CN114784455A - Diaphragm, preparation method thereof and battery application - Google Patents
Diaphragm, preparation method thereof and battery application Download PDFInfo
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- CN114784455A CN114784455A CN202210356139.4A CN202210356139A CN114784455A CN 114784455 A CN114784455 A CN 114784455A CN 202210356139 A CN202210356139 A CN 202210356139A CN 114784455 A CN114784455 A CN 114784455A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/431—Inorganic material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
- H01M50/497—Ionic conductivity
Abstract
The invention relates to a diaphragm, a preparation method thereof and battery application. Adding sodium hydroxide into MXene solution, stirring for a certain time under the condition of argon, filtering and washing to be neutral; adding a PDDA solution into the solution, stirring for a certain time, adding a porous oxide into the solution, obtaining a MXene @ porous oxide solution in a self-assembly mode, filtering and washing to obtain high-concentration slurry, coating the slurry into a diaphragm, and drying in vacuum to obtain the MXene @ porous oxide modified diaphragm. The diaphragm prepared by the invention can effectively make the electric field uniformly distributed, promote the diffusion of ions and reduce the local current density, thereby inducing uniform zinc deposition; the diaphragm has good zinc affinity, and can also effectively inhibit the growth of dendritic crystals; the adopted commercial porous oxide can effectively reduce the cost and obtain a low-cost diaphragm; if the vacuum distillation method is adopted to obtain the porous oxide, the large specific surface and uniform porous structure presented by the porous oxide are beneficial to obtaining better electrochemical performance.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a diaphragm, a preparation method of the diaphragm and application of a battery.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
With the use of fossil energy and the increasing increase of environmental pollution, secondary batteries have been widely spotlighted due to their unique advantages. However, in some battery systems, dendrite growth can result in the production of large amounts of by-products, which in turn consume electrolyte and salt, resulting in low coulombic efficiency. In addition, the numerous growing dendrites can pierce the separator, causing short circuits of the battery, thereby causing some safety problems. In a battery system, the separator is one of the important and indispensable components. Designing a low-cost separator that can suppress dendrite growth is of great importance in promoting the development of secondary batteries.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the diaphragm, the preparation method thereof and the battery application, the diaphragm provided by the invention is a diaphragm modified by MXene composite porous oxide, the diaphragm can effectively inhibit dendritic crystal growth, has good electrochemical performance and low production cost, and can realize industrial production.
In a first aspect of the present invention, there is provided a method for manufacturing a separator, comprising the steps of:
adding a sodium hydroxide solution into the MXene solution, stirring for a certain time under the condition of argon, filtering and washing to be neutral;
adding a PDDA solution into the solution, stirring for a certain time, adding a porous oxide into the solution, obtaining a MXene @ porous oxide solution in a self-assembly mode, filtering and washing to obtain high-concentration slurry, coating the slurry into a diaphragm, and performing vacuum drying to obtain the MXene @ porous oxide membrane.
Further, after adding sodium hydroxide to the MXene solution, stirring for 2h-120 h.
Further, PDDA is added and stirred for 0.2h-5 h.
Further, the concentration of the sodium hydroxide is 1-10mol L-1。
Furthermore, the volume ratio of the sodium hydroxide solution to the MXene solution is 1:5-3: 1.
Furthermore, the volume ratio of the MXene solution to the PDDA solution is 100: 4-12.
Further, the concentration of the porous oxide in the solution is 0.1-10mg mL-1。
Further, the thickness of the coating is 50nm to 10 μm.
The porous oxide is a commercial porous oxide or a porous oxide prepared from hydroxide by a vacuum distillation method; preferably, the porous oxide is prepared from a hydroxide by vacuum distillation.
The porous oxide is one or a mixture of more than two of porous nickel oxide, porous cobalt oxide, porous copper oxide, porous magnesium oxide, porous indium oxide, porous bismuth oxide, porous iron oxide, porous niobium oxide, porous aluminum oxide and porous zinc oxide.
The hydroxide is porous nickel hydroxide, porous cobalt hydroxide, porous copper hydroxide, porous magnesium hydroxide, porous indium hydroxide, porous bismuth hydroxide, porous iron hydroxide, porous niobium hydroxide, porous aluminum hydroxide, or porous zinc hydroxide.
The temperature of the vacuum distillation is 200 ℃ and 1500 ℃, and the time is 0.1-10 h.
The diaphragm is one of a polyolefin diaphragm, a cellulose membrane, a polyimide membrane and a polyester membrane.
