CN111952516A - Preparation method of rubidium-doped lithium battery composite diaphragm - Google Patents
Preparation method of rubidium-doped lithium battery composite diaphragm Download PDFInfo
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- CN111952516A CN111952516A CN202010823437.0A CN202010823437A CN111952516A CN 111952516 A CN111952516 A CN 111952516A CN 202010823437 A CN202010823437 A CN 202010823437A CN 111952516 A CN111952516 A CN 111952516A
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- rubidium
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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
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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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a rubidium-doped lithium battery composite diaphragm, which comprises the following steps: s1) according to the mass ratio of 0.5-1: 3-5: 4-5: 0.5-1: 50-80 dispersing and mixing a rubidium source, a lithium source, sodium hydroxide and urea in deionized water to obtain a mixed aqueous solution containing rubidium and lithium; s2) placing the flax cellulose in an environment with the temperature of 150-200 ℃ for heat activation for 0.5-1 h to obtain heat activated flax cellulose; s3) according to the mass ratio of 1: 1-2, dispersing the thermally activated flax cellulose in the mixed aqueous solution, and freezing for 5-10 hours at-18 to-50 ℃; s4) standing and thawing the thermally activated flax cellulose mixture frozen in the step S3) for 3-10 h in sequence at the temperature of 10-25 ℃, stirring and thawing for 1-2 h to obtain a cellulose membrane casting solution; s5) forming a film from the cellulose membrane casting solution after standing and defoaming, and cleaning and drying the film to obtain the rubidium-doped lithium battery composite diaphragm. According to the invention, the rubidium ions are doped to form the ion channel with large aperture, and meanwhile, the excellent mechanical property of the flax cellulose under the high-temperature condition is fully utilized.
Description
Technical Field
The invention belongs to the field of preparation of lithium battery diaphragms, and particularly relates to a preparation method of a rubidium-doped lithium battery composite diaphragm.
Background
The separator is one of the key internal components of a lithium battery, and its performance determines the interface structure, internal resistance, etc. of the battery. In order to ensure the capacity, circulation, safety and other properties of the lithium battery, the diaphragm needs to have a certain aperture and porosity, ensure low resistance and high ionic conductivity, and simultaneously need to have sufficient mechanical properties.
At present, polyolefin membrane materials are mostly adopted for lithium battery diaphragms, for example, the melting point of PE is 128-135 ℃, the PP is 150-160 ℃, and the aperture and the mechanical property of the lithium battery diaphragm can be reduced under the high-temperature condition, so that the internal resistance of the battery is high, the ionic conductivity is low, and the safety performance is poor.
Disclosure of Invention
Aiming at the technical problems of low ionic conductivity and poor mechanical property of a lithium battery diaphragm material in the prior art, the invention provides a preparation method of a rubidium-doped lithium battery composite diaphragm, which is characterized in that a large-aperture ion channel is formed by doping rubidium ions/cesium ions to promote lithium ion conduction; meanwhile, the excellent mechanical property of the flax cellulose under the high-temperature condition is fully utilized, and the mechanical strength required by the lithium battery diaphragm material is provided.
The technical scheme adopted by the invention for solving the problems is as follows:
a preparation method of a rubidium-doped lithium battery composite diaphragm comprises the following steps:
s1) according to the mass ratio of 0.5-1: 3-5: 4-5: 0.5-1: 50-80 mixing a rubidium source, a lithium source, sodium hydroxide, urea and water to obtain a mixed aqueous solution containing rubidium and lithium;
s2) placing the flax cellulose in an environment with the temperature of 150-200 ℃ for heat activation for 0.5-1 h to obtain heat activated flax cellulose;
s3) according to the mass ratio of 1: 1-2, dispersing the thermally activated flax cellulose prepared in the step S2) in the mixed aqueous solution prepared in the step S1), and freezing for 5-10 hours at-18 to-50 ℃;
s4) standing and thawing the mixture frozen in the step S3) for 3-10 h in sequence at the temperature of 10-25 ℃, and stirring and thawing for 1-2 h to obtain a casting solution;
s5) forming a film from the casting solution after standing and defoaming, and cleaning and drying the film to obtain the rubidium-doped lithium battery composite diaphragm.
