CN107416807A - A kind of preparation method of the three-D nano-porous graphene of nitrogen oxygen codope - Google Patents
A kind of preparation method of the three-D nano-porous graphene of nitrogen oxygen codope Download PDFInfo
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- CN107416807A CN107416807A CN201710751422.6A CN201710751422A CN107416807A CN 107416807 A CN107416807 A CN 107416807A CN 201710751422 A CN201710751422 A CN 201710751422A CN 107416807 A CN107416807 A CN 107416807A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Abstract
The present invention relates to a kind of preparation method of the three-D nano-porous graphene of nitrogen oxygen codope, comprise the following steps:Prepare alloy foil sheet;Prepare nanoporous nickel;Prepare the three-D nano-porous graphene of nitrogen oxygen codope:Tube furnace furnace temperature is warming up to 150 300 DEG C under argon gas, hydrogen, acetylene atmosphere, by nanoporous nickel foil piece be placed in tube furnace center carry out hydrogenate graphite growth, after reaction 30 minutes, turn off acetylene, hydrogen, and it is passed through ammonia, remove nanoporous nickel foil piece, ammonia, argon gas mixed atmosphere in furnace temperature is risen to 700 900 DEG C after by nanoporous nickel foil piece be quickly moved to reaction tube high-temperature constant warm area calcining;Nanoporous nickel is eroded afterwards to obtain the three-D nano-porous grapheme material of N doping, is acidified after cleaning in concentrated nitric acid.
Description
Technical field
The invention belongs to the technology of preparing of nano material and application field, and in particular to a kind of three-D nano-porous graphene
Preparation method and its application in carbon-based supercapacitor field.
Background technology
With the rapid advances of society and flourishing for miniaturized electronic device, the development for minimizing energy storage device is more next
It is more important.Ultracapacitor is as a kind of new energy storage device, with power density is high, charge-discharge velocity is fast, service life
The features such as long, all it is widely used in many practical fields.And with high power density, the miniature electrochemical capacitance of high-energy-density
Development it is even more very urgent, and the electrode material for forming ultracapacitor be determine performance of the supercapacitor determinant,
Therefore, how to rationally design and using the electrode material with excellent properties with very important effect.
Nano porous metal is a kind of new nano-porous materials system that developed recently gets up, by the gold of nanoscale
Category hole wall and hole form and have the basic attribute of metal body phase material.Nanoporous nickel has being total to for nano porous metal
Property, meanwhile, nanoporous nickel has less metal hole wall and hole (5-10nm), and has excellent catalytic activity, is storing up
Energy field has obtained the extensive attention of researcher.
Graphene is used as by the closelypacked monoatomic layer two-dimensional material of carbon atom, with excellent electrical and thermal conductivity, by force
The features such as toughness, optical property, stability, the huge attention of every field researchers is obtained.But because graphene sheet layer it
Between have interaction force and easily mutually accumulation, it is impossible to give full play to the advantages such as its high-specific surface area and superior electrical conductivity, so as to
Limit its and the application in electrochemical capacitance energy storage field.Therefore, two-dimentional (2D) graphene is assembled into specific three dimensional (3D)
The graphene of structure, the characteristic such as excellent electron transport property and higher specific surface area is made it have, and then processability is excellent
Different function element is for expanding the macroscopic view of graphene using significant.But from document report, it is most of to grind
The aperture of 3D graphenes for studying carefully to obtain is larger, causes electrode activity thing quality in unit volume relatively low, so that volume specific volume
It can not effectively play, limit its application in miniaturization energy storage field.
Meanwhile studies have reported that, the doping of heteroatom can adjust the electronic structure and chemical property of graphene, and nitrogen is former
The processing of the codope of son and oxygen atom can not only improve the hydrophily of graphene, and then improve its electrolyte and electrode material
Engagement capacity, and more avtive spots can be improved, make grapheme material that fake capacitance reaction occur, further improve graphite
The energy-storage property of alkene material.Therefore, the doping of effective heteroatom how is carried out to graphene, and is led improving electrode material
Electrically and it is hydrophilic simultaneously, there is provided fake capacitance react, there is very important meaning in electrochemical capacitance energy storage field for carbon material
Justice.
