CN109841428A - Preparation method of high-density graphene electrode material for lithium ion capacitor - Google Patents
Preparation method of high-density graphene electrode material for lithium ion capacitor Download PDFInfo
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- CN109841428A CN109841428A CN201711204042.7A CN201711204042A CN109841428A CN 109841428 A CN109841428 A CN 109841428A CN 201711204042 A CN201711204042 A CN 201711204042A CN 109841428 A CN109841428 A CN 109841428A
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- electrode material
- graphene
- ion capacitor
- density
- lithium
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 45
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 40
- 239000003990 capacitor Substances 0.000 title claims abstract description 37
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 34
- 239000007772 electrode material Substances 0.000 title claims abstract description 28
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 57
- 239000010439 graphite Substances 0.000 claims abstract description 57
- 238000000034 method Methods 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 21
- 239000006185 dispersion Substances 0.000 claims abstract description 18
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 17
- 230000003647 oxidation Effects 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000002243 precursor Substances 0.000 claims abstract description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 5
- -1 graphite alkene Chemical class 0.000 claims description 35
- 238000001035 drying Methods 0.000 claims description 30
- 238000010438 heat treatment Methods 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 150000001336 alkenes Chemical class 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 239000004575 stone Substances 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000010907 mechanical stirring Methods 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000002441 X-ray diffraction Methods 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- 238000001228 spectrum Methods 0.000 abstract description 4
- 238000001132 ultrasonic dispersion Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000011056 performance test Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Classifications
-
- 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
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- Electric Double-Layer Capacitors Or The Like (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates to a preparation method of a high-density graphene electrode material for a lithium ion capacitor. The invention belongs to the technical field of graphene electrode materials. A preparation method of a high-density graphene electrode material for a lithium ion capacitor comprises the following process steps: the graphene powder is subjected to oxidation treatment, the graphene oxide powder is mixed with a graphite oxide dispersion solution, after stirring and ultrasonic dispersion, the precursor solution is transferred into a hydrothermal kettle, the hydrothermal kettle is continuously heated for 6-24 hours at the temperature of 150-. The method has the advantages that the feeding amount and the preparation amount of the preorder are increased, the preparation conditions and the method are simplified, and the high-density graphene has no obvious diffraction peak in an X-ray diffraction spectrum, belongs to short-range order and long-range disorder; the production efficiency is improved, the production cost is reduced, and the method is very suitable for large-scale production of graphene.
Description
Technical field
The invention belongs to Graphene electrodes field of material technology, more particularly to a kind of lithium-ion capacitor high density stone
Black alkene electrode material preparation method.
Background technique
Graphene is by the sp with hexagonal structure2The two-dimension single layer film that hydbridized carbon atoms are constituted.Due to graphene
Unique structure makes it have above-mentioned unique property, such as the specific surface area of super large, good electron conduction and excellent
Optical characteristics etc..And so be also doomed can in a variety of manners for excellent carbon material, Yu Tigao lithium ion battery, electrochemical capacitor
And the electrochmical power sources aspect of performance such as fuel cell, indelible effect will be played.For grapheme material its super large
Specific surface area is its advantage under certain condition, but disadvantage brought by its extra specific surface area is exactly extremely low tap density,
The density of the great grapheme material of some porositys is even lower than 0.00016g/mL.This is for grapheme material as electrode
The application of material in the capacitor is fatal defect, and the material of such low-density is not only difficult to be prepared into electrode, and electrode
Carrying capacity be very big problem, and then affect active material proportion in entire capacitor, be finally unfavorable for capacitor
The performance of energy density and power density.
Currently, for high-density graphite alkene material preparation research, most representational treatise: SCIENTIFIC
REPORTS.2013,3,2975；Chem.Mater.2015,27,3291-3298.And mainly asking in existing preparation process
Topic: 1) batch preparation amount is less.Since graphite oxide is in certain volume solvent, dispersion amount and its limited, about 0.1g/L, therefore batch
Secondary preparation amount is only in several gram-grades.2) preparation condition and method are complex.Existing process requirement after post treatment, and needs
Drying condition is controlled, so strongly limiting preparation efficiency.
Summary of the invention
The present invention is to solve technical problem present in well-known technique and provide a kind of lithium-ion capacitor high density stone
Black alkene electrode material preparation method.
The object of the present invention is to provide a kind of inventory and preparation amount with increased preamble, simplify preparation condition with
Method, high-density graphite alkene, without obvious diffraction maximum, belong to shortrange order, longrange disorder in X-ray diffraction spectrum；It is given birth to improving
While producing efficiency, the lithium-ion capacitor for the features such as reducing production cost, being very suitable for the large-scale production of graphene
With high-density graphite alkene electrode material preparation method.
