CN115642305A - Sodium battery composite solid electrolyte and preparation method and application thereof - Google Patents
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Abstract
The invention discloses a preparation method of a composite solid electrolyte of a sodium battery, which comprises the following steps: s1, preparing a modified solid sodium electrolyte; s2: completely dissolving a polymer in an organic solvent, adding sodium salt and the modified solid sodium electrolyte prepared by S1, and stirring to obtain a mixed solution; and S3, coating the prepared mixed solution on the surface of an electrode plate, and drying and hot-pressing to obtain the sodium battery composite solid electrolyte. The surface of the modified solid sodium electrolyte contains active functional groups such as hydroxyl, amino and the like, and can react with isocyanate active groups of a polymer solid electrolyte to form carbamate and carbamido covalent bonds, so that the dispersibility of the solid sodium electrolyte in the polymer solid electrolyte is improved, and meanwhile, the composite solid electrolyte forms a cross-linked network structure, so that the regularity of polymer molecular chain arrangement is reduced, the crystallinity of the polymer solid electrolyte is obviously reduced, the ionic conductivity of the electrolyte is improved, and the mechanical strength and the thermal stability of the composite solid electrolyte are also improved.
Description
Technical Field
The invention belongs to the technical field of solid sodium batteries, and particularly relates to a sodium battery composite solid electrolyte and a preparation method and application thereof.
Background
The lithium ion battery has the outstanding advantages of high energy density, high working voltage, long cycle life, small self-discharge rate, environmental protection and the like, is widely applied to the fields of mobile phones, notebook computers, digital cameras, electric tools and the like, and gradually expands to the fields of new energy automobiles, energy storage and the like. However, the lithium resources on the earth are very poor and the distribution is very uneven, so that the cost of the lithium ion battery is very high, and the large-scale application of the lithium ion battery in the fields of new energy automobiles and energy storage is limited to a certain extent.
The sodium ion battery system has abundant resources, low price, environmental protection and similar electrochemical properties with lithium ion batteries, so the sodium ion battery system is widely concerned in recent years and provides a new choice for electrochemical energy storage. However, the conventional liquid sodium battery contains organic liquid electrolyte, which has poor thermal stability and flammability, and has potential safety hazards such as leakage, ignition, explosion and the like when the battery is abused and generates heat. Compared with the traditional liquid sodium battery, the solid sodium battery adopts the nonflammable solid electrolyte with good thermal stability to replace the organic electrolyte, and has better safety and higher energy density. However, many challenges still exist with existing solid-state sodium batteries, wherein low ionic conductivity and large interfacial resistance of the solid-state electrolyte at room temperature become key challenges for technology development.
Disclosure of Invention
In order to solve the above problems, the present invention adopts the following technical solutions:
the invention provides a preparation method of a sodium battery composite solid electrolyte, which comprises the following specific steps:
s1, preparing a modified solid sodium electrolyte;
s2: completely dissolving a polymer in an organic solvent, adding sodium salt and modified solid sodium electrolyte prepared by S1, heating to 60-100 ℃, and stirring to obtain a mixed solution;
and S3, coating the prepared mixed solution on the surface of an electrode plate, and drying and hot-pressing to obtain the sodium battery composite solid electrolyte.
Further, the preparation method of the modified solid sodium electrolyte in the step S1 comprises the following steps:
a. preparation of initial modified solid sodium electrolyte: uniformly mixing the solid sodium electrolyte and dopamine hydrochloride buffer solution, adjusting the pH value, stirring for 2-10 h at room temperature, and cleaning and filtering to obtain an initial modified solid sodium electrolyte;
b. adding the initial modified solid sodium electrolyte and diisocyanate into an organic solvent according to the mass ratio of 1 (2.5-9), heating to 50-100 ℃, and continuously stirring for 2-25 hours to obtain the modified solid sodium electrolyte.
Further, the polymer is selected from any one or more of polyethylene oxide, polyacrylonitrile, polymethyl methacrylate, polyvinyl alcohol, polyvinylidene fluoride-hexafluoropropylene, polycarbonate and polyacrylamide.