The content of the invention
It is an object of the invention to provide a kind of process is simple, cost it is cheap prepare the three-D nano-porous of nitrogen oxygen codope
The method of grapheme material.The three-D nano-porous graphene pore-size distribution of nitrogen oxygen codope obtained by the preparation method technique is equal
It is even and in nano-grade size, it is adapted to industrialized production.Technical scheme is as follows:
A kind of preparation method of the three-D nano-porous graphene of nitrogen oxygen codope, comprises the following steps:
1) alloy foil sheet is prepared
First, it is 100% according to Ni and Mn atomicity percentage sum, wherein Ni is 30%, Mn 70%, prepares and closes
Gold foil.
2) nanoporous nickel is prepared
By alloy foil sheet made from the first step, it is placed in 1M ammonium sulfates at 50 DEG C and is entered using the own etch of chemistry
The processing of row removal alloying, three-dimensional continuous communicating structure nanoporous nickel foil piece is prepared.
3) the three-D nano-porous graphene of nitrogen oxygen codope is prepared
Second step is obtained into nanoporous nickel foil piece to be placed in quartzy Noah's ark, and quartzy Noah's ark is placed in the cold temperature of quartz ampoule
Area, it is passed through argon gas, hydrogen, acetylene and carries out mixed gas after 5 minutes, mixed gas system pressure is adjusted to 100Torr, and by tube furnace
Furnace temperature is warming up to 150-300 DEG C, and quartzy Noah's ark is dragged in into tube furnace center after furnace temperature rises to assigned temperature carries out hydrogenation graphite
Growth, the ratio of acetylene, argon gas and hydrogen presses 1-50:200-500:50-200 flow configuration, after reacting 30 minutes, is closed
Fall acetylene, hydrogen, and be passed through ammonia, ammonia flow 5-50sccm, and by quartzy Noah's ark quickly from tube furnace center flat-temperature zone
Move to cold warm area, and ammonia, argon gas mixed atmosphere in furnace temperature risen to 700-900 DEG C.It is specified to treat that tubular type furnace temperature rises to
During temperature, quartzy Noah's ark is quickly moved to reaction tube high-temperature constant warm area, calcines 1-3min at this temperature, after calcining finishes,
Quartzy Noah's ark is quickly moved to cold warm area, and bell is opened, sample is down to room temperature in argon gas protects gas.By sample from pipe
Take out, and immerse in 3M hydrochloric acid solutions 15 hours in formula stove, nanoporous nickel is eroded to obtain N doping three-D nano-porous
Grapheme material, then, dense nitre is placed in after the three-D nano-porous grapheme material of N doping is cleaned up with deionized water
4h is acidified in acid, after acidifying is completed, is cleaned and is dried to obtain repeatedly with absolute ethyl alcohol again after being cleaned repeatedly with deionized water
The three-D nano-porous grapheme material of self-supporting nitrogen oxygen codope.
Compared with prior art, the present invention is grown by low temperature CVD using nanoporous nickel as matrix and combines high temperature and forged
The method of burning, obtain the three-D nano-porous grapheme material of N doping.In low-temperature CVD process, grown in nanoporous nickel surface
One layer of hydrogenation graphite, during high-temperature calcination, by the use of graphite is hydrogenated as solid-state carbon source, makes it be carbonized and carries out doping treatment, receiving
The three-D nano-porous graphene of N doping is obtained under the catalytic action of rice porous nickel, while nanoporous is eroded with hydrochloric acid solution
After nickel, and it is acidified with concentrated nitric acid to obtain the three-D nano-porous grapheme material of nitrogen oxygen codope.This method has following excellent
Gesture:(1) preparation technology is simple, and cost is cheap, can obtain nano-porous materials by the method for chemical vapor deposition, simplifies
Technological process, reduce process costs;(2) the three-D nano-porous graphene that this technique obtains is the complete membrane of self-supporting,
It can be used directly as working electrode, it is not necessary to traditional slurry coating processes and do not need binding agent, conductive black etc., effectively
The utilization rate of electrode material is added, has expanded the application field of graphene;(3) three-D nano-porous graphite prepared by this technique
Alkene film is obtained by hydrogenating the high-temperature calcination of graphite, and whole process is carried out under stable friendly environment, is a kind of green
The technology of color.