By graphene powder through the oxidation processes that kick the beam, then it is mixed with graphite oxide dispersion, by stirring and is surpassed
After sound dispersion.Precursor liquid is transferred in water heating kettle, the continuous heating 6-24h at 150-200 DEG C, directly by gained Graphene gel
It is dried in normal pressure, drying mode is ladder drying mode, then crushes and obtains high-density graphite alkene powder, is then used as lithium
Ionistor positive electrode carries out electric performance test.
The light oxidation of graphene powder carries out normal temperature oxidation including the use of the acid solution of 1%-60% (volume ratio)；It is used
Acid includes: nitric acid, perchloric acid, hypochlorous acid, permanganic acid, phosphoric acid etc.；Mode of oxidizing used include: ultrasonic vibration, mechanical stirring,
Airflow stirring etc.；Oxidization time 1-12h.
Light graphene oxide is mixed with graphite oxide dispersion, stirring and ultrasonic disperse time 1-12h.
Hydro-thermal process, condition: temperature is 150-200 DEG C, reaction time 6-24h.
The drying of Graphene gel, condition are atmospheric pressure, without post-processing；Drying mode is ladder drying: first in 40-
60 DEG C of baking 12-24h, then in 60-100 DEG C of baking 6-12h.
Lithium-ion capacitor high-density graphite alkene electrode material preparation method of the present invention is adopted the technical scheme that:
A kind of lithium-ion capacitor high-density graphite alkene electrode material preparation method, its main feature is that: lithium-ion capacitor
With the technical process of high-density graphite alkene electrode material preparation method: graphene powder passes through oxidation processes, by graphene oxide
Powder is mixed with graphite oxide dispersion, by stirring with after ultrasonic disperse, precursor liquid is transferred in water heating kettle, in 150-200
Continuous heating 6-24h under the conditions of DEG C dries gained Graphene gel using ladder drying mode, and crushing obtains high density powder
Graphene electrodes material.
Lithium-ion capacitor high-density graphite alkene electrode material preparation method of the present invention can also use following technical side
Case:
Lithium-ion capacitor high-density graphite alkene electrode material preparation method, its main feature is that: graphene powder
Oxidation processes are to carry out normal temperature oxidation using the acid solution of 1%-60% volume ratio；Mode of oxidizing is stirred using ultrasonic vibration, machinery
It mixes or airflow stirring.
Lithium-ion capacitor high-density graphite alkene electrode material preparation method, its main feature is that: sour acid solution is
Nitric acid, perchloric acid, hypochlorous acid, permanganic acid or phosphoric acid solution, oxidization time 1-12h.
Lithium-ion capacitor high-density graphite alkene electrode material preparation method, its main feature is that: graphene oxide
Powder is mixed with graphite oxide dispersion, and graphite oxide dispersion is graphite oxide aqueous solution, graphene oxide and graphite oxide
Dispersion liquid mixing is to increase batch preparation amount, stirring and ultrasonic disperse time 1-12h.
Lithium-ion capacitor high-density graphite alkene electrode material preparation method, its main feature is that: drying mode is adopted
Ladder drying, first in 40-60 DEG C of baking 12-24h, then in 60-100 DEG C of baking 6-12h.
The advantages and positive effects of the present invention are:
Lithium-ion capacitor is with high-density graphite alkene electrode material preparation method due to using the completely new technology of the present invention
Scheme, compared with prior art, the inventory and preparation amount of present invention process not only increased preamble, and simplify and prepare item
Part and method, high-density graphite alkene, without obvious diffraction maximum, belong to shortrange order, longrange disorder in X-ray diffraction spectrum.It is mentioning
While high efficiency, production cost is reduced, is very suitable for the large-scale production of graphene.
Detailed description of the invention
Fig. 1, Fig. 2 and Fig. 3 are the TEM figures that embodiment 1 obtains high-density graphite alkene；
Fig. 4, Fig. 5 are the electrical property curves that embodiment 1 obtains high-density graphite alkene.
Specific embodiment
In order to further understand the content, features and effects of the present invention, the following examples are hereby given, and cooperate attached drawing
Detailed description are as follows:
Refering to attached drawing 1, Fig. 2 and Fig. 3.