In a second aspect of the present invention, a separator prepared by the above preparation method is provided. The MXene composite porous oxide modified diaphragm.
In a third aspect of the present invention, there is provided a use of the above separator in a secondary battery, such as a lithium ion battery, a sodium ion battery, a potassium ion battery, a zinc ion battery, a magnesium ion battery, a calcium ion battery, and others.
The beneficial effects of one or more of the above technical solutions are as follows:
according to the invention, the porous oxide and MXene are combined in an electrostatic self-assembly mode, and the MXene has better hydrophilicity and zinc affinity, so that the electric field distribution can be effectively uniform, the diffusion of ions is promoted, and uniform zinc deposition can be induced.
If the vacuum distillation method is adopted to obtain the porous oxide, the porous oxide has a large specific surface and a uniform porous structure, is favorable for promoting the transmission of ions, and reduces the local current density, so that better electrochemical performance is obtained.
The porous oxide adopted by the invention can effectively reduce the cost and obtain the diaphragm with low cost.
According to the invention, the membrane is modified, so that the growth of dendritic crystals can be effectively inhibited, the nucleation overpotential and the platform overpotential are effectively reduced, and high coulombic efficiency and stable cycle performance are obtained.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the application and, together with the description, serve to explain the application and are not intended to limit the application.
Fig. 1 is (a) XRD and (b) XPS of the commercial membrane and MXene @ NiO modified membrane of example 1.
FIG. 2 is SEM for (a-b) commercial membrane and (c-d) MXene @ NiO modified membrane of example 1.
Fig. 3 is the SEM evolution of metallic zinc on a stainless steel current collector in example 1. (a, c-f) commercial membranes and (b, g-j) MXene @ NiO modified membranes.
Fig. 4 is the coulombic efficiency of Zn | | | | Cu half-cells assembled with MXene @ NiO modified separator in example 1.
Fig. 5 is the cycling performance of Zn | Zn cells assembled in example 1 using a commercial separator and an MXene @ NiO modified separator.
Fig. 6 is (a) time-voltage curve, (b) capacity-voltage curve, (c) coulombic efficiency, and (d) cycle performance of Li cell assembled with commercial membrane and MXene @ NiO modified membrane in example 2.
Fig. 7 is (a) time-voltage curve, (b) capacity-voltage curve, (c) coulombic efficiency, and (d) cycling performance of Na | Na cell assembled with commercial membrane and MXene @ NiO modified membrane in example 3.
Fig. 8 is (a) a time-voltage curve, (b) a capacity-voltage curve, (c) coulombic efficiency, and (d) cycling performance of a K | K cell assembled with the commercial separator and the MXene @ NiO modified separator in example 4.
Fig. 9 is the cycling performance of Mg cells assembled with commercial membranes and MXene @ NiO modified membranes in example 5.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
Example 1
An MXene @ NiO modified membrane and a preparation method thereof are as follows:
preparing porous nickel oxide: weighing 1g of nickel hydroxide, putting the nickel hydroxide into a tube furnace, and heating the nickel hydroxide under a vacuum condition to obtain the porous nickel oxide.
Preparation of PDDA modified MXene solution: 100mL of 6M NaOH solution is prepared, added into 100mL of MXene solution under the protection of argon, stirred for 20 hours to obtain alkalized MXene solution, and then filtered and washed to be neutral to obtain the required solution. 5ml of PDDA solution was added to the above solution and stirred for 1 h.
Preparation of MXene @ NiO modified membranes: and adding 0.1g of porous nickel oxide into the 100mL solution, uniformly stirring, centrifuging and washing to obtain high-concentration slurry, coating the slurry on a glass fiber diaphragm, and drying to obtain the MXene @ NiO modified diaphragm.
Testing the electrochemical performance of the zinc metal battery:
the current also adopts 2M ZnSO4The solution and zinc foil are used as a counter electrode and a reference electrode, and the battery is assembled by adopting the diaphragm.
Coulomb efficiency test: the copper foil is adopted as a current collector, and the current density is 5mA cm-2And 10mAcm-2Discharge capacity of 5mAh cm-2The charge cut-off voltage was 0.5V.
And (3) testing a symmetrical battery: the current density was 2mA cm-2Capacity of 2mAh cm-2。
Example 2
An MXene @ NiO modified diaphragm and a preparation method thereof are as follows:
preparing porous nickel oxide: weighing 1g of nickel hydroxide, putting the nickel hydroxide into a tube furnace, and heating the nickel hydroxide under a vacuum condition to obtain the porous nickel oxide.