Further, the solid sodium electrolyte is selected from Na 2 Zr 2 Si 2 PO 12 、NaFeO 2 、Na 2/3 MnO 2 、Na 2/3 Mn 1/2 Fe 1/ 2 O 2 、Na 7/9 Cu 2/9 Mn 2/3 Fe 1/3 O 2 、Na 2 MnP 2 O 7 、Na 2 FeP 2 O 7 、Na 3 V 2 (PO 4 ) 3 、Na 3 V 2 (PO 4 ) 2 F 3 、NaFePO 4 、Na 2 MnFe(CN) 6 、Na 2 CoFe(CN) 6 Any one or more of them.
Further, the sodium salt is selected from any one or more of sodium hexafluorophosphate, sodium bis (trifluoromethylsulfonyl) imide, sodium difluoromethylsulfonylimide, sodium perchlorate, sodium tetrafluoroborate and sodium dioxalate.
Further, the diisocyanate is selected from any one or more of toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate, naphthalene diisocyanate, tetramethylxylylene diisocyanate, hexamethylene diisocyanate and hexamethylene diisocyanate; the organic solvent is N-methyl pyrrolidone.
Further, the mass ratio of the polymer, the modified solid sodium electrolyte and the sodium salt in step S2 is 50 to 85.
Further, the electrode sheet in the step S3 includes a positive electrode sheet and a negative electrode sheet, and the porosity of the electrode sheet is 35 to 50%; the drying process of the electrode plate in the step S3 is that the electrode plate is dried for 5-30 min at room temperature and then dried at the temperature of 60-100 ℃.
The invention also provides the sodium battery composite solid electrolyte, which is prepared by the preparation method of the sodium battery composite solid electrolyte.
The invention provides a solid sodium battery which is provided with the sodium battery composite solid electrolyte.
The invention has the beneficial effects that:
1. the surface of the modified solid sodium electrolyte contains a coating layer with high adhesion, so that the contact property of the electrolyte and an electrode plate can be effectively improved, the interface impedance is reduced, and the electrical property of the solid sodium battery is improved.
2. The surface of the modified solid sodium electrolyte contains active functional groups such as hydroxyl, amino and the like, and can react with isocyanate active groups of a polymer solid electrolyte to form carbamate and carbamido covalent bonds, so that the dispersibility of the solid sodium electrolyte in the polymer solid electrolyte is improved, and meanwhile, the composite solid electrolyte forms a cross-linked network structure, so that the regularity of the molecular chain arrangement of the polymer is reduced, the crystallinity of the polymer solid electrolyte is obviously reduced, the ionic conductivity of the electrolyte is further improved, and the mechanical strength and the thermal stability of the composite solid electrolyte are also improved.
3. The mixed liquid of the composite solid electrolyte is directly coated on the surface of the electrode plate, is dried for a certain time at room temperature, can fully permeate the mixed liquid into the electrode plate, is dried at high temperature, can promote the mixed liquid to be continuously crosslinked, improves the mechanical strength of the electrode plate, simultaneously enables the composite solid electrolyte to fully contact materials in the electrode plate, further reduces the interface impedance through hot pressing, and improves the electrical property of the solid sodium battery.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to a plurality of examples so that those skilled in the art can more clearly understand the contents of the technical solution. Furthermore, the description is to be construed as illustrative and explanatory only and should not be taken as limiting the scope of the present invention in any way.
Example 1:
in the embodiment, the sodium battery composite solid electrolyte is prepared by the following steps:
s1, mixing 5g of Na 2 Zr 2 Si 2 PO 12 Mixing with 10g dopamine hydrochloride buffer solution, adjusting pH to 8.5, stirring at room temperature for 2h, washing, and filtering to obtain initial modified Na 2 Zr 2 Si 2 PO 12 (ii) a 5g of initial Na 2 Zr 2 Si 2 PO 12 Adding 20g of isophorone diisocyanate into 500mL of N-methyl pyrrolidone, heating to 80 ℃, and continuing stirring for 25h to obtain modified Na 2 Zr 2 Si 2 PO 12 ；
S2, 50g of polyoxyethylene is completely dissolved in 500mL of N-methylpyrrolidone, and 20g of sodium (trifluoromethylsulfonyl) imide and 30g of modified Na prepared from S1 are added 2 Zr 2 Si 2 PO 12 Stirring uniformly, heating to 80 ℃, and continuing stirring for 5 hours to obtain a mixed solution;
and S3, coating the prepared mixed solution on the surface of an electrode plate, drying at room temperature for 10min, drying at 60 ℃, and carrying out hot pressing to obtain the sodium battery composite solid electrolyte. The electrode sheet adopted in the method comprises a positive electrode sheet and a negative electrode sheet, and the porosity of the electrode sheet is 35%.
