CN109763263B - Process for preparing silicon-carbon tab material by electrostatic spinning - Google Patents
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Abstract
The invention provides a process for preparing a silicon-carbon tab material by electrostatic spinning, and relates to the technical field of lithium ion batteries. The method comprises the following steps: preparing a polyimide solution; preparing nano silicon, silicon monoxide and lithium element composite powder; ultrasonically dispersing the polyimide solution and the composite powder to form a suspension, and preparing an integrated fibrous membrane by an electrostatic spinning machine; and carrying out heat treatment on the integrated fiber membrane to prepare the silicon-carbon tab material. The polyimide is adopted to replace the traditional copper foil as a tab material, 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. 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 technical field of lithium ion batteries, in particular to a process for preparing a silicon carbon electrode lug material by electrostatic spinning.
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 blocked, 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 process for preparing a silicon-carbon tab material by electrostatic spinning, which solves the technical 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 process for preparing a silicon-carbon tab material by electrostatic spinning comprises the following steps:
preparing a polyimide solution;
preparing nano silicon, silicon monoxide and lithium element compound composite powder;
ultrasonically dispersing the polyimide solution and the composite powder to form a suspension, and preparing an integrated fibrous membrane by an electrostatic spinning machine;
and carrying out heat treatment on the integrated fiber membrane to prepare the silicon-carbon tab material.
Preferably, the preparation of the polyimide solution comprises the steps of:
s1-1, dissolving ketone anhydride and sodium methoxide solvent in a mixed solution of DMF and DMAc;
s1-2, slowly dripping TDI and MDr into the polar solvent of the step S1-1 for dissolving, and carrying out polycondensation reaction to obtain a viscous PI solution;
s1-3, precipitating the prepared PI polymer solution in an acetone solvent, and filtering and purifying;
s1-4, dissolving the powder obtained by filtering in the step S1-3 in a mixed solution of DMF and DMAc, and adding a proper solution to prepare a spinning solution with the viscosity of 50-600 Pa.s and the concentration of 2-20 wt%; wherein the moderate solution is one or more of acetone, alcohol and PAN.
Preferably, the preparation of the nano-silicon, silicon monoxide and lithium element compound composite powder comprises the following steps:
s2-1, mixing high-purity silicon with silicon monoxide;
s2-2, preparing composite powder of nano silicon, silicon monoxide and lithium element compounds from the mixture obtained in the step S2-1 by one or more methods of high-energy ball milling, electric arc method and plasma spraying method;
s2-3, dispersing and collecting the composite powder.
Preferably, the heat treatment conditions are as follows: and carrying out carbonization heat treatment on the integrated fiber membrane under the protection of nitrogen or argon.
Preferably, in the step S1-1, the reaction is carried out under the protection of nitrogen, and the volume ratio of DMF to DMAc is 1-50: 1-50.
Preferably, the mass ratio of the high-purity silicon to the silicon monoxide in the step S2-1 is 5-1: 1-20.
Preferably, the step S2-2 includes the following steps:
adding the mixture obtained in the step S2-1, performing wet grinding for high-energy ball milling, and performing repeated circulating ball milling for 4-20 hours;
the dispersing agent is one or more of DMF, acetone, alcohol and PAN.
Preferably, the temperature of the heat treatment is 600-1200 ℃, and the treatment time is 0.5-10 h.
(III) advantageous effects
The invention provides a process for preparing a silicon-carbon tab material by electrostatic spinning. Compared with the prior art, the method has the following beneficial effects:
the polyimide is adopted to replace the traditional copper foil as the tab material, so that the 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.
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 process for preparing the silicon-carbon tab material through electrostatic spinning, 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 adhesive property is influenced by poor compatibility between a copper interface and a negative electrode 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 above crosstalk problem, the technical solution in the embodiment of the present application has the following general idea: the polyimide is adopted to replace copper foil, so that the tolerance performance of a copper interface and a negative electrode material interface is improved; because no polymer adhesive is added, the cathode active material is directly contacted 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 above technical solutions, the following detailed descriptions will be provided for the above technical solutions with specific embodiments.
A process for preparing a silicon-carbon tab material by electrostatic spinning comprises the following steps:
preparing a polyimide solution;
preparing nano silicon, silicon monoxide and lithium element composite powder;
ultrasonically dispersing the polyimide solution and the composite powder to form a suspension, and preparing an integrated fibrous membrane by an electrostatic spinning machine;
and carrying out heat treatment on the integrated fiber membrane to prepare the silicon-carbon tab material.
