CN114583095A - Electrode, preparation method thereof and lithium ion battery - Google Patents
Electrode, preparation method thereof and lithium ion battery Download PDFInfo
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- CN114583095A CN114583095A CN202011388808.3A CN202011388808A CN114583095A CN 114583095 A CN114583095 A CN 114583095A CN 202011388808 A CN202011388808 A CN 202011388808A CN 114583095 A CN114583095 A CN 114583095A
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses an electrode, a preparation method thereof and a lithium ion battery. The electrode comprises a current collector, wherein the current collector is provided with two oppositely arranged surfaces, an electrode active layer is formed on at least one of the two surfaces, a protective film layer is further combined on the outer surface of one electrode active layer or protective film layers are further respectively combined on the outer surfaces of the two electrode active layers, a plurality of through holes for electrolyte to pass through to the electrode active layers are formed in the protective film layers, the materials of the protective film layers comprise first resin, second resin and heat-resistant framework materials for a membrane framework, and the first resin and the second resin are crosslinked in a thermal environment. The electrode can effectively avoid or inhibit thermal failure and improve the safety of the electrode, thereby improving the safety of the lithium ion battery and meeting the requirements of GB38031-2020 national standard.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a composition, an electrode, a preparation method of the electrode and a lithium ion battery.
Background
Lithium ion batteries are widely used due to their high energy density, long cycle, and high stability. With the wide application of electronic products and the vigorous development of electric automobiles, the market of lithium ion batteries is increasingly wide, but higher requirements on the safety of the lithium ion batteries are provided.
The state puts higher requirements on the runaway of the lithium ion battery in a mandatory standard GB38031-2020 (5-minute escape time when failure occurs) on the battery. Therefore, the fundamental factor of the safety of the unit, which is high energy, is also the most important factor.
As is known, the lithium ion battery is more likely to cause potential safety hazards when used under conditions of high rate, high and low temperature, excessive amount of corresponding cathode active material, and the like. When lithium is excessively inserted into an electrode using metal lithium, graphite and the like as a matrix of the lithium ion battery or the lithium insertion speed is too low, lithium ions are separated out from the surface of the electrode, and the lithium dendrite is generally sharp and irreversible and easily pierces a diaphragm to cause instant energy release so as to cause safety accidents.
During the process of coating the lithium ion electrode, the electrode may be in an uneven state, and factors such as excessive positive electrode and insufficient negative electrode coating recess are very likely to cause lithium precipitation. When a general battery core fails in use, the battery is not abnormal wholly, but is often caused by local abnormality of the battery core, namely short circuit caused by penetration of a membrane by lithium dendrite or impurity burrs and the like. Generally, the closed pores of the diaphragm are relied on to isolate the positive electrode and the negative electrode, but once thermal runaway occurs, heat is gathered and rises, and even the heat rises to the melting and shrinking temperature of the diaphragm, and the holes of the diaphragm are broken to aggravate the runaway of the battery.
Although it is reported that a protective layer is formed on the surface of an electrode in order to improve the safety of a battery, the conventional protective layer only functions as an insulator, but the protective layer is softened and fails by heat when thermal runaway is encountered. Therefore, how to effectively reduce the local failure of the battery or prolong the thermal runaway time or completely prevent the thermal runaway from occurring is a technical problem which is continuously tried to solve in the field.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides an electrode, a preparation method thereof and a lithium ion battery containing the electrode, so as to solve the technical problem that the safety of the lithium ion battery is not ideal due to partial failure of the conventional electrode.
In order to achieve the above object, according to one aspect of the present invention, an electrode is provided. The electrode includes the mass flow body, the mass flow body has two surfaces of relative setting, two at least one in the surface is formed with electrode active layer on the surface, one electrode active layer still combine protective film layer or two on the surface electrode active layer still combine protective film layer respectively on the surface, protective film layer has been seted up a plurality ofly and has been used for electrolyte to pass extremely electrode active layer's through-hole, just protective film layer's material includes first resin, second resin and is used for the heat-resisting skeleton material of rete skeleton, first resin and second resin take place the crosslinking in the thermal environment.
Therefore, as the protective film layer contained in the electrode is provided with the plurality of through holes, when the electrode is contacted with the electrolyte, the electrolyte can directly reach the electrode active layer through the through holes, so that the infiltration of the electrolyte and the migration and the intercalation and deintercalation of lithium ions are not influenced in the charging and discharging processes. When the electrode is subjected to local thermal failure in the charging and discharging processes, the first resin and the second resin contained in the material of the protective film layer are sensitive to temperature, when the temperature of the electrode reaches the crosslinking temperature of the composition, the first resin and the second resin increase fluidity due to heating and migrate and gather at the abnormal surface of the electrode, and an implosion crosslinking reaction occurs in the skeleton film layer formed by the heat-resistant skeleton material to form a tough, compact, insulating and high-temperature-resistant polymer protective layer which covers the abnormal surface tightly attached to the electrode to play an isolation role and play a decisive thermal runaway closing protection role, so that the local thermal runaway of the local electrode is inhibited, the local thermal runaway is prevented from spreading the whole electrode or battery, more escape time is strived, and the electrode meets the requirements of GB38031-2020 national standard.
Preferably, the mass ratio of the heat-resistant framework material to the first resin to the second resin is (50-70): (15-50): (15-50). Through the adjustment and optimization of the proportion of the three resins, the toughness, compactness and high temperature resistance of a high-molecular protective layer formed by crosslinking the protective film layer after the thermal runaway of the electrode can be improved.
Specifically, the heat-resistant framework material comprises at least one of polyimide, polyethylene terephthalate and polyphenylene sulfide. The heat-resistant framework material has excellent high-temperature stability, and can improve the toughness and high-temperature resistance of a high-molecular protective layer formed by crosslinking a protective film layer after the thermal runaway of an electrode.
