CN102467990B - Positive electrode as well as preparation method and application thereof - Google Patents
Positive electrode as well as preparation method and application thereof Download PDFInfo
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- CN102467990B CN102467990B CN201010536812XA CN201010536812A CN102467990B CN 102467990 B CN102467990 B CN 102467990B CN 201010536812X A CN201010536812X A CN 201010536812XA CN 201010536812 A CN201010536812 A CN 201010536812A CN 102467990 B CN102467990 B CN 102467990B
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Abstract
The invention discloses a positive electrode, which comprises a positive electrode substrate and a positive electrode coating combined on the surface of the positive electrode substrate, wherein the positive electrode coating comprises a graphene derivant material, conductive agent and binding agent, and the graphene derivant material has the following molecular structural formula. The preparation method of the positive electrode comprises the following steps: obtaining the graphene derivant material, the conductive agent, the binding agent and the positive electrode substrate; mixing the graphene derivant material, the conductive agent and the binding agent to obtain positive electrode coating liquid; coating the positive electrode coating liquid onto the surface of the positive electrode substrate; and drying to obtain the positive electrode. According to the positive electrode disclosed by the invention, faradic pseudocapacitance and double layer capacitance can be provided, and larger energy density and power density can be provided. The preparation method of the positive electrode has the advantages of simple working procedure and low requirement on the equipment and is suitable for industrial production, production efficiency is improved, and production cost is lowered.
Description
Technical field
The invention belongs to technical field of electrochemistry, relate to a kind of positive electrode and preparation method thereof and application specifically.
Background technology
Since the strong K of the peace moral of Univ Manchester UK sea nurse (Andre K.Geim) etc. was prepared grapheme material in 2004.Because its particular structure and photoelectric property have been subjected to people and have paid attention to widely.Mono-layer graphite has big specific area, good conduction, heat conductivility and low thermal coefficient of expansion and be considered to desirable material.Especially its high conductivity matter, the structural property of big specific surface character and the nanoscale of its monolayer two dimension can be widely used in electrode material.Therefore, grapheme material is used as the electrode material of ultracapacitor and lithium ion battery.
Nineteen ninety, Japanese Sony Corporation successfully releases commercial lithium rechargeable battery first, and the active material of its positive electrode adopts cobalt acid lithium (LiCoO
2).Because cobalt acid lithium manufacture craft is simple, material thermal stability performance is good, have extended cycle life, therefore, be still topmost lithium ion secondary battery anode material up to now, but the shortcoming that it exists is expensive, poisonous, security performance is not high.Afterwards, along with to the improving constantly of the low cost of battery, high-energy-density, good cycle, high security and environmentally friendly etc. requirement, lithium ion secondary battery anode material steps into the stage that develops rapidly.Except the cobalt acid lithium of layer structure, the LiNiO of transition metal oxide such as layer structure
2LiMn with spinel structure
2O
4Active material as positive electrode is widely used.Wherein, LiNiO
2Theoretical capacity is than higher (275mAh/g), but thermally-stabilised poor, preparation difficulty, the product that easily side reaction, generation takes place influence capacity and the cycle performance of battery; And LiMn
2O
4Cycle performance is poor, specific capacity is lower (theoretical specific capacity only is about 148mAh/g), and this mainly is because Mn
3+Disproportionation and Jahn-Telle distortion effect easily take place.The LiMPO of olivine structural
4The compound of (M=Fe, Co, Mn, Ni etc.) polyanion is because its special structure causes this class material to have extremely low electronic conductivity and ions diffusion speed.No matter top which class positive electrode all can not satisfy high power and the requirement of energy density.
Lithium ion battery has high energy density, but its power density is lower.How making system have high energy density and higher power density simultaneously is present stage be badly in need of solving one very important problem.In order to improve the power density of lithium ion battery, adopt the method for nanometer and raising conductance, but its degree that improves power density is limited more.
Summary of the invention
The objective of the invention is to overcome the above-mentioned deficiency of prior art, provide a kind of and can have wild goose electric capacity and electric double layer capacitance, and positive electrode than macro-energy density and power density and preparation method thereof is provided.
