CN110890547B - Slurry stabilizer for preparing nitrogen-boron doped carbon fiber and composite electrode - Google Patents
Slurry stabilizer for preparing nitrogen-boron doped carbon fiber and composite electrode Download PDFInfo
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Abstract
The invention relates to a slurry stabilizer for preparing nitrogen-boron doped carbon fibers and composite electrodes, which is prepared by mixing a high-polarity organic compound and N-methylpyrrolidone and dispersing a binder. The high-polarity organic compound is one or two of amide and sulfoxide, and the amide is one or two of dimethylacetamide, diethylformamide, diethylacetamide, methylethylformamide and methylethylacetamide; the sulfoxide is one or two of dimethyl sulfoxide, diethyl sulfoxide and methyl ethyl sulfoxide; the volume ratio of the high-polarity organic compound to the N-methyl pyrrolidone solvent is 0.03-3. The slurry stabilizer is used for preparing nitrogen-boron doped carbon fiber, nitrogen-boron doped carbon fiber/molybdenum sulfide, nitrogen-boron doped carbon fiber/zinc sulfide, nitrogen-boron doped carbon fiber/iron sulfide and nitrogen-boron doped carbon fiber/manganese sulfide electrodes; the stability and the electrochemical performance of the electrode material are greatly improved, so that the electrode material has wide application prospect in the field of energy storage.
Description
Technical Field
The invention relates to the field of lithium ion batteries, in particular to a slurry stabilizer for preparing nitrogen-boron doped carbon fibers and composite electrodes.
Background
The lithium ion battery has the advantages of high energy storage density, long service life, small environmental pollution and the like, and is widely applied to the fields of various portable electronic equipment and electric automobiles. In the preparation process of the negative electrode, the negative electrode active material, the conductive agent and the binder are uniformly, stably and dispersedly dispersed in the solvent, which is the key for determining the coating quality and the yield of the subsequent slurry. Therefore, finding a suitable binder and a solvent for dissolving the binder has been a problem to be solved urgently in the preparation of the negative electrode. At present, the commonly used lithium ion battery cathode slurry stabilizer (the binder is acrylic resin and polyvinylidene fluoride, and the dissolving solvent is N-methyl pyrrolidone) is easy to cause poor rheological property or stability, and poor phenomena such as sedimentation or edge bulging of slurry coating and the like.
Patent 1(CN109817985A) discloses a stabilizer for negative electrode slurry of lithium ion battery, which adopts polyacrylonitrile and N-methylpyrrolidone and ethanol solvent for dissolving polyacrylonitrile, and can significantly reduce instability index of negative electrode slurry, improve stability of negative electrode slurry, and further inhibit slurry sedimentation, and prevent adverse phenomena such as edge bulging of slurry coating edge. However, the cathode slurry stabilizer is only suitable for battery cathode slurry of artificial graphite, natural graphite, lithium titanate and silicon carbon; other negative electrode materials, particularly nitrogen-boron doped carbon fibers and composite electrode materials are not involved.
Disclosure of Invention
Aiming at the defects, the invention provides a slurry stabilizer for preparing nitrogen-boron doped carbon fibers and composite electrodes, which comprises the following steps: a slurry stabilizer for preparing nitrogen-boron doped carbon fibers and composite electrodes comprises a binder and a solvent for dissolving the binder; the binder is 0.1-50% of the solvent for dissolving the binder by mass percent; the binder is one of acrylic resin, polyvinylidene fluoride, aqueous sodium alginate and polytetrafluoroethylene;
the solvent is a mixture of N-methyl pyrrolidone and a high-polarity organic compound;
the high-polarity organic compound is one or two of amide and sulfoxide;
the amide is one or two of dimethylacetamide, diethylformamide, diethylacetamide, methylethylformamide and methylethylacetamide;
the sulfoxide is one or two of dimethyl sulfoxide, diethyl sulfoxide and methyl ethyl sulfoxide;
the volume ratio of the high-polarity organic compound to the N-methyl pyrrolidone solvent is 0.03-3;
the slurry stabilizer is applied to the preparation of nitrogen-boron doped carbon fibers and composite electrodes;
the nitrogen-boron-doped carbon fiber and composite electrode material is one of nitrogen-boron-doped carbon fiber, nitrogen-boron-doped carbon fiber/molybdenum sulfide, nitrogen-boron-doped carbon fiber/zinc sulfide, nitrogen-boron-doped carbon fiber/iron sulfide and nitrogen-boron-doped carbon fiber/manganese sulfide.