Specifically, the first resin comprises at least one of thermoplastic modified acrylic resin, polyvinyl alcohol and low-density polyethylene.
Specifically, the second resin comprises at least one of vinyl acetate and polytetrafluoroethylene.
The first resin and the second resin can effectively flow after the thermal runaway of the electrode, gather on the surface of the thermal runaway position and generate polymerization crosslinking under the action of heat, so that a high-molecular protective layer with toughness, compactness and high temperature resistance is formed.
Preferably, the material of the protective film layer further comprises a thermistor material, and the mass ratio of the thermistor material to the heat-resistant framework material is (0.1-10): (50-70). Specifically, the thermistor material includes a PTC. Adding thermistor materials into the materials of the protective film layer, and optimizing the content and the type of the thermistor materials, so that the protective film layer has conductivity when the electrode works normally; when the electrode is out of control thermally, the thermistor material can play the role of insulation, and the insulation and isolation protection of the polymer protective layer formed by polymerization crosslinking can be improved.
Preferably, the material of the protective film layer further comprises an insulating inorganic additive, and the mass ratio of the insulating inorganic additive to the heat-resistant framework material is (0.1-5): (50-70). In particular, the insulating inorganic additive comprises an insulating metal oxide. Insulating inorganic additives are added into the material of the protective film layer, and the content and the type of the insulating inorganic additives are optimized, so that the protective film layer has good wettability to electrolyte when the electrode normally works; when the electrode is out of control thermally, the insulating inorganic additive exerts the characteristics of the insulating inorganic substance, and improves the high temperature resistance and the isolation protection effect of the high molecular protective layer formed by crosslinking.
Preferably, the aperture of the through hole is 0.1-5 mm.
Preferably, the distribution density of the through holes in the protective film layer is 100-3000/cm2。
Preferably, the thickness of the protective film layer is 0.01-10 μm.
The thickness of the protective film layer, the aperture of the contained through holes and the distribution density of the through holes are controlled and optimized, so that the protective film layer does not influence the electrochemical performance of the electrode in the normal working process of the electrode, the toughness, the compactness and the high temperature resistance of a high-molecular protective layer formed by crosslinking are improved when the electrode is out of control thermally, and the isolation protection effect of the high-molecular protective layer is improved.
Preferably, the electrode is a positive electrode, and the electrode active layer is a positive electrode active material layer; or the electrode is a negative electrode, and the electrode active layer is a negative electrode active material layer. Thus, the battery negative electrode or/and the battery positive electrode can be made to be an electrode containing a protective film layer, and the safety of the battery can be improved.
In another aspect of the present invention, a method for preparing an electrode is provided. The preparation method of the electrode comprises the following steps:
providing an electrode body, wherein the electrode body comprises a current collector, the current collector is provided with two oppositely-arranged surfaces, and an electrode active layer is formed on at least one of the two surfaces;
preparing resin slurry, wherein the resin slurry comprises a first resin, a second resin and a heat-resistant framework material for a film-layer framework, and the first resin and the second resin are crosslinked in a thermal environment;
and forming a protective film layer by performing film forming treatment on the outer surface of one electrode active layer or performing film forming treatment on the outer surfaces of the two electrode active layers respectively.
Thus, the preparation method of the electrode directly forms the protective film layer on the outer surface of the electrode active layer contained in the existing electrode body. The protective film layer contains a heat-resistant framework material, a first resin and a second resin. The electrode thus prepared is the electrode of the present invention having high safety as described above. The electrode preparation method has the advantages of simple process steps, controllable conditions, capability of effectively ensuring the stability of the prepared electrode and high production efficiency.
In yet another aspect, the present invention provides a composition. The composition includes a first resin, a second resin, and a heat-resistant skeletal material for a film skeletal, the first resin and the second resin being cross-linked in a thermal environment. The heat-resistant framework material contained in the composition plays a role of a film-forming framework and has excellent high-temperature resistance, so that a film layer formed by the composition has high heat resistance and good mechanical property. The first resin and the second resin can migrate and aggregate in a thermal environment, and undergo an implosion crosslinking reaction to form a tough, dense, insulating and high-temperature-resistant high polymer material.
Specifically, the heat-resistant framework material comprises at least one of polyimide, polyethylene terephthalate and polyphenylene sulfide. The heat-resistant framework material has excellent high-temperature stability and plays a framework role.
Specifically, the first resin comprises at least one of thermoplastic modified acrylic resin, polyvinyl alcohol and low-density polyethylene.
Specifically, the second resin comprises at least one of vinyl acetate and polytetrafluoroethylene.
The first resin and the second resin can flow and aggregate in a thermal environment and undergo violent crosslinking under the action of heat, and form a tough, compact and high-temperature-resistant high polymer material together with the heat-resistant framework material.
Preferably, the composition further comprises a thermistor material, and the mass ratio of the thermistor material to the heat-resistant framework material is (0.1-10): (50-70). Specifically, the thermistor material includes a PTC. The thermistor material is added into the composition, and the content and the type of the thermistor material are optimized, so that the composition has certain conductivity at the temperature lower than the crosslinking temperature, and when the composition is in a thermal environment, the thermistor material plays a role in insulation, and the insulation and isolation protection effects of a high polymer material formed by crosslinking through polymerization are improved.
