CN108493420A - A kind of graphited graphene derived material of aluminium ion battery local - Google Patents
A kind of graphited graphene derived material of aluminium ion battery local Download PDFInfo
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- CN108493420A CN108493420A CN201810299394.3A CN201810299394A CN108493420A CN 108493420 A CN108493420 A CN 108493420A CN 201810299394 A CN201810299394 A CN 201810299394A CN 108493420 A CN108493420 A CN 108493420A
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- graphene
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- ion battery
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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
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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
Abstract
The invention belongs to energy-storage battery technologies, more particularly to a kind of graphited graphene derived material of aluminium ion battery local, the material is overlapped by 3 ~ 10 layer graphene lamella three-dimensionals, and the degree of graphitization of graphene sheet layer is 10% ~ 99%, the lateral dimension of the graphene sheet layer is 10 μm ~ 100 μm, and the material is prepared by high-temperature process method or method of chemical treatment.Compared with the existing technology, the beneficial effects of the invention are as follows：(1) the present invention provides a kind of graphited graphene derived materials of local, by changing heat treatment temperature（Or the amount of reducing agent type and reducing agent）And processing time, the finely regulating of the degree of graphitization of grapheme material may be implemented.(2) it innovatively proposes the graphited graphene derived material of local to act on the storage of electroactive substance and charge and discharge product, to promote the multiplying power property of electrochemical energy storing device.
Description
Technical field
The invention belongs to energy-storage battery technologies more particularly to a kind of graphited graphene of aluminium ion battery local to derive
Material.
Background technology
Graphene is the sp for having bi-dimensional cellular shape lattice structure2Hydridization single layer of carbon atom crystal is out-of-flatness, has pleat
The two dimensional crystal of wrinkle, it is considered to be construct other sp2The primitive unit of carbonaceous material.Excellent electricity, the heat that graphene has
, mechanics, optical property become the research hotspot of people in recent years.
Grapheme material has higher specific surface area active and high reaction activity due to its microcosmic nanoscale,
Electrochemical energy storage field embodies larger advantage.Although grapheme material itself has higher specific surface area, it is based on
The performance of graphene energy storage device is unsatisfactory.This is because the specific surface area of grapheme material is excessive, for aluminium ion electricity
Chi Shihui forms huge SEI films, consumes excessive aluminium ion, reduces the cycle performance of battery.Simultaneously as aluminium ion when charging
AlCl in battery electrolyte4 -It need to be inserted into negative material, but the grapheme material of monolithic layer obviously cannot be satisfied AlCl4 -
Intercalation need.And it is all limited for the capacity and high rate performance of the natural graphite of aluminium ion battery at this stage.
In view of this, the present invention is intended to provide a kind of graphited graphene derived material of aluminium ion battery local,
By carrying out local graphitization processing to grapheme material, electrochemical energy storing device high rate performance, cycle characteristics can be solved not
Foot, the relatively low technical problem of energy density.
Invention content
It is an object of the invention to：In view of the deficiencies of the prior art, a kind of aluminium ion battery is provided to be graphitized with local
Graphene derived material, by grapheme material carry out local graphitization processing, electrochemical energy storing device can be solved
High rate performance, cycle characteristics are insufficient, the relatively low technical problem of energy density.
In order to achieve the above object, the present invention adopts the following technical scheme that：
A kind of graphited graphene derived material of aluminium ion battery local, the material is by 3~10 layer graphene pieces
Layer three-dimensional overlaps, and the degree of graphitization of graphene sheet layer is 10%~99%, the lateral dimension of the graphene sheet layer
It it is 10 μm~100 μm, the material is prepared by high-temperature process method or method of chemical treatment.
The present invention derives material by the local graphitization processing to grapheme material, the graphited graphene of local of preparation
Material is conducive to the transmission of ion in charge and discharge process, and the capacity and high rate performance to promote energy storage device are laid a good foundation.
The present invention promotes the capacity characteristic of energy storage device by the degree of graphitization of control local graphitized carbon.The local
Graphited graphene derived material has the less graphene film number of plies, and the high rate performance to promoting energy storage device also has aobvious
Write effect.
As a kind of improvement of the graphited graphene derived material of aluminium ion battery local of the present invention, the graphene
The specific surface area of lamella is 100m2·g-1~3000m2·g-1。
As a kind of improvement of the graphited graphene derived material of aluminium ion battery local of the present invention, the graphene
The degree of graphitization of lamella is 20%~75%.
