
The catalyst of platinum, since content is less in earth resource and involves great expense for platinum metals, therefore the extensive quotient of such catalyst
Industry production is not real enough, in this case, develops low platinum or is just provided with critically important development meaning without platinum catalyst.
MXene is a kind of novel two-dimensional material with class graphene-structured, chemical formula Mn+1XnTx, wherein n=
1,2,3, M is early transition metal element (such as Ti, Sc, Zr, Nb etc.), and X is carbon or/and nitrogen, TxFor surface functional group (as-
OH ,-O ,-F).The presoma MAX phase of MXene is a kind of ternary layered compound, is provided simultaneously with the excellent spy of ceramics and metal
Property, chemical formula Mn+1AXn, wherein M, X, n is same as described above, and A is III or IV major element.At present by the method for etching
More than 20 kinds of MXene, including Ti are prepared3C2Tx, Ti2CTx, Nb4C3TxDeng wherein Ti3C2TxIt is that the first is prepared out
MXene, and most deep supercapacitor, lithium ion battery, Dye Adsorption, the biology of most widely can be applied to of research at present pass
The two-dimensional material of sensor etc..
Poly phosphazene nano material as it is a kind of rich in there is the heteroatomic mutual hydridization of novel organic/inorganic such as N, P, S and
At high molecular material, be more commonly used for pharmaceutical carrier, sensor, electrochemical catalysis etc., especially make
There is huge potential using value in catalytic field for catalyst carrier.
ZIFs is zeolite imidazole ester frame structure material, and in this special structure, imidazoles is connected to transition metal
On, the structure that imidazate includes transition metal is formed, this cage structure has biggish specific surface area, is carbonized it at high temperature
Afterwards, the structure that just will form carbon-nitrogen doped material cladding transition metal, meets the optimum structure of elctro-catalyst just.
Transition metal iron, cobalt, nickel are a kind of materials for being most expected to replace business platinum catalyst at present at present, because its content is rich
The advantages that richness, catalytic activity are high, inexpensive and cause global concern, transient metal sulfide, phosphide, nitride and
Transition metal hydroxide presents excellent characteristic in terms of electro-catalysis.By way of in-situ polymerization, gather between MXene film
Close PZS polyphosphazene, make it have excellent electrochemical performance after high temperature cabonization, the synergistic effect between them improve electronics flowing and
Mass transfer, this is exactly electrochemical structure excellent in electrochemical catalysis.
Summary of the invention
A solution proposed the present invention be directed to some problems existing for current fuel-cell catalyst, at this
MXene thin layer is prepared by hydrochloric acid and lithium fluoride in-situ preparation hydrofluoric acid selective etch in invention, passes through in-situ preparation
ZIF-67 loads MXene, then adulterates PZS in MXene/ZIF, generates MXene/ZIF/PZS, prepares after high temperature cabonization a kind of high
The catalyst of performance.
The technology that the present invention uses is as follows:
(1) MXene is prepared using the method for selective etch,
(2) it is constantly centrifuged and adjusts pH to neutrality, stable black is collected by centrifugation in the black product collected after ultrasonic
Colloid upper liquid, the blackish green liquid in upper layer are single layer MXene, and lower part is precipitated as multilayer.By the way of suction filtration, collection is obtained
MXene film.The film being collected into is dry.
(3) the MXene sample after taking drying is dissolved in dimethyl sulfoxide under ultrasound condition, six nitric hydrates added
Cobalt, 2-methylimidazole after ultrasonic dissolution, are placed under magnetic agitation and stir, centrifugal drying obtains MXene/ZIF.
(4) it takes MXene/ZIF obtained above to be dissolved in methanol solution, adds hexachlorocyclotriph,sphazene and 4,4- is to two
Hydroxyl diphenyl sulphone (DPS), is added dropwise triethylamine solution dropwise under stiring, and stirring generates MXene/ZIF/PZS.
(5) by the MXene/ZIF/PZS film of synthesis, high-temperature calcination is handled under nitrogen atmosphere.To improve its electrocatalysis
Can, so that preparation has the elctro-catalyst of excellent properties.
Preferably, it takes dry MXene sample to be dissolved in dimethyl sulfoxide under ultrasound condition, then adds by different proportion
Enter cabaltous nitrate hexahydrate, 2-methylimidazole after ultrasonic dissolution, is placed under magnetic agitation and stirs.
Preferably, the MXene/ZIF sample after taking drying is dissolved in methanol under ultrasound condition, is separately added by different proportion
Enter hexachlorocyclotriph,sphazene and 4,4- is added dropwise triethylamine to dihydroxydiphenylsulisomer dropwise, stirs to get MXene/ZIF/PZS.
Preferably, the carbonization technique of film are as follows: heating rate is 5 DEG C/min, and carburizing temperature is 700 DEG C -900 DEG C, carbonization
Time is 1-2h.
