CN109742307B - Preparation process of polyimide silicon tab material - Google Patents
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Abstract
The invention provides a preparation process of a polyimide silicon tab material, and relates to the field of lithium batteries. The method comprises the following steps: preparing cellular porous polyimide; mixing silicon, silicon monoxide and lithium element compound into mixed powder; filling the mixed powder into honeycomb porous polyimide by a plasma gas phase method to obtain a deposition material; the deposition material is prepared into the cathode material through carbon deposition. The mixed powder of silicon, silicon monoxide and lithium element compound is filled into the cellular porous polyimide by a plasma gas phase method to obtain a deposition material, and the deposition material is used as a tab material, so that the poor compatibility of a copper interface and a negative electrode material interface is improved, the conductivity of the whole tab is improved, and the battery rate is improved; because no polymer adhesive is added, the cathode active material is in direct contact with the polyimide, and the electron transmission speed and the electron circulation stability are effectively improved. The technical problem of poor conductivity of the conventional pole lug is solved from the source of the material for preparing the pole lug.
Description
Technical Field
The invention relates to the field of lithium batteries, in particular to a preparation process of a polyimide silicon tab material.
Background
With the great progress and rapid development of the information age, multifunctional portable electronic equipment, electric automobiles, aircrafts, artificial power assistance and other equipment put higher requirements on energy storage materials. Therefore, the research and development of novel lithium battery electrode materials with high specific capacity, high rate, high safety and the like are urgent.
The tab is a raw material of a lithium ion polymer battery product. The battery is divided into positive and negative electrodes, the tabs are metal conductors leading out the positive and negative electrodes from the battery core, and the ears of the positive and negative electrodes of the battery are contact points during charging and discharging.
In the existing tab preparation process, a high-molecular binder is required to be added when a negative electrode material is combined with a copper foil, and the binder is a non-conductive high polymer, so that an electronic conductive channel is obstructed, the transmission speed is reduced, and the conductive performance of the tab is poor.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a preparation process of a polyimide silicon tab material, which solves the problem of poor conductivity of the conventional tab.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme:
a preparation process of a polyimide silicon tab material specifically comprises the following steps:
preparing cellular porous polyimide;
mixing silicon, silicon monoxide and lithium element compound into mixed powder;
filling the mixed powder into honeycomb porous polyimide by a plasma gas phase method to obtain a deposition material;
the deposition material is prepared into the cathode material through carbon deposition.
Preferably, in step S1, preparing honeycomb porous polyimide:
s1-1, dissolving pyromellitic dianhydride, 4' -diaminodiphenyl ether, dimethylacetamide, N-methyl-2-pyrrolidone and fluorine compounds serving as raw materials under the protection of nitrogen;
s1-2, adding polystyrene into the solution obtained in the step S1-1, stirring and refluxing for 2-10 hours under the protection of nitrogen;
s1-3, preparing a film with the thickness of 25-100 mu m by injection-calendaring molding through the solution refluxed in the step S1-2, and drying at 40-80 ℃;
and S1-4, graphitizing the dried film obtained in the step S1-3 at 2500-3000 ℃, and preserving heat for 5-10 hours.
Preferably, the preparation process of the mixed powder comprises the following steps:
taking 20-40 parts of high-purity silicon, 30-80 parts of silicon monoxide and 2-10 parts of lithium element compound, and placing the mixture in a ball mill for ball milling for 8-10 hours, wherein a ball milling medium is zirconium oxide.
Preferably, the specific steps of filling the mixed powder into the honeycomb-shaped porous polyimide by a plasma gas phase method are as follows:
s3-1: placing the mixed powder in a plasma processor, vacuumizing, and introducing jet gas;
s3-2: starting plasma heating;
s3-3: and (6) cooling.
Preferably, the carbon deposition comprises the following specific steps:
and (3) placing the deposition material in a vapor deposition furnace, introducing carbon source gas, and performing vapor-phase jet deposition.
Preferably, the lithium element compound is one or more of a lithium-based inorganic compound and a lithium-based organic compound.
Preferably, the conditions of step S3-1 are: the vacuum degree is 10-150 Pa, the jet gas is argon, and the jet speed is 1-30 m/s.
