CN114759253A - Preparation method of ultra-thin, light and high-mechanical-strength PEO-based solid electrolyte with cellulose membrane as supporting layer - Google Patents
Preparation method of ultra-thin, light and high-mechanical-strength PEO-based solid electrolyte with cellulose membrane as supporting layer Download PDFInfo
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Abstract
The invention relates to a preparation method of an ultrathin, light and high-mechanical-strength PEO-based solid electrolyte with a cellulose membrane as a supporting layer, which is characterized in that a cellulose membrane is introduced as the supporting layer, and the ultrathin, light and high-mechanical-strength PEO-based solid electrolyte membrane is prepared by simple coating and hot-pressing technologies. The surface of the cellulose membrane has a large number of hydroxyl groups, so that the compatibility of the cellulose membrane with PEO can be improved. Making it one of the most desirable support layers for PEO-based solid electrolytes. Compared with the traditional PEO-based solid electrolyte, the PEO-based solid electrolyte with the cellulose membrane as the supporting layer has extremely excellent mechanical property and electrochemical property in ultrathin thickness, and the assembled battery has high rate capability and high cycle performance, thereby being beneficial to realizing high energy density of the lithium battery. The PEO-based solid electrolyte prepared by the method has the advantages of cost advantage and simple operation, and is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of lithium battery materials, and relates to a preparation method of an ultrathin, light and high-mechanical-strength PEO-based solid electrolyte with a cellulose membrane as a supporting layer.
Background
Due to the rapid development of portable devices and electric vehicles, the current lithium battery has not been able to meet future demands in terms of energy density, cycle life, and safety. And by adopting the solid electrolyte and the lithium metal cathode to be combined for use, the energy density can be improved, and meanwhile, the safety problem brought by the traditional liquid electrolyte is relieved. The polymer electrolyte composed of the polymer matrix and the lithium salt has the advantages of flexibility, light weight, good interface compatibility with electrodes, easy large-scale production and the like, and has better development prospect in practical application. Among them, polyacetylene oxide (PEO) and solid electrolyte have been widely studied due to their excellent solubility of lithium salts and stability with lithium metal negative electrodes.
However, the mechanical strength of PEO by itself is not sufficient to inhibit the growth of lithium dendrites well enough to make it incompatible with high surface capacity anodes. Therefore, the PEO solid electrolyte used today is thick, which is not conducive to achieving high energy density. To increase the Li dendrite suppression capability of PEO-based solid electrolytes at relatively thin thicknesses, this problem is often ameliorated by the addition of a support layer in the PEO-based electrolyte. The support layers currently used are mainly crosslinked reticulated polymer scaffolds, inorganic inert scaffolds, and commonly used commercial membranes. But the ion conductivity of the crosslinked reticular polymer bracket is lower, the thickness of the inorganic inert supporting layer is still thicker, and the density is higher, so that the realization of high energy density is not facilitated; the conventional commercial separator has poor thermal stability and insufficient compatibility with a solid electrolyte, and thus rapid transfer of lithium ions is hindered to some extent. Therefore, the ideal support layer should have the characteristics of flexibility, light weight, ultra-thin property, easy processing, good compatibility with PEO, thermal stability and the like. Cellulose is a material with abundant reserves, strong sustainability, low price, simple processing, excellent flexibility, relatively good thermal stability, light weight and high porosity. Meanwhile, a large number of hydroxyl groups exist on the surface of the PEO, so that the compatibility of the PEO with the PEO can be improved, and the PEO is possible. Among various types of Cellulose, Cladophora Cellulose (CC) has a characteristic that it is not easy to absorb water and can maintain its porous structure after drying because of its high crystallinity. Therefore, we believe that Cladophora Cellulose (CC) can be used as a suitable support layer to prepare a high mechanical performance, ultra-thin, lightweight, thermally stable PEO-based electrolyte, thereby increasing the energy density of an all-solid-state lithium metal battery.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a method for preparing an ultrathin, light and high-mechanical-strength PEO-based solid electrolyte with a cellulose membrane as a supporting layer.