Preferably, the rubidium source in step S1) is rubidium hydroxide (RbOH) or rubidium carbonate (Rb)2CO3) Etc.; the lithium source is lithium hydroxide (LiOH) or lithium carbonate (Li)2CO3) And the like.
Preferably, the polymerization degree of the flax cellulose in the step S2) is 1500-2000.
Preferably, the average diameter of the flax cellulose in the step S2) is 1-3 μm, and the length-diameter ratio is 50-300.
Preferably, the mixed aqueous solution in step S1) further includes a cesium source, and the cesium source is added according to a mass ratio of 0.5-1: 3-5: 4-5: 0.5-1: 0.3-0.6: 50-80 blending rubidium source, lithium source, sodium hydroxide, urea, cesium source and water.
Preferably, the cesium source is cesium carbonate (Cs)2CO3) Or cesium bicarbonate (CsHCO)3) And the like.
Preferably, the blending temperature in the step S1) is 40-60 ℃, and the blending time is 0.5-1 h.
In general, compared with the prior art, the above technical solution contemplated by the present invention can achieve the following beneficial effects: according to the invention, the rubidium ions/cesium ions are doped to form the ion channel with large aperture, so that the lithium ion conduction is promoted, and meanwhile, the excellent mechanical property of the flax cellulose at high temperature is fully utilized, so that the mechanical strength required by the lithium battery diaphragm material is provided, the mechanical strength is ensured while the conductivity is improved, and the practicability is greatly enhanced.
Drawings
Fig. 1 is a cycle test chart of the rubidium-doped lithium battery composite membrane obtained in example 1 of the present invention at a current density of 0.2C;
fig. 2 is a cycle test chart of the rubidium-doped lithium battery composite diaphragm obtained in example 3 of the present invention at a current density of 0.2C.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
A preparation method of a rubidium-doped lithium battery composite diaphragm comprises the following specific steps:
step 1: according to the mass ratio of 0.5: 3: 4: 0.5: 50 mixing rubidium hydroxide, lithium carbonate, sodium hydroxide, urea and deionized water, heating to 40 ℃, and blending for 1h to obtain a mixed aqueous solution containing rubidium and lithium;
step 2: weighing 500g of a flax cellulose material with the polymerization degree of 1500, placing the flax cellulose material in a drying oven, and thermally activating for 1h at 150 ℃ to obtain a thermally activated flax cellulose material; wherein, the average diameter of the flax cellulose material selected by the embodiment is about 1 μm, and the length-diameter ratio is about 50;
and step 3: according to the mass ratio of 1: 1, dispersing the heat-activated flax cellulose material prepared in the step 2 in the mixed aqueous solution prepared in the step 1, and freezing for 10 hours at-18 ℃;
and 4, step 4: standing and thawing the mixture frozen in the step 3 for 3 hours at the temperature of 25 ℃, and stirring and thawing for 1 hour to obtain a membrane casting solution;
and 5: and (3) forming a film by using the casting film liquid after standing and defoaming, then placing the film into deionized water for cleaning, taking out the film, and then placing the film into an oven at 80 ℃ for drying for 5 hours to obtain the rubidium-doped lithium battery composite diaphragm.
In addition, a lithium battery composite separator not doped with a rubidium source was prepared as comparative sample 1 according to the procedure of this example.