In the specific implementation of the embodiment, the polyimide is adopted to replace the copper foil, so that the technical problems of the tolerance between a copper interface and a negative electrode material interface and the like are solved; 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 root of preparing pole lug materials.
Specifically, the preparation of the polyimide solution comprises the following steps:
s1-1, dissolving ketone anhydride and sodium methoxide solvent in a mixed solution of DMF and DMAc;
s1-2, slowly dripping TDI and MDr into the polar solvent of the step S1-1 for dissolving, and carrying out polycondensation reaction to obtain a viscous PI solution;
s1-3, precipitating the prepared PI polymer solution in an acetone solvent, and filtering and purifying;
s1-4, dissolving the powder obtained by filtering in the step S1-3 in a mixed solution of DMF and DMAc, and adding a proper solution to prepare a spinning solution with the viscosity of 50-600 Pa.s and the concentration of 2-20 wt%; the moderate solution is one or more of acetone, alcohol and PAN. The preparation of the polyimide solution by the above examples provides a basis for the subsequent electrostatic protection of the filaments.
In the specific implementation process, the preparation of the nano silicon, silicon monoxide and lithium element compound composite powder comprises the following steps:
s2-1, mixing high-purity silicon, silicon monoxide and lithium element compound; the high-purity silicon is silicon with purity of more than 99.5 percent;
s2-2, preparing composite powder of nano silicon, silicon monoxide and lithium element compounds from the mixture obtained in the step S2-1 by one or more methods of high-energy ball milling, electric arc method and plasma spraying method;
s2-3, dispersing and collecting the composite powder; specifically, DMF is taken as a dispersing agent and is doped into the composite powder in the later preparation stage to prevent powder agglomeration.
In the specific implementation process, the heat treatment conditions are as follows: and carrying out carbonization heat treatment on the integrated fiber membrane under the protection of nitrogen or argon.
In the specific implementation process, in the step S1-1, the oxidation-reduction reaction is sufficiently reduced by performing under the protection of nitrogen and by setting the volume ratio of DMF to DMAc to be 1-50: 1-50.
In the specific implementation process, the mass ratio of the high-purity silicon to the silicon monoxide in the step S2-1 is 5-1: 1-20, so that the volume expansion is reduced sufficiently.
In a specific implementation process, the step S2-2 specifically includes the following steps:
adding the mixture obtained in the step S2-1, performing wet grinding for high-energy ball milling, and performing repeated circulating ball milling for 4-20 hours;
the dispersing agent is one or more of DMF, acetone, alcohol and PAN.
In the specific implementation process, the temperature of the heat treatment in the step S4 is 600-1200 ℃, and the treatment time is 0.5-10 h.
The following is a detailed description of the specific examples:
example 1:
a process for preparing a silicon-carbon tab material by electrostatic spinning comprises the following steps:
(1) preparing a polyimide solution;
s1-1, dissolving ketone anhydride and sodium methoxide solvent in a mixed solution of DMF and DMAc; in the step S1-1, the reaction is carried out under the protection of nitrogen, and the volume ratio of DMF to DMAc is 1: 1.
S1-2, slowly dripping TDI and MDr into the polar solvent of the step S1-1 for dissolving, and carrying out polycondensation reaction to obtain a viscous PI solution; the mass ratio of the high-purity silicon to the silicon monoxide in the step S2-1 is 5: 1.
S1-3, precipitating the prepared PI polymer solution in an acetone solvent, and filtering and purifying;
s1-4, dissolving the powder obtained by filtering in the step S1-3 in a mixed solution of DMF and DMAc, and adding a moderate solution to prepare a spinning stock solution with the viscosity of 50Pa.s and the concentration of 2 wt%; wherein the moderate solution is one or more of acetone, alcohol and PAN.
(2) Preparing nano silicon, silicon monoxide and lithium element compound composite powder;
s2-1, mixing high-purity silicon, silicon monoxide and lithium element compound;
s2-2, preparing composite powder of nano silicon, silicon monoxide and lithium element compounds from the mixture obtained in the step S2-1 by one or more methods of high-energy ball milling, electric arc method and plasma spraying method; the step S2-2 comprises the following steps:
adding the mixture obtained in the step S2-1, performing wet grinding by high-energy ball milling, and performing repeated circulating ball milling for 4 hours;
the dispersing agent is one or more of DMF, acetone, alcohol and PAN.
