CN110010897B - Graphene lithium battery positive electrode slurry, preparation method and lithium battery positive electrode piece - Google Patents
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Abstract
The invention discloses a graphene lithium battery positive electrode slurry which comprises raw materials of a positive electrode active substance, a conductive agent, a binder and azomethidone, wherein the conductive agent is formed by combining a carbon conductive material and a negative thermal expansion material, the carbon conductive material contains graphene, and the negative thermal expansion material is ZrW2O8And/or hetero-metal ion doped ZrW2O8. The positive electrode slurry of the lithium battery is added with a negative thermal expansion material ZrW2O8And/or hetero-metal ion doped ZrW2O8In a charging and discharging state, the temperature of the battery rises, the positive active material expands under heating, micro cracks in the negative thermal expansion material and contraction gaps between the negative thermal expansion material and the positive active material and between the negative thermal expansion material and the carbon conductive material are increased, the diffusion path of lithium ions is increased, the diffusion capacity of the lithium ions in the positive electrode is improved, and the rate performance of the battery is improved. The invention also discloses a preparation method of the graphene lithium battery positive electrode slurry and a lithium battery positive electrode plate.
Description
Technical Field
The invention relates to the technical field of lithium batteries, in particular to graphene lithium battery positive electrode slurry, a preparation method and a lithium battery positive electrode piece.
Background
The lithium battery is a battery which uses lithium metal or lithium alloy as a positive electrode material and uses a non-aqueous electrolyte solution, during the charging process, the active substance of the positive electrode material undergoes a phase change reaction under the condition of potential, lithium ions are released from the crystal structure of the positive electrode material, gradually separate from crystals, are transferred to a negative electrode material through the electrolyte and are embedded, and meanwhile, electrons are also removed from the interior of the crystals and transferred to the negative electrode through an external circuit. The discharging process is the reverse of the charging process. The crystal structures of the positive electrode materials before and after lithium intercalation are similar. The commonly used active material of the positive electrode material comprises lithium iron phosphate, a ternary material of iron manganese lithium cobaltate, lithium nickel manganate and lithium manganate, wherein the most commonly used lithium iron phosphate has good thermal stability and chemical stability. Lithium iron phosphate as a positive electrode material has disadvantages of low electron conductivity and low ion conductivity. The current optimization direction mainly comprises surface modification and ion nanocrystallization, wherein the surface modification refers to coating carbon, metal, conductive polymer and other materials on the surface of a material in a certain mode, and the ion electron transmission rate of the material can be improved.
The graphene is applied to the lithium battery anode material in the prior art such as CN104409729A, CN107528054A and CN107546389A, and the gram capacity and the multiplying power of the lithium battery anode obtained after the graphene is added are both improved. However, the following technical problems exist in the test: the sheet structure of the graphene can hinder the diffusion of lithium ions, so that the diffusion path of the lithium ions is prolonged, the diffusion impedance of the lithium ions is increased, and the rate performance of the battery is reduced.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the lithium battery anode slurry, which has a negative thermal expansion material at the use temperature of the battery, the battery releases heat in the charging and discharging process, the negative thermal expansion material positioned between graphene sheets shrinks in at least one direction, and the lithium ion diffusion capacity is improved.
The technical scheme of the invention is as follows: the graphene lithium battery positive electrode slurry comprises raw materials of a positive electrode active substance, a carbon conductive material, a binder and azomethidone, and is characterized by further comprising a negative thermal expansion material, wherein the carbon conductive material contains graphene, and the negative thermal expansion material is ZrW2O8And/or hetero-metal ion doped ZrW2O8。
The optimized technical scheme is that the heterogeneous metal ion doped ZrW2O8The heterogeneous metal in (2) is one or the combination of more than two of aluminum, yttrium, ytterbium, tungsten and molybdenum.
The preferable technical scheme is that the graphene lithium battery positive electrode slurry according to claim 1 is characterized by comprising the following components in parts by weight: 92-96 parts of positive electrode active substance, 0.7-4 parts of carbon conductive material, 0.8-2.5 parts of binder, 0.3-2 parts of negative thermal expansion material and 36-43 parts of azomethyl pyrrolidone.