Preparation of PDDA modified MXene solution: 100mL of 6M NaOH solution is prepared, added into 100mL of MXene solution under the protection of argon, stirred for 20 hours to obtain alkalized MXene solution, and then filtered and washed to be neutral to obtain the required solution. 5ml of PDDA solution was added to the above solution and stirred for 1 h.
Preparation of MXene @ NiO modified membranes: and adding 0.1g of porous nickel oxide into the 100mL solution, uniformly stirring, centrifuging and washing to obtain high-concentration slurry, coating the slurry on a PE diaphragm, and drying to obtain the MXene @ NiO modified diaphragm.
The electrochemical performance of the lithium metal battery was tested.
Example 3
An MXene @ NiO modified diaphragm and a preparation method thereof are as follows:
preparing porous nickel oxide: weighing 1g of nickel hydroxide, putting the nickel hydroxide into a tube furnace, and heating the nickel hydroxide under a vacuum condition to obtain the porous nickel oxide.
Preparation of PDDA modified MXene solution: 100mL of 6M NaOH solution is prepared, added into 100mL of MXene solution under the protection of argon, stirred for 20 hours to obtain alkalized MXene solution, and then filtered and washed to be neutral to obtain the required solution. 7ml of PDDA solution were added to the above solution and stirred for 1 h.
Preparation of MXene @ NiO modified membranes: and adding 0.1g of porous nickel oxide into the 100mL solution, uniformly stirring, centrifuging and washing to obtain high-concentration slurry, coating the slurry on a glass fiber diaphragm, and drying to obtain the MXene @ NiO modified diaphragm.
Testing its application in sodium metal batteries.
Example 4
An MXene @ NiO modified diaphragm and a preparation method thereof are as follows:
preparing porous nickel oxide: weighing 1g of nickel hydroxide, putting the nickel hydroxide into a tube furnace, and heating the nickel hydroxide under a vacuum condition to obtain the porous nickel oxide.
Preparation of PDDA modified MXene solution: 100mL of 6M NaOH solution is prepared, added into 100mL of MXene solution under the protection of argon, stirred for 20 hours to obtain alkalized MXene solution, and then filtered and washed to be neutral to obtain the required solution. 10ml of PDDA solution was added to the above solution and stirred for 1 h.
Preparation of MXene @ NiO modified membranes: and adding 0.1g of porous nickel oxide into the 100mL solution, uniformly stirring, centrifuging and washing to obtain high-concentration slurry, coating the slurry on a glass fiber diaphragm, and drying to obtain the MXene @ NiO modified diaphragm.
Testing its application in potassium metal batteries.
Example 5
An MXene @ NiO modified diaphragm and a preparation method thereof are as follows:
preparing porous nickel oxide: weighing 1g of nickel hydroxide, putting the nickel hydroxide into a tube furnace, and heating the nickel hydroxide under a vacuum condition to obtain the porous nickel oxide.
Preparation of PDDA modified MXene solution: 100mL of 6M NaOH solution is prepared and added into 100mL of MXene solution under the protection of argon, the mixture is stirred for 20 hours to obtain alkalified MXene solution, and then the alkalified MXene solution is filtered and washed to be neutral to obtain the required solution. 4ml of PDDA PDDA solution was added to the above solution and stirred for 1 h.
Preparation of MXene @ NiO modified membranes: and adding 0.1g of porous nickel oxide into the 100mL solution, uniformly stirring, centrifuging and washing to obtain high-concentration slurry, coating the slurry on a glass fiber diaphragm, and drying to obtain the MXene @ NiO modified diaphragm.
Testing the application of the magnesium alloy in magnesium metal batteries.
Fig. 1 is (a) XRD and (b) XPS of the commercial membrane and MXene @ NiO modified membrane of example 1. Characteristic peaks for MXene and NiO were observed in the modified separator, indicating that MXene @ NiO was successfully coated on the surface of the separator.
FIG. 2 is SEM of (a-b) commercial membranes and (c-d) MXene @ NiO modified membranes of example 1. The surface of the modified diaphragm is flat, and MXene @ NiO layers are clearly observed.
Fig. 3 is the SEM evolution of metallic zinc on a stainless steel current collector in example 1. (a, c-f) commercial membranes and (b, g-j) MXene @ NiO modified membranes. With commercial separators, a large amount of zinc dendrites are observed on the stainless steel surface, and as the deposition time is prolonged, the zinc dendrites grow continuously, causing more side reactions, resulting in low coulombic efficiency. Severe dendrites can puncture the separator causing a short circuit in the cell. After modification by the diaphragm, uniform zinc deposition was shown on the stainless steel. The prepared diaphragm can effectively make the electric field distribution uniform, promote the diffusion of ions and reduce the local current density, thereby inducing uniform zinc deposition. The modified diaphragm has good zinc affinity and can also effectively inhibit the growth of dendritic crystals.