The nitrogen-boron doped carbon fiber is nitrogen-boron co-doped carbonized bacterial cellulose.
1) According to the invention, the high-polarity solvent amide, sulfoxide and N-methyl pyrrolidone are mixed to form the polar solvent, the stable and uniform dispersion of the binder in the solvent is greatly promoted through the bond-bond action of functional groups such as amino, carbonyl, sulfinyl and the like, and the adverse phenomena such as edge bulging and the like during slurry coating are prevented in the electrode preparation process.
Compared with the prior art, the invention has the beneficial effects that:
2) the cathode slurry stabilizer is applied to cathode active substances such as nitrogen-boron doped carbon fiber, nitrogen-boron doped carbon fiber/molybdenum sulfide, nitrogen-boron doped carbon fiber/zinc sulfide, nitrogen-boron doped carbon fiber/iron sulfide and nitrogen-boron doped carbon fiber/manganese sulfide, can improve the stability of cathode slurry, further can inhibit slurry sedimentation, and can prevent adverse phenomena such as edge bulging of slurry coating edges.
3) The cathode slurry stabilizer provided by the invention is simple in preparation method, low in cost and large in market prospect.
4) The mixed solvent of N-methyl pyrrolidone and high-polarity organic compounds is adopted, and the electrochemical performance of the nitrogen-boron doped carbon fiber and the composite electrode prepared by the method is obviously higher than that of the same electrode which singly uses the N-methyl pyrrolidone solvent.
Detailed Description
In order to further understand the contents, features and effects of the present invention, the following embodiments are described in detail as follows:
example 1
Designing a nitrogen-boron doped carbon fiber and negative electrode slurry stabilizer:
1. the active substance is nitrogen-boron doped carbon fiber, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; active material: acetylene black: the proportion of the binder is 8: 1: 1; the solvent is N-methyl pyrrolidone and dimethyl acetamide; the polyvinylidene fluoride accounts for 5% of the weight of the solvent; the volume of the dimethylacetamide accounts for 10 percent of that of the N-methylpyrrolidone;
2. the active substance is nitrogen-boron doped carbon fiber, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; active material: acetylene black: the proportion of the binder is 8: 1: 1; the solvent is N-methyl pyrrolidone; the polyvinylidene fluoride accounts for 5% of the weight of the solvent;
the preparation method of the nitrogen-boron doped carbon fiber and the composite electrode comprises the following steps: 1) mixing N-methyl pyrrolidone and dimethyl acetamide according to a proportion to form a mixed solvent; 2) and weighing polyvinylidene fluoride, adding the polyvinylidene fluoride into a solvent, and stirring and dispersing to obtain a solution, namely the cathode slurry stabilizer. 2) Weighing active substances, a conductive agent and a negative electrode slurry stabilizer in proportion; 3) stirring, smearing, drying, slicing and the like to prepare a negative plate; 4) the button cells were assembled and tested for electrochemical performance.
The experimental results show that: the solvent is N-methyl pyrrolidone; the active substance is nitrogen-boron doped carbon fiber, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; the electrochemical capacity of the battery is 101mAh/g under the current density of 0.5C; under the same conditions, the solvents are N-methyl pyrrolidone and dimethyl acetamide; under the current density of 0.5C of the nitrogen-boron doped carbon fiber electrode, the electrochemical capacity is 233 mAh/g; obviously, the addition of the dimethylacetamide obviously improves the electrochemical performance of the nitrogen-boron doped carbon fiber electrode.