Example 2:
in the embodiment, the sodium battery composite solid electrolyte is prepared by the following steps:
s1, mixing 5g of Na 2 Zr 2 Si 2 PO 12 Mixing with 10g dopamine hydrochloride buffer solution, adjusting pH to 8.5, stirring at room temperature for 2h, washing, and filtering to obtain initial modified Na 2 Zr 2 Si 2 PO 12 (ii) a 5g of initial Na 2 Zr 2 Si 2 PO 12 And 45g of isophorone diisocyanate are added into 500mL of N-methyl pyrrolidone, the temperature is raised to 100 ℃, the mixture is continuously stirred for 2 hours, and modified Na is obtained 2 Zr 2 Si 2 PO 12 ；
S2, 50g of polymethyl methacrylate is completely dissolved in 500mL of N-methylpyrrolidone, and 20g of sodium (trifluoromethylsulfonyl) imide and 20g of modified Na prepared from S1 are added 2 Zr 2 Si 2 PO 12 Stirring uniformly, heating to 80 ℃, and continuing stirring for 5 hours to obtain a mixed solution;
and S3, coating the prepared mixed solution on the surface of an electrode plate, drying at room temperature for 20min, drying at 70 ℃, and carrying out hot pressing to obtain the sodium battery composite solid electrolyte. The electrode sheet used herein includes a positive electrode sheet and a negative electrode sheet, and the porosity of the electrode sheet is 40%.
Example 3:
in the embodiment, the sodium battery composite solid electrolyte is prepared by adopting the following steps:
s1, mixing 5g of Na 2/3 Mn 1/2 Fe 1/2 O 2 Mixing with 10g dopamine hydrochloride buffer solution, adjusting pH to 8.5, stirring at room temperature for 2h, cleaning, and filtering to obtain initial modified Na 2/3 Mn 1/2 Fe 1/2 O 2 (ii) a 5g of initial Na 2/3 Mn 1/2 Fe 1/2 O 2 And 12.5g of naphthalene diisocyanate are added into 500mL of N-methyl pyrrolidone, the temperature is increased to 80 ℃, the stirring is continued for 10 hours, and modified Na is obtained 2/3 Mn 1/ 2 Fe 1/2 O 2 ；
S2, 70g of polyoxyethylene is completely dissolved in 500mL of N-methylpyrrolidone, and 20g of sodium (trifluoromethylsulfonyl) imide and 30g of modified Na prepared from S1 are added 2/3 Mn 1/2 Fe 1/2 O 2 Stirring uniformly, heating to 80 deg.C, and continuing stirringObtaining a mixed solution after 5 hours;
and S3, coating the prepared mixed solution on the surface of an electrode plate, drying at room temperature for 10min, drying at 100 ℃, and carrying out hot pressing to obtain the sodium battery composite solid electrolyte. The electrode sheet adopted in the method comprises a positive electrode sheet and a negative electrode sheet, and the porosity of the electrode sheet is 35%.