As a kind of improvement of the graphited graphene derived material of aluminium ion battery local of the present invention, at the high temperature
Logos includes at least following steps：
Step 1: the preparation of grapheme material：Graphite oxide is heat-treated under inert gas protection, is had
The grapheme material of monolithic layer；
Step 2: it is small that the single-layer graphene obtained by step 1 is heat-treated to h under inert gas protection, under temperature T
When, obtain the graphited graphene derived material of local.
As a kind of improvement of the graphited graphene derived material of aluminium ion battery local of the present invention, in step 1
The temperature of heat treatment is 300 DEG C~1200 DEG C.
As a kind of improvement of the graphited graphene derived material of aluminium ion battery local of the present invention, step 1 and two
Described in inert gas be at least one of nitrogen, argon gas and helium；Temperature T described in step 2 is 1000 DEG C~
3000℃；H described in step 2 is 0.5~3.It should be understood that temperature is excessively high or processing time is too long, to grapheme material
Local graphitization it is unfavorable, it is intended to completely graphitization.Likewise, temperature is too small or processing time is too short, grapheme material without
Method is graphitized.
As a kind of improvement of the graphited graphene derived material of aluminium ion battery local of the present invention, at the chemistry
Logos includes at least following steps：
Step 1: graphite oxide is mixed with reducing agent, dissolved, is ultrasonically treated t minutes with solvent；
Step 2: obtaining the graphited graphene derived material of local after centrifuging, taking precipitation, cleaning, drying.
As a kind of improvement of the graphited graphene derived material of aluminium ion battery local of the present invention, institute in step 1
It is at least one of hydrazine hydrate, sodium ascorbate, glucose to state reducing agent；The solvent is water, methanol, ethyl alcohol, hexamethylene
At least one of, the time t of the supersound process is 10~60min, and the molar ratio of the graphite oxide and reducing agent is 1：
The mass ratio of (0.05~0.5), the graphite oxide and solvent is 1：(5~20).
As a kind of improvement of the graphited graphene derived material of aluminium ion battery local of the present invention, done in step 2
Dry temperature is 60 DEG C~90 DEG C, and the dry duration is 1h~10h.
It is another object of the present invention to provide a kind of aluminium ion battery, including anode, cathode, electrolyte and it is located at institute
The isolation film between anode and the cathode is stated, active material is material of the present invention used in the cathode, described
Contain AlCl in electrolyte4 -。
Compared with the existing technology, when charging to the aluminium ion battery, AlCl4 -Ion is inserted into negative electrode active material
In, the graphited graphene derived material of the local has less piece layer number and moderate lateral dimension, can effectively be promoted
The capacity characteristic and high rate performance of aluminium ion battery.Therefore, the high conductivity and graphite material of present invention combination grapheme material
Interlayer advantage, design the graphited graphene derived material of local, it is close to battery high rate performance, cycle characteristics and energy
The promotion of degree has theoretical research value and practical application meaning.
In short, the beneficial effects of the invention are as follows：
(1) the present invention provides a kind of graphited graphene derived material of local, by change heat treatment temperature (or
The amount of reducing agent type and reducing agent) and processing time, the finely regulating of the degree of graphitization of grapheme material may be implemented.
(2) the graphited graphene derived material of local is innovatively proposed to electroactive substance and charge and discharge
The storage of product acts on, to promote the multiplying power property of electrochemical energy storing device.
Description of the drawings
With reference to the accompanying drawings and detailed description, the present invention and its advantageous effects are described in detail.
Fig. 1 is the transmission electron microscope figure of the graphited graphene derived material of local prepared by embodiment 1.
Fig. 2 is the charge and discharge that the graphited graphene derived material of local prepared by embodiment 1 is applied in aluminium ion battery
Electric curve.
Specific implementation mode
Below the technical scheme of the invention is illustrated by a specific example, but the scope of the present invention is not limited thereto.
Embodiment 1：
A kind of graphited graphene derived material of aluminium ion battery local is present embodiments provided, the material is by 3 layers
Graphene sheet layer three-dimensional overlaps, and the degree of graphitization of graphene sheet layer is 87%, and the lateral dimension of graphene sheet layer is
10 μm~100 μm, the specific surface area of graphene sheet layer is 1300m2g-1。
The material is prepared using high-temperature process method：Weigh graphite oxide prepared by the improved Hummer methods of 200mg
Powder body material is placed in heat treatment, 5 DEG C of min in the tube furnace for being connected with argon atmospher-1Heating is heated to 300 DEG C of constant temperature 120min, obtains
To grapheme material.Grapheme material obtained is placed in the high temperature furnace for being connected with argon gas, 2800 DEG C of high-temperature process 1h obtain office
The graphited graphene derived material in domain.