Technical scheme
A method for preparing an ultrathin, light and high-mechanical-strength PEO-based solid electrolyte with a cellulose membrane as a supporting layer is characterized by comprising the following steps:
step 1: uniformly dispersing a Cladophora Cellulose raw material in an aqueous solution to obtain a precursor solution;
step 2: carrying out vacuum filtration on the obtained precursor solution and then drying;
and step 3: mixing and stirring PEO, LiTFSI and LLZTO in acetonitrile to obtain slurry of PEO-based solid electrolyte; wherein the ratio of LLZTO is 20%, and the ratio of PEO to LiTFSI is [ EO/Li + ] -16: 1;
and 4, step 4: coating the slurry of the PEO-based solid electrolyte on two sides of Cladophora Cellulose by a coating machine and drying; the drying process is that room temperature is firstly 12 hours, and then a vacuum oven is used for 12 hours at 60 ℃;
and 5: hot-pressing the dried PEO-based solid electrolyte to obtain the ultrathin, light and high-mechanical-strength PEO-based solid electrolyte with the cellulose membrane as a supporting layer; the hot pressing pressure is 40MPa, the hot pressing temperature is 70 ℃, and the hot pressing time is 10-30 min.
In the step 1: the Cladophora Cellulose raw material is dispersed in the water solution through an ultrasonic wall breaking machine; the power of the ultrasonic wall breaking machine is 650W; the dispersion time is 10-30 min.
In the step 2: the drying temperature is 100 ℃, and the drying time is 12 hours.
The stirring time of the step 3 is 12 hours.
In the step 4: the coating scale of the slurry of PEO-based solid electrolyte was 15-35.
Advantageous effects
The invention provides a preparation method of an ultrathin, light and high-mechanical-strength PEO-based solid electrolyte with a cellulose membrane as a supporting layer, which is characterized in that a cellulose membrane is introduced as the supporting layer, and the ultrathin, light and high-mechanical-strength PEO-based solid electrolyte membrane is prepared by simple coating and hot pressing technologies. PEO-based solid electrolytes have hindered practical applications due to insufficient mechanical properties at ultra-thin thicknesses. The cellulose membrane is a material with abundant reserves, strong sustainability, low price, simple processing, excellent flexibility, relatively good thermal stability, light weight and high porosity. Meanwhile, a large number of hydroxyl groups exist on the surface of the PEO, so that the compatibility of the PEO with the PEO can be improved. Making it one of the most desirable support layers for PEO-based solid electrolytes. Compared with the traditional PEO-based solid electrolyte, the PEO-based solid electrolyte with the cellulose membrane as the supporting layer has extremely excellent mechanical property and electrochemical property at ultrathin thickness, and the assembled battery has high rate performance and high cycle performance, thereby being beneficial to realizing high energy density of the lithium battery. The PEO-based solid electrolyte prepared by the method has the advantages of cost advantage and simple operation, and is suitable for industrial production.
The thickness of the PEO-based solid electrolyte is a key problem that prevents the high energy density from being achieved only when the solid electrolyte has a low specific gravity. The demand of ultra-thin, light, flexible and high mechanical strength of PEO-based solid electrolyte can be realized by the Cladophora Cellulose with flexibility, thermal stability, light weight and high porosity. Meanwhile, a large amount of hydroxyl groups on the surface of the cellulose membrane can improve the compatibility of the cellulose membrane with PEO, and the electrochemical performance of the PEO-based solid electrolyte is improved to a certain extent. By combining the characteristics, the preparation of the ultrathin, flexible, light and high-mechanical-strength PEO-based solid electrolyte can be realized, and the high energy density of the all-solid-state lithium metal battery can be realized.
Therefore, the Cladophora Cellulose is used as a supporting layer to prepare the ultrathin, light and high-mechanical-strength PEO-based solid electrolyte, the mechanical property and the electrochemical property are improved, the assembled battery has high rate performance and high cycle performance, and the realization of the high energy density of the lithium battery is facilitated.
