CN107827103A - The preparation method and applications of N doping porous graphene - Google Patents
The preparation method and applications of N doping porous graphene Download PDFInfo
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- CN107827103A CN107827103A CN201711281693.6A CN201711281693A CN107827103A CN 107827103 A CN107827103 A CN 107827103A CN 201711281693 A CN201711281693 A CN 201711281693A CN 107827103 A CN107827103 A CN 107827103A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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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
- Y02E60/10—Energy storage using batteries
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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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a kind of preparation method and applications of N doping porous graphene.The preparation method of N doping porous graphene includes：Graphene and/or modified graphene are mixed with etchant, obtain mixture；Mixture and nitrogen-containing compound are placed in closed container, 30 minutes are incubated under the conditions of 50 ~ 200 DEG C, is put into the micro-wave oven reaction several seconds, and carry out acid treatment and obtain N doping porous graphene；The etchant is metallic compound.Compared with prior art, operation equipment is simple, and production cost is relatively low, it is most important that during porous graphene is prepared while realizes N doping is carried out to it, and greatly shorten the reaction time using microwave heating method.Due to the excellent properties of N doping porous graphene, it can be applied to the electrode material of ultracapacitor and for lithium ion battery negative material.
Description
Technical field
The present invention relates to novel nano carbon material technical field, specially a kind of preparation method of N doping porous graphene
And its application, it can apply to the fields such as nano-device, ultracapacitor, lithium ion battery.
Background technology
Graphene has leading for huge theoretical specific surface area and superelevation as a kind of new two-dimensional nano-carbon material
Electricity, heat conductivility, are most thin, maximum intensity materials known today.Graphene is due to a series of excellent physico
Learn characteristic, there is huge potential using value in fields such as nano-device, ultracapacitor, lithium ion batteries, one it is found that
Just the extensive concern of scientist is enjoyed, turns into study hotspot in recent years.
In order to improve the performance of graphene, its band structure can be changed by carrying out Heteroatom doping to it, while can
To extend its application.Such as：Electrode material of the nitrogen-doped graphene as ultracapacitor, shows high specific volume
Amount, excellent high rate performance and cyclical stability.And porous graphene material not only has the excellent specific property of graphene in itself, together
When graphene sheet surfaces there is unique nano aperture structure so that porous graphene is as the energy, catalysis or absorption
During material, the advantage of its two-dimensional structure has been given full play to.Therefore, nitrogen-doped graphene and porous graphene have become numerous
The focus of section researcher.And N doping porous graphene has the advantage of both porous graphene and nitrogen-doped graphene concurrently,
With important researching value and it is widely applied prospect
The method for preparing porous graphene at present is to carry out chemical activation at high temperature to graphene using potassium hydroxide；And prepare
Nitrogen-doped graphene to graphene under ammonia atmosphere mainly by carrying out the high temperature anneal.Both approaches be required for compared with
High heating-up temperature, preparation condition are harsh, it is most important that time-consuming, constrains the popularization and application of graphene；It is moreover, existing
Technology of preparing is difficult to realize a kind of method and prepares N doping porous graphene.
The content of the invention
In order to solve prior art N doping porous graphene preparation method condition harshness, popularization and application are restricted the present invention
The problem of, there is provided a kind of preparation method of N doping porous graphene.
The present invention is achieved by the following technical solution：A kind of preparation method of N doping porous graphene, including
Following steps：
Step 1：Graphene and/or modified graphene are well mixed in aqueous with etchant, dry after with nitrogenous chemical combination
Thing is placed in closed container, and 30 minutes are incubated under the conditions of 50 ~ 200 DEG C；
Step 2：Closed container in step 1 is put into the micro-wave oven reaction several seconds, reaction carries out acid treatment after terminating and obtains nitrogen
Adulterate porous graphene.
The present invention is during N doping porous graphene is prepared, by graphene and/or modified graphene and metallization
Compound etchant fully contacts, and is placed in nitrogen-containing compound in closed container, microwave heating under conditions of, make graphene and/
Or modified graphene reacts with metallic compound and nitrogen-containing compound, obtains N doping porous graphene.
Preferably, the etchant is one in oxometallate, metal nitrate, metal acetate and metal oxide
Kind is a variety of.
Preferably, the nitrogen-containing compound is in ammonia, nitrogen dioxide, urea, ammonium carbonate, ammonium hydrogen carbonate and melamine
One or more.
Preferably, the modified graphene is graphene oxide or fluorinated graphene.
Preferably, the microwave reaction time is 1~100 s, and the microwave power is 200~1000 W.