And, the application of above-mentioned positive electrode in lithium ion battery and/or ultracapacitor.
In order to realize the foregoing invention purpose, technical scheme of the present invention is as follows:
A kind of positive electrode comprises anodal substrate and the anodal coating that is combined in described anodal substrate surface, and described anodal coating comprises Graphene derivant material, conductive agent and binding agent; Described Graphene derivant material molecular structural formula is as follows:
And a kind of positive electrode preparation method comprises the steps:
Obtain Graphene derivant material, conductive agent, binding agent and anodal substrate, wherein, described Graphene derivant material molecular structural formula is as follows:
Graphene derivant material, conductive agent and binding agent are mixed, be prepared into anodal coating liquid;
Anodal coating liquid is coated to anodal substrate surface, and drying obtains described positive electrode.
Further, the application of above-mentioned positive electrode provided by the invention in lithium ion battery and/or ultracapacitor.
(C=O), make this Graphene derivant material have big theoretical capacity, environmentally friendly, energy consumes less and surface area is big owing to contain carbonyl in the contained Graphene derivant material molecular structure in the anodal coating of positive electrode of the present invention.When containing this Graphene derivant material in the anodal coating of positive electrode, make positive electrode have wild goose electric capacity and electric double layer capacitance, and bigger energy density and power density is provided.The anodal coating liquid that the positive electrode preparation only need form Graphene derivant material, conductive agent and binding agent mixed preparing is coated on the anodal substrate and gets final product, the its preparation method operation is simple, and is low for equipment requirements, improved production efficiency, reduce production cost, be suitable for suitability for industrialized production.
Description of drawings
Fig. 1 is the positive electrode structural representation of the embodiment of the invention;
Fig. 2 is the Graphene derivant material molecular structural formula of the embodiment of the invention;
Fig. 3 is the positive electrode preparation method process chart of the embodiment of the invention;
Fig. 4 is Graphene derivant material preparation method process chart in the anodal coating of positive electrode of the embodiment of the invention.
The charging and discharging curve figure of Fig. 5 embodiment 1 gained lithium ion battery under the 1A/g condition.
Embodiment
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearer, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explaining the present invention, and be not used in restriction the present invention.
The embodiment of the invention provides a kind of positive electrode, and as shown in Figure 1, this positive electrode comprises anodal substrate 1 and be combined in the anodal coating 2 of described anodal substrate surface that described anodal coating comprises Graphene derivant material, conductive agent and binding agent; Described Graphene derivant material molecular structural formula is as follows, sees also Fig. 2 simultaneously.
Like this, (C=O), make this Graphene derivant material have big theoretical capacity, environmentally friendly, energy consumes less and surface area is big owing to contain carbonyl in the Graphene derivant material molecular structure.When containing the Graphene derivant material in the anodal coating of positive electrode, make positive electrode that wild goose electric capacity and electric double layer capacitance effectively are provided, and bigger energy density and power density is provided.
Particularly, in the anodal coating 2 of this positive electrode, the mass content of Graphene derivant material, conductive agent and binding agent is respectively x, y, z, and wherein, x, y, z preferably satisfy: x+y+z=1,0＜x, y, z＜1.The anodal coating that Graphene derivant material, conductive agent and the binding agent of this proportion prepared makes embodiment of the invention positive electrode more can effectively provide wild goose electric capacity and electric double layer capacitance, bigger energy density and power density, thus embodiment of the invention positive electrode performance further improved.The thickness of the anodal coating 2 of this positive electrode adopts this area class thickness commonly used.
The embodiment of the invention also provides above-mentioned positive electrode preparation method, and this method technological process is seen shown in Figure 3, simultaneously referring to Fig. 1, comprises the steps:
S1. obtain Graphene derivant material, conductive agent, binding agent and anodal substrate 1, wherein, described Graphene derivant material molecular structural formula is as follows:
S2. Graphene derivant material, conductive agent and binding agent are mixed, be prepared into anodal coating liquid;
S3. anodal coating liquid is coated to anodal substrate 1 surface, drying obtains described positive electrode.