Preferably, the composition further comprises an insulating inorganic additive, and the mass ratio of the insulating inorganic additive to the heat-resistant framework material is (0.1-5): (50-70). In particular, the insulating inorganic additive comprises an insulating metal oxide. The insulating inorganic additive is added into the composition, and the content and the type of the insulating inorganic additive are optimized, so that the composition has good wettability on the electrolyte at the temperature lower than the crosslinking temperature; when in a hot environment, the insulating inorganic additive plays the characteristic of an insulating inorganic substance, and improves the high temperature resistance and the insulation protection effect of a high polymer material formed by crosslinking.
In yet another aspect, the present invention provides a lithium ion battery. The lithium ion battery comprises an anode, a cathode and a diaphragm which is stacked between the anode and the cathode, wherein the anode and/or the cathode are/is the electrode. Therefore, the electrode has the structure and the function, so that the lithium ion battery has high safety and meets the national standard of GB 38031-2020.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic diagram of an electrode structure according to an embodiment of the present invention; fig. 1(a) shows an electrode with an active layer formed on one surface of a current collector; fig. 1(b) shows an electrode in which active layers are formed on both surfaces of a current collector;
FIG. 2 is a schematic structural diagram of a protective film 3 included in an electrode according to an embodiment of the present invention; wherein, fig. 1(a) is a schematic structural diagram of the protective film layer 3, and fig. 1(b) is a schematic structural diagram of the protective film layer 3;
FIG. 3 is a schematic diagram of a raised electrode structure resulting from a large local coating amount of an active layer according to an embodiment of the present invention;
FIG. 4 is a schematic view of an electrode according to an embodiment of the present invention, in which lithium dendrites are formed on the surface of an active layer;
FIG. 5 is a schematic structural diagram of a polymer protective layer formed after a crosslinking reaction occurs in abnormal thermal runaway of a protective film layer 3 included in an electrode according to an embodiment of the present invention;
fig. 6 is a schematic diagram of a cell structure included in a lithium ion battery according to an embodiment of the present invention;
FIG. 7 is a graph showing temperature change curves in cycles of artificial treatment of negative electrodes included in lithium ion batteries according to example 23 and comparative examples of the present invention;
wherein the reference numerals in the figures are as follows:
1-current collector;
2-electrode active layer, 21-lithium dendrite, 22-electrode active material, 22-conductive agent;
3-a protective film layer; 31-a through hole contained in the protective film layer;
3' -a polymer protective layer;
01-positive electrode, 02-negative electrode, 03-diaphragm.
Detailed Description
In order to make the objects, technical solutions and technical effects of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described, and the embodiments described below are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments obtained by a person of ordinary skill in the art without any inventive step in connection with the embodiments of the present invention shall fall within the scope of protection of the present invention. Those whose specific conditions are not specified in the examples are carried out according to conventional conditions or conditions recommended by the manufacturer; the reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the description of the present invention, the term "and/or" describing an association relationship of associated objects means that there may be three relationships, for example, a and/or B, may mean: a is present alone, A and B are present simultaneously, and B is present alone. Wherein A and B can be singular or plural. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship.
In the description of the present invention, "at least one" means one or more, "a plurality" means two or more. "at least one of the following" or similar expressions refer to any combination of these items, including any combination of the singular or plural items. For example, "at least one (a), b, or c", or "at least one (a), b, and c", may each represent: a, b, c, a-b (i.e., a and b), a-c, b-c, or a-b-c, wherein a, b, and c may be single or plural, respectively.
It should be understood that the weight of the related components mentioned in the embodiments of the present invention may not only refer to the specific content of each component, but also represent the proportional relationship of the weight among the components, and therefore, it is within the scope of the disclosure that the content of the related components is scaled up or down according to the embodiments of the present invention. Specifically, the weight described in the embodiments of the present invention may be a unit of mass known in the chemical field such as μ g, mg, g, kg, etc.
In addition, unless the context clearly uses otherwise, an expression of a word in the singular is to be understood as including the plural of the word. The terms "comprises" or "comprising" are intended to specify the presence of stated features, quantities, steps, operations, elements, portions, or combinations thereof, but are not intended to preclude the presence or addition of one or more other features, quantities, steps, operations, elements, portions, or combinations thereof.
In one aspect, embodiments of the invention provide a composition. The composition includes a first resin and a second resin and a heat resistant skeletal material for a film skeletal.
Wherein the first resin and the second resin contained in the composition are crosslinked in a thermal environment, that is, at a temperature that triggers the crosslinking reaction of the first resin and the second resin, the crosslinking reaction of the first resin and the second resin can occur. The heat-resistant framework material contained in the composition plays a role of a film-forming framework and has excellent high-temperature resistance. Therefore, when the temperature of the component formed from the composition, such as the film layer, is lower than or equal to the temperature at which the crosslinking of the first resin and the second resin is triggered, the original state of the component, such as the film layer, can be ensured, and the components are uniformly dispersed. When a member formed from the composition, such as a film layer, is at a temperature that triggers crosslinking of the first and second resins, the first and second resins are capable of migrating and aggregating in a thermal environment and undergoing an imploding crosslinking reaction to form a polymeric material that is tough, dense, and insulating, and has high temperature resistance. When the relevant component such as the film layer is formed, the component such as the film layer is endowed with good mechanical properties.
In one embodiment, the heat-resistant framework material contained in the composition comprises at least one of Polyimide (PI), polyethylene terephthalate (PET) and polyphenylene sulfide (PPS). The heat-resistant framework materials have excellent high-temperature stability and play a framework role, if the heat-resistant framework materials are PI, the heat-resistant framework materials can resist high temperature of more than or equal to 260 ℃, and even the high-temperature modified PI can resist high temperature of 350 ℃. In a specific embodiment, the high temperature modified PI may be an existing high temperature resistant modified PI. When a component formed by the composition, such as a film layer, triggers the crosslinking temperature of the first resin and the second resin, the first resin and the second resin can be crosslinked in the component, the heat-resistant framework material forms the framework effect of the component and gives the component excellent high-temperature resistance, and the resin plays a role in synergy with the first resin and the second resin crosslinking polymer and gives the component excellent mechanical properties such as toughness and the like, and is dense in insulation.