Fig. 1 is the transmission electron micrograph for the material that the present embodiment is prepared, as seen from Figure 1：Graphite flake
The number of plies is three layers, and degree of graphitization is high.
Embodiment 2：The temperature being heat-treated in embodiment 1 is adjusted to 200 DEG C, remaining is same as Example 1, here no longer
It repeats.
Embodiment 3：The temperature being heat-treated in embodiment 1 is adjusted to 500 DEG C, remaining is same as Example 1, here no longer
It repeats.
Embodiment 4：The temperature being heat-treated in embodiment 1 is adjusted to 800 DEG C, remaining is same as Example 1, here no longer
It repeats.
Embodiment 5：The temperature being heat-treated in embodiment 1 is adjusted to 1000 DEG C, remaining is same as Example 1, here not
It repeats again.
Comparative example 1：The temperature being heat-treated in embodiment 1 is adjusted to room temperature, remaining is same as Example 1, here no longer
It repeats.
The graphene film number of plies of the product of embodiment 1 to 5 and comparative example 1 is characterized, acquired results are shown in Table 1：
Table 1：Include the graphene film number of plies test result of the material prepared by embodiment 1-5 and comparative example.
| Project | Heat treatment temperature (DEG C) | The product graphene film number of plies |
| Embodiment 1 | 300 | 3 |
| Embodiment 2 | 200 | 6 |
| Embodiment 3 | 500 | 8 |
| Embodiment 4 | 800 | 7 |
| Embodiment 5 | 1000 | 5 |
| Comparative example 1 | 25 | 0 |
As shown in table 1：Heat treatment temperature has a significant impact to the stripping of graphene sheet layer, when treatment temperature is too low, stripping
From not enriching, single-layer graphene cannot be formed；When treatment temperature is excessively high, the graphene sheet layer formed after stripping can further stone
Mo Hua.By probing into above, it has been found that：Heat treatment temperature has a significant impact to the stripping tool of graphene.
Embodiment 6：The temperature of 1 high temperature of embodiment processing is adjusted to 1000 DEG C, remaining is same as Example 1, here
It repeats no more.
Embodiment 7：The temperature of 1 high temperature of embodiment processing is adjusted to 1800 DEG C, remaining is same as Example 1, here
It repeats no more.
Embodiment 8：The temperature of 1 high temperature of embodiment processing is adjusted to 2500 DEG C, remaining is same as Example 1, here
It repeats no more.
Embodiment 9：The temperature of 1 high temperature of embodiment processing is adjusted to 3000 DEG C, remaining is same as Example 1, here
It repeats no more.
Comparative example 2：The temperature of 1 high temperature of embodiment processing is adjusted to room temperature, remaining is same as Example 1, here not
It repeats again.
Electrochemical property test：
By embodiment 1, electrode is made in the local graphitized material prepared by 6-9 and comparative example 2, is pressed in collector molybdenum foil
On, aluminium ion battery is formed with ionic liquid (1- ethyl -3- methylimidazolium chlorides aluminium salt), the aluminium flake of just extremely 0.1mm thickness,
Electro-chemical test is carried out to the battery.After high-temperature process temperature, the specific capacity of degree of graphitization and battery and 5000 cycles
Capacity retention ratio, as shown in table 2.
Table 2：Include the performance test results of the aluminium ion battery of material prepared by embodiment 1,6-9 and comparative example 2.
As shown in table 2：High-temperature process temperature has degree of graphitization and final electrode specific capacity and cycle conservation rate very big
It influences, when treatment temperature is too low, degree of graphitization is not enriched, and is unfavorable for aluminum ions insertion, causes specific capacity relatively low；Work as place
When the temperature is excessively high, the piece number of plies is excessive after graphitization for reason, is unfavorable for aluminium ion diffusion, causes high rate performance relatively low.By visiting above
Study carefully, it has been found that：The degree of graphitization of the graphited graphene derived material for the treatment of temperature local area and its aluminium ion of assembling
Battery performance tool has a significant impact.
Wherein, the graphited graphene derived material of local that prepared by embodiment 1 is applied to the charge and discharge in aluminium ion battery
Electric curve is as shown in Figure 2.
Embodiment 10：Inertia protection gas in embodiment 1 is adjusted to nitrogen, remaining is same as Example 1, no longer superfluous here
It states.
Embodiment 11：Inertia protection gas in embodiment 1 is adjusted to helium, remaining is same as Example 1, no longer superfluous here
It states.