By above-mentioned S1 to S3 as can be known, the anodal coating liquid that this positive electrode preparation only need form Graphene derivant material, conductive agent and binding agent mixed preparing is coated on the anodal substrate and gets final product, and this positive electrode preparation method operation is simple, low for equipment requirements, the production efficiency height is suitable for suitability for industrialized production.
Particularly, in above-mentioned positive electrode preparation method's the S1 step, conductive agent is preferably acetylene black, binding agent is preferably polyvinylidene fluoride (PVDF), anodal substrate 1 is preferably aluminium flake, and certainly, conductive agent, binding agent and anodal substrate 1 also can adopt this area material commonly used to replace.
In the S1 step, Graphene derivant material acquisition methods process chart as shown in Figure 4, its acquisition methods is preferably as follows:
S11. obtain multi-walled carbon nano-tubes or natural flake graphite;
S12. under acid condition, described multi-walled carbon nano-tubes or natural flake graphite are mixed stirring with liquor potassic permanganate, oxidation reaction is carried out in heating then;
S13. after treating that oxidation reaction finishes, product is carried out cancellation handle, filter then, washing, drying obtains described Graphene derivant material.
Further, in the S11 step of above-mentioned Graphene derivant material acquisition methods, multi-walled carbon nano-tubes or natural flake graphite can commercially obtain.
In above-mentioned Graphene derivant material preparation method's the S12 step, the process that oxidation reaction is carried out in described heating preferably includes the following step: after handling 1～12h earlier under acid condition in described multi-walled carbon nano-tubes or the natural flake graphite, add liquor potassic permanganate again, at room temperature stir 1～3h, be heated to 55 ℃～70 ℃ then and carry out oxidation reaction 1～5h.
In the step of this oxidation reaction, the mass ratio of multi-walled carbon nano-tubes or natural flake graphite and described potassium permanganate is preferably 1: 5～and 20, liquor potassic permanganate concentration is preferably 500%; Acid under multi-walled carbon nano-tubes or natural flake graphite and the described acid condition be preferably the strong acid that adds 20～50ml in every 0.5g multi-walled carbon nano-tubes or the natural flake graphite with magnitude relation.Wherein, the acid under the acid condition can be organic acid and/or inorganic acid, and organic acid can be sulfonic acid, and inorganic acid can be the concentrated sulfuric acid, concentrated hydrochloric acid and/or red fuming nitric acid (RFNA).Certainly, also Bronsted acid commonly used of the acid under the acid condition.The existence of this acid is for oxidation reaction provides sour environment, strengthens the oxidizability of potassium permanganate.In addition, adding acid earlier is to carrying out intercalation with the natural flake graphite interlayer between multi-walled carbon nano-tubes (MWCNT) tube wall and tube wall, make adding potassium permanganate (KMnO as concentrated sulfuric acid main purpose
4) after, can make every layer of nanotube and natural flake graphite better oxidized.
The chemical equation of this oxidation reaction is as follows:
In the above-mentioned chemical equation, compound 1 is multi-walled carbon nano-tubes or natural flake graphite source reactant; Compound 2,3, the 4th, the intermediate product of this oxidation reaction; The end product of compound 5 oxidation reactions, i.e. embodiment of the invention Graphene derivant material.
In above-mentioned Graphene derivant material preparation method's the S13 step, cancellation is handled to be preferably the product of oxidation reaction gained poured in the ice that contains hydrogen peroxide and is mixed.Wherein, the content of hydrogen peroxide in ice should capacity, its content at least should the product with the oxidation reaction gained in unnecessary potassium permanganate just consume fully.The purpose that cancellation is handled is to consume unnecessary potassium permanganate in the product of oxidation reaction gained.The ice that contains hydrogen peroxide when preferred employing carries out cancellation when handling, and the reaction mechanism of hydrogen peroxide and potassium permanganate is as follows:
2MnO
4 -+5H
2O
2+6H
+＝2Mn
2++5O
2↑+8H
2O
In this S13 step, filter operation and be preferably handling product through cancellation by the PTFE membrane filtration, collect the solid of gained.Certainly filter operation and can also adopt other modes, as suction filtration etc.