In one embodiment, the first resin contained in the composition comprises at least one of a thermoplastic modified acrylic resin, polyvinyl alcohol (PVA), Low Density Polyethylene (LDPE). In another embodiment, the second resin comprises at least one of vinyl acetate, polytetrafluoroethylene. The preferred first and second resins are capable of flowing and aggregating in a thermal environment, such as an environment that triggers a cross-linking reaction between the two, and undergo a cross-linking reaction under exposure to heat, to form a tough, dense, and high temperature resistant polymeric material with a heat resistant backbone material. The crosslinking reaction may occur between the first resins and between the second resins, and may occur between the first resins and the second resins. In addition, the second resin, particularly preferably the second resin of the above-mentioned composition, can also function as a binder and a dispersant, can impart good film layer and dispersion stability to the composition, can improve the film forming property of the composition to be formed, and can improve the film layer quality such as uniformity of the film layer.
In a further embodiment, the composition further comprises a thermistor material. Preferably, the mass ratio of the thermistor material to the heat-resistant framework material is controlled to be (0.1-10): (50-70). In a specific embodiment, the thermistor material comprises a PTC, and the PTC is selected from PTC containing barium titanate doped with a small amount of niobium, manganese, cerium, iridium, and the like. The thermistor material is added into the composition, and the content and the type of the thermistor material are optimized, so that the composition has certain conductivity and reduces the resistance when the temperature of the composition is lower than the crosslinking temperature, and when the composition is in a thermal environment, the thermistor material exerts the insulating property and improves the insulating and insulating properties of high polymer materials formed by polymerization crosslinking, thereby improving the insulating and insulating protective effects of components formed by the composition, such as a film layer.
In a further embodiment, the composition further comprises an insulating inorganic additive, and the mass ratio of the insulating inorganic additive to the heat-resistant framework material is preferably controlled to be (0.1-5): (50-70). In a particular embodiment, the insulating inorganic additive comprises an insulating metal oxide. Wherein, the insulating metal oxide can be at least one of aluminum oxide, zinc oxide, cesium oxide and titanium dioxide. The insulating inorganic additive is added into the composition, and the content and the type of the insulating inorganic additive are optimized, so that the composition has good wettability on the electrolyte at the temperature lower than the crosslinking temperature; when in the environment of temperature for triggering the cross-linking reaction of the first resin and the second resin, the insulating inorganic additive exerts the characteristics of the insulating inorganic substance, and improves the high-temperature resistance and the insulating property of the high-molecular material formed by cross-linking, thereby improving the protective effects of components formed by the composition, such as the insulation and the insulation of a film layer.
In addition, the composition can be prepared by mixing the components in proportion according to the components contained therein to form a uniform mixture in a dispersion system. Before use, it should be ensured that the composition is at a temperature below the temperature at which the first resin and the second resin contained therein crosslink. The composition may be formulated into a slurry or the like to form each member, such as a film layer, according to the requirements of the application, when required by the application. If the film layer is required to have toughness, compactness, insulation, high temperature resistance and other performances finally, the component is subjected to heat treatment to trigger the first resin and the second resin to perform a crosslinking reaction, so that the corresponding component such as the film layer is endowed with excellent toughness, compactness, insulation, high temperature resistance and other performances.
In another aspect, an embodiment of the present invention provides an electrode. The electrode has a structure as shown in fig. 1 and 2, and includes a current collector 1 having two oppositely disposed surfaces, at least one of which has an electrode active layer 2 formed thereon. Specifically, an electrode active layer 2 may be formed on one of two oppositely disposed surfaces of the current collector 1, and at this time, a protective film layer 3 is further bonded to an outer surface of the electrode active layer 2, that is, a surface facing away from the current collector, as shown in fig. 1 (a).
Of course, the electrode active layers 2 may be formed on both surfaces of the current collector 1 facing each other, as shown in fig. 1, in which case the protective film 3 is further bonded to the outer surface of one of the electrode active layers 2 or the protective films 3 are further bonded to the outer surfaces of the two electrode active layers 2, respectively. A structure in which the protective film layers 3 are further bonded to the outer surfaces of the two electrode active layers 2, respectively, is also preferred in the embodiment of the present invention, as shown in fig. 1 (b).
Regardless of the electrode structure shown in fig. 1(a) or fig. 1(b), the protective film 3 is provided with a plurality of through holes 31 for passing the electrolyte to the electrode active layer 2, and the material of the protective film 3 is the composition described above.
Thus, since the protective film layer 3 is provided with the plurality of through holes 31, after the electrode contacts the electrolyte, the electrolyte can directly reach the electrode active layer 2 through the through holes 31, so that the infiltration of the electrolyte and the migration, insertion and extraction of lithium ions are not influenced in the charging and discharging processes, preferably, the protective film layer 3 preferably contains a thermistor material and/or an insulating inorganic additive, and before the protective film layer 3 undergoes a cross-linking reaction, namely when the electrode is locally thermally failed, the protective film layer 3 also has excellent electrolyte infiltration and certain conductivity.