Example 2
Designing a nitrogen-boron doped carbon fiber composite electrode and a negative electrode slurry stabilizer:
3. the active substance is nitrogen-boron doped carbon fiber/molybdenum sulfide, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; active material: acetylene black: the proportion of the binder is 8: 1: 1; the solvent is N-methyl pyrrolidone and diethyl acetamide; the polyvinylidene fluoride accounts for 20% of the weight of the solvent; the volume of the diethyl acetamide is 50 percent of that of the N-methyl pyrrolidone;
4. the active substance is nitrogen-boron doped carbon fiber/molybdenum sulfide, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; active material: acetylene black: the proportion of the binder is 8: 1: 1; the solvent is N-methyl pyrrolidone; the polyvinylidene fluoride accounts for 20% of the weight of the solvent;
5. the active substance is nitrogen-boron doped carbon fiber/zinc sulfide, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; active material: acetylene black: the proportion of the binder is 8: 1: 1; the solvent is N-methyl pyrrolidone and methyl ethyl formamide; the polyvinylidene fluoride accounts for 40% of the weight of the solvent; the methyl ethyl formamide accounts for 100 percent of the volume of the N-methyl pyrrolidone;
6. the active substance is nitrogen-boron doped carbon fiber/zinc sulfide, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; active material: acetylene black: the proportion of the binder is 8: 1: 1; the solvent is N-methyl pyrrolidone; the polyvinylidene fluoride accounts for 40% of the weight of the solvent;
7. the active substance is nitrogen-boron doped carbon fiber/ferric sulfide, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; active material: acetylene black: the proportion of the binder is 8: 1: 1; the solvent is N-methyl pyrrolidone and methyl ethyl acetamide; the polyvinylidene fluoride accounts for 50% of the weight of the solvent; the volume of the methyl ethyl acetamide is 150 percent of that of the N-methyl pyrrolidone;
8. the active substance is nitrogen-boron doped carbon fiber/ferric sulfide, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; active material: acetylene black: the proportion of the binder is 8: 1: 1; the solvent is N-methyl pyrrolidone; the polyvinylidene fluoride accounts for 50% of the weight of the solvent;
9. the active substance is nitrogen-boron doped carbon fiber/manganese sulfide, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; active material: acetylene black: the proportion of the binder is 8: 1: 1; the solvent is N-methyl pyrrolidone and diethyl formamide; the weight of the polyvinylidene fluoride accounts for 1% of the weight of the solvent; the volume of the diethyl formamide is 200 percent of that of the N-methyl pyrrolidone;
10. the active substance is nitrogen-boron doped carbon fiber/manganese sulfide, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; active material: acetylene black: the proportion of the binder is 8: 1: 1; the solvent is N-methyl pyrrolidone; the weight of the polyvinylidene fluoride accounts for 1% of the weight of the solvent;
the preparation method of the nitrogen-boron doped carbon fiber and the composite electrode comprises the following steps: 1) mixing N-methyl pyrrolidone and amide in proportion to form a mixed solvent; 2) and weighing polyvinylidene fluoride, adding the polyvinylidene fluoride into the mixed solvent, and stirring and dispersing to obtain a solution, namely the cathode slurry stabilizer. 2) Weighing active substances, a conductive agent and a negative electrode slurry stabilizer in proportion; 3) stirring, smearing, drying, slicing and the like to prepare a negative plate; 4) the button cells were assembled and tested for electrochemical performance.
The experimental results show that: the addition of the high-polarity amide solvent obviously improves the electrochemical performance of the nitrogen-boron doped carbon fiber composite electrode.