Preferably, the plasma heating conditions in step S3-2 are as follows: the temperature is 2000-3500 ℃, and the processing time is 10-100 s.
Preferably, the vapor-phase spray deposition conditions are: the temperature is 600-1000 ℃, and the treatment time is 100-1000 s.
Preferably, the carbon source gas in the step of vapor-phase spray deposition is one or more of methane, acetylene, propylene, natural gas, coal gas and the like.
(III) advantageous effects
The invention provides a preparation process of a polyimide silicon tab material. Compared with the prior art, the method has the following beneficial effects: the mixed powder of silicon, silicon monoxide and lithium element compound is filled into the cellular porous polyimide by a plasma gas phase method to obtain a deposition material, and the deposition material is used as a tab material, so that the poor compatibility of a copper interface and a negative electrode material interface is improved, the conductivity of the whole tab is improved, and the battery rate is improved; because no polymer adhesive is added, the cathode active material is in direct contact with the polyimide, and the electron transmission speed and the electron circulation stability are effectively improved. The technical problem of poor conductivity of the conventional pole lug is solved from the source of the material for preparing the pole lug.
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, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a scanned view of a honeycomb polyimide;
FIG. 2 is a scanning view of an integrated tab;
FIG. 3 is a schematic process diagram of step 3-1.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
According to the preparation process of the polyimide silicon tab material, in the existing preparation process of the negative electrode material tab, a high-molecular binder is required to be added when the negative electrode material is combined with copper foil, and the binder is a non-conductive high polymer, so that an electronic conductive channel is blocked, and the transmission speed is reduced; meanwhile, the high-molecular bonding property is influenced by poor compatibility between a copper interface and a cathode material interface along with the transmission of electrons, so that the cycling stability and the capacity of the battery are influenced. Therefore, the conventional pole lug has the technical problem of poor conductivity.
In order to solve the problem of crosstalk, the technical scheme in the embodiment of the present application has the following general idea: polyimide is adopted to replace copper foil, so that poor compatibility of a copper interface and a negative electrode material interface is improved; because no polymer adhesive is added, the cathode active material is in direct contact with the polyimide, and the electron transmission speed and the electron circulation stability are effectively improved. The technical problem of poor conductivity of the conventional pole lug is solved from the source of the material for preparing the pole lug.
In order to better understand the technical solution, the technical solution will be described in detail with reference to the drawings and the specific embodiments.
A preparation process of a polyimide silicon tab material specifically comprises the following steps:
preparing cellular porous polyimide;
mixing silicon, silicon monoxide and lithium element compound into mixed powder;
filling the mixed powder into honeycomb porous polyimide by a plasma gas phase method to obtain a deposition material;
the deposition material is prepared into the cathode material through carbon deposition.
As shown in fig. 1, the scanning graph of the prepared honeycomb polyimide is shown, and the mixed powder is filled into the honeycomb porous polyimide by a plasma gas phase method to obtain a deposition material, which is specifically shown in fig. 3. Fig. 2 shows a scanning diagram of the integrated tab.
In the embodiment, the copper foil is replaced by the polyimide, so that the compatibility of a copper interface and a negative electrode material interface is improved; because no polymer adhesive is added, the cathode active material is in direct contact with the polyimide, and the electron transmission speed and the electron circulation stability are effectively improved. Because the heat conduction speed of the polyimide is better than that of the copper foil, potential safety hazards such as high temperature of the battery are effectively avoided, the electric conductivity of the integral lug is improved, and the battery rate is improved. The technical problem of poor conductivity of the conventional pole lug is solved from the source of the material for preparing the pole lug. And the technical problems that the copper pole lug is easy to corrode and the like are avoided.
In a specific implementation process, in the step S1, preparing honeycomb-shaped porous polyimide:
s1-1, dissolving pyromellitic dianhydride, 4' -diaminodiphenyl ether, dimethylacetamide, N-methyl-2-pyrrolidone and fluorine compounds serving as raw materials under the protection of nitrogen; specifically, the fluorine-containing compound is one or more selected from (3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10, 10-heptadecafluorodecyl) silane which is one or more selected from fluorotriethoxysilane, triethoxytrifluoromethylsilane, 1,2, 2-tetrahydroperfluorohexyltriethoxysilane, triethoxy-3, 3,4,4,5,5,6,6, 6-nonafluorohexylsilane, triethoxy [4- (trifluoromethyl) phenyl ] silane and triethoxy.