Drawings
FIG. 1 is an SEM image of an ultra-thin, lightweight, high mechanical strength PEO-based solid electrolyte having cellulose films obtained in example 1, comparative example and comparative example 2 of the present invention as a support layer;
a: thickness of example 2 15 μm; b. thickness of 25 μm for comparative example 1; c. thickness of comparative example 2 35 μm;
FIG. 2 is a graph of tensile properties, i.e., stress-strain curves, of ultra-thin, lightweight, flexible, thermally stable, high mechanical strength PEO-based solid electrolytes (15 μm, 25 μm, 35 μm) of various thicknesses prepared in example 2, comparative example 1, and comparative example 2 of the present invention compared to conventional PEO-based solid electrolytes obtained in comparative example 3;
FIG. 3 is a comparison of critical current densities of ultra-thin, lightweight, flexible, thermally stable, high mechanical strength PEO-based solid electrolytes (15 μm, 25 μm, 35 μm) of different thicknesses prepared in example 2, comparative example 1, and comparative example 2 of the present invention and conventional PEO-based solid electrolytes obtained in comparative example 3;
FIG. 4 is a comparison of the ion conductivity of an ultra-thin, lightweight, high mechanical strength PEO-based solid electrolyte obtained from the cellulose membrane of example 2 of the present invention as a support layer, with that of a conventional PEO-based solid electrolyte obtained from comparative example 3;
FIG. 5a is the lithium ion transport number of an ultrathin, lightweight, high mechanical strength PEO-based solid electrolyte with a cellulose membrane as a support layer obtained in example 2 of the present invention; 5b is the transference number of lithium ions for the conventional PEO-based solid state electrolyte obtained in comparative example 3;
FIG. 6 is a comparison of the cycle performance of an ultra-thin, lightweight, high mechanical strength PEO-based solid electrolyte obtained from example 2 of the present invention as a support layer, with a conventional PEO-based solid electrolyte obtained from comparative example 3;
FIG. 7 is a comparison of rate capability of an ultra-thin, lightweight, high mechanical strength PEO-based solid electrolyte obtained from a cellulose membrane of example 2 of the present invention as a support layer with that of a conventional PEO-based solid electrolyte obtained from comparative example 3;
Detailed Description
The invention will now be further described with reference to the following examples, and the accompanying drawings:
the invention discloses a preparation method of an ultrathin, light and high-mechanical-strength PEO-based solid electrolyte with a cellulose membrane as a supporting layer. The PEO-based solid electrolyte membrane with ultrathin, flexible and high mechanical strength is prepared by simple coating and hot pressing technologies. The requirements of ultra-thin, light weight, flexibility and high mechanical strength of the PEO-based solid electrolyte can be realized by the Cladophora Cellulose with flexibility, thermal stability, light weight and high porosity. Meanwhile, a large number of hydroxyl groups on the surface of the cellulose membrane can improve the compatibility of the cellulose membrane with PEO, and the electrochemical performance of the PEO-based solid electrolyte is improved to a certain extent. By combining the characteristics, the preparation of the ultrathin, flexible, light and high-mechanical-strength PEO-based solid electrolyte can be realized, and the high energy density of the all-solid-state lithium metal battery can be realized. Meanwhile, in consideration of the characteristics of rich cellulose reserves, strong sustainability, low price and simple processing, the PEO-based solid electrolyte prepared by the method has the advantages of cost advantage and simple operation, and is suitable for industrial production. In view of this, the invention is particularly proposed.