Example 3
Designing a nitrogen-boron doped carbon fiber composite electrode and a negative electrode slurry stabilizer:
11. the active substance is nitrogen-boron doped carbon fiber/molybdenum sulfide, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; active material: acetylene black: the proportion of the binder is 8: 1: 1; the solvent is N-methyl pyrrolidone and dimethyl sulfoxide; the polyvinylidene fluoride accounts for 20% of the weight of the solvent; dimethyl sulfoxide accounts for 50% of the volume of the N-methyl pyrrolidone;
12. the active substance is nitrogen-boron doped carbon fiber/zinc sulfide, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; active material: acetylene black: the proportion of the binder is 8: 1: 1; the solvent is N-methyl pyrrolidone and diethyl sulfoxide; the polyvinylidene fluoride accounts for 40% of the weight of the solvent; the volume of the diethyl sulfoxide is 100 percent of that of the N-methyl pyrrolidone;
13. the active substance is nitrogen-boron doped carbon fiber/ferric sulfide, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; active material: acetylene black: the proportion of the binder is 8: 1: 1; the solvent is N-methyl pyrrolidone and methyl ethyl sulfoxide; the polyvinylidene fluoride accounts for 50% of the weight of the solvent; the volume of the methyl ethyl sulfoxide is 150 percent of that of the N-methyl pyrrolidone;
the preparation method of the nitrogen-boron doped carbon fiber and the composite electrode comprises the following steps: 1) mixing N-methyl pyrrolidone and sulfoxide in proportion to form a mixed solvent; 2) and weighing polyvinylidene fluoride, adding the polyvinylidene fluoride into the mixed solvent, and stirring and dispersing to obtain a solution, namely the cathode slurry stabilizer. 2) Weighing active substances, a conductive agent and a negative electrode slurry stabilizer in proportion; 3) stirring, smearing, drying, slicing and the like to prepare a negative plate; 4) the button cells were assembled and tested for electrochemical performance.
The experimental results show that: the addition of the high-polarity sulfoxide solvent obviously improves the electrochemical performance of the nitrogen-boron doped carbon fiber composite electrode.
Example 4
Designing a nitrogen-boron doped carbon fiber composite electrode and a negative electrode slurry stabilizer:
14. the active substance is nitrogen-boron doped carbon fiber, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; active material: acetylene black: the proportion of the binder is 8: 1: 1; the solvent is N-methyl pyrrolidone, dimethyl acetamide and diethyl acetamide; the polyvinylidene fluoride accounts for 5% of the weight of the solvent; the total volume of the dimethylacetamide and the diethylacetamide is 10% of the volume of the N-methylpyrrolidone;
15. the active substance is nitrogen-boron doped carbon fiber/molybdenum sulfide, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; active material: acetylene black: the proportion of the binder is 8: 1: 1; the solvent is N-methyl pyrrolidone, methyl ethyl formamide and dimethyl sulfoxide; the polyvinylidene fluoride accounts for 20% of the weight of the solvent; the total volume of the methyl ethyl formamide and the dimethyl sulfoxide is 50 percent of the volume of the N-methyl pyrrolidone;
16. the active substance is nitrogen-boron doped carbon fiber/zinc sulfide, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; active material: acetylene black: the proportion of the binder is 8: 1: 1; the solvent is N-methyl pyrrolidone, dimethyl sulfoxide and diethyl sulfoxide; the polyvinylidene fluoride accounts for 40% of the weight of the solvent; the total volume of the dimethyl sulfoxide and the diethyl sulfoxide is 100 percent of the volume of the N-methyl pyrrolidone;
17. the active substance is nitrogen-boron doped carbon fiber/ferric sulfide, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; active material: acetylene black: the proportion of the binder is 8: 1: 1; the solvent is N-methyl pyrrolidone, dimethyl sulfoxide and methyl ethyl sulfoxide; the polyvinylidene fluoride accounts for 50% of the weight of the solvent; the total volume of the dimethyl sulfoxide and the methyl ethyl sulfoxide is 150 percent of the volume of the N-methyl pyrrolidone;
18. the active substance is nitrogen-boron doped carbon fiber/manganese sulfide, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; active material: acetylene black: the proportion of the binder is 8: 1: 1; the solvent is N-methyl pyrrolidone, methyl ethyl sulfoxide and diethyl formamide; the weight of the polyvinylidene fluoride accounts for 1% of the weight of the solvent; the total volume of the methyl ethyl sulfoxide and the diethyl formamide is 200 percent of the volume of the N-methyl pyrrolidone;