S1-2, adding polystyrene into the solution obtained in the step S1-1, wherein the specific particle size of the polystyrene is 50-200 nm, the using amount of the polystyrene is 1-5 wt%, stirring and refluxing for 2-10h under the protection of nitrogen;
s1-3, preparing a film with the thickness of 25-100 mu m by injection-calendaring molding through the solution refluxed in the step S1-2, and drying at 40-80 ℃;
and S1-4, graphitizing the dried film obtained in the step S1-3 at 2500-3000 ℃, and preserving heat for 5-10 hours.
In a specific implementation process, the preparation process of the mixed powder comprises the following steps:
taking 20-40 parts of high-purity silicon, 30-80 parts of silicon monoxide and 2-10 parts of lithium element compound; by controlling reasonable raw material proportion, volume expansion is reduced, energy density is improved, material lithium wedge is improved, and first effect is increased.
And (4) placing the mixture in a ball mill for ball milling for 8-10 h, wherein a ball milling medium is zirconium oxide.
In the specific implementation process, the specific steps of filling the mixed powder into the cellular porous polyimide by using a plasma gas phase method are as follows:
s3-1: placing the mixed powder in a plasma processor, vacuumizing, and introducing jet gas, as shown in FIG. 3;
s3-2: starting plasma heating;
s3-3: and (6) cooling.
In a specific implementation process, the carbon deposition comprises the following specific steps:
and (3) placing the deposition material in a vapor deposition furnace, introducing carbon source gas, and performing vapor-phase jet deposition.
In the specific implementation process, the lithium inorganic compound is as follows: one or more of lithium metasilicate, lithium carbonate, lithium halide and lithium nitrate. Other lithium-based compounds may also be selected by those skilled in the art.
In a specific implementation process, the conditions of the step S4-1 are as follows: the vacuum degree is 10-150 Pa, the jet gas is argon, and the jet speed is 1-30 m/s.
In a specific implementation process, the plasma heating conditions in the step S4-2 are as follows: the temperature is 2000-3500 ℃, and the processing time is 10-100 s.
In the specific implementation process, the vapor phase spray deposition conditions are as follows: the temperature is 600-1000 ℃, and the treatment time is 100-1000 s;
in a specific implementation process, in the vapor phase spray deposition in step S4-3, the carbon source gas is one or more of methane, acetylene, propylene, natural gas, coal gas, and the like.
The following is a detailed description of the specific examples:
example 1:
a preparation process of a polyimide silicon tab material specifically comprises the following steps:
(1) preparing cellular porous polyimide;
s1-1, dissolving pyromellitic dianhydride, 4' -diaminodiphenyl ether, dimethylacetamide, N-methyl-2-pyrrolidone and fluorine compounds serving as raw materials under the protection of nitrogen;
s1-2, stirring and refluxing the solution obtained in the step S1-1 for 2 hours under the protection of nitrogen;
s1-3, preparing a 25 mu m film by injection-calendaring molding the solution refluxed in the step S1-2, and drying at 40 ℃;
and S1-4, graphitizing the dried film obtained in the step S1-3 at 2500 ℃, and preserving heat for 5 hours.
(2) Mixing silicon, silicon monoxide and lithium element compound into mixed powder;
and (3) placing 20 parts of high-purity silicon, 80 parts of silicon monoxide and 2 parts of lithium element compound in a ball mill for ball milling for 10 hours, wherein a ball milling medium is zirconium oxide.
(3) Filling the mixed powder into honeycomb porous polyimide by a plasma gas phase method to obtain a deposition material;
s3-1: placing the mixed powder in a plasma processor, vacuumizing, and introducing jet gas; the concrete conditions are as follows: the vacuum degree is 10Pa, the jet gas is argon, and the jet speed is 30 m/s.