Fig. 4 is the coulombic efficiency of Zn | | | | Cu half-cells assembled with MXene @ NiO modified separator in example 1. The battery still obtains stable and high coulombic efficiency under high current density, and further shows the superiority of the modified diaphragm.
Fig. 5 is the cycling performance of Zn | Zn cells assembled in example 1 using a commercial separator and an MXene @ NiO modified separator. The battery assembled with the commercial separator showed voltage fluctuation after cycle 680 h. In contrast, the modified separator can effectively inhibit the growth of zinc dendrites, thereby obtaining stable cycle performance.
Fig. 6 is (a) a time-voltage curve, (b) a capacity-voltage curve, (c) coulombic efficiency, and (d) cycling performance of Li | Cu half cells assembled from example 2 using a commercial separator and an MXene @ NiO modified separator. Fig. 7 is the (a) time-voltage curve, (b) capacity-voltage curve, (c) coulombic efficiency, and (d) cycling performance of Na | Cu half cells assembled from example 3 with a commercial separator and an MXene @ NiO modified separator. Fig. 8 is (a) time-voltage curve, (b) capacity-voltage curve, (c) coulombic efficiency, and (d) cycle performance of K | K cell assembled with commercial membrane and MXene @ NiO modified membrane in example 4. Fig. 9 is the cycle performance of Mg cells assembled in example 5 using a commercial separator and an MXene @ NiO modified separator. As can be seen from fig. 9, the modified membrane can effectively reduce nucleation overpotential and plateau overpotential, and obtain high coulombic efficiency and stable cycle performance.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (10)
1. A preparation method of a diaphragm is characterized by comprising the following steps:
adding sodium hydroxide into MXene solution, stirring under argon condition, filtering and washing to neutrality; adding the PDDA solution into the solution, stirring, adding the porous oxide into the solution, obtaining MXene @ porous oxide solution in a self-assembly mode, filtering and washing to obtain high-concentration slurry, coating the slurry into a diaphragm, and drying in vacuum to obtain the MXene @ porous oxide slurry.
2. The method according to claim 1, wherein the hydroxide is present in a concentration of 1 to 10mol L-1。
3. The method according to claim 1, wherein the porous oxide is a commercially available porous oxide or a porous oxide prepared from a hydroxide by a vacuum distillation method; preferably, the porous oxide is prepared from a hydroxide by vacuum distillation.
4. The production method according to claim 3, wherein the porous oxide is one or a mixture of two or more of porous nickel oxide, porous cobalt oxide, porous copper oxide, porous magnesium oxide, porous indium oxide, porous bismuth oxide, porous iron oxide, porous niobium oxide, porous aluminum oxide, and porous zinc oxide; the hydroxide is porous nickel hydroxide, porous cobalt hydroxide, porous copper hydroxide, porous magnesium hydroxide, porous indium hydroxide, porous bismuth hydroxide, porous iron hydroxide, porous niobium hydroxide, porous aluminum hydroxide, or porous zinc hydroxide.
5. The preparation method as claimed in claim 3, wherein the temperature of the vacuum distillation is 200-1500 ℃ and the time is 0.1-10 h.
6. The preparation method of claim 1, wherein the volume ratio of the sodium hydroxide solution to the MXene solution is 1:5-3: 1; the volume ratio of the MXene solution to the PDDA solution is 100: 4-12; the concentration of the porous oxide in the solution is 0.1-10mg mL-1。
7. The production method according to claim 1, wherein the separator is one of a polyolefin-based separator, a cellulose film, a polyimide film, and a polyester film; the coating thickness is 50nm-10 μm.
8. A separator produced by the production method according to any one of the preceding claims.
9. Use of the separator according to claim 8 in a secondary battery.
10. Use according to claim 9, characterized in that the secondary battery comprises a lithium ion battery, a sodium ion battery, a potassium ion battery, a zinc ion battery, a magnesium ion battery, a calcium ion battery.
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Cited By (2)
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| CN117673647A (en) * | 2024-02-02 | 2024-03-08 | 吉林大学 | Ion conductor coating modified diaphragm, preparation method and application thereof |
| CN117673647B (en) * | 2024-02-02 | 2024-04-23 | 吉林大学 | Ion conductor coating modified diaphragm, preparation method and application thereof |
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