The invention provides an ultrathin, light, flexible, thermally stable and high-mechanical-strength PEO-based solid electrolyte, which is realized by the following steps:
step 3, mixing and stirring PEO, LiTFSI and LLZTO in acetonitrile according to a certain ratio to obtain slurry of the PEO-based solid electrolyte; the ratio of LLZTO is 20%, the ratio of PEO to LiTFSI is [ EO/Li + ] -16: 1, and the stirring time is 12 hours;
step 4, coating the slurry of the PEO-based solid electrolyte on two sides of Cladophora Cellulose by a coating machine and drying; the coating scale of the slurry of the PEO-based solid electrolyte is 15-35; the drying process is that room temperature is firstly 12 hours, and then a vacuum oven is used for 12 hours at 60 ℃;
Example 2
step 3, mixing 520mg of PEO, 212mg of LiTFSI and 183mg of LLZTO in 10ml of acetonitrile, and stirring to obtain slurry of the PEO-based solid electrolyte; the stirring time is 12 hours;
step 4, coating the slurry of the PEO-based solid electrolyte on two sides of Cladophora Cellulose by a coating machine and drying; the coating scale of the slurry of PEO-based solid electrolyte was 25; the drying process is that room temperature is firstly 12 hours, and then a vacuum oven is used for 12 hours at 60 ℃;
And (4) SEM characterization:
SEM characterization of the ultra-thin, light, flexible, thermally stable, and high mechanical strength PEO-based solid electrolyte prepared in example 2 of the present invention, as shown in fig. 1, it can be seen that the thickness of the prepared PEO-based solid electrolyte is about 25 μm;
mechanical Property test
When the ultra-thin, light, flexible, thermally stable, and high mechanical strength PEO-based solid electrolytes (15 μm, 25 μm, and 35 μm) having different thicknesses prepared in example 2, comparative example 1, and comparative example 2 according to the present invention and the conventional PEO-based solid electrolyte obtained in comparative example 3 were subjected to a stress-strain test, as shown in fig. 2, it was observed that the mechanical properties of the ultra-thin, light, flexible, thermally stable, and high mechanical strength PEO-based solid electrolyte prepared in example 2 were greatly improved;
Critical current density test
When the ultra-thin, light, flexible, thermally stable, and high mechanical strength PEO-based solid electrolytes (15 μm, 25 μm, and 35 μm) of different thicknesses prepared in examples 2, 1, and 2 according to the present invention and the conventional PEO-based solid electrolyte obtained in comparative example 3 were subjected to critical current density tests, as shown in fig. 3, it was observed that the ultra-thin, light, flexible, thermally stable, and high mechanical strength PEO-based solid electrolyte prepared in example 1 had a higher critical current density and a lower overpotential than comparative example 3, and the combination of critical current density, overpotential, and mechanical property tests, the combination of example 2 was the most excellent;
ion conductivity test
When the ultra-thin, light, flexible, thermally stable, and high-mechanical strength PEO-based solid electrolyte prepared in example 2 of the present invention and the conventional PEO-based solid electrolyte obtained in comparative example 1 were subjected to an ion conductivity test, as shown in fig. 4, it can be observed that the ultra-thin, light, flexible, thermally stable, and high-mechanical strength PEO-based solid electrolyte prepared in example 2 has higher ion conductivity;
lithium ion transference number test
The ultra-thin, light, flexible, thermally stable, high mechanical strength PEO-based solid electrolyte prepared in example 2 of the present invention was subjected to a lithium ion transport number test, and the result is shown in fig. 5 a; the conventional PEO-based solid state electrolyte obtained in comparative example 1 was subjected to a lithium ion transport number test, and the result is shown in fig. 5 b; it can be observed that the ultra-thin, lightweight, flexible, thermally stable, high mechanical strength PEO-based solid electrolyte prepared in example 1 has a higher transference number of lithium ions (0.56);
Electrochemical Performance test
The ultra-thin, light, flexible, thermally stable, high mechanical strength PEO-based solid electrolyte obtained in example 2 of the present invention and that obtained in comparative example 1 were usedConventional PEO-based solid electrolyte and LiFePO4Electrochemical performance tests of the button cell assembled by the positive electrode and the lithium metal negative electrode show that the results are shown in fig. 6 and 7, and the ultrathin, light, flexible, thermally stable and high-mechanical-strength PEO-based solid electrolyte prepared in example 2 has better cycle performance and rate performance.
Comparative example 1
step 3, mixing 520mg of PEO, 212mg of LiTFSI and 183mg of LLZTO in 10ml of acetonitrile, and stirring to obtain slurry of the PEO-based solid electrolyte; stirring for 12 hours;
step 4, coating the slurry of the PEO-based solid electrolyte on two sides of Cladophora Cellulose by a coating machine and drying; the coating scale of the slurry of PEO-based solid electrolyte was 35; the drying process is that room temperature is firstly 12 hours, and then a vacuum oven is used for 12 hours at 60 ℃;
Comparative example 2
step 3, mixing 520mg of PEO, 212mg of LiTFSI and 183mg of LLZTO in 10ml of acetonitrile, and stirring to obtain slurry of the PEO-based solid electrolyte; the stirring time is 12 hours;
step 4, coating the slurry of the PEO-based solid electrolyte on two sides of Cladophora Cellulose by a coating machine and drying; the coating scale of the slurry of PEO-based solid electrolyte was 15; the drying process is that room temperature is firstly 12 hours, and then a vacuum oven is used for 12 hours at 60 ℃;
Comparative example 3
the above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention.