By embodiment 1, electrode is made in the local graphitized material prepared by 10-11, is pressed on collector molybdenum foil, with ion
Liquid (1- ethyl -3- methylimidazolium chlorides aluminium salt) forms aluminium ion battery, the aluminium foil of just extremely 0.1mm thickness, to the battery
Carry out electro-chemical test.Capacity after high-temperature process temperature, the specific capacity of degree of graphitization and battery and 5000 cycles is protected
Holdup, as shown in table 3.
Table 3：Include the performance test results of the aluminium ion battery of material prepared by embodiment 1-3.
As shown in table 3, very little, electrode material are influenced to gained grapheme material using inert atmosphere in high-temperature process
Embody higher capacity and excellent multiplying power property.Therefore, this to grapheme material graphitizing method to different heat
Processing atmosphere also has certain universality.
Embodiment 12：The time of 1 high temperature of embodiment processing is adjusted to 0.5h, remaining is same as Example 1, here not
It repeats again.
Embodiment 13：The time of 1 high temperature of embodiment processing is adjusted to 1.5h, remaining is same as Example 1, here not
It repeats again.
Embodiment 14：The time of 1 high temperature of embodiment processing is adjusted to 2h, remaining is same as Example 1, here no longer
It repeats.
Embodiment 15：The time of 1 high temperature of embodiment processing is adjusted to 3h, remaining is same as Example 1, here no longer
It repeats.
Comparative example 3
The time of 1 high temperature of embodiment processing is adjusted to 0h, remaining is same as Example 1, and which is not described herein again.
By embodiment 1, electrode is made in the local graphitized material prepared by 12-15 and comparative example 3, is pressed in collector molybdenum foil
On, aluminium ion battery is formed with ionic liquid (1- ethyl -3- methylimidazolium chlorides aluminium salt), the aluminium foil of just extremely 0.1mm thickness,
Electro-chemical test is carried out to the battery.After high-temperature process temperature, the specific capacity of degree of graphitization and battery and 5000 cycles
Capacity retention ratio, as shown in table 4.
Table 4：Include the performance test results of the aluminium ion battery of material prepared by embodiment 1,12-15 and comparative example 3.
As shown in table 4：There are degree of graphitization and final electrode specific capacity and cycle conservation rate in the high-temperature process time very big
Influence, when treated between it is too short when, degree of graphitization is not enriched, and aluminum ions insertion is unfavorable for, and causes specific capacity relatively low；Work as place
When managing overlong time, the piece number of plies is excessive after graphitization, is unfavorable for aluminium ion diffusion, causes high rate performance relatively low.By visiting above
Study carefully, it has been found that：The degree of graphitization of the graphited graphene derived material of processing time local area and its aluminium ion of assembling
Battery performance tool has a significant impact.
Embodiment 16
A kind of graphited graphene derived material of aluminium ion battery local is present embodiments provided, the material is by 7 layers
Graphene sheet layer three-dimensional overlaps, and the degree of graphitization of graphene sheet layer is 85%, and the lateral dimension of graphene sheet layer is
10 μm~100 μm, the specific surface area of graphene sheet layer is 1300m2·g-1。
The material is prepared using high-temperature process method：
Step 1: graphite oxide is mixed with reducing agent hydrazine hydrate, with solvent water dissolution, it is ultrasonically treated 30 minutes, oxidation
The molar ratio of graphite and reducing agent is 1：0.1, the mass ratio of the graphite oxide and solvent is 1：10；
Step 2: centrifugation, take precipitation, cleaning, dry 5h at 70 DEG C after obtain the graphited graphene derived material of local.
Embodiment 17
A kind of graphited graphene derived material of aluminium ion battery local is present embodiments provided, the material is by 8 layers
Graphene sheet layer three-dimensional overlaps, and the degree of graphitization of graphene sheet layer is 80%, and the lateral dimension of graphene sheet layer is
10 μm~100 μm, the specific surface area of graphene sheet layer is 1600m2·g-1。
The material is prepared using high-temperature process method：
Step 1: graphite oxide is mixed with reducing agent sodium ascorbate, dissolved with solvent methanol, is ultrasonically treated 40 points
The molar ratio of clock, graphite oxide and reducing agent is 1：0.2, the mass ratio of the graphite oxide and solvent is 1：15；
Step 2: centrifugation, take precipitation, cleaning, dry 7h at 80 DEG C after obtain the graphited graphene derived material of local.