Example 4:
in the embodiment, the sodium battery composite solid electrolyte is prepared by the following steps:
s1, mixing 5g of Na 2 Zr 2 Si 2 PO 12 Mixing with 10g dopamine hydrochloride buffer solution, adjusting pH to 8.5, stirring at room temperature for 2h, washing, and filtering to obtain initial modified Na 2 Zr 2 Si 2 PO 12 (ii) a 5g of initial Na 2 Zr 2 Si 2 PO 12 Adding 20g of isophorone diisocyanate into 500mL of N-methyl pyrrolidone, heating to 80 ℃, and continuing stirring for 25h to obtain modified Na 2 Zr 2 Si 2 PO 12 ；
S2, 85g of polyethylene oxide was completely dissolved in 500mL of N-methylpyrrolidone, and 10g of sodium (trifluoromethylsulfonyl) imide and 10g of modified Na prepared in S1 were added 2 Zr 2 Si 2 PO 12 Stirring uniformly, heating to 80 ℃, and continuing stirring for 5 hours to obtain a mixed solution;
and S3, coating the prepared mixed solution on the surface of an electrode plate, drying at room temperature for 10min, drying at 60 ℃, and carrying out hot pressing to obtain the sodium battery composite solid electrolyte. The electrode sheet used herein includes a positive electrode sheet and a negative electrode sheet, and the porosity of the electrode sheet is 35%.
Example 5:
in the embodiment, the sodium battery composite solid electrolyte is prepared by the following steps:
s1, mixing 5g of Na 2/3 Mn 1/2 Fe 1/2 O 2 Mixing with 10g dopamine hydrochloride buffer solution, adjusting pH to 8.5, stirring at room temperature for 5h, washing, and filtering to obtain initial modified Na 2/3 Mn 1/2 Fe 1/2 O 2 (ii) a 5g of initial Na 2/3 Mn 1/2 Fe 1/2 O 2 Adding 20g of toluene diisocyanate into 500mL of N-methyl pyrrolidone, heating to 80 ℃, and continuing stirring for 10h to obtain modified Na 2/3 Mn 1/ 2 Fe 1/2 O 2 ；
S2, completely dissolving 60g of polyacrylonitrile in 500mL of N-methyl pyrrolidone, and adding 20g of sodium hexafluorophosphate and 20g of modified Na prepared from S1 2/3 Mn 1/2 Fe 1/2 O 2 Stirring uniformly, heating to 80 ℃, and continuing stirring for 5 hours to obtain a mixed solution;
and S3, coating the prepared mixed solution on the surface of an electrode plate, drying at room temperature for 10min, drying at 90 ℃, and carrying out hot pressing to obtain the sodium battery composite solid electrolyte. The electrode sheet used herein includes a positive electrode sheet and a negative electrode sheet, and the porosity of the electrode sheet is 50%.
Example 6:
in the embodiment, the sodium battery composite solid electrolyte is prepared by adopting the following steps:
s1, mixing 5g of Na 2 MnFe(CN) 6 Mixing with 10g dopamine hydrochloride buffer solution, adjusting pH to 8.5, stirring at room temperature for 3h, washing, and filtering to obtain initial modified Na 2 MnFe(CN) 6 (ii) a 5g of initial Na 2 MnFe(CN) 6 Adding 20g of diphenylmethane diisocyanate into 500mL of N-methylpyrrolidone, heating to 80 ℃, and continuing stirring for 10h to obtain modified Na 2 MnFe(CN) 6 ；
S2, completely dissolving 60g of polycarbonate in 500mL of N-methylpyrrolidone, and adding 20g of sodium tetrafluoroborate and 20g of modified Na prepared from S1 2 MnFe(CN) 6 Stirring uniformly, heating to 80 ℃, and continuing stirring for 5 hours to obtain a mixed solution;
and S3, coating the prepared mixed solution on the surface of an electrode plate, drying at room temperature for 30min, drying at 100 ℃, and carrying out hot pressing to obtain the sodium battery composite solid electrolyte. The electrode plate adopted in the method comprises a positive electrode plate and a negative electrode plate, and the porosity of the electrode plate is 45%.