When the electrode has local thermal failure in the charging and discharging process, or the closed pore of the diaphragm still can not prevent thermal runaway to cause the melting and the hole breaking of the diaphragm, because the first resin and the second resin contained in the material of the protective film layer 3 are sensitive to the temperature, when the local thermal failure temperature of the electrode reaches the cross-linking temperature of the composition, if the local thermal failure temperature reaches 80 ℃, the first resin and the second resin can migrate and gather at the abnormal surface of the electrode due to the reason that the heat increases the fluidity, so that the imploding cross-linking reaction occurs, and the cross-linking is irreversible to form a tough, compact, insulating and high-temperature resistant polymer protective layer which covers and tightly clings to the abnormal surface of the electrode to play a role in isolation, and play a decisive thermal runaway closing protection, namely equal to the isolation of the positive electrode and the negative electrode, the positive electrode and the electrolyte, and the negative electrode and the electrolyte, the suppression of local thermal runaway is realized, the local thermal runaway is prevented from spreading the whole electrode or battery, so that more escape time is strived for, and the safety of the battery meets the escape requirement of 5min after national mandatory national standard for lithium ion battery safety warning. Preferably, when the protective film layer 3 preferably contains a thermistor material and/or an insulating inorganic additive, the high-molecular protective layer formed after the crosslinking reaction has more excellent properties such as high temperature resistance, insulating property and the like, and has a better insulating and protecting effect.
Empirical research shows that the local abnormal thermal runaway of the electrode generally results from the fact that a broken hole is formed in the diaphragm and the diaphragm cannot be recovered due to the instant discharge pulverization of the tip electron aggregation such as lithium dendrite/metal impurities and the like at the interface of the electrode and the diaphragm. Once the current is slightly large (micro short circuit exists at the broken hole), the diaphragm can be continuously torn and melted along the broken hole, and the short circuit transient thermal runaway of a larger surface is caused to cause safety accidents. In one embodiment, the electrode active layer 2 of the electrode, such as the positive and negative electrodes, has a protrusion with a large local coating amount as shown in fig. 3, or a recess with a local deficiency as shown in fig. 3, which results in an uneven surface of the electrode active layer 2, so that excessive lithium ions are not properly inserted into the electrode during the charging and discharging process and are precipitated in the state of metallic lithium, i.e., lithium dendrites 21 are precipitated on the surface of the electrode active layer 2, especially in the area with a large local coating amount, thereby easily causing the lithium precipitation phenomenon as shown in fig. 4. When abnormal thermal runaway occurs locally on the electrode, such as in the recessed area of the electrode active layer 2 or in the raised area or area in fig. 3, due to the increase of temperature, the first resin and the second resin in the protective film layer 3 are triggered to migrate and gather in the recessed or raised area and perform a crosslinking reaction in the film skeleton constructed by the heat-resistant skeleton material, so that the polymer protective layer is constructed together with the heat-resistant skeleton material, and the polymer protective layer is endowed with excellent toughness, compactness and insulation and has high temperature resistance. Specifically, as shown in fig. 4, a polymer protective layer 3' is formed in the abnormal thermal runaway region of the electrode active layer 2.
In one embodiment, the aperture of the through hole contained in the protective film layer 3 in each of the above embodiments is 0.1 to 5 mm. In another embodiment, the distribution density of the through holes in the protective film layer is 100-3000/cm2. In another embodiment, the thickness of the protective film layer 3 is 0.01 to 10 μm. By controlling and optimizing the aperture of the through holes 31 and the distribution density of the through holes 31 contained in the protective film layer 3, the protective film layerThe protective film layer 3 is effectively combined on the surface of the electrode active layer 2 in the normal work of the electrode, and simultaneously, the infiltration of electrolyte and the insertion and extraction of lithium ions are not influenced, so that the electrochemical performance of the electrode is not adversely influenced; when the electrode is out of control by heat, the toughness, compactness, insulation and high temperature resistance of the macromolecular protective layer 3' formed by crosslinking can be improved, and the isolation protection effect of the macromolecular protective layer is improved. In addition, the protective film layer 3 may cover the whole surface of the electrode active layer 2, or may partially cover the surface of the electrode active layer 2, for example, in an embodiment, the area of the protective film layer 3 covering the surface of the electrode active layer 2 is 40% to 70% of the surface of the electrode active layer 2.
In addition, as shown in fig. 3 to 5, the electrode active layer 2 included in the electrode in each of the above embodiments, the material of the electrode active layer 2 may be a conventional electrode active layer material, such as including the electrode active material 22 and the conductive agent 23, and may also include a binder or other additives.
Among them, the electrode active material 22 may be provided with a corresponding electrode active material according to the properties of the electrode such as a positive electrode or a negative electrode. When the electrode is an anode, the electrode active layer 2 is an anode active material layer, and then the electrode active material 22 is an anode active material. As in one embodiment, the negative active material is preferably at least one of graphite, hard carbon, soft carbon, silicon oxide, and nano silicon (the mass fraction of the negative active material in the electrode active layer 2 is 85%). In this case, the binder contained in the electrode active layer 2 is preferably at least one of sodium carboxymethylcellulose, styrene-butadiene rubber, phenylacetic acid, terpene resin, and tragacanth gum (mass fraction of the binder in the electrode active layer 2: 0.3 to 10%).
When the electrode is a positive electrode, the electrode active layer 2 is a positive electrode active material layer, and then the electrode active material 22 is a positive electrode active material. As in one embodiment, the positive electrode active material is preferably at least one of lithium cobaltate, lithium nickel cobalt manganese oxide, lithium nickel manganese oxide, lithium iron phosphate, and lithium nickel cobalt aluminate (the mass fraction of the positive electrode active material in the electrode active layer 2 is equal to or greater than 85%). In this case, the binder contained in the electrode active layer 2 is preferably at least one of polyvinylidene fluoride, acrylic resin, and polytetrafluoroethylene (mass fraction of the binder in the electrode active layer 2: 0.3 to 5%). The other functional additive contained in the electrode active layer 2 may be at least one of alumina, zinc oxide, and cesium oxide (mass fraction of the other functional additive in the electrode active layer 2: 0.1 to 1.5%).