Modified MXene film, which can be used as oxygen reduction catalyst, to be come using need to be changed with this when testing its chemical property
Property after MXene membrane material modification glass-carbon electrode as working electrode, calomel electrode and platinum electrode are respectively as reference electrode
With to electrode, constitutes three-electrode system and tested.Electrolyte then uses the KOH solution of 0.1M.
Catalyst of the invention is used for fuel battery negative pole oxygen reduction reaction elctro-catalyst, with document report phase before
Than having the advantages that
(1) due to planar forming new complicated active site, metal Co, Co-NxComplex compound and CoOxSubstance coexists
It may be conductive to catalytic activity.Wherein, Co-NxCenter can reduce oxygen absorption energy and extend O -- O bond to activate ORR
Process.Meanwhile CoOxSpecies and metal Co facilitate electrochemical catalysis.
(2) a large amount of defects that the doping of N, P element generate will increase catalytic activity, and active site is more.Therefore, abundant
Pyridine-N and graphite can not only promote ORR performance, can also enhance the catalytic activity of N doping carbon material.
(3) this catalyst is derived from ZIF-67 and Ti3C2TxNanometer sheet, and the hetero atoms such as N, P are adulterated, it shows good
The nano particle of catalytic structure, formation is uniformly distributed, and appropriate partial size.It is all these to promote O2It is fast with electrolyte
Speed diffusion, so as to cause the fine dispersion and advantageous exposure in high activity site.Ti3C2The high electric conductivity of Tx nanometer sheet is advantageous
In the electronics transfer of catalytic process, accelerate catalytic process.
Detailed description of the invention:
Fig. 1 is the electron microscope of MXene
Fig. 2 is the section electron microscope for the MXene film collected
Specific embodiment
Embodiment 1
Prepare MXene.1g lithium fluoride and 9M 20mL hydrochloric acid stir 30min in tetrafluoroethene beaker.It is slowly added to 1g
MAX-Ti3AlC2, persistently stirred for 24 hours at 35 DEG C.With deionized water with the revolving speed of 3500rpm, be centrifuged repeatedly, until pH value extremely
It is neutral.Lower sediment thing is collected, is filtered, it is dry.
Prepare MXene/ZIF.It weighs 10mg MXene and ultrasonic disperse in the DMSO of 30mL is added, the cobalt nitrate of 2mM is molten
Above-mentioned solution is added in the dispersion liquid of the DMSO of MXene, then by the methylimidazole of 10mM in solution, and product is collected by centrifugation, uses first
Pure and mild deionized water washing three times, is dried in vacuo.
Take MXene/ZIF obtained above to be dissolved in methanol solution, in molar ratio 1:1 add hexachlorocyclotriph,sphazene and
4,4-, to dihydroxydiphenylsulisomer, are added dropwise triethylamine, are stirred for 18h.Obtain MXene/ZIF/PZS.
MXene/ZIF/PZS is risen to 700 DEG C in tube furnace nitrogen atmosphere with the heating rate of 5 DEG C/min, keeps the temperature 2h, from
So it is cooled to room temperature.
Embodiment 2
Prepare MXene.1g lithium fluoride and 9M 20mL hydrochloric acid stir 30min in tetrafluoroethene beaker.It is slowly added to 1g
MAX-Ti3AlC2, persistently stirred for 24 hours at 35 DEG C.With deionized water with the revolving speed of 3500rpm, be centrifuged repeatedly, until pH value extremely
It is neutral.Lower sediment thing is collected, is filtered, it is dry.
Prepare MXene/ZIF.It weighs 20mg MXene and ultrasonic disperse in the DMSO of 30mL is added, the cobalt nitrate of 2mM is molten
Above-mentioned solution is added in the dispersion liquid of the DMSO of MXene, then by the methylimidazole of 10mM in solution, and product is collected by centrifugation, uses first
Pure and mild deionized water washing three times, is dried in vacuo.
Take MXene/ZIF obtained above to be dissolved in methanol solution, in molar ratio 1:1 add hexachlorocyclotriph,sphazene and
4,4-, to dihydroxydiphenylsulisomer, are added dropwise triethylamine, are stirred for 18h.Obtain MXene/ZIF/PZS.
MXene/ZIF/PZS is risen to 700 DEG C in tube furnace nitrogen atmosphere with the heating rate of 5 DEG C/min, keeps the temperature 2h, from
So it is cooled to room temperature.
Embodiment 3
Prepare MXene.1g lithium fluoride and 9M 20mL hydrochloric acid stir 30min in tetrafluoroethene beaker.It is slowly added to 1g
MAX-Ti3AlC2, persistently stirred for 24 hours at 35 DEG C.With deionized water with the revolving speed of 3500rpm, be centrifuged repeatedly, until pH value extremely
It is neutral.Lower sediment thing is collected, is filtered, it is dry.