Embodiment 1
A kind of lithium-ion capacitor high-density graphite alkene electrode material preparation method, technical process:
By graphene powder in 1% nitric acid solution oxidation processes 12h, after by itself and graphite oxide ultrasonic vibration dispersion liquid
Mix 12h, precursor liquid is transferred in water heating kettle, at 180 DEG C continuous heating for 24 hours, directly by gained Graphene gel in normal pressure
Drying, drying mode are ladder drying mode: being baked at 40 DEG C for 24 hours, then in 100 DEG C of baking 6h, then crushing is obtained highly dense
Graphene powder is spent, lithium-ion capacitor positive electrode is then used as and carries out electric performance test.
Embodiment 2
A kind of lithium-ion capacitor high-density graphite alkene electrode material preparation method, technical process:
By graphene powder in 60% phosphoric acid solution oxidation processes 1h, after by itself and graphite oxide ultrasonic vibration dispersion liquid
12h is mixed, precursor liquid is transferred in water heating kettle, the continuous heating 12h at 150 DEG C, directly by gained Graphene gel in normal pressure
Drying, drying mode are ladder drying mode: in 60 DEG C of baking 12h, then in 100 DEG C of baking 12h, then crushing is obtained highly dense
Graphene powder is spent, lithium-ion capacitor positive electrode is then used as and carries out electric performance test.
Embodiment 3
A kind of lithium-ion capacitor high-density graphite alkene electrode material preparation method, technical process:
By graphene powder in 50% perchloric acid solution oxidation processes 1h, after itself and graphite oxide ultrasonic vibration are dispersed
Liquid mixing 12h, precursor liquid is transferred in water heating kettle, the continuous heating 6h at 200 DEG C, directly by gained Graphene gel in normal pressure
Drying, drying mode are ladder drying mode: in 60 DEG C of baking 12h, then in 100 DEG C of baking 6h, then crushing is obtained highly dense
Graphene powder is spent, lithium-ion capacitor positive electrode is then used as and carries out electric performance test.
Embodiment 4
A kind of lithium-ion capacitor high-density graphite alkene electrode material preparation method, technical process:
By graphene powder in 50% hypochlorite solution oxidation processes 1h, after itself and graphite oxide ultrasonic vibration are dispersed
Liquid mixing 12h, precursor liquid is transferred in water heating kettle, the continuous heating 12h at 180 DEG C, directly by gained Graphene gel normal
Pressure drying, drying mode are ladder drying mode: in 60 DEG C of baking 12h, then in 90 DEG C of baking 12h, then crushing and obtain height
Density graphite alkene powder is then used as lithium-ion capacitor positive electrode and carries out electric performance test.
Comparative embodiment
Comparative example 1
Graphite oxide is dispersed in water with the concentration of 1mg/mL, dispersion liquid is transferred in water heating kettle, 180 DEG C of hydro-thermals are anti-
Answer 6h, Graphene gel taken out, squeezed (pressure 1Mpa) with press machine, then it is dried in vacuo (vacuum degree be-
0.1Mpa), drying temperature control persistently dries 36h at 70 DEG C.It then crushes and obtains high-density graphite alkene powder, then by it
Electric performance test is carried out as lithium-ion capacitor positive electrode.
This technique, initial charge amount is limited, and in addition subsequent drying condition is more harsh, time-consuming, low efficiency and at high cost, sternly
The relatively large preparation of recasting about high-density graphite alkene.
1 embodiment 1 of table and comparative example preparation efficiency contrast table
| Serial number | Embodiment 1 | Comparative example | Comparative example | Comparative example |
| Preparation efficiency (g/ days) | 1.3 | 0.1 | 0.1 | 0.06 |
Comparative example 2
Graphite oxide will be dispersed in water with the concentration of 1mg/mL, dispersion liquid is transferred in water heating kettle, 180 DEG C of hydro-thermals
React 6h, Graphene gel is taken out, using ethyl alcohol or acetone soak 12h, then it is dried in vacuo (vacuum degree be-
0.1Mpa), drying temperature control persistently dries 36h at 60 DEG C.It then crushes and obtains high-density graphite alkene powder, then by it
Electric performance test is carried out as lithium-ion capacitor positive electrode.
This technique, initial charge amount is limited, and in addition subsequent drying condition is more harsh, time-consuming, low efficiency and at high cost, sternly
The relatively large preparation of recasting about high-density graphite alkene.