And S2-3, dispersing and collecting the composite powder, taking DMF as a dispersing agent, and mixing the DMF into the composite powder to prevent the powder from agglomerating at the later stage of preparation.
(3) Ultrasonically dispersing the polyimide solution and the composite powder to form a suspension, and preparing an integrated fibrous membrane by an electrostatic spinning machine;
(4) and carrying out heat treatment on the integrated fiber membrane to prepare the silicon-carbon tab material.
The conditions of the heat treatment are as follows: and carrying out carbonization heat treatment on the integrated fiber membrane under the protection of nitrogen or argon. The temperature of the heat treatment in the step S4 is 600 ℃, and the treatment time is 0.5 hh.
Example 2:
a process for preparing a silicon-carbon tab material by electrostatic spinning comprises the following steps:
(1) preparing a polyimide solution;
s1-1, dissolving ketone anhydride and sodium methoxide solvent in a mixed solution of DMF and DMAc; in the step S1-1, the reaction is carried out under the protection of nitrogen, and the volume ratio of DMF to DMAc is 1: 50.
S1-2, slowly dripping TDI and MDr into the polar solvent of the step S1-1 for dissolving, and carrying out polycondensation reaction to obtain a viscous PI solution; the mass ratio of the high-purity silicon to the silicon monoxide in the step S2-1 is 1: 1.
S1-3, precipitating the prepared PI polymer solution in an acetone solvent, and filtering and purifying;
s1-4, dissolving the powder obtained by filtering in the step S1-3 in a mixed solution of DMF and DMAc, and adding a moderate solution to prepare a spinning stock solution with the viscosity of 600Pa.s and the concentration of 20 wt%; wherein the moderate solution is one or more of acetone, alcohol and PAN.
(2) Preparing nano silicon, silicon monoxide and lithium element composite powder;
s2-1, mixing high-purity silicon, silicon monoxide and lithium element compound;
s2-2, preparing composite powder of nano silicon, silicon monoxide and lithium element compounds from the mixture obtained in the step S2-1 by one or more methods of high-energy ball milling, electric arc method and plasma spraying method; the step S2-2 comprises the following steps:
adding the mixture obtained in the step S2-1, performing wet grinding by high-energy ball milling, and performing repeated circulating ball milling for 20 hours;
the dispersing agent is one or more of DMF, acetone, alcohol and PAN.
And S2-3, dispersing and collecting the composite powder, taking DMF as a dispersing agent, and mixing the DMF into the composite powder to prevent the powder from agglomerating at the later stage of preparation.
(3) Ultrasonically dispersing the polyimide solution and the composite powder to form a suspension, and preparing an integrated fibrous membrane by an electrostatic spinning machine;
(4) and carrying out heat treatment on the integrated fiber membrane to prepare the silicon-carbon tab material.
The conditions of the heat treatment are as follows: and carrying out carbonization heat treatment on the integrated fiber membrane under the protection of nitrogen or argon. The temperature of the heat treatment in the step S4 is 61200 ℃, and the treatment time is 10 h.
Example 3:
a process for preparing a silicon-carbon tab material by electrostatic spinning comprises the following steps:
(1) preparing a polyimide solution;
s1-1, dissolving ketone anhydride and sodium methoxide solvent in a mixed solution of DMF and DMAc; in the step S1-1, the reaction is carried out under the protection of nitrogen, and the volume ratio of DMF to DMAc is 50: 1.
S1-2, slowly dripping TDI and MDr into the polar solvent of the step S1-1 for dissolving, and carrying out polycondensation reaction to obtain a viscous PI solution; the mass ratio of the high-purity silicon to the silicon monoxide in the step S2-1 is 1: 20.
S1-3, precipitating the prepared PI polymer solution in an acetone solvent, and filtering and purifying;
s1-4, dissolving the powder obtained by filtering in the step S1-3 in a mixed solution of DMF and DMAc, and adding a moderate solution to prepare a spinning stock solution with the viscosity of 200Pa.s and the concentration of 10 wt%; wherein the moderate solution is one or more of acetone, alcohol and PAN.