In this S13 step, washing procedure is that the solid of gained is after filtration washed with water earlier, again with the washing of low boiling water-miscible organic solvent.Wherein, the purpose of washing is salt and the inorganic ions of removing in the product, low boiling water-miscible organic solvent washing is preferably at least a in ethanol, methyl alcohol, the acetonitrile in order to remove the organic substance low boiling water-miscible organic solvent that may exist in the product, more preferably ethanol, because ethanol is nontoxic, economy.
In this S13 step, drying process is that solid after washing is preferably placed 40-60 ℃ of following vacuumize 24-72h.This drying both can more effectively have been removed and filtered the gained solid to be the moisture in the Graphene derivant material and to remove low boiling water-miscible organic solvent residual in washing process, can also prevent effectively that the Graphene derivant material is in this contaminated and possible oxidation.Certainly other drying modes also can reach the purpose of dry Graphene derivant material, as dry low temperature drying etc.
Particularly, in above-mentioned positive electrode preparation method's the S2 step, the mass content in the anodal coating liquid of Graphene derivant material, conductive agent and binding agent is x, y, z, and wherein, x, y, z preferably satisfy: x+y+z=1,0＜x, y, z＜1.Graphene derivant material, conductive agent and the binding agent of this proportion anodal coating make performance that embodiment of the invention positive electrode has as mentioned above, in order to save length, do not repeat them here.
Particularly, in above-mentioned positive electrode preparation method's the S3 step, the method that anodal coating liquid is coated to anodal substrate 1 surface can be modes such as brushing, dip-coating or spraying.No matter take any mode, so long as anodal coating liquid is applied anodal substrate 1 surface, all within the category of embodiment of the invention technical scheme.Certainly, anodal coating liquid is coated to anodal substrate 1 surface, and after drying, can also carries out operations such as roll extrusion, cut-parts, the actual concrete required positive electrode of preparation.
Because above-mentioned positive electrode has above-mentioned performance, therefore, the positive electrode of the embodiment of the invention can be used in lithium ion battery and/or ultracapacitor.As, when positive electrode was used in lithium ion battery, redox reaction can take place by its Li+ that gets in betatopic and the lithium ion battery in this positive electrode, thereby can improve the lithium ion battery discharge performance.
Now in conjunction with instantiation, the present invention is further elaborated.
The positive electrode structure as shown in Figure 1, this positive electrode comprises anodal substrate 1 and is combined in the anodal coating 2 of anodal substrate surface.Wherein, anodal coating 2 comprises Graphene derivant material, conductive agent and binding agent; Graphene derivant material molecular structural formula is as follows,
The preparation method is as follows for this positive electrode, simultaneously referring to Fig. 3:
(1) obtain Graphene derivant material, acetylene black, polyvinylidene fluoride, the anodal substrate 1 of aluminium, wherein, described Graphene derivant material molecular structure such as above-mentioned;
(2) Graphene derivant material, conductive agent and binding agent are mixed by 0.84: 0.08: 0.08 mass ratio, be prepared into anodal coating liquid;
(3) anodal coating liquid is sprayed to anodal substrate 1 surface, drying, roll extrusion, cut-parts obtain described positive electrode.
Have bigger confession wild goose electric capacity and electric double layer capacitance through recording this positive plate, and bigger energy density and power density.