The conductive agent 23 contained in the electrode active layer 2 is preferably at least one of carbon black, conductive graphite, carbon nanotubes, carbon fibers, and graphene (the mass fraction of the conductive agent 23 in the electrode active layer 2 is 0.01 to 8%).
Also, the current collector 1 may select a corresponding current collector material according to the properties of the electrode, such as a positive electrode or a negative electrode.
Therefore, the electrode in each of the above embodiments may be either a positive electrode or a negative electrode. Therefore, the negative electrode or/and the positive electrode of the battery can be set as the electrode containing the protective film layer 3, so that the safety of the battery is improved, and the safety requirement of the national standard on the lithium ion battery is met.
Correspondingly, the embodiment of the invention also provides a preparation method of the electrode. Referring to fig. 1 to 5, the method for manufacturing the electrode includes the steps of:
s01: providing an electrode body, wherein the electrode body comprises a current collector 1, the current collector 1 is provided with two oppositely-arranged surfaces, and an electrode active layer 2 is formed on at least one surface of the two surfaces;
s02: preparing resin slurry, wherein the resin slurry comprises a first resin, a second resin and a heat-resistant framework material for a film-layer framework, and the first resin and the second resin are crosslinked in a thermal environment;
s03: the protective film layer 3 is formed by film-forming the resin slurry on the outer surface of one electrode active layer 2 or by film-forming the resin slurry on the outer surfaces of the two electrode active layers 2.
The current collector 1, the electrode active layer 2 and the protective film 3 in step S03 in step S01 are all as the current collector 1, the electrode active layer 2 and the protective film 3 included in the electrode in the embodiment of the present invention, and for the sake of brevity, the structures, materials and the like of the current collector 1, the electrode active layer 2 and the protective film 3 are not described again.
The resin paste in step S02 is a paste of the composition of the embodiment of the present invention, that is, a film-forming paste prepared by mixing the composition of the embodiment of the present invention with a solvent is used to form the protective film layer 3 on the outer surface of the electrode active layer 2. Therefore, the first resin, the second resin and the heat-resistant skeleton material for the film layer skeleton contained in the resin slurry in the step S02 are the same as those contained in the composition of the embodiment of the invention and the heat-resistant skeleton material for the film layer skeleton, and the first resin, the second resin and the heat-resistant skeleton material for the film layer skeleton will not be described herein again for the sake of brevity. Further, the resin paste in step S02 may further contain a thermistor material and/or an insulating inorganic additive contained in the composition of the embodiment of the invention described above.
The film formation processing method in step S03 is to form the resin slurry prepared in step S02 on the surface of the electrode active layer 2, and therefore any method capable of forming a film of the resin slurry on the surface of the electrode active layer 2 is within the scope of the disclosure of the embodiments of the present invention, such as but not limited to casting, printing, and the like. The temperature during film formation should, of course, be below the temperature at which crosslinking of the first and second resins is triggered. The protective film 3 formed by the film formation process may have other patterns than the two patterns shown in fig. 2.
In this way, the electrode manufacturing method forms the protective film layer 3 directly on the outer surface of the electrode active layer 2 included in the conventional electrode body. Since the protective film layer 3 contains the heat-resistant skeleton material, the first resin, and the second resin, the electrode obtained is a highly safe electrode according to the embodiment of the present invention. The electrode preparation method is simple in process steps, controllable in conditions, capable of effectively guaranteeing stability of the prepared electrode and high in production efficiency.
In another aspect, based on the electrode and the preparation method thereof, the embodiment of the invention also provides a lithium ion battery. The lithium ion battery comprises a battery cell as shown in fig. 6, and comprises a positive electrode 01, a negative electrode 02 and a diaphragm 03 stacked between the positive electrode 01 and the negative electrode 02, wherein the positive electrode 01, the negative electrode 02 and the diaphragm 03 are assembled into the battery cell according to a lithium ion battery assembling method. Wherein, the positive electrode 01 and/or the negative electrode 02 are/is the electrode of the embodiment of the invention. When the positive electrode 01 and the negative electrode 02 are assembled into a cell, the protective film layer 3 included in the positive electrode 01 and/or the negative electrode 02 is laminated at least on the side close to the separator 03. In a specific embodiment, the separator 03 may be made of polyethylene, polypropylene, or a polypropylene-polyethylene interlayer (PP/PE/PP), the electrolyte of the lithium ion battery may be made of lithium hexafluorophosphate as a solvent, and EC/PC/DMC as a solvent.
In this way, the positive electrode 01 and/or the negative electrode 02 of the lithium ion battery are/is the electrodes described above. Based on the structure and the function of the electrode, the lithium ion battery provided by the embodiment of the invention has high safety and meets the national standard GB 38031-2020.
The compositions, electrodes, etc. of the embodiments of the present invention are illustrated by the following specific examples.
Composition of the embodiments
Example 11
The present example provides a composition. The composition comprises the following components in percentage by mass of 60: 30: 30 of a mixture of a polyimide, a thermoplastic modified acrylic resin, and vinyl acetate.
Example 12
The present example provides a composition. The composition comprises the following components in percentage by mass of 60: 30: 30: 3, a thermoplastic modified acrylic resin, a mixture of vinyl acetate and a mixture of PTC.
Example 13
The present example provides a composition. The composition comprises the following components in percentage by mass of 60: 30: 30: 3: 5, a thermoplastic modified acrylic resin, a mixture of vinyl acetate and PTC, and a mixture of insulating metal oxides. Wherein the insulating metal oxide is aluminum oxide.