Preferably, the oxometallate is sodium molybdate, sodium tungstate, potassium molybdate, sodium aluminate, Sodium Caprylate, potassium octanoate, metatitanic acid
One or more in sodium, potassium titanate, nickel acid sodium, nickel acid potassium；
Preferably, the metal nitrate is one or more metal nitrates in iron, cobalt, nickel, aluminium, copper, zinc, silver and chromium；
Preferably, the metal acetate is one or more metal acetates in cobalt, nickel, aluminium, copper, zinc, silver and chromium；
Preferably, the metal oxide is the oxidation of one or more metals in iron, cobalt, nickel, aluminium, copper, zinc, vanadium and chromium
Thing.
Preferably, the mass ratio of the graphene and/or modified graphene and etchant is 1:20~20:1.
Preferably, the mass ratio of the graphene and/or modified graphene and nitrogen-containing compound is 1:10~30:1.
Preferably, the acid solution is the one or more in hydrochloric acid, sulfuric acid and nitric acid.
Compared with prior art, the present invention realizes while porous graphene is prepared carries out N doping to it, uses
Microwave heating method greatly shortens the reaction time.Test result indicates that N doping porous graphene nitrogen content prepared by the present invention
Higher and surface hole size is in 0.5 ~ 300nm scopes；N doping porous graphene prepared by the present invention is applied to super electricity
The electrode material of container, during current density 1A/g, the specific capacity of ultracapacitor is 182F/g；For negative electrode of lithium ion battery material
Material, is circulated 100 times, capability retention 98.6% under the conditions of the A/g of current density 2.
Brief description of the drawings
Fig. 1 is the transmission electron microscope photo of N doping porous graphene.
Fig. 2 is the stereoscan photograph of the N doping porous graphene before acid treatment.
Fig. 3 is the transmission electron microscope photo of the N doping porous graphene before acid treatment.
Fig. 4 is the x-ray photoelectron energy spectrum diagram of N doping porous graphene.
Fig. 5 is curve of double curvature figure of the N doping porous graphene electrode material under different current densities.
Fig. 6 is cyclic curve figure of the N doping porous graphene electrode material under the A/g of current density 2.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
A kind of preparation method of N doping porous graphene, comprises the following steps：
Step 1：Graphene and/or modified graphene are well mixed in aqueous with etchant, dry after with nitrogenous chemical combination
Thing is placed in closed container, and 30 minutes are incubated under the conditions of 50 ~ 200 DEG C；
Step 2：Closed container in step 1 is put into the micro-wave oven reaction several seconds, reaction carries out acid treatment after terminating and obtains nitrogen
Adulterate porous graphene.
In embodiment, graphene and/or modified graphene are heated with etchant, nitrogen-containing compound microwave, make graphite
Alkene and/or modified graphene react with etchant and nitrogen-containing compound, and the modified graphene is preferably graphene oxide or fluorine
Graphite alkene, the etchant are metallic compound.If modified graphene, such as graphene oxide or fluorinated graphene
The activation energy required for reaction can be substantially reduced Deng, active function groups existing for its surface, improves reaction efficiency.The graphite
The mass ratio of alkene and/or modified graphene and etchant is preferably 1:20~20:1, more preferably 1:10~10:1.The metallization
Compound is the one or more in oxometallate, metal nitrate, metal acetate and metal oxide；The oxometallic acid
Salt is in sodium molybdate, sodium tungstate, potassium molybdate, sodium aluminate, Sodium Caprylate, potassium octanoate, sodium titanate, potassium titanate, nickel acid sodium, nickel acid potassium
It is one or more；The metal oxide is the oxidation of one or more metals in iron, cobalt, nickel, aluminium, copper, zinc, vanadium and chromium
Thing.The metal nitrate is one or more metal nitrates in iron, cobalt, nickel, aluminium, copper, zinc, silver and chromium；The metal
Acetate is one or more metal acetates in cobalt, nickel, aluminium, copper, zinc, silver and chromium.The nitrogen-containing compound is preferably ammonia
One or more in gas, nitrogen dioxide, urea, ammonium carbonate, ammonium hydrogen carbonate and melamine.The time of the heating is preferably
1 ~ 100s, more preferably 5 ~ 60s, most preferably 5 ~ 20s；The microwave power is preferably 200 ~ 1000W, more preferably 600 ~
1000 W。
The graphene and/or modified graphene with after etchant reaction, the etchant in the graphene and/or
Modified graphene surface completes pore-creating, and preferably, obtained N doping porous graphene is cleaned, by described in
The etchant on N doping porous graphene surface removes, and displays the hole of graphenic surface.The present invention is preferably by described in
N doping porous graphene is cleaned in acid solution, and the acid solution is preferably the one or more in hydrochloric acid, sulfuric acid and nitric acid.