(2) Preparing nano silicon, silicon monoxide and lithium element compound composite powder;
s2-1, mixing high-purity silicon, silicon monoxide and lithium element compound;
s2-2, preparing composite powder of nano silicon, silicon monoxide and lithium element compounds from the mixture obtained in the step S2-1 by one or more methods of high-energy ball milling, electric arc method and plasma spraying method; the step S2-2 comprises the following steps:
adding the mixture obtained in the step S2-1, performing wet grinding by high-energy ball milling, and performing repeated circulating ball milling for 12 hours;
the dispersing agent is one or more of DMF, acetone, alcohol and PAN.
And S2-3, dispersing and collecting the composite powder, taking DMF as a dispersing agent, and mixing the DMF into the composite powder to prevent the powder from agglomerating at the later stage of preparation.
(3) Ultrasonically dispersing the polyimide solution and the composite powder to form a suspension, and preparing an integrated fibrous membrane by an electrostatic spinning machine;
(4) and carrying out heat treatment on the integrated fiber membrane to prepare the silicon-carbon tab material.
The conditions of the heat treatment are as follows: and carrying out carbonization heat treatment on the integrated fiber membrane under the protection of nitrogen or argon. The temperature of the heat treatment in the step S4 is 900 ℃, and the treatment time is 6 h.
The resistance of the products prepared in the above examples 1 to 3 was measured by using a full-automatic four-probe resistance tester, and the results of the measurements were as shown in the following table 1, with reference to comparative example 1 and comparative example 2:
TABLE 1 comparison of conductivity
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 data clearly show that the conductivity of the tab material prepared by the invention is greatly improved.
It is noted that, in this document, relational terms such as first and second, and the like are 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 like 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 (5)
1. A process for preparing a silicon-carbon tab material by electrostatic spinning is characterized by comprising the following steps:
preparing a polyimide solution;
preparing nano silicon, silicon monoxide and lithium element compound composite powder;
ultrasonically dispersing the polyimide solution and the composite powder to form a suspension, and preparing an integrated fibrous membrane by an electrostatic spinning machine;
carrying out heat treatment on the integrated fiber membrane to obtain a silicon-carbon tab material;
the conditions of the heat treatment are as follows: carrying out carbonization heat treatment on the integrated fiber membrane under the protection of nitrogen or argon;
the preparation of the polyimide solution comprises the following steps:
s1-1, dissolving ketone anhydride and sodium methoxide solvent in a mixed solution of DMF and DMAc;
s1-2, slowly dripping TDI and MDr into the polar solvent of the step S1-1 for dissolving, and carrying out polycondensation reaction to obtain a viscous PI solution;
s1-3, precipitating the prepared PI polymer solution in an acetone solvent, filtering and purifying;
s1-4, dissolving the powder obtained by filtering in the step S1-3 in a mixed solution of DMF and DMAc, and adding a proper solution to prepare a spinning stock solution with the viscosity of 50-600 Pa.s and the concentration of 2-20 wt%; wherein the moderate solution is one or more of acetone, alcohol and PAN;
the preparation method of the nano silicon, silicon monoxide and lithium element compound composite powder comprises the following steps:
s2-1, mixing high-purity silicon, silicon monoxide and lithium element compound;
s2-2, preparing composite powder of nano silicon, silicon monoxide and lithium element compound by one or more methods of high-energy ball milling, electric arc method and plasma spraying method from the mixture obtained in the step S2-1;
s2-3, dispersing and collecting the composite powder.
2. The process for preparing the silicon-carbon tab material through electrostatic spinning according to claim 1, wherein the step S1-1 is performed under the protection of nitrogen, and the volume ratio of DMF to DMAc is 1-50: 1-50.
3. The process for preparing the silicon-carbon tab material through electrostatic spinning according to claim 1, wherein the mass ratio of the high-purity silicon to the silicon monoxide in the step S2-1 is 5-1: 1-20.
4. The process for preparing the silicon-carbon tab material through electrostatic spinning according to claim 1, wherein the step S2-2 comprises the following steps:
and (4) adding the mixture obtained in the step (S2-1), performing wet grinding by adopting high-energy ball milling, and performing repeated circulating ball milling for 4-20 hours.
5. The process for preparing the silicon-carbon tab material through electrostatic spinning according to claim 1, wherein the temperature of the heat treatment is 600-1200 ℃, and the treatment time is 0.5-10 h.
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