Brief description of the drawings
Fig. 1 is the photomacrograph of nickel-manganese paillon foil used in the present invention;
Fig. 2 is the nanoporous nickel SEM image prepared by the present invention;
Fig. 3 is the SEM image of the three-D nano-porous graphene of the nitrogen oxygen codope prepared by the embodiment of the present invention 1;
Fig. 4 is the TEM image of the three-D nano-porous graphene of the nitrogen oxygen codope prepared by the embodiment of the present invention 1;
Fig. 5 is the STEM images of the three-D nano-porous graphene of the nitrogen oxygen codope prepared by the embodiment of the present invention 1;
Fig. 6 be prepared by the embodiment of the present invention 1 undoped with three-D nano-porous graphene and nitrogen oxygen codope three
The cyclic voltammetry curve figure of wiener rice porous graphene.
Embodiment
The specific embodiment of preparation method of the present invention given below.These embodiments are only used for describing preparation of the present invention in detail
Method, it is not intended to limit the application scope of the claims.
Comparison example
First, according to Ni and Mn atomicity percentage sum be 100%, wherein Ni is 30%, Mn 70%, by Ni,
Mn bulks, which are put into vacuum melting furnace, prepares Ni30Mn70Alloy side's ingot, the alloy sheet through wire cutting post-processing into 2mm thickness,
Again the alloy foil sheet that thickness is 100 μ m thicks is obtained by rolling-annealing-rolling mill practice repeatedly.By obtained Ni30Mn70Close
Gold foil intercepts 1*0.5cm2, it is placed in 1M ammonium sulfates at 50 DEG C and is carried out using the own etch of chemistry at removal alloying
Reason 10 hours, the three-dimensional nanoporous nickel foil piece continuously penetrated is prepared.By obtained nanoporous nickel sheet spend respectively from
After sub- water is cleaned and cleaned repeatedly with absolute ethyl alcohol repeatedly, it is dried in vacuo to obtain fresh nanoporous nickel foil at room temperature
Piece.Nanoporous nickel foil piece is placed in quartzy Noah's ark, and quartzy Noah's ark is placed in the cold warm area of quartz ampoule, is passed through argon gas, hydrogen
Gas, acetylene carried out mixed gas after 5 minutes, mixed gas system pressure were adjusted into 100Torr, and tube furnace furnace temperature is warming up into 230
DEG C, after furnace temperature rises to assigned temperature by quartzy Noah's ark be dragged in tube furnace center flat-temperature zone carry out hydrogenate graphite growth, acetylene,
The ratio of argon gas and hydrogen presses 40:500:200 flow configuration, after reaction 30 minutes, turn off acetylene, hydrogen, and by quartz
Noah's ark quickly moves to cold warm area from flat-temperature zone, and furnace temperature is risen into 700 DEG C in argon gas atmosphere.It is specified to treat that tubular type furnace temperature rises to
During temperature, quartzy Noah's ark is quickly moved to reaction tube high-temperature constant warm area, calcines 3min at this temperature., will after calcining finishes
Quartzy Noah's ark is quickly moved to cold warm area, and bell is opened, and sample is down into room temperature in argon gas protects gas.By sample from tubular type
Take out, and immerse in 3M hydrochloric acid solutions 15 hours in stove, nanoporous nickel is eroded to obtain three-D nano-porous graphene material
Material.Then, cleaned and done repeatedly with absolute ethyl alcohol after three-D nano-porous grapheme material is cleaned up with deionized water
It is dry to obtain the three-D nano-porous grapheme material of self-supporting.