Wherein, the preparation method is as follows for the Graphene derivant material, simultaneously referring to Fig. 4:
(11) obtain multi-walled carbon nano-tubes;
(12) add 98% the concentrated sulfuric acid in the multi-walled carbon nano-tubes earlier by adding the 30ml concentrated sulfuric acid in every 0.5g multi-walled carbon nano-tubes, add potassium permanganate in the ratio of adding 6g potassium permanganate in every 0.5g natural flake graphite again after 6 hours, mixed under the room temperature 2 hours, and heated 60 ℃ then and carried out oxidation reaction 3 hours;
(13) treat that above-mentioned oxidation reaction finishes after, the product of oxidation reaction gained is contained cancellation in the ice of hydrogen peroxide, filter then, adopt water, ethanol washing successively, in 50 ℃ of following vacuumizes 36 hours, obtain the Graphene derivant material of following structural formula.
The application of positive electrode in lithium ion battery: positive electrode and the lithium sheet of present embodiment 1 preparation are assembled in the lithium ion housing, adopt polypropylene diaphragm to separate between positive electrode and the negative electrode, and in housing, inject il electrolyte, adopt the existing method encapsulation in this area, obtain lithium ion battery.
The lithium ion battery discharge performance resolution chart of present embodiment preparation is seen Fig. 5, the charge/discharge capacity of this lithium ion battery under the 1A/g condition is up to 120mAh/g, because Graphene derivative positive electrode can provide wild goose electric capacity and electric double layer capacitance simultaneously, fake capacitance has high energy density, electric double layer capacitance has good high rate during charging-discharging, so gained material capacity under big electric current 1A/g condition can reach 120mAh/g, cycle performance is better.
The positive electrode structure is identical with embodiment 1, and this positive electrode performance is similar to positive electrode among the embodiment 1.
The preparation method is as follows for this positive electrode, simultaneously referring to Fig. 3:
(1) obtain Graphene derivant material, acetylene black, polyvinylidene fluoride, the anodal substrate 1 of aluminium, wherein, among described Graphene derivant material molecular structure such as the above-mentioned embodiment 1;
(2) Graphene derivant material, conductive agent and binding agent are mixed by 0.94: 0.04: 0.02 mass ratio, be prepared into anodal coating liquid;
(3) anodal coating liquid is sprayed to anodal substrate 1 surface, drying, roll extrusion, cut-parts obtain described positive electrode.
Have bigger confession wild goose electric capacity and electric double layer capacitance through recording this positive plate, and bigger energy density and power density.
Wherein, the preparation method is as follows for the Graphene derivant material, simultaneously referring to Fig. 4:
(11) obtain natural flake graphite;
(12) in natural flake graphite, add analytically pure red fuming nitric acid (RFNA) by adding the 20ml red fuming nitric acid (RFNA) in every 0.5g natural flake graphite earlier, add potassium permanganate in the ratio of adding 2.5g potassium permanganate in every 0.5g natural flake graphite again after 1 hour, mixed under the room temperature 3 hours, and heated 55 ℃ then and carried out oxidation reaction 5 hours;
(13) treat that above-mentioned oxidation reaction finishes after, the product of oxidation reaction gained is contained cancellation in the ice of hydrogen peroxide, suction filtration adopts water, methanol wash successively then, in 40 ℃ of following vacuumizes 72 hours, obtains the Graphene derivant material of following structural formula.
The application of positive electrode in lithium ion battery: positive electrode and the lithium titanate of present embodiment 2 preparations are assembled in the lithium ion housing, adopt polypropylene diaphragm to separate between positive electrode and the negative electrode, and in housing, inject il electrolyte, adopt the existing method encapsulation in this area, obtain lithium ion battery.
Embodiment 3
The positive electrode structure is identical with embodiment 1, and this positive electrode performance is similar to positive electrode among the embodiment 1.
The preparation method is as follows for this positive electrode, simultaneously referring to Fig. 3:
(1) obtain Graphene derivant material, acetylene black, polyvinylidene fluoride, the anodal substrate 1 of aluminium, wherein, among described Graphene derivant material molecular structure such as the above-mentioned embodiment 1;
(2) Graphene derivant material, conductive agent and binding agent are mixed by 0.70: 0.15: 0.15 mass ratio, be prepared into anodal coating liquid;
(3) anodal coating liquid is sprayed to anodal substrate 1 surface, drying, roll extrusion, cut-parts obtain described positive electrode.