Example 2
A preparation method of a rubidium-doped lithium battery composite diaphragm comprises the following specific steps:
step 1: according to the mass ratio of 1: 5: 5: 1: 80 mixing rubidium carbonate, lithium hydroxide, sodium hydroxide, urea and deionized water, heating to 60 ℃, and blending for 0.5h to obtain a mixed aqueous solution containing rubidium and lithium;
step 2: weighing 500g of flax cellulose material with polymerization degree of 2000, placing the flax cellulose material in a drying oven, and thermally activating for 0.5h at 200 ℃ to obtain a thermally activated flax cellulose material; wherein, the average diameter of the flax cellulose material selected in the embodiment is about 3 μm, and the length-diameter ratio is about 300;
and step 3: according to the mass ratio of 1: 2, dispersing the heat-activated flax cellulose material prepared in the step 2 into the mixed aqueous solution prepared in the step 1, and freezing for 5 hours at-50 ℃;
and 4, step 4: standing and thawing the mixture frozen in the step 3 for 10 hours at the temperature of 10 ℃, and stirring and thawing for 2 hours to obtain a membrane casting solution;
and 5: and (3) forming a film by using the casting film liquid after standing and defoaming, then placing the film into deionized water for cleaning, taking out the film, and then placing the film into an oven at 80 ℃ for drying for 5 hours to obtain the rubidium-doped lithium battery composite diaphragm.
In addition, a lithium battery composite separator not doped with a rubidium source was prepared as comparative sample 2 according to the procedure of this example.
Example 3
A preparation method of a rubidium-doped lithium battery composite diaphragm comprises the following specific steps:
step 1: according to the mass ratio of 0.5: 3: 0.3: 4: 0.5: 50 mixing rubidium hydroxide, lithium carbonate, cesium bicarbonate, sodium hydroxide, urea and deionized water, heating to 40 ℃, and blending for 1h to obtain a mixed aqueous solution containing rubidium and lithium;
step 2: weighing 500g of a flax cellulose material with the polymerization degree of 1500, placing the flax cellulose material in a drying oven, and thermally activating for 1h at 150 ℃ to obtain a thermally activated flax cellulose material; wherein, the average diameter of the flax cellulose material selected by the embodiment is about 1 μm, and the length-diameter ratio is about 50;
and step 3: according to the mass ratio of 1: 1, dispersing the heat-activated flax cellulose material prepared in the step 2 in the mixed aqueous solution prepared in the step 1, and freezing for 10 hours at-18 ℃;
and 4, step 4: standing and thawing the mixture frozen in the step 3 for 3 hours at the temperature of 25 ℃, and stirring and thawing for 1 hour to obtain a membrane casting solution;
and 5: and (3) forming a film by using the casting film liquid after standing and defoaming, then placing the film into deionized water for cleaning, taking out the film, and then placing the film into an oven at 80 ℃ for drying for 5 hours to obtain the rubidium-doped lithium battery composite diaphragm.
In addition, a lithium battery composite separator not doped with a rubidium source was prepared as comparative sample 3 according to the procedure of this example.
Example 4
A preparation method of a rubidium-doped lithium battery composite diaphragm comprises the following specific steps:
step 1: according to the mass ratio of 1: 5: 0.6: 5: 1: 80 mixing rubidium carbonate, lithium hydroxide, cesium carbonate, sodium hydroxide, urea and deionized water, heating to 60 ℃, and blending for 0.5h to obtain a mixed aqueous solution containing rubidium and lithium;
step 2: weighing 500g of flax cellulose material with polymerization degree of 2000, placing the flax cellulose material in a drying oven, and thermally activating for 0.5h at 200 ℃ to obtain a thermally activated flax cellulose material; wherein, the average diameter of the flax cellulose material selected in the embodiment is about 3 μm, and the length-diameter ratio is about 300;
and step 3: according to the mass ratio of 1: 2, dispersing the heat-activated flax cellulose material prepared in the step 2 into the mixed aqueous solution prepared in the step 1, and freezing for 5 hours at-50 ℃;
and 4, step 4: standing and thawing the mixture frozen in the step 3 for 10 hours at the temperature of 10 ℃, and stirring and thawing for 2 hours to obtain a membrane casting solution;
and 5: and (3) forming a film by using the casting film liquid after standing and defoaming, then placing the film into deionized water for cleaning, taking out the film, and then placing the film into an oven at 80 ℃ for drying for 5 hours to obtain the rubidium-doped lithium battery composite diaphragm.