Embodiment 18
A kind of graphited graphene derived material of aluminium ion battery local is present embodiments provided, the material is by 10 layers
Graphene sheet layer three-dimensional overlaps, and the degree of graphitization of graphene sheet layer is 90%, and the lateral dimension of graphene sheet layer is
10 μm~100 μm, the specific surface area of graphene sheet layer is 1700m2·g-1。
The material is prepared using high-temperature process method：
Step 1: graphite oxide is mixed with reducing agent glucose, dissolved, is ultrasonically treated 20 minutes, oxygen with etoh solvent
Graphite and the molar ratio of reducing agent are 1：0.4, the mass ratio of the graphite oxide and solvent is 1：12；
Step 2: centrifugation, take precipitation, cleaning, dry 3h at 85 DEG C after obtain the graphited graphene derived material of local.
By embodiment 1, electrode is made in the local graphitized material prepared by 12-15 and comparative example 3, is pressed in collector molybdenum foil
On, aluminium ion battery is formed with ionic liquid (1- ethyl -3- methylimidazolium chlorides aluminium salt), the aluminium foil of just extremely 0.1mm thickness,
Electro-chemical test is carried out to the battery.After high-temperature process temperature, the specific capacity of degree of graphitization and battery and 5000 cycles
Capacity retention ratio, as shown in table 4.
Table 4：Include the performance test results of the aluminium ion battery of material prepared by embodiment 16-18.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, embodiment of above are only for interpreting the claims.Right protection scope of the present invention is not limited to specification.Appoint
What those familiar with the art is in the technical scope of present disclosure, the variation or replacement that can be readily occurred in,
It is included within the scope of the present invention.
Claims (10)
1. a kind of graphited graphene derived material of aluminium ion battery local, it is characterised in that：The material is by 3 ~ 10 layers
Graphene sheet layer three-dimensional overlaps, and the degree of graphitization of graphene sheet layer is 10% ~ 99%, the transverse direction of the graphene sheet layer
Size is 10 μm ~ 100 μm, and the material is prepared by high-temperature process method or method of chemical treatment.
2. the graphited graphene derived material of aluminium ion battery local according to claim 1, it is characterised in that：Institute
The specific surface area for stating graphene sheet layer is 100 m2·g-1~3000 m2·g-1。
3. the graphited graphene derived material of aluminium ion battery local according to claim 1, it is characterised in that：Institute
The degree of graphitization for stating graphene sheet layer is 20% ~ 75%.
4. the graphited graphene derived material of aluminium ion battery local according to claim 1, which is characterized in that institute
It states high-temperature process method and includes at least following steps：
Step 1: the preparation of grapheme material：Graphite oxide is heat-treated under inert gas protection, is obtained with monolithic
The grapheme material of layer；
Step 2: the single-layer graphene obtained by step 1 is heat-treated h hours under inert gas protection, under temperature T, obtain
To the graphited graphene derived material of local.
5. the graphited graphene derived material of aluminium ion battery local according to claim 4, which is characterized in that step
The temperature of heat treatment in rapid one is 300 DEG C ~ 1200 DEG C.
6. the graphited graphene derived material of aluminium ion battery local according to claim 4, which is characterized in that step
Inert gas described in rapid one and two is at least one of nitrogen, argon gas and helium；Temperature T described in step 2 is
1000℃~3000℃；H described in step 2 is 0.5 ~ 3.
7. the graphited graphene derived material of aluminium ion battery local according to claim 1, which is characterized in that institute
It states method of chemical treatment and includes at least following steps：
Step 1: graphite oxide is mixed with reducing agent, dissolved, is ultrasonically treated t minutes with solvent；
Step 2: obtaining the graphited graphene derived material of local after centrifuging, taking precipitation, cleaning, drying.
8. the graphited graphene derived material of aluminium ion battery local according to claim 7, which is characterized in that step
Reducing agent described in rapid one is at least one of hydrazine hydrate, sodium ascorbate, glucose；The solvent is water, methanol, second
At least one of alcohol, hexamethylene, the time t of the supersound process are 10 ~ 60min, and the graphite oxide and reducing agent rub
You are than being 1：（0.05~0.5）, the mass ratio of the graphite oxide and solvent is 1：（5~20）.
9. the graphited graphene derived material of aluminium ion battery local according to claim 7, which is characterized in that step
Dry temperature is 60 DEG C ~ 90 DEG C in rapid two, and the dry duration is 1h ~ 10h.
10. a kind of aluminium ion battery, including anode, cathode, electrolyte and positioned at the anode and being isolated between the cathode
Film, it is characterised in that：Active material used in the cathode is claim 1 to 9 any one of them material, the electrolysis
Contain AlCl in liquid4 -。
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