The preferred technical scheme is that the carbon conductive material is formed by combining acetylene black and graphene, and the weight ratio of the acetylene black to the graphene is 1: (0.8-1.3), wherein the diameter-thickness ratio of the graphene is not less than 500; the weight ratio of the graphene to the negative thermal expansion material is 1: (0.2-0.65).
The preferable technical scheme is that the anode active material is lithium iron phosphate, and the binder is polyvinylidene fluoride.
The invention also aims to provide a preparation method of the graphene lithium battery positive electrode slurry, which is characterized by comprising the following steps of:
s1: mixing the carbon conductive material, the negative thermal expansion material and the polar organic solvent to prepare a dispersion liquid, then placing the dispersion liquid in a ball milling tank for ball milling and mixing, removing the polar organic solvent, drying solid components in the dispersion liquid, and sieving to obtain conductive mixed powder;
s2: putting the conductive mixed powder obtained in the step S1 into a mold, placing the mold in a furnace chamber of a discharge plasma sintering furnace, and performing discharge plasma sintering treatment under the protection of inert gas to obtain conductive composite powder;
s3: and dissolving the binder in N-methyl pyrrolidone, adding the conductive composite powder obtained in the step S2, uniformly dispersing, adding the positive active substance, and uniformly mixing to obtain the finished product of the positive slurry of the lithium battery.
The preferable technical scheme is that the ball-to-material ratio of grinding balls subjected to S1 ball milling to powder in the dispersion liquid is 1: (1.2-1.6), wherein the weight ratio of the powder to the polar organic solvent in the dispersion is 1: (1.7-2.5) and the ball milling time is 24-48 h.
The preferred technical scheme is that the axial pressure in the furnace chamber of the discharge plasma sintering furnace is 40-60 Mpa, the sintering temperature is 630-680 ℃, the sintering time is 3-5 min, and the vacuum degree in the furnace chamber of the discharge plasma sintering furnace in the sintering process is 0.1-0.2 Pa.
The preferable technical scheme is that the polar organic solvent is an alcohol organic solvent of C2-C5.
The invention also aims to provide a lithium battery positive pole piece, which is characterized in that solid dry materials of the positive pole piece mainly comprise positive active substances, carbon conductive materials, adhesives and negative thermal expansion materials, wherein the carbon conductive materials contain graphene, and the negative thermal expansion materials are ZrW2O8And/or hetero-metal ion doped ZrW2O8(ii) a The compaction density of the positive pole piece is 2.1-2.3 g/cm3。
The invention has the advantages and beneficial effects that:
the positive electrode slurry of the lithium battery is added with a negative thermal expansion material ZrW2O8And/or hetero-metal ion doped ZrW2O8Under the charging and discharging state, the temperature of the battery is increased, the negative thermal expansion material is isotropically or anisotropically shrunk, namely, the negative thermal expansion material crystal is shrunk in at least one direction, the positive active material is heated to expand, microcracks in the negative thermal expansion material and shrinkage gaps among the positive active material and the carbon conductive material are increased, the diffusion path of lithium ions is increased, the diffusion capacity of the lithium ions in the positive electrode is improved, and the multiplying power performance of the battery is improved;
the preparation method of the graphene lithium battery positive electrode slurry comprises the steps of carrying out discharge plasma sintering treatment on a carbon conductive material and a negative thermal expansion material under the protection of inert gas, wherein the crystal of zirconium tungstate in the composite powder is complete, the adhesion between the zirconium tungstate and the carbon conductive material is stable, and a three-dimensional conductive layer formed by the positive electrode slurry is more stereoscopic and has good conductive performance and heat conduction performance.
Detailed Description
The following further describes embodiments of the present invention with reference to examples. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Positive electrode active material
The selection range of the positive electrode active material includes, but is not limited to, known lithium cobaltate, lithium manganate, lithium iron phosphate, lithium nickelate, layered lithium manganate, lithium manganese phosphate, lithium nickel cobalt manganate, and solid solution material, preferably common lithium iron phosphate.
Carbon conductive material
The carbon conductive material is used for forming a three-dimensional conductive network of the battery anode pole piece, and the selection and combination of the carbon conductive material are related to the internal resistance of the conductive network. The selection range comprises carbon nano tubes, conductive carbon black, acetylene black, graphite, Super P and graphene.