Example 14
The present example provides a composition. The composition comprises the following components in percentage by mass of 70: 15: 15: 5: 1 (mass ratio of 1:1), a first resin (mass ratio of 1:1) compounded by thermoplastic modified acrylic resin and polyvinyl alcohol, polytetrafluoroethylene, PTC and a mixture of insulating metal oxides. Wherein the insulating metal oxide is zinc oxide.
Example 15
The present example provides a composition. The composition comprises the following components in percentage by mass: 40: 50: 1: 10 of polyimide and polyethylene terephthalate composite heat-resistant framework material (mass ratio is 1:1), polyvinyl alcohol, polytetrafluoroethylene, PTC and insulating metal oxide mixture (mass ratio is 1: 1). Wherein the insulating metal oxide is a mixture of aluminum oxide and titanium dioxide (mass ratio is 1: 1).
Electrode and lithium ion battery embodiments
Example 21
The embodiment provides a lithium ion battery electrode and a lithium ion battery. The lithium ion battery comprises the following structure:
and (3) positive electrode: including 12um aluminium foil and formation and the relative anodal active layer on two surfaces of aluminium foil, all be formed with the protection rete at the surface of two anodal active layers. The material of the positive active layer comprises a positive material of nickel cobalt lithium manganate with the mass fraction of 94%, a conductive carbon black conductive agent with the mass fraction of 3%, a PVDF binder with the mass fraction of 3% and the surface density of 350 g/cc; the protective film layer was the composition of example 11 coated to form a through-hole film layer as shown in fig. 2 (a);
negative electrode: including 12um copper foil and formation and the relative negative pole active layer on two surfaces of copper foil, all be formed with the protective film layer at the surface of two negative pole active layers. The material of the negative active layer comprises 92.5% of artificial graphite negative electrode material, 3% of conductive carbon black conductive agent and 1.5% of CMC binder (3% of SBR emulsion is also added in the preparation process), and the surface density is 150 g/cc; protective film layer the composition of example 11 was coated to form a through-hole-provided film layer as shown in FIG. 2(a), which had a thickness of 2 μm and an average through-hole diameter of 3 mm.
A diaphragm: polyethylene, polypropylene polyethylene (PP/PE/PP) composite film layer.
Electrolyte solution: lithium hexafluorophosphate is used as solvent, and EC/PC/DMC is used as solvent.
Assembling the battery: and assembling the anode, the cathode and the diaphragm into a battery cell according to the lithium ion battery, and then assembling the battery cell, the diaphragm and the electrolyte into the lithium ion battery.
Example 22
The embodiment provides a lithium ion battery electrode and a lithium ion battery. The lithium ion battery comprises the following structure:
and (3) positive electrode: referring to example 21, except that the protective film layer was included in the composition of example 12, which was coated to form a through-hole-provided film layer as shown in fig. 2 (a);
negative electrode: a negative electrode of example 21 was fabricated, except that the composition of example 12 was coated to form a through-hole-provided film layer as shown in fig. 2 (a);
a diaphragm: as in the example 21 separator.
Electrolyte solution: the same electrolyte as in example 21 was used.
Assembling the battery: and assembling the positive electrode, the negative electrode and the diaphragm into a battery cell according to the lithium ion battery, and then assembling the battery cell, the diaphragm and the electrolyte into the lithium ion battery.
Example 23
The embodiment provides a lithium ion battery electrode and a lithium ion battery. The lithium ion battery comprises the following structure:
and (3) positive electrode: referring to example 21, except that the protective film layer was included in the composition of example 13, which was coated to form a through-hole-provided film layer as shown in fig. 2 (a);
negative electrode: a negative electrode of example 21 was fabricated, except that the composition of example 13 was coated to form a through-hole-provided film layer as shown in fig. 2 (a);
a diaphragm: as in the example 21 separator.
Electrolyte solution: the same electrolyte as in example 21 was used.
Assembling the battery: and assembling the anode, the cathode and the diaphragm into a battery cell according to the lithium ion battery, and then assembling the battery cell, the diaphragm and the electrolyte into the lithium ion battery.
Examples 24 to 25
The embodiment provides a lithium ion battery electrode and a lithium ion battery. Including the lithium ion battery reference example 21 battery assembly, wherein, example 24 battery positive and negative: the composition of the positive and negative electrode examples 14 in reference example 21 was coated to form a through-hole-provided film layer as shown in fig. 2 (a); example 25 positive and negative electrodes of battery: the composition of positive and negative electrode examples 15 in reference example 21 was coated to form a through-hole-provided film layer as shown in fig. 2 (a).
Comparative example 1
The embodiment provides a lithium ion battery electrode and a lithium ion battery. The lithium ion battery comprises the following structure:
and (3) positive electrode: a cathode as referred to in example 21 except that it does not include the protective film layer as included in example 21;
negative electrode: a negative electrode of example 21 except that it did not contain the protective film layer contained in example 21;
a diaphragm: as in the example 21 separator.
Electrolyte solution: the same electrolyte as in example 21 was used.
Assembling the battery: and assembling the anode, the cathode and the diaphragm into a battery cell according to the lithium ion battery, and then assembling the battery cell, the diaphragm and the electrolyte into the lithium ion battery.
Correlation characteristic test
1. A small piece of the active layer (length 4mm × width 4mm × thickness 50um) containing artificial graphite was artificially removed from the negative electrode active layer contained in the negative electrode provided in example 23, and then the negative electrode in example 23 was formed with the protective film; the negative electrode active layer of the negative electrode provided in comparative example 1 was artificially removed a small piece of the active layer (length 4mm × width 4mm × thickness 50um) containing artificial graphite, and then the negative electrode of comparative example 1 was formed with the protective film layer on the negative electrode active layer; the areas, shapes and positions of the two negative electrode active layers which are artificially removed are kept the same to the maximum extent.