Embodiment 1
（1）According to mass ratio it is 1 by graphene and cobalt nitrate:1 is well mixed in aqueous, and freeze-drying obtains mixture；
Mixture and ammonium carbonate are placed in closed container, wherein the mass ratio of graphene and ammonium carbonate is 1:2,100 DEG C are heated to, is protected
Warm 30min；
（2）Above-mentioned closed container is placed in micro-wave oven, with 1000 W power, microwave heating 5s；
（3）Reaction is handled product after terminating in watery hydrochloric acid, clean dry, that is, obtains N doping porous graphene.
Fig. 1 is the transmission electron microscope photo of N doping porous graphene manufactured in the present embodiment, and graphenic surface is distributed with
Even hole, a diameter of 50nm of porous graphene or so.
Embodiment 2
（1）According to mass ratio it is 1 by graphene oxide and nickel acetate:3 are well mixed in aqueous, dry in 40 DEG C of vacuum drying oven
It is dry to obtain mixture；Mixture and ammonium hydrogen carbonate are placed in closed container, wherein the quality of graphene oxide and ammonium hydrogen carbonate
Than for 1:5,90 DEG C are heated to, is incubated 30min；
（2）Above-mentioned closed container is placed in micro-wave oven, with 800 W power, microwave heating 10s；
（3）Reaction is handled product after terminating in dilute sulfuric acid, clean dry, that is, obtains N doping porous graphene.
Fig. 2 is the stereoscan photograph before N doping porous graphene acid treatment manufactured in the present embodiment, it can be seen that stone
Substantial amounts of nano nickle granules and equally distributed nano-pore be present in black alkene surface.
Embodiment 3
（1）According to mass ratio it is 4 by fluorinated graphene and sodium tungstate:1 is well mixed in aqueous, dry in 60 DEG C of vacuum drying oven
It is dry to obtain mixture；Mixture and ammonia are placed in closed container, wherein the mass ratio of fluorinated graphene and ammonia is 2:1,
60 DEG C are heated to, is incubated 30min；
（2）Above-mentioned closed container is placed in micro-wave oven, with 1000 W power, microwave heating 20s；
（3）Reaction is handled product after terminating in watery hydrochloric acid, clean dry, that is, obtains N doping porous graphene.
Fig. 3 is the transmission electron microscope photo before N doping porous graphene acid treatment manufactured in the present embodiment, it can be seen that erosion
Carve agent and graphenic surface is etched into a large amount of nano apertures.
Embodiment 4
（1）According to mass ratio it is 7 by graphene oxide and sodium aluminate:1 is well mixed in aqueous, dry in 50 DEG C of vacuum drying oven
It is dry to obtain mixture；Mixture and ammonium carbonate are placed in closed container, the mass ratio of wherein graphene oxide and ammonium carbonate is
5:1,100 DEG C are heated to, is incubated 30min；
（2）Above-mentioned closed container is placed in micro-wave oven, with 500 W power, microwave heating 50s；
（3）Reaction is handled product after terminating in dust technology, clean dry, that is, obtains N doping porous graphene.
Fig. 4 is the x-ray photoelectron energy spectrum diagram of N doping porous graphene manufactured in the present embodiment, it follows that reaction
There is obvious nitrogen-doping peak in graphene afterwards.
Embodiment 5
（1）According to mass ratio it is 10 by graphene and nickel acid potassium:1 is well mixed in aqueous, in 60 DEG C of dryings of vacuum drying oven
Obtain mixture；Mixture and urea are placed in closed container, wherein the mass ratio of graphene and urea is 1:7, it is heated to
160 DEG C, it is incubated 30min；
（2）Above-mentioned closed container is placed in micro-wave oven, with 600 W power, microwave heating 5s；
（3）Reaction is handled product after terminating in watery hydrochloric acid, clean dry, that is, obtains N doping porous graphene.
N doping porous graphene is used for the electrode material of ultracapacitor, electro-chemical test shows, as shown in figure 5,
Under the conditions of current density 1A/g, its specific capacity is up to 182F/g, and has excellent high rate performance.
Embodiment 6
（1）According to mass ratio it is 1 by fluorinated graphene and silver nitrate:5 are well mixed in aqueous, and drying process is mixed
Thing；Mixture and ammonium dihydrogen phosphate are placed in closed container, wherein the mass ratio of fluorinated graphene and ammonium dihydrogen phosphate is 1:
1,150 DEG C are heated to, is incubated 30min；
（2）Above-mentioned closed container is placed in micro-wave oven, with 400 W power, microwave heating 100s；
（3）Reaction is handled product after terminating in watery hydrochloric acid, clean dry, that is, obtains N doping porous graphene.