Example 7:
in the embodiment, the sodium battery composite solid electrolyte is prepared by adopting the following steps:
s1, mixing 5g of Na 3 V 2 (PO 4 ) 2 F 3 Mixing with 10g dopamine hydrochloride buffer solution, adjusting pH to 8.5, stirring at room temperature for 10h, washing, and filtering to obtain initial modified Na 2 Zr 2 Si 2 PO 12 (ii) a 5g of initial Na 3 V 2 (PO 4 ) 2 F 3 And 20g of diphenylmethane diisocyanate are added into 500mL of N-methylpyrrolidone, the temperature is increased to 80 ℃, the stirring is continued for 8 hours, and modified Na is obtained 3 V 2 (PO 4 ) 2 F 3 ；
S2, completely dissolving 60g of polyacrylamide in 500mL of N-methylpyrrolidone, and adding 20g of sodium (trifluoromethylsulfonyl) imide and 20g of modified Na prepared from S1 3 V 2 (PO 4 ) 2 F 3 Stirring uniformly, heating to 80 ℃, and continuing stirring for 5 hours to obtain a mixed solution;
and S3, coating the prepared mixed solution on the surface of an electrode plate, drying at room temperature for 5min, drying at 70 ℃, and carrying out hot pressing to obtain the sodium battery composite solid electrolyte.
It should be noted that: in the above embodiment, the polymer may be selected from any one or more of polyethylene oxide, polyacrylonitrile, polymethyl methacrylate, polyvinyl alcohol, polyvinylidene fluoride-hexafluoropropylene, polycarbonate, and polyacrylamide. The solid sodium electrolyte is selected from Na 2 Zr 2 Si 2 PO 12 、NaFeO 2 、Na 2/3 MnO 2 、Na 2/3 Mn 1/2 Fe 1/2 O 2 、Na 7/9 Cu 2/9 Mn 2/3 Fe 1/3 O 2 、Na 2 MnP 2 O 7 、Na 2 FeP 2 O 7 、Na 3 V 2 (PO 4 ) 3 、Na 3 V 2 (PO 4 ) 2 F 3 、NaFePO 4 、Na 2 MnFe(CN) 6 、Na 2 CoFe(CN) 6 One or more of (a). The sodium salt is selected from any one or more of sodium hexafluorophosphate, sodium bis (trifluoromethylsulfonyl) imide, sodium difluoromethylsulfonylimide, sodium perchlorate, sodium tetrafluoroborate and sodium dioxalate. The diisocyanate is selected from any one or more of toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate, naphthalene diisocyanate, tetramethylxylylene diisocyanate, hexamethylene diisocyanate and hexamethylene diisocyanate.
Comparative example 1:
s1, 60g of polyethylene oxide was completely dissolved in 500mL of N-methylpyrrolidone, and 20g of sodium (trifluoromethylsulfonyl) imide and 20g of Na prepared in S1 were added 2 Zr 2 Si 2 PO 12 Stirring uniformly, heating to 80 ℃, and continuing stirring for 5 hours to obtain a mixed solution;
and S2, coating the prepared mixed solution on the surface of an electrode plate, drying at room temperature for 10min, drying at 90 ℃, and carrying out hot pressing to obtain the sodium battery composite solid electrolyte.
The test method comprises the following steps:
and (3) testing the ionic conductivity: the ionic conductivity of the electrolyte is determined by assembling symmetrical cells with steel plates as blocking electrodes on an electrochemical workstation at a frequency ranging from 0.1Hz to 10 Hz 6 Hz, the ionic conductivity was calculated as the following man-hours: σ = L/(R × S), σ is the ionic conductivity of the composite solid electrolyte membrane, L is the composite solid electrolyte membrane thickness, S is the area of the composite solid electrolyte membrane, and R is the bulk resistance of the composite solid electrolyte membrane.
After testing each of the examples and comparative examples, the ionic conductivity results at room temperature were as follows:
from the above results, it can be seen that the ionic conductivity of the sodium battery composite solid electrolyte prepared by the method of the present invention at room temperature is much higher than that of the sodium battery solid electrolyte prepared by the method of the prior art, and the mechanical strength is also much higher than that of the sodium battery solid electrolyte prepared by the method of the prior art.
The technical solution of the present invention is explained in detail above. It is obvious that the invention is not limited to what has been described. Many variations will be apparent to those skilled in the art in light of this disclosure, but any variations that are equivalent or similar to the present invention are within the scope of the present invention.