Comparative example 3
Graphite oxide will be dispersed in water with the concentration of 1mg/mL, dispersion liquid is transferred in water heating kettle, 180 DEG C of hydro-thermals
6h is reacted, Graphene gel is taken out, then to its vacuum air drying (vacuum degree is -0.1Mpa), drying temperature control exists
25 DEG C, persistently dry 70h or more.It then crushes and obtains high-density graphite alkene powder, be then used as lithium-ion capacitor just
Pole material carries out electric performance test.
This technique, initial charge amount is limited, and in addition subsequent drying condition is more harsh, time-consuming, low efficiency and at high cost, sternly
The relatively large preparation of recasting about high-density graphite alkene.
The present embodiment has the inventory and preparation amount of the technique not only increased preamble, and simplifies and prepare item
Part and method, high-density graphite alkene, without obvious diffraction maximum, belong to shortrange order, longrange disorder in X-ray diffraction spectrum.It is mentioning
While high efficiency, production cost is reduced, is very suitable for the good effects such as the large-scale production of graphene.
Claims (5)
1. a kind of lithium-ion capacitor high-density graphite alkene electrode material preparation method, it is characterized in that: lithium-ion capacitor is used
The technical process of high-density graphite alkene electrode material preparation method: graphene powder passes through oxidation processes, by graphene oxide powder
Body is mixed with graphite oxide dispersion, by stirring with after ultrasonic disperse, precursor liquid is transferred in water heating kettle, at 150-200 DEG C
Under the conditions of continuous heating 6-24h, by gained Graphene gel using ladder drying mode dry, crushing obtain high density powder stone
Black alkene electrode material.
2. lithium-ion capacitor according to claim 1 high-density graphite alkene electrode material preparation method, it is characterized in that:
Graphene powder oxidation processes are to carry out normal temperature oxidation using the acid solution of 1%-60% volume ratio；Mode of oxidizing is using ultrasound shake
It swings, mechanical stirring or airflow stirring.
3. lithium-ion capacitor according to claim 2 high-density graphite alkene electrode material preparation method, it is characterized in that:
Sour acid solution is nitric acid, perchloric acid, hypochlorous acid, permanganic acid or phosphoric acid solution, oxidization time 1-12h.
4. lithium-ion capacitor according to claim 1 or 2 high-density graphite alkene electrode material preparation method, feature
Be: graphene oxide powder is mixed with graphite oxide dispersion, and graphite oxide dispersion is graphite oxide aqueous solution, graphite oxide
Alkene is mixed with graphite oxide dispersion to increase batch preparation amount, stirring and ultrasonic disperse time 1-12h.
5. lithium-ion capacitor according to claim 1 high-density graphite alkene electrode material preparation method, it is characterized in that:
The ladder drying that drying mode uses, first in 40-60 DEG C of baking 12-24h, then in 60-100 DEG C of baking 6-12h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711204042.7A CN109841428A (en) | 2017-11-27 | 2017-11-27 | Preparation method of high-density graphene electrode material for lithium ion capacitor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711204042.7A CN109841428A (en) | 2017-11-27 | 2017-11-27 | Preparation method of high-density graphene electrode material for lithium ion capacitor |
Publications (1)
| Publication Number | Publication Date |
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| CN109841428A true CN109841428A (en) | 2019-06-04 |
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ID=66880044
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| CN201711204042.7A Pending CN109841428A (en) | 2017-11-27 | 2017-11-27 | Preparation method of high-density graphene electrode material for lithium ion capacitor |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW201343548A (en) * | 2012-03-09 | 2013-11-01 | 巴地斯顏料化工廠 | Aerogel based on doped graphene |
| CN105590757A (en) * | 2014-11-18 | 2016-05-18 | 中国科学院宁波材料技术与工程研究所 | Carbon nanotube/graphene composite gel and preparation method thereof |
-
2017
- 2017-11-27 CN CN201711204042.7A patent/CN109841428A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW201343548A (en) * | 2012-03-09 | 2013-11-01 | 巴地斯顏料化工廠 | Aerogel based on doped graphene |
| CN105590757A (en) * | 2014-11-18 | 2016-05-18 | 中国科学院宁波材料技术与工程研究所 | Carbon nanotube/graphene composite gel and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| QINQIN ZHOU等: "Composite organogels of graphene and activated carbon for electrochemical capacitors", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
| TIANYUAN LIU等: "High-Density Lithium-Ion Energy Storage Utilizing the Surface Redox Reactions in Folded Graphene Films", 《CHEM. MATER.》 * |
| YUNFU LIU等: "Solvothermal synthesis of graphene nanosheets as the electrode materials for supercapacitors", 《IONICS》 * |
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Application publication date: 20190604 |