S3-2: starting plasma heating, wherein the plasma heating conditions are as follows: the temperature was 2000 ℃ and the treatment time was 100 s.
S3-3: and (6) cooling.
(4) The deposition material is prepared into the cathode material by carbon deposition
And (3) placing the deposition material in a vapor deposition furnace, introducing carbon source gas, and performing vapor-phase jet deposition. The vapor phase spray deposition conditions are as follows: the temperature is 600 ℃, and the treatment time is 100 s; the carbon source gas is one or more of methane, acetylene, propylene, natural gas, coal gas and the like.
Example 2:
a preparation process of a polyimide silicon tab material specifically comprises the following steps:
(1) preparing cellular porous polyimide;
s1-1, dissolving pyromellitic dianhydride, 4' -diaminodiphenyl ether, dimethylacetamide, N-methyl-2-pyrrolidone and fluorine compounds serving as raw materials under the protection of nitrogen;
s1-2, stirring and refluxing the solution obtained in the step S1-1 for 10 hours under the protection of nitrogen;
s1-3, preparing a 2100 mu m film by injection-calendaring molding the solution refluxed in the step S1-2, and drying at 80 ℃;
and S1-4, graphitizing the dried film obtained in the step S1-3 at 3000 ℃, and preserving heat for 10 hours.
(2) Mixing silicon, silicon monoxide and lithium element compound into mixed powder;
40 parts of high-purity silicon, 30 parts of silicon monoxide and 10 parts of lithium element compound are taken and put into a ball mill for ball milling for 10 hours, and the ball milling medium is zirconium oxide.
(3) Filling the mixed powder into honeycomb porous polyimide by a plasma gas phase method to obtain a deposition material;
s3-1: placing the mixed powder in a plasma processor, vacuumizing, and introducing jet gas; the concrete conditions are as follows: the vacuum degree is 150Pa, the jet gas is argon, and the jet speed is 30 m/s.
S3-2: starting plasma heating, wherein the plasma heating conditions are as follows: the temperature was 3500 ℃ and the treatment time was 100 s.
S3-3: and (6) cooling.
(4) The deposition material is prepared into the cathode material by carbon deposition
And (3) placing the deposition material in a vapor deposition furnace, introducing carbon source gas, and performing vapor-phase jet deposition. The vapor phase spray deposition conditions are as follows: the temperature is 1000 ℃, and the treatment time is 1000 s; the carbon source gas is one or more of methane, acetylene, propylene, natural gas, coal gas and the like.
Example 3
A preparation process of a polyimide silicon tab material specifically comprises the following steps:
(1) preparing cellular porous polyimide;
s1-1, dissolving pyromellitic dianhydride, 4' -diaminodiphenyl ether, dimethylacetamide, N-methyl-2-pyrrolidone and fluorine compounds serving as raw materials under the protection of nitrogen;
s1-2, stirring and refluxing the solution obtained in the step S1-1 for 6 hours under the protection of nitrogen;
s1-3, preparing a film with the thickness of 60 microns by injection-calendaring molding the solution refluxed in the step S1-2, and drying at 60 ℃;
and S1-4, graphitizing the dried film obtained in the step S1-3 at 2800 ℃ and preserving heat for 7 hours.
(2) Mixing silicon, silicon monoxide and lithium element compound into mixed powder;
30 parts of high-purity silicon, 50 parts of silicon monoxide and 6 parts of lithium element compound are taken and put into a ball mill for ball milling for 9 hours, and the ball milling medium is zirconium oxide.
(3) Filling the mixed powder into honeycomb porous polyimide by a plasma gas phase method to obtain a deposition material;
s3-1: placing the mixed powder in a plasma processor, vacuumizing, and introducing jet gas; the concrete conditions are as follows: the vacuum degree is 80Pa, the jet gas is argon, and the jet speed is 15 m/s.
S3-2: starting plasma heating, wherein the plasma heating conditions are as follows: the temperature was 3000 ℃ and the treatment time was 60 s.
S3-3: and (6) cooling.