N doping porous graphene is prepared into lithium ion battery negative material, electro-chemical test shows, as shown in fig. 6,
Circulated 100 times under the conditions of current density 2A/g, specific capacity remains at 398mAh/g.
The foregoing description of the disclosed embodiments, professional and technical personnel in the field are enable to realize or using the present invention.
A variety of modifications to these embodiments will be apparent for those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, it is of the invention
The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one
The most wide scope caused.
Claims (10)
1. a kind of preparation method of N doping porous graphene, it is characterised in that comprise the following steps：
Step 1：Graphene and/or modified graphene are well mixed in aqueous with etchant, dry after with nitrogenous chemical combination
Thing is placed in closed container, and 30 minutes are incubated under the conditions of 50 ~ 200 DEG C；
Step 2：Closed container in step 1 is put into the micro-wave oven reaction several seconds, reaction carries out acid treatment after terminating and obtains nitrogen
Adulterate porous graphene.
2. the preparation method of N doping porous graphene according to claim 1, it is characterised in that：The etchant is gold
Belong to the one or more in oxygen hydrochlorate, metal nitrate, metal acetate and metal oxide.
3. the preparation method of N doping porous graphene according to claim 1, it is characterised in that：The nitrogen-containing compound
For the one or more in ammonia, nitrogen dioxide, urea, ammonium carbonate, ammonium hydrogen carbonate and melamine.
4. the preparation method of N doping porous graphene according to claim 1, it is characterised in that：The modified graphene
For graphene oxide or fluorinated graphene.
5. the preparation method of N doping porous graphene according to claim 1, it is characterised in that：During the microwave reaction
Between be 1~100 s, the microwave power is 200~1000W.
6. the preparation method of N doping porous graphene according to claim 2, it is characterised in that：The oxometallate
For one in sodium molybdate, sodium tungstate, potassium molybdate, sodium aluminate, Sodium Caprylate, potassium octanoate, sodium titanate, potassium titanate, nickel acid sodium, nickel acid potassium
Kind is a variety of；
The metal nitrate is one or more metal nitrates in iron, cobalt, nickel, aluminium, copper, zinc, silver and chromium；
The metal acetate is one or more metal acetates in cobalt, nickel, aluminium, copper, zinc, silver and chromium；
The metal oxide is one or more metal oxides in iron, cobalt, nickel, aluminium, copper, zinc, vanadium and chromium.
7. the preparation method of N doping porous graphene according to claim 1, it is characterised in that：The graphene and/
Or the mass ratio of modified graphene and etchant is 1:20~20:1.
8. the preparation method of N doping porous graphene according to claim 1, it is characterised in that：The graphene and/
Or the mass ratio of modified graphene and nitrogen-containing compound is 1:10~30:1.
9. the preparation method of N doping porous graphene according to claim 1, it is characterised in that：The acid solution is salt
One or more in acid, sulfuric acid and nitric acid.
10. the N doping porous graphene described in claim 1-9, electro-catalysis, fuel-cell catalyst, ultracapacitor or
Application in terms of lithium ion battery.
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| CN108772040A (en) * | 2018-05-05 | 2018-11-09 | 安徽乐金环境科技有限公司 | A kind of preparation method of porous graphite alkenyl air purifying preparation |
| CN108816281A (en) * | 2018-05-07 | 2018-11-16 | 常州大学 | A kind of solid catalyst and preparation method thereof for brain text reaction grid |
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| CN110247032A (en) * | 2019-05-28 | 2019-09-17 | 北京汽车股份有限公司 | Nitrogen-doped graphene negative electrode material and preparation method thereof and lithium ion battery |
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| CN114068886A (en) * | 2020-07-30 | 2022-02-18 | 湖南中科星城石墨有限公司 | Modified graphite material and preparation method and application thereof |
| CN112661145A (en) * | 2020-12-24 | 2021-04-16 | 中国科学院过程工程研究所 | Nitrogen-doped graphene and preparation method and application thereof |
| CN114014306A (en) * | 2021-12-15 | 2022-02-08 | 陇东学院 | Preparation method and application of oxygen-enriched layered porous graphene |
| CN114014306B (en) * | 2021-12-15 | 2022-08-09 | 陇东学院 | Preparation method and application of oxygen-enriched layered porous graphene |
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