The ultra-thin, light, flexible, thermally stable and high-mechanical strength PEO-based solid electrolyte prepared by the invention has better comprehensive performances of mechanical property, ionic conductivity and critical current density when the thickness is about 25 mu m as can be seen by the example 2 and the comparative examples 1 and 2, and the ultra-thin, light, flexible, thermally stable and high-mechanical strength PEO-based solid electrolyte (25 mu m thick) prepared by the invention has more excellent mechanical property, ionic conductivity, lithium ion migration number and critical current density as can be seen by the example 1 and the comparative examples 3, and the assembled battery has better cycle performance and rate capability. By combining the advantages, the electrolyte membrane is beneficial to realizing the high energy density of the all-solid-state lithium metal battery.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. A method for preparing an ultrathin, light and high-mechanical-strength PEO-based solid electrolyte with a cellulose membrane as a supporting layer is characterized by comprising the following steps:
step 1: uniformly dispersing Cladophora Cellulose raw material in an aqueous solution to obtain a precursor solution;
step 2: carrying out vacuum filtration on the obtained precursor solution and then drying;
and step 3: mixing and stirring PEO, LiTFSI and LLZTO in acetonitrile to obtain slurry of PEO-based solid electrolyte; wherein the ratio of LLZTO is 20%, and the ratio of PEO to LiTFSI is [ EO/Li + ] -16: 1;
and 4, step 4: coating the slurry of the PEO-based solid electrolyte on two sides of Cladophora Cellulose by a coating machine and drying; the drying process is that room temperature is firstly 12 hours, and then a vacuum oven is used for 12 hours at 60 ℃;
and 5: hot-pressing the dried PEO-based solid electrolyte to obtain the ultrathin, light and high-mechanical-strength PEO-based solid electrolyte with the cellulose membrane as a supporting layer; the hot pressing pressure is 40MPa, the hot pressing temperature is 70 ℃, and the hot pressing time is 10-30 min.
2. The method for preparing the ultrathin, light and high mechanical strength PEO-based solid electrolyte with the cellulose membrane as the support layer according to claim 1, is characterized in that: in the step 1: dispersing Cladophora Cellulose raw material in water solution by an ultrasonic wall breaking machine; the power of the ultrasonic wall breaking machine is 650W; the dispersion time is 10-30 min.
3. The method for preparing the ultra-thin, light and high mechanical strength PEO-based solid electrolyte with the cellulose membrane as the support layer according to claim 1, is characterized in that: in the step 2: the drying temperature is 100 ℃, and the time is 12 hours.
4. The method for preparing the ultrathin, light and high mechanical strength PEO-based solid electrolyte with the cellulose membrane as the support layer according to claim 1, is characterized in that: the stirring time of the step 3 is 12 hours.
5. The method for preparing the ultrathin, light and high mechanical strength PEO-based solid electrolyte with the cellulose membrane as the support layer according to claim 1, is characterized in that: in the step 4: the coating scale of the slurry of PEO-based solid electrolyte was 15-35.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115332624A (en) * | 2022-10-13 | 2022-11-11 | 西北工业大学 | Preparation method of thermal-stable, ultrathin, light and flame-retardant PEO-based solid electrolyte |
| CN116231067A (en) * | 2023-05-09 | 2023-06-06 | 西北工业大学 | Preparation method of flame-retardant ultrathin PEO-based solid electrolyte |
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2022
- 2022-04-18 CN CN202210415560.8A patent/CN114759253A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115332624A (en) * | 2022-10-13 | 2022-11-11 | 西北工业大学 | Preparation method of thermal-stable, ultrathin, light and flame-retardant PEO-based solid electrolyte |
| CN115332624B (en) * | 2022-10-13 | 2023-01-31 | 西北工业大学 | Preparation method of heat-stable, ultrathin, light and flame-retardant PEO-based solid electrolyte |
| CN116231067A (en) * | 2023-05-09 | 2023-06-06 | 西北工业大学 | Preparation method of flame-retardant ultrathin PEO-based solid electrolyte |
| CN116231067B (en) * | 2023-05-09 | 2023-08-04 | 西北工业大学 | Preparation method of flame-retardant ultrathin PEO-based solid electrolyte |
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