Prepare MXene/ZIF.It weighs 30mg MXene and ultrasonic disperse in the DMSO of 30mL is added, the cobalt nitrate of 2mM is molten
Above-mentioned solution is added in the dispersion liquid of the DMSO of MXene, then by the methylimidazole of 10mM in solution, and product is collected by centrifugation, uses first
Pure and mild deionized water washing three times, is dried in vacuo.
Take MXene/ZIF obtained above to be dissolved in methanol solution, in molar ratio 1:1 add hexachlorocyclotriph,sphazene and
4,4-, to dihydroxydiphenylsulisomer, are added dropwise triethylamine, are stirred for 18h.Obtain MXene/ZIF/PZS.
MXene/ZIF/PZS is risen to 700 DEG C in tube furnace nitrogen atmosphere with the heating rate of 5 DEG C/min, keeps the temperature 2h, from
So it is cooled to room temperature.
Embodiment 4
Prepare MXene.1g lithium fluoride and 9M 20mL hydrochloric acid stir 30min in tetrafluoroethene beaker.It is slowly added to 1g
MAX-Ti3AlC2, persistently stirred for 24 hours at 35 DEG C.With deionized water with the revolving speed of 3500rpm, be centrifuged repeatedly, until pH value extremely
It is neutral.Lower sediment thing is collected, is filtered, it is dry.
Prepare MXene/ZIF.It weighs 40mg MXene and ultrasonic disperse in the DMSO of 30mL is added, the cobalt nitrate of 2mM is molten
Above-mentioned solution is added in the dispersion liquid of the DMSO of MXene, then by the methylimidazole of 10mM in solution, and product is collected by centrifugation, uses first
Pure and mild deionized water washing three times, is dried in vacuo.
Take MXene/ZIF obtained above to be dissolved in methanol solution, in molar ratio 1:1 add hexachlorocyclotriph,sphazene and
4,4-, to dihydroxydiphenylsulisomer, are added dropwise triethylamine, are stirred for 18h.Obtain MXene/ZIF/PZS.
MXene/ZIF/PZS is risen to 700 DEG C in tube furnace nitrogen atmosphere with the heating rate of 5 DEG C/min, keeps the temperature 2h, from
So it is cooled to room temperature.
Embodiment 5
Prepare MXene.1g lithium fluoride and 9M 20mL hydrochloric acid stir 30min in tetrafluoroethene beaker.It is slowly added to 1g
MAX-Ti3AlC2, persistently stirred for 24 hours at 35 DEG C.With deionized water with the revolving speed of 3500rpm, be centrifuged repeatedly, until pH value extremely
It is neutral.Lower sediment thing is collected, is filtered, it is dry.
Prepare MXene/ZIF.It weighs 40mg MXene and ultrasonic disperse in the DMSO of 30mL is added, the cobalt nitrate of 2mM is molten
Above-mentioned solution is added in the dispersion liquid of the DMSO of MXene, then by the methylimidazole of 10mM in solution, and product is collected by centrifugation, uses first
Pure and mild deionized water washing three times, is dried in vacuo.
Take MXene/ZIF obtained above to be dissolved in methanol solution, in molar ratio 1:2 add hexachlorocyclotriph,sphazene and
4,4-, to dihydroxydiphenylsulisomer, are added dropwise triethylamine, are stirred for 18h.Obtain MXene/ZIF/PZS.
MXene/ZIF/PZS is risen to 700 DEG C in tube furnace nitrogen atmosphere with the heating rate of 5 DEG C/min, keeps the temperature 2h, from
So it is cooled to room temperature.
Embodiment 6
Prepare MXene.1g lithium fluoride and 9M 20mL hydrochloric acid stir 30min in tetrafluoroethene beaker.It is slowly added to 1g
MAX-Ti3AlC2, persistently stirred for 24 hours at 35 DEG C.With deionized water with the revolving speed of 3500rpm, be centrifuged repeatedly, until pH value extremely
It is neutral.Lower sediment thing is collected, is filtered, it is dry.
Prepare MXene/ZIF.It weighs 40mg MXene and ultrasonic disperse in the DMSO of 30mL is added, the cobalt nitrate of 2mM is molten
Above-mentioned solution is added in the dispersion liquid of the DMSO of MXene, then by the methylimidazole of 10mM in solution, and product is collected by centrifugation, uses first
Pure and mild deionized water washing three times, is dried in vacuo.
Take MXene/ZIF obtained above to be dissolved in methanol solution, in molar ratio 1:3 add hexachlorocyclotriph,sphazene and
4,4-, to dihydroxydiphenylsulisomer, are added dropwise triethylamine, are stirred for 18h.Obtain MXene/ZIF/PZS.