Claims (10)
1. The preparation method of the sodium battery composite solid electrolyte is characterized by comprising the following specific steps of:
s1, preparing a modified solid sodium electrolyte;
s2: completely dissolving a polymer in an organic solvent, adding a sodium salt and a modified solid sodium electrolyte prepared by S1, heating to 60 to 100 ℃, and stirring to obtain a mixed solution;
and S3, coating the prepared mixed solution on the surface of an electrode plate, and drying and hot-pressing to obtain the sodium battery composite solid electrolyte.
2. The method for preparing the sodium battery composite solid electrolyte according to claim 1, wherein the method for preparing the modified solid sodium electrolyte in the step S1 comprises the following steps:
a. preparation of initial modified solid sodium electrolyte: uniformly mixing the solid sodium electrolyte with a dopamine hydrochloride buffer solution, adjusting the pH value, stirring at room temperature for 2-10h, cleaning, and filtering to obtain an initial modified solid sodium electrolyte;
b. adding the initial modified solid sodium electrolyte and diisocyanate into an organic solvent according to the mass ratio of 1 (2.5 to 9), heating to 50 to 100 ℃, and continuously stirring for 2 to 25h to obtain the modified solid sodium electrolyte.
3. The method of claim 1, wherein the polymer is selected from one or more of polyethylene oxide, polyacrylonitrile, polymethyl methacrylate, polyvinyl alcohol, polyvinylidene fluoride-hexafluoropropylene, polycarbonate, and polyacrylamide.
4. The method of claim 2, wherein the solid sodium electrolyte is selected from Na 2 Zr 2 Si 2 PO 12 、NaFeO 2 、Na 2/3 MnO 2 、Na 2/3 Mn 1/2 Fe 1/2 O 2 、Na 7/9 Cu 2/9 Mn 2/3 Fe 1/3 O 2 、Na 2 MnP 2 O 7 、Na 2 FeP 2 O 7 、Na 3 V 2 (PO 4 ) 3 、Na 3 V 2 (PO 4 ) 2 F 3 、NaFePO 4 、Na 2 MnFe(CN) 6 、Na 2 CoFe(CN) 6 Any one or more of them.
5. The method of claim 1, wherein the sodium salt is selected from one or more of sodium hexafluorophosphate, sodium bis (trifluoromethylsulfonyl) imide, sodium difluoromethylsulfonylimide, sodium perchlorate, sodium tetrafluoroborate, and sodium dioxalate.
6. The method for preparing the composite solid electrolyte of the sodium battery according to claim 2, wherein the diisocyanate is any one or more selected from the group consisting of toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate, naphthalene diisocyanate, tetramethylxylylene diisocyanate, hexamethylene diisocyanate, and hexamethylene diisocyanate; the organic solvent is N-methyl pyrrolidone.
7. The method for preparing the composite solid electrolyte of the sodium battery according to claim 1, wherein the mass ratio of the polymer, the modified solid sodium electrolyte and the sodium salt in the step S2 is 50 to 85 to 5 to 20.
8. The method for preparing the composite solid electrolyte of the sodium battery according to claim 1, wherein the electrode sheet in the step S3 comprises a positive electrode sheet and a negative electrode sheet, and the porosity of the electrode sheet is 35 to 50 percent; the drying process of the electrode sheet in the step S3 is to dry the electrode sheet at room temperature for 5 to 30min and then dry the electrode sheet at the temperature of 60 to 100 ℃.
9. A composite solid electrolyte for sodium battery is characterized in that: the composite solid electrolyte for sodium battery of any one of claims 1-8.
10. A solid state sodium battery characterized by: the solid state sodium battery has the sodium battery composite solid state electrolyte of claim 9.
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| CN117039127A (en) * | 2023-09-11 | 2023-11-10 | 浙江煌能新能源科技有限公司 | Sodium battery composite solid electrolyte, preparation method thereof and sodium battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117039127A (en) * | 2023-09-11 | 2023-11-10 | 浙江煌能新能源科技有限公司 | Sodium battery composite solid electrolyte, preparation method thereof and sodium battery |
| CN117039127B (en) * | 2023-09-11 | 2024-02-06 | 浙江煌能新能源科技有限公司 | Sodium battery composite solid electrolyte, preparation method thereof and sodium battery |
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