(4) The deposition material is prepared into the cathode material by carbon deposition
And (3) placing the deposition material in a vapor deposition furnace, introducing carbon source gas, and performing vapor-phase jet deposition. The vapor phase spray deposition conditions are as follows: the temperature is 800 ℃, and the processing time is 600 s; the carbon source gas is one or more of methane, acetylene, propylene, natural gas, coal gas and the like.
The resistance of the products prepared in the above examples 1 to 3 was measured by a full-automatic four-probe resistance tester, and the comparative example 1 and the comparative example 2 were selected as references, and the measurement results are shown in the following table 1:
TABLE 1 comparison of conductivity
| Serial number | Resistance (RC) |
| Comparative example 1 | 580mΩ/sq |
| Comparative example 2 | 600mΩ/sq |
| Example 1 | 20mΩ/sq |
| Example 2 | 25mΩ/sq |
| Example 2 | 21mΩ/sq |
Wherein comparative examples 1 and 2 are common lithium battery coating electrode lugs, and the preparation method comprises the following steps: copper foil is used as a negative electrode carrier, polymer PVDF is used as a binder, carbon black and an active substance are stirred, coated on a copper sheet, dried and the like.
The above data can show that the conductivity of the tab prepared by the embodiment of the invention is significantly improved.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. A preparation process of a polyimide silicon tab material is characterized by comprising the following steps:
preparing cellular porous polyimide;
mixing silicon, silicon monoxide and lithium element compound into mixed powder;
filling the mixed powder into honeycomb porous polyimide by a plasma gas phase method to obtain a deposition material;
preparing the deposition material into a negative electrode material through carbon deposition;
preparing the cellular porous polyimide:
s1-1, dissolving pyromellitic dianhydride, 4' -diaminodiphenyl ether, dimethylacetamide, N-methyl-2-pyrrolidone and fluorine compounds serving as raw materials under the protection of nitrogen;
s1-2, stirring and refluxing the solution obtained in the step S1-1 for 2-10 hours under the protection of nitrogen;
s1-3, preparing a film with the thickness of 25-100 mu m by injection-calendaring molding through the solution refluxed in the step S1-2, and drying at 40-80 ℃;
and S1-4, graphitizing the dried film obtained in the step S1-3 at 2500-3000 ℃, and preserving heat for 5-10 hours.
2. The process for preparing the polyimide silicon tab material according to claim 1, wherein the process for preparing the mixed powder comprises the following steps:
taking 20-40 parts of high-purity silicon, 30-80 parts of silicon monoxide and 2-10 parts of lithium element compound, and placing the mixture in a ball mill for ball milling for 8-10 hours, wherein a ball milling medium is zirconium oxide.
3. The preparation process of the polyimide silicon tab material according to claim 1, wherein the step of filling the mixed powder into the cellular porous polyimide by a plasma gas phase method comprises the following specific steps:
s3-1: placing the mixed powder in a plasma processor, vacuumizing, and introducing jet gas;
s3-2: starting plasma heating;
s3-3: and (6) cooling.
4. The process for preparing the polyimide silicon tab material according to claim 1, wherein the carbon deposition comprises the following specific steps:
and (3) placing the deposition material in a vapor deposition furnace, introducing carbon source gas, and performing vapor-phase jet deposition.
5. The process for preparing the polyimide silicon tab material according to claim 1, wherein the lithium element compound is one or more of a lithium-based inorganic compound and a lithium-based organic compound.
6. The process for preparing a polyimide silicon tab material according to claim 3, wherein the conditions of the step S3-1 are as follows: the vacuum degree is 10-150 Pa, the jet gas is argon, and the jet speed is 1-30 m/s.
7. The process for preparing a polyimide silicon tab material according to claim 3, wherein the plasma heating conditions in step S3-2 are as follows: the temperature is 2000-3500 ℃, and the processing time is 10-100 s.
8. The process for preparing the polyimide silicon tab material according to claim 4, wherein the vapor phase spray deposition conditions are as follows: the temperature is 600-1000 ℃, and the treatment time is 100-1000 s.
9. The process for preparing the polyimide silicon tab material according to claim 4, wherein the carbon source gas in the vapor phase spray deposition is one or more of methane, acetylene, propylene, natural gas, coal gas and the like.
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