Embodiment 1
First, according to Ni and Mn atomicity percentage sum be 100%, wherein Ni is 30%, Mn 70%, by Ni,
Mn bulks, which are put into vacuum melting furnace, prepares Ni30Mn70Alloy side's ingot, the alloy sheet through wire cutting post-processing into 2mm thickness,
Again the alloy foil sheet that thickness is 100 μ m thicks is obtained by rolling-annealing-rolling mill practice repeatedly.By obtained Ni30Mn70Close
Gold foil intercepts 1*0.5cm2, it is placed in 1M ammonium sulfates at 50 DEG C and is carried out using the own etch of chemistry at removal alloying
Reason 10 hours, the three-dimensional nanoporous nickel foil piece continuously penetrated is prepared.By obtained nanoporous nickel sheet spend respectively from
After sub- water is cleaned and cleaned repeatedly with absolute ethyl alcohol repeatedly, it is dried in vacuo to obtain fresh nanoporous nickel foil at room temperature
Piece.Nanoporous nickel foil piece is placed in quartzy Noah's ark, and quartzy Noah's ark is placed in the cold warm area of quartz ampoule, is passed through argon gas, hydrogen
Gas, acetylene carried out mixed gas after 5 minutes, mixed gas system pressure were adjusted into 100Torr, and tube furnace furnace temperature is warming up into 230
DEG C, after furnace temperature rises to assigned temperature by quartzy Noah's ark be dragged in flat-temperature zone carry out hydrogenate graphite growth, acetylene, argon gas and hydrogen
Ratio press 40:500:200 flow configuration, after reacting 30 minutes, turns off acetylene, hydrogen, and is passed through ammonia, ammonia flow
For 10sccm, and quartzy Noah's ark is quickly moved into cold warm area from flat-temperature zone, and ammonia, argon gas mixed atmosphere in by furnace temperature liter
To 700 DEG C, wherein ammonia, argon gas press 10:200 flow configuration.When tubular type furnace temperature rises to assigned temperature, by quartzy Noah's ark
Reaction tube high-temperature constant warm area is quickly moved to, calcines 3min at this temperature.After calcining finishes, quartzy Noah's ark is quickly moved to cold
Warm area, and bell is opened, sample is down to room temperature in argon gas protects gas.Sample is taken out from tube furnace, and immerses 3M
15 hours in hydrochloric acid solution, nanoporous nickel is eroded to obtain the three-D nano-porous grapheme material of N doping.Then, by nitrogen
Adulterate to be placed in concentrated nitric acid after three-D nano-porous grapheme material is cleaned up with deionized water and be acidified 4h, acidifying completion
Afterwards, cleaned repeatedly with absolute ethyl alcohol again after being cleaned repeatedly with deionized water and be dried to obtain the three-dimensional of self-supporting nitrogen oxygen codope
Nano-size Porous Graphite alkene material.