Negative thermal expansion material
ZrW2O8Having isotropic negative thermal expansion in the temperature range of the battery in use, foreign metal ions, e.g. doped ZrW2O8Including but not limited to ZrW doped with one of aluminum, yttrium, ytterbium, tungsten, molybdenum2O8ZrW codoped with two or more of aluminum, yttrium, ytterbium, tungsten and molybdenum2O8And doped ZrW with negative thermal expansion obtained by doping other metals2O8. The aluminum ions provide vacant orbital electrons and contribute to an increase in the electron diffusion ability, and therefore ZrW doped with aluminum ions is preferable2O8。
Binder
The binder is selected from the group consisting of but not limited to polyvinylidene fluoride (PVDF), polyvinyl alcohol, polyurethane, epoxy resin, and polyvinylidene fluoride (PVDF).
Examples (S) 1 to 3 and comparative examples
The compositions of the lithium battery positive electrode pastes of examples 1-3 and comparative examples in parts by weight are given in the following table:
examples 4 to 5
Examples 4 to 5Based on example 3, the difference is that the negative thermal expansion material of example 4 is ytterbium doped ZrW2O8，Zr0.94Yb0.06W2O8-n(n is determined by oxygen vacancies due to unequal doping); example 5 doping of ZrW with aluminum ions2O8The doping amount of aluminum is 3.2%.
The graphene used in examples 1 to 5 and comparative example was mechanically exfoliated graphene, with few structural defects and a aspect ratio of not less than 500.
Example 3 a and 3B were set in parallel, and the group a samples were physically blended in the order of azomethylpyrrolidone, polyvinylidene fluoride, carbon conductive material, negative thermal expansion material, and lithium iron phosphate, and uniformly dispersed by high-speed stirring. The examples and comparative examples employ the following process steps set B:
s1: mixing a carbon conductive material, a negative thermal expansion material and ethanol to prepare a dispersion liquid, then placing the dispersion liquid in a ball milling tank for ball milling and mixing, removing a polar organic solvent, drying solid components in the dispersion liquid, and sieving to obtain conductive mixed powder, wherein the ball-material ratio of grinding balls to powder in the dispersion liquid is 1: 1.2, the weight ratio of the powder to the polar organic solvent in the dispersion is 1: 2.5, the ball milling time is 24 hours;
s2: putting the conductive mixed powder obtained in the step S1 into a mold, placing the mold into a furnace chamber of a discharge plasma sintering furnace, and performing discharge plasma sintering treatment under the protection of inert gas to obtain conductive composite powder, wherein the axial pressure in the furnace chamber of the discharge plasma sintering furnace is 50Mpa, the sintering temperature is 650 ℃, the sintering time is 3min, and the vacuum degree in the furnace chamber of the discharge plasma sintering furnace is 0.1Pa in the sintering process;
s3: and dissolving the binder in N-methyl pyrrolidone, adding the conductive composite powder obtained in the step S2, uniformly dispersing, adding the positive active substance, and uniformly mixing to obtain the finished product of the positive slurry of the lithium battery.