Then, after the lithium ion battery of example 23 containing the modified negative electrode and the lithium ion battery of comparative example 1 containing the modified negative electrode were subjected to charge and discharge for multiple times at 0.3C under the same conditions, discharge was performed at a rate of 2C, and temperature comparison monitoring was performed, with the results shown in fig. 7. As can be seen from fig. 7, the lithium ion battery of example 23 having the modified negative electrode has a significant difference in temperature after the two lithium ion batteries have the same cycle number during the discharging process, wherein the lithium ion battery of comparative example 1 having the modified negative electrode has a significantly higher battery temperature than the lithium ion battery of example 23 having the modified negative electrode as the cycle number increases. Therefore, when the electrode containing the protective film layer provided by the embodiment of the invention has local thermal failure in the charging and discharging processes, the protective film layer is heated to increase the fluidity and migrates and gathers on the abnormal surface of the electrode, so that the implosion crosslinking reaction occurs, a tough, compact, insulating and high-temperature-resistant polymer protective layer is formed, the isolation and protection effects are achieved, the local thermal runaway is inhibited, the local thermal runaway is prevented from spreading the whole electrode or battery, more escape time is strived for, and the safety of the lithium ion battery is improved.
The lithium ion battery negative electrodes provided in examples 21 to 22 and 24 to 25 were treated in the same manner as in example 23, and the temperature change measured after the same cycle as in example 23 was very close to that of the lithium ion battery in example 23.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (13)
1. An electrode comprising a current collector having two oppositely disposed surfaces, at least one of said surfaces having an electroactive layer formed thereon, wherein: the electrode comprises an electrode active layer, a protective film layer and a heat-resistant framework material, wherein the outer surface of the electrode active layer is combined with the protective film layer or the outer surface of the electrode active layer is combined with the protective film layer respectively, the protective film layer is provided with a plurality of through holes for enabling electrolyte to pass through the electrode active layer, the material of the protective film layer comprises first resin, second resin and the heat-resistant framework material for the framework of the membrane layer, and the first resin and the second resin are crosslinked in a thermal environment.
2. The electrode of claim 1, wherein: the mass ratio of the heat-resistant framework material to the first resin to the second resin is 50-70: (15-50): (15-50).
3. The electrode of claim 1 or 2, wherein: the heat-resistant framework material comprises at least one of polyimide, polyethylene terephthalate and polyphenylene sulfide; and/or
The first resin comprises at least one of thermoplastic modified acrylic resin, polyvinyl alcohol and low-density polyethylene; and/or
The second resin comprises at least one of vinyl acetate and polytetrafluoroethylene.
4. The electrode of claim 1 or 2, wherein: the material of the protective film layer also comprises a thermistor material, and the mass ratio of the thermistor material to the heat-resistant framework material is 0.1-10: (50-70); and/or
The material of the protective film layer also comprises an insulating inorganic additive, and the mass ratio of the insulating inorganic additive to the heat-resistant framework material is 0.1-5: (50-70).
5. The electrode of claim 4, wherein: the thermistor material includes a PTC;
the insulating inorganic additive includes an insulating metal oxide.
6. The electrode of any one of claims 1, 2 and 5, wherein: the aperture of the through hole is 0.1-5 mm; and/or
The distribution density of the through holes in the protective film layer is 100-3000/cm2(ii) a And/or
The thickness of the protective film layer is 0.01-10 mu m; and/or
The protective film layer is combined on the outer surface of the electrode active layer in a grid shape.
7. The electrode of any one of claims 1, 2 and 5, wherein: the electrode is a positive electrode, and the electrode active layer is a positive electrode active material layer; or
The electrode is a negative electrode, and the electrode active layer is a negative electrode active material layer.
8. A preparation method of an electrode comprises the following steps:
providing an electrode body, wherein the electrode body comprises a current collector, the current collector is provided with two oppositely-arranged surfaces, and an electrode active layer is formed on at least one of the two surfaces;
preparing resin slurry, wherein the resin slurry comprises a first resin, a second resin and a heat-resistant framework material for a film-layer framework, and the first resin and the second resin are crosslinked in a thermal environment;
and forming a protective film layer by performing film forming treatment on the outer surface of one electrode active layer or performing film forming treatment on the outer surfaces of the two electrode active layers respectively.
9. A composition characterized by: the heat-resistant composite material comprises a first resin, a second resin, a heat-resistant framework material for a film framework, the first resin and the second resin, wherein the first resin and the second resin are crosslinked in a thermal environment.
10. The composition of claim 9, wherein: the heat-resistant framework material comprises at least one of polyimide, polyethylene terephthalate and polyphenylene sulfide; and/or
The first resin comprises at least one of thermoplastic modified acrylic resin, polyvinyl alcohol and low-density polyethylene; and/or
The second resin comprises at least one of vinyl acetate and polytetrafluoroethylene.
11. The electrode of claim 9 or 10, wherein: the material of the protective film layer also comprises a thermistor material, and the mass ratio of the thermistor material to the heat-resistant framework material is 0.1-10: (50-70); and/or
The composite material also comprises an insulating inorganic additive, wherein the mass ratio of the insulating inorganic additive to the heat-resistant framework material is 0.1-5: (50-70).
12. The electrode of claim 11, wherein: the thermistor material includes a PTC;
the insulating inorganic additive includes an insulating metal oxide.
13. A lithium ion battery comprising a positive electrode, a negative electrode and a separator stacked between the positive electrode and the negative electrode, wherein the positive electrode and/or the negative electrode is the electrode according to any one of claims 1 to 7.
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