Embodiment 2
First, according to Ni and Mn atomicity percentage sum be 100%, wherein Ni is 30%, Mn 70%, by Ni,
Mn bulks, which are put into vacuum melting furnace, prepares Ni30Mn70Alloy side's ingot, the alloy sheet through wire cutting post-processing into 2mm thickness,
Again the alloy foil sheet that thickness is 100 μ m thicks is obtained by rolling-annealing-rolling mill practice repeatedly.By obtained Ni30Mn70Close
Gold foil intercepts 1*1cm2, it is placed in 1M ammonium sulfates at 50 DEG C and carries out removal alloying processing using the own etch of chemistry
10 hours, the three-dimensional nanoporous nickel foil piece continuously penetrated is prepared.Obtained nanoporous nickel sheet is used into deionization respectively
After water is cleaned and cleaned repeatedly with absolute ethyl alcohol repeatedly, it is dried in vacuo to obtain fresh nanoporous nickel foil at room temperature
Piece.Nanoporous nickel foil piece is placed in quartzy Noah's ark, and quartzy Noah's ark is placed in the cold warm area of quartz ampoule, is passed through argon gas, hydrogen
Gas, acetylene carried out mixed gas after 5 minutes, mixed gas system pressure were adjusted into 100Torr, and tube furnace furnace temperature is warming up into 300
DEG C, after furnace temperature rises to assigned temperature by quartzy Noah's ark be dragged in tube furnace center flat-temperature zone carry out hydrogenate graphite growth, acetylene,
The ratio of argon gas and hydrogen presses 50:500:200 flow configuration, after reacting 30 minutes, turns off acetylene, hydrogen, and be passed through ammonia
Gas, ammonia flow 20sccm, and quartzy Noah's ark is quickly moved into cold warm area from flat-temperature zone, and in ammonia, the gaseous mixture of argon gas
Furnace temperature is risen to 800 DEG C in atmosphere, wherein ammonia, argon gas presses 20:200 flow configuration treats that tubular type furnace temperature rises to assigned temperature
When, quartzy Noah's ark is quickly moved to reaction tube high-temperature constant warm area, calcines 3min at this temperature.After calcining finishes, by quartz
Noah's ark is quickly moved to cold warm area, and bell is opened, and sample is down into room temperature in argon gas protects gas.By sample from tube furnace
Take out, and immerse in 3M hydrochloric acid solutions 15 hours, nanoporous nickel is eroded to obtain the three-D nano-porous graphene of N doping
Material.Then, it is placed in after the three-D nano-porous grapheme material of N doping is cleaned up with deionized water sour in concentrated hydrochloric acid
Change 4h, after acidifying is completed, cleaned repeatedly with absolute ethyl alcohol again after being cleaned repeatedly with deionized water and be dried to obtain self-supporting
The three-D nano-porous grapheme material of nitrogen oxygen codope.
Embodiment 3
First, according to Ni and Mn atomicity percentage sum be 100%, wherein Ni is 30%, Mn 70%, by Ni,
Mn bulks, which are put into vacuum melting furnace, prepares Ni30Mn70Alloy side's ingot, the alloy sheet through wire cutting post-processing into 2mm thickness,
Again the alloy foil sheet that thickness is 100 μ m thicks is obtained by rolling-annealing-rolling mill practice repeatedly.By obtained Ni30Mn70Close
Gold foil intercepts 1*0.5cm2, it is placed in 1M ammonium sulfates at 50 DEG C and is carried out using the own etch of chemistry at removal alloying
Reason 10 hours, the three-dimensional nanoporous nickel foil piece continuously penetrated is prepared.By obtained nanoporous nickel sheet spend respectively from
After sub- water is cleaned and cleaned repeatedly with absolute ethyl alcohol repeatedly, it is dried in vacuo to obtain fresh nanoporous nickel foil at room temperature
Piece.Nanoporous nickel foil piece is placed in quartzy Noah's ark, and quartzy Noah's ark is placed in the cold warm area of quartz ampoule, is passed through argon gas, hydrogen
Gas, acetylene carried out mixed gas after 5 minutes, mixed gas system pressure were adjusted into 100Torr, and tube furnace furnace temperature is warming up into 250
DEG C, after furnace temperature rises to assigned temperature by quartzy Noah's ark be dragged in flat-temperature zone carry out hydrogenate graphite growth, acetylene, argon gas and hydrogen
Ratio press 30:500:200 flow configuration, after reacting 30 minutes, turns off acetylene, hydrogen, and is passed through ammonia, ammonia flow
For 10sccm, and quartzy Noah's ark is quickly moved into cold warm area from flat-temperature zone, and ammonia, argon gas mixed atmosphere in by furnace temperature liter
To 900 DEG C.When tubular type furnace temperature rises to assigned temperature, quartzy Noah's ark is quickly moved to reaction tube high-temperature constant warm area, it is warm herein
The lower calcining 3min of degree.After calcining finishes, quartzy Noah's ark is quickly moved to cold warm area, and bell is opened, gas is protected in argon gas
It is middle that sample is down to room temperature.Sample is taken out from tube furnace, and immersed in 3M hydrochloric acid solutions 15 hours, nanoporous nickel is rotten
Eating away obtains the three-D nano-porous grapheme material of N doping.Then, the three-D nano-porous grapheme material of N doping is spent
Ionized water is placed in concentrated nitric acid after cleaning up and is acidified 4h, after acidifying is completed, is used again after being cleaned repeatedly with deionized water
Absolute ethyl alcohol cleans and is dried to obtain the three-D nano-porous grapheme material of self-supporting nitrogen oxygen codope repeatedly.