The lithium iron phosphate (M121 produced by Taiwan, China) in the examples and the comparative examples, the lithium battery positive electrode slurry was coated on the positive electrode plate with a single-sided surface density of 103g/M2The negative electrode uses a lithium sheet, the model of the experimental battery is CR2025, and the designed capacity2mAh, a compacted density of 2.1g/cm3In the test of the conductivity of the lithium batteries of the examples and the comparative examples, the conductivity of S1-B, S2-B, S3-A, S3-B, S4-B, S5-B, D-B is respectively as follows: 0.520X 10-3S/cm、0.517×10-3S/cm、0.379×10-3S/cm、0.588×10-3S/cm、0.602×10-3S/cm、0.635×10-3S/cm、0.462×10-3S/cm。
The conductivity is the ability to transport electrons, and it can be seen from the above table that, in example 2, compared with example 3, the negative thermal expansion material is added in an excessive amount, and the contact resistance increases, which is not favorable for transporting electrons. In the group B subjected to ball milling and spark plasma sintering treatment, compared with the group a not subjected to the above treatment, contact sites between the carbon conductive materials and the negative thermal expansion material are increased, contact resistance is reduced, and the rate of electron transfer is increased. ZrW doped with aluminum ions2O8When the doping amount of the medium aluminum ions is 2.8-4.5%, the conductivity of the prepared positive electrode battery is superior to that of the battery with ZrW2O8And ZrW doped with other metal ions2O8。
Under the high-rate discharge condition of 4C, the rate performance of the embodiment 3-B, the embodiment 4-B and the embodiment 5-B is superior to that of other embodiments and comparative examples, and the reversible specific capacity retention rate reaches over 70 percent.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the technical principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. The preparation method of the graphene lithium battery positive electrode slurry is characterized by comprising the following steps:
s1: mixing the carbon conductive material, the negative thermal expansion material and the polar organic solvent to prepare a dispersion liquid, then placing the dispersion liquid in a ball milling tank for ball milling and mixing, removing the polar organic solvent, drying solid components in the dispersion liquid, and sieving to obtain conductive mixed powder;
s2: putting the conductive mixed powder obtained in the step S1 into a mold, placing the mold in a furnace chamber of a discharge plasma sintering furnace, and performing discharge plasma sintering treatment under the protection of inert gas to obtain conductive composite powder;
s3: dissolving a binder in the N-methyl pyrrolidone, adding the conductive composite powder obtained in the step S2, uniformly dispersing, adding a positive active substance, and uniformly mixing to obtain a finished product of the positive slurry of the lithium battery;
the carbon conductive material contains graphene, and the negative thermal expansion material is ZrW2O8And/or hetero-metal ion doped ZrW2O8。
2. The method for preparing positive electrode slurry of graphene lithium battery according to claim 1, wherein the heterogeneous metal ion doped ZrW2O8The heterogeneous metal in (2) is one or the combination of more than two of aluminum, yttrium, ytterbium, tungsten and molybdenum.
3. The preparation method of the positive electrode slurry for the graphene lithium battery as claimed in claim 1, wherein the positive electrode slurry for the graphene lithium battery comprises the following components in parts by weight: 92-96 parts of positive electrode active substance, 0.7-4 parts of carbon conductive material, 0.8-2.5 parts of binder, 0.3-2 parts of negative thermal expansion material and 36-43 parts of azomethyl pyrrolidone.
4. The method for preparing the positive electrode slurry of the graphene lithium battery as claimed in claim 3, wherein the carbon conductive material is formed by combining acetylene black and graphene, and the weight ratio of the acetylene black to the graphene is 1: (0.8-1.3), wherein the diameter-thickness ratio of the graphene is not less than 500; the weight ratio of the graphene to the negative thermal expansion material is 1: (0.2-0.65).
5. The method for preparing the positive electrode slurry for the graphene lithium battery as claimed in claim 3, wherein the positive electrode active material is lithium iron phosphate, and the binder is polyvinylidene fluoride.
6. The preparation method of the positive slurry for the graphene lithium battery as claimed in claim 1, wherein the ball-to-material ratio of the grinding balls subjected to the S1 ball milling to the powder in the dispersion liquid is 1: (1.2-1.6), wherein the weight ratio of the powder to the polar organic solvent in the dispersion is 1: (1.7-2.5) and the ball milling time is 24-48 h.
7. The preparation method of the positive electrode slurry for the graphene lithium battery, according to claim 1, is characterized in that the axial pressure in a furnace chamber of the discharge plasma sintering furnace is 40-60 MPa, the sintering temperature is 630-680 ℃, the sintering time is 3-5 min, and the vacuum degree in the furnace chamber of the discharge plasma sintering furnace in the sintering process is 0.1-0.2 Pa.
8. The method for preparing the positive electrode slurry for the graphene lithium battery as claimed in claim 1, wherein the polar organic solvent is an alcohol organic solvent of C2-C5.
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| CN115939382A (en) * | 2021-09-22 | 2023-04-07 | 四川大学 | Method for improving electrochemical performance and safety of positive electrode material |
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| CN116093460B (en) * | 2023-04-07 | 2023-06-20 | 河南锂动电源有限公司 | Semi-solid lithium ion battery pole piece, manufacturing method thereof and battery |
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| CN110010897A (en) | 2019-07-12 |
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