19. the active substance is nitrogen-boron doped carbon fiber, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; active material: acetylene black: the proportion of the binder is 8: 1: 1; the solvent is N-methyl pyrrolidone, dimethyl sulfoxide, dimethylacetamide and diethylacetamide; the polyvinylidene fluoride accounts for 5% of the weight of the solvent; the total volume of the dimethyl sulfoxide, the dimethylacetamide and the diethylacetamide is 10% of the volume of the N-methylpyrrolidone;
20. the active substance is nitrogen-boron doped carbon fiber/molybdenum sulfide, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; active material: acetylene black: the proportion of the binder is 8: 1: 1; the solvent is N-methyl pyrrolidone, diethyl sulfoxide, methyl ethyl formamide and dimethyl sulfoxide; the polyvinylidene fluoride accounts for 20% of the weight of the solvent; the total volume of the diethyl sulfoxide, the methyl ethyl formamide and the dimethyl sulfoxide is 50 percent of the volume of the N-methyl pyrrolidone;
21. the active substance is nitrogen-boron doped carbon fiber/zinc sulfide, the conductive agent is acetylene black, and the binder is polyvinylidene fluoride; active material: acetylene black: the proportion of the binder is 8: 1: 1; the solvent is N-methyl pyrrolidone, dimethyl sulfoxide, diethyl sulfoxide, dimethyl acetamide and diethyl acetamide; the polyvinylidene fluoride accounts for 40% of the weight of the solvent; the total volume of the dimethyl sulfoxide, the diethyl sulfoxide, the dimethylacetamide and the diethylacetamide is 100 percent of the volume of the N-methylpyrrolidone;
the preparation method of the nitrogen-boron doped carbon fiber and the composite electrode comprises the following steps: 1) mixing N-methyl pyrrolidone and a high-polarity solvent in proportion to form a mixed solvent; 2) and weighing polyvinylidene fluoride, adding the polyvinylidene fluoride into the mixed solvent, and stirring and dispersing to obtain a solution, namely the cathode slurry stabilizer. 2) Weighing active substances, a conductive agent and a negative electrode slurry stabilizer in proportion; 3) stirring, smearing, drying, slicing and the like to prepare a negative plate; 4) the button cells were assembled and tested for electrochemical performance.
The experimental results show that: the addition of two, three or four high-polarity solvents obviously improves the electrochemical performance of the nitrogen-boron doped carbon fiber composite electrode.
The foregoing detailed description is exemplary only, and is not intended to limit the scope of the patent, as defined by the appended claims; any equivalent alterations or modifications made according to the spirit of the disclosure of this patent are intended to be included in the scope of this patent.
Claims (1)
1. A preparation method of a nitrogen-boron doped carbon fiber composite electrode is characterized by comprising the following steps: the nitrogen-boron-doped carbon fiber composite electrode material is one of nitrogen-boron-doped carbon fiber/molybdenum sulfide, nitrogen-boron-doped carbon fiber/zinc sulfide, nitrogen-boron-doped carbon fiber/iron sulfide and nitrogen-boron-doped carbon fiber/manganese sulfide, and the nitrogen-boron-doped carbon fiber is nitrogen and boron co-doped carbonized bacterial cellulose; the cathode slurry stabilizer for preparing the nitrogen-boron doped carbon fiber composite electrode comprises a binder and a solvent for dissolving the binder, wherein the mass percentage of the binder to the solvent for dissolving the binder is 0.1-50%; the solvent for dissolving the binder is a mixture of N-methyl pyrrolidone and a high-polarity organic compound; the high-polarity organic compound is one or two of dimethylacetamide, diethylacetamide, methylethylacetamide, diethylsulfoxide and methylethylsulfoxide; the volume ratio of the high-polarity organic compound to the N-methyl pyrrolidone is 0.03-3; the preparation method of the nitrogen-boron doped carbon fiber composite electrode comprises the following steps:
1) mixing N-methyl pyrrolidone and a high-polarity organic compound in proportion to form a mixed solvent;
2) weighing a certain mass of binder, adding the binder into the mixed solvent obtained in the step 1), and stirring and dispersing to obtain a cathode slurry stabilizer;
3) weighing the cathode slurry stabilizer, the nitrogen-boron doped carbon fiber composite electrode material and the conductive agent in the step 2) according to the proportion;
4) stirring, smearing, drying and slicing to obtain the nitrogen-boron doped carbon fiber composite electrode.
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