Claims (1)
1. a kind of preparation method of the three-D nano-porous graphene of nitrogen oxygen codope, comprises the following steps:
1) alloy foil sheet is prepared
First, it is 100% according to Ni and Mn atomicity percentage sum, wherein Ni is 30%, Mn 70%, prepares Alloy Foil
Piece.
2) nanoporous nickel is prepared
By alloy foil sheet made from the first step, it is placed in 1M ammonium sulfates at 50 DEG C and is gone using the own etch of chemistry
Alloying Treatment, three-dimensional continuous communicating structure nanoporous nickel foil piece is prepared.
3) the three-D nano-porous graphene of nitrogen oxygen codope is prepared
Second step is obtained into nanoporous nickel foil piece to be placed in quartzy Noah's ark, and quartzy Noah's ark is placed in the cold warm area of quartz ampoule,
It is passed through argon gas, hydrogen, acetylene and carries out mixed gas after 5 minutes, mixed gas system pressure is adjusted to 100Torr, and by tube furnace stove
Temperature is warming up to 150-300 DEG C, and quartzy Noah's ark is dragged in into tube furnace center after furnace temperature rises to assigned temperature carries out hydrogenating graphite
Growth, the ratio of acetylene, argon gas and hydrogen press 1-50:200-500:50-200 flow configuration, after reacting 30 minutes, turns off
Acetylene, hydrogen, and ammonia is passed through, ammonia flow 5-50sccm, and quartzy Noah's ark is quickly moved from tube furnace center flat-temperature zone
To cold warm area, and ammonia, argon gas mixed atmosphere in furnace temperature risen to 700-900 DEG C;Treat that tubular type furnace temperature rises to and specify temperature
When spending, quartzy Noah's ark is quickly moved to reaction tube high-temperature constant warm area, calcines 1-3min at this temperature, will after calcining finishes
Quartzy Noah's ark is quickly moved to cold warm area, and bell is opened, and sample is down into room temperature in argon gas protects gas;By sample from tubular type
Take out, and immerse in 3M hydrochloric acid solutions 15 hours in stove, nanoporous nickel is eroded to obtain the three-D nano-porous stone of N doping
Black alkene material, then, concentrated nitric acid is placed in after the three-D nano-porous grapheme material of N doping is cleaned up with deionized water
Middle acidifying 4h, after acidifying is completed, cleaned and be dried to obtain certainly repeatedly with absolute ethyl alcohol again after being cleaned repeatedly with deionized water
Support the three-D nano-porous grapheme material of nitrogen oxygen codope.
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Cited By (2)
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CN108636438A (en) * | 2018-05-16 | 2018-10-12 | 成都理工大学 | A kind of nitrogen co-doped graphene photo-catalyst of oxygen and its preparation method and application |
CN114577874A (en) * | 2022-03-04 | 2022-06-03 | 清华大学 | Electrode and preparation method thereof, sensor and preparation method and application thereof |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108636438A (en) * | 2018-05-16 | 2018-10-12 | 成都理工大学 | A kind of nitrogen co-doped graphene photo-catalyst of oxygen and its preparation method and application |
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CN114577874A (en) * | 2022-03-04 | 2022-06-03 | 清华大学 | Electrode and preparation method thereof, sensor and preparation method and application thereof |
CN114577874B (en) * | 2022-03-04 | 2022-11-18 | 清华大学 | Electrode and preparation method thereof, sensor and preparation method and application thereof |
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