In addition, a lithium battery composite separator not doped with a rubidium source was prepared as comparative sample 4 according to the procedure of this example.
The characteristics of the rubidium-doped lithium battery composite membranes prepared in examples 1 to 4 are shown in table 1, and the overall results show that rubidium ions/cesium ions can significantly improve the ionic conductivity of the lithium battery composite membranes, and the flax cellulose provides good tensile strength, so that the mechanical strength required by the lithium battery composite membranes is provided while the conductivity is improved.
TABLE 1 comparative tests of ionic conductivity and mechanical Properties
| Examples of the invention | Conductivity (mS/cm) | Transference number of lithium ion (60 ℃ C.) | Tensile Strength (MPa) |
| Example 1 | 0.45 | 0.58 | 141 |
| Comparative sample 1 | 0.24 | 0.40 | 141 |
| Example 2 | 0.50 | 0.61 | 145 |
| Comparative sample 2 | 0.26 | 0.42 | 145 |
| Example 3 | 0.55 | 0.71 | 141 |
| Comparative sample 3 | 0.42 | 0.55 | 141 |
| Example 4 | 0.59 | 0.73 | 145 |
| Comparative sample 4 | 0.44 | 0.57 | 145 |
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (7)
1. A preparation method of a rubidium-doped lithium battery composite diaphragm is characterized by comprising the following steps:
s1) according to the mass ratio of 0.5-1: 3-5: 4-5: 0.5-1: 50-80 mixing a rubidium source, a lithium source, sodium hydroxide, urea and water to obtain a mixed aqueous solution containing rubidium and lithium;
s2) placing the flax cellulose in an environment with the temperature of 150-200 ℃ for heat activation for 0.5-1 h to obtain heat activated flax cellulose;
s3) according to the mass ratio of 1: 1-2, dispersing the thermally activated flax cellulose prepared in the step S2) in the mixed aqueous solution prepared in the step S1), and freezing for 5-10 hours at-18 to-50 ℃;
s4) standing and thawing the mixture frozen in the step S3) for 3-10 h in sequence at the temperature of 10-25 ℃, and stirring and thawing for 1-2 h to obtain a casting solution;
s5) standing and defoaming the casting solution, forming a film, and drying to obtain the rubidium-doped lithium battery composite diaphragm.
2. The production method according to claim 1, wherein the rubidium source in step S1) is rubidium hydroxide or rubidium carbonate; the lithium source is lithium hydroxide or lithium carbonate.
3. The preparation method according to claim 1, wherein the polymerization degree of the flax cellulose in the step S2) is 1500-2000.
4. The preparation method of claim 1, wherein the average diameter of the flax cellulose in the step S2) is 1-3 μm, and the length-diameter ratio is 50-300.
5. The method according to claim 1, wherein the mixed aqueous solution in step S1) further comprises a cesium source in a mass ratio of 0.5 to 1: 3-5: 4-5: 0.5-1: 0.3-0.6: 50-80 blending rubidium source, lithium source, sodium hydroxide, urea, cesium source and water.
6. The method of claim 5, wherein the cesium source is cesium carbonate or cesium bicarbonate.
7. The preparation method according to claim 1, wherein the blending temperature in step S1) is 40-60 ℃ and the blending time is 0.5-1 h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113078348A (en) * | 2021-03-19 | 2021-07-06 | 光鼎铷业(广州)集团有限公司 | Preparation method of rubidium-doped high-conductivity solid electrolyte |
| CN113088134A (en) * | 2021-03-19 | 2021-07-09 | 光鼎铷业(广州)集团有限公司 | Rubidium doped coating for lithium battery diaphragm, film, diaphragm and preparation method |
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Application publication date: 20201117 |