MXene/ZIF/PZS is risen to 700 DEG C in tube furnace nitrogen atmosphere with the heating rate of 5 DEG C/min, keeps the temperature 2h, from
So it is cooled to room temperature.
Embodiment 7
Prepare MXene.1g lithium fluoride and 9M 20mL hydrochloric acid stir 30min in tetrafluoroethene beaker.It is slowly added to 1g
MAX-Ti3AlC2, persistently stirred for 24 hours at 35 DEG C.With deionized water with the revolving speed of 3500rpm, be centrifuged repeatedly, until pH value extremely
It is neutral.Lower sediment thing is collected, is filtered, it is dry.
Prepare MXene/ZIF.It weighs 40mg MXene and ultrasonic disperse in the DMSO of 30mL is added, the cobalt nitrate of 2mM is molten
Above-mentioned solution is added in the dispersion liquid of the DMSO of MXene, then by the methylimidazole of 10mM in solution, and product is collected by centrifugation, uses first
Pure and mild deionized water washing three times, is dried in vacuo.
Take MXene/ZIF obtained above to be dissolved in methanol solution, in molar ratio 1:3 add hexachlorocyclotriph,sphazene and
4,4-, to dihydroxydiphenylsulisomer, are added dropwise triethylamine, are stirred for 18h.Obtain MXene/ZIF/PZS.
MXene/ZIF/PZS is risen to 800 DEG C in tube furnace nitrogen atmosphere with the heating rate of 5 DEG C/min, keeps the temperature 2h, from
So it is cooled to room temperature.
Embodiment 8
Prepare MXene.1g lithium fluoride and 9M 20mL hydrochloric acid stir 30min in tetrafluoroethene beaker.It is slowly added to 1g
MAX-Ti3AlC2, persistently stirred for 24 hours at 35 DEG C.With deionized water with the revolving speed of 3500rpm, be centrifuged repeatedly, until pH value extremely
It is neutral.Lower sediment thing is collected, is filtered, it is dry.
Prepare MXene/ZIF.It weighs 40mg MXene and ultrasonic disperse in the DMSO of 30mL is added, the cobalt nitrate of 2mM is molten
Above-mentioned solution is added in the dispersion liquid of the DMSO of MXene, then by the methylimidazole of 10mM in solution, and product is collected by centrifugation, uses first
Pure and mild deionized water washing three times, is dried in vacuo.
Take MXene/ZIF obtained above to be dissolved in methanol solution, in molar ratio 1:3 add hexachlorocyclotriph,sphazene and
4,4-, to dihydroxydiphenylsulisomer, are added dropwise triethylamine, are stirred for 18h.Obtain MXene/ZIF/PZS.
MXene/ZIF/PZS is risen to 900 DEG C in tube furnace nitrogen atmosphere with the heating rate of 5 DEG C/min, keeps the temperature 2h, from
So it is cooled to room temperature.
Claims (4)
1. the preparation method of the cell catalyst of efficient two-dimensional material (MXene) titanium carbide, synthetic method are as described below:
(1) MXene is prepared using the method for selective etch, the MXene sample after taking drying is dissolved in two under ultrasound condition
In methyl sulfoxide, cabaltous nitrate hexahydrate is added, 2-methylimidazole after ultrasonic dissolution, is placed under magnetic agitation and stirs, centrifugation is dry
It is dry to obtain MXene/ZIF；
(2) it takes MXene/ZIF obtained above to be dissolved in methanol solution, adds hexachlorocyclotriph,sphazene and 4,4- is to dihydroxy
Triethylamine is added dropwise in diphenyl sulphone (DPS) dropwise under stiring, is stirred for preparation PZS microballoon insertion MXene interlayer, obtains MXene/ZIF/
PZS；
(3) MXene/ZIF/PZS is risen to 900 DEG C in tube furnace nitrogen atmosphere with the heating rate of 5 DEG C/min, keeps the temperature 2h, from
It is so cooled to room temperature, to prepare high performance catalyst.
2. preparation method according to claim 1, it is characterised in that cabaltous nitrate hexahydrate and 2-methylimidazole is successively added
It is dissolved in the dimethyl sulphoxide solution of MXene, wherein the molar ratio of cabaltous nitrate hexahydrate and 2-methylimidazole is 1:4~1:1,
Middle MXene is 10~100mg.
3. preparation method according to claim 1, it is characterised in that the raw material of synthesis PZS is successively added, realizes growth in situ
PZS microballoon, wherein hexachlorocyclotriph,sphazene and 4,4- are 1:1~1:6 to the molar ratio of dihydroxydiphenylsulisomer.
4. preparation method according to claim 1, the doping introducing hetero-atoms of PZS, when carbonization heating rate be about 5 DEG C/
Min, carburizing temperature are 700 DEG C, 800 DEG C, 900 DEG C, carbonization time 2h.
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