Have bigger confession wild goose electric capacity and electric double layer capacitance through recording this positive plate, and bigger energy density and power density.
Wherein, the preparation method is as follows for the Graphene derivant material, simultaneously referring to Fig. 4:
S31. obtain multi-walled carbon nano-tubes;
S32. in multi-walled carbon nano-tubes, add sulfonic acid by adding 50ml sulfonic acid in every 0.5g multi-walled carbon nano-tubes earlier, press again after 12 hours and add the 10g liquor potassic permanganate in every 0.5g natural flake graphite, mixed 1 hour, and heated 70 ℃ then and carried out oxidation reaction 1 hour;
S33. after treating that above-mentioned oxidation reaction finishes, the product of oxidation reaction gained is contained cancellation in the ice of hydrogen peroxide, adopt the PTFE membrane filtration then, adopt water, acetonitrile washing successively, in 60 ℃ of following vacuumizes 24 hours, obtain the Graphene derivant material of following structural formula.
The application of positive electrode in ultracapacitor: positive electrode and the existing negative electrode of present embodiment 3 preparations are assembled in the lithium ion housing, and in housing, inject il electrolyte, adopt the existing method encapsulation in this area, obtain ultracapacitor.
The above only is preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. a positive electrode comprises anodal substrate and the anodal coating that is combined in described anodal substrate surface, and described anodal coating comprises Graphene derivant material, conductive agent and binding agent; Described Graphene derivant material molecular structural formula I is as follows:
2. positive electrode according to claim 1, it is characterized in that: the mass content of described Graphene derivant material, conductive agent and binding agent is respectively x, y, z, wherein, x+y+z=1,0＜x, y, z＜1.
3. a positive electrode preparation method comprises the steps:
Obtain Graphene derivant material, conductive agent, binding agent and anodal substrate, wherein, described Graphene derivant material molecular structural formula I is as follows:
Graphene derivant material, conductive agent and binding agent are mixed, be prepared into anodal coating liquid;
Anodal coating liquid is coated to anodal substrate surface, and drying obtains described positive electrode.
4. positive electrode preparation method according to claim 3, it is characterized in that: the mass content of described Graphene derivant material, conductive agent and binding agent is x, y, z, wherein, x+y+z=1,0＜x, y, z＜1.
5. positive electrode preparation method according to claim 3, it is characterized in that: described Graphene derivant material acquisition methods is as follows:
Obtain multi-walled carbon nano-tubes or natural flake graphite;
Under acid condition, described multi-walled carbon nano-tubes or natural flake graphite are mixed stirring with liquor potassic permanganate, oxidation reaction is carried out in heating then; Particularly, after elder generation handles 1～12h in described multi-walled carbon nano-tubes or the natural flake graphite under acid condition, add liquor potassic permanganate again, at room temperature stir 1～3h, be heated to 55 ℃～70 ℃ then and carry out oxidation reaction 1～5h; Wherein, the mass ratio of described multi-walled carbon nano-tubes or natural flake graphite and described potassium permanganate is 1: 5～20, the acid under described multi-walled carbon nano-tubes or natural flake graphite and the described acid condition be the acid of adding 20～50ml in every 0.5g multi-walled carbon nano-tubes or the natural flake graphite with magnitude relation;
After treating that oxidation reaction finishes, product is carried out cancellation handle, filter then, washing, drying obtains described Graphene derivant material.
6. positive electrode preparation method according to claim 5 is characterized in that: described washing is that the solid of gained is after filtration washed with water earlier, again with the washing of low boiling water-miscible organic solvent;
Described drying is that the solid after washing is placed 40-60 ℃ of following vacuumize 24-72h.
7. positive electrode preparation method according to claim 6 is characterized in that: described low boiling water-miscible organic solvent is at least a in ethanol, methyl alcohol, the acetonitrile.
8. the application of positive electrode according to claim 1 and 2 in lithium ion battery and/or ultracapacitor.
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