CN112993244A - Room-temperature full-liquid-state lithium-sulfur battery and preparation method thereof - Google Patents
Room-temperature full-liquid-state lithium-sulfur battery and preparation method thereof Download PDFInfo
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H—ELECTRICITY
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- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/40—Alloys based on alkali metals
- H01M4/405—Alloys based on lithium
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Abstract
The invention provides a room-temperature full-liquid lithium-sulfur battery and a preparation method thereof, wherein the room-temperature full-liquid lithium-sulfur battery comprises a diaphragm, a room-temperature liquid alloy negative electrode and a liquid polysulfide positive electrode which are respectively arranged on two sides of the diaphragm, and a current collector connected with the liquid polysulfide positive electrode; the room-temperature liquid alloy cathode is formed by reacting lithium and mercury according to a preset proportion, and the diaphragm is lithium ions with a boron nitride coatingA battery separator; the liquid polysulfide positive electrode is
(ii) a The current collector includes an aluminum foil coated with a conductive carbon material. According to the invention, the liquid alloy is used for replacing metal lithium, so that the generation of lithium dendrite is inhibited, and the cycle life and the safety performance of the battery are improved; the liquid polysulfide replaces the elemental sulfur anode, so that the conductivity of the anode is greatly improved, and the problem of volume expansion in the charging and discharging process is effectively solved; by carrying out surface modification and structure improvement on the diaphragm, shuttling of polysulfide is effectively inhibited, loss of active substances and self-discharge are reduced, and the coulomb efficiency of the lithium-sulfur battery is improved.
Description
Technical Field
The invention relates to the technical field of lithium batteries, in particular to a room-temperature all-liquid-state lithium-sulfur battery and a preparation method thereof.
Background
In recent years, liquid batteries have a wide prospect in the field of energy storage batteries, and have the following advantages: 1) the liquid battery has no volume change in the charging and discharging processes; 2) the liquid metal electrode has no dendritic crystal growth problem; 3) the liquid electrode has good conductivity, simple electrode structure and the like. The liquid lithium-sulfur battery can solve the existing problems of the lithium-sulfur battery, such as poor mechanical property and serious active substance loss of the battery caused by great volume expansion in the charging and discharging processes; the positive electrode has poor elemental sulfur conductivity, and the shuttle of polysulfide can cause active substance loss and self-discharge; the growth of negative lithium dendrites results in lower coulombic efficiency and shorter cycle life with poorer safety. Because the alkali metal is solid under the conditions of normal temperature and normal pressure, the liquid battery generally needs to operate at higher temperature (> 300 ℃), and the lithium-sulfur battery electrolyte cannot normally work under the condition of high temperature; so that no liquid lithium-sulfur battery at room temperature exists.
Disclosure of Invention
The invention provides a room-temperature all-liquid-state lithium-sulfur battery and a preparation method thereof, aiming at solving the technical problem that the existing solid-state lithium-sulfur battery is inconvenient to use.
The invention provides a room-temperature full-liquid lithium-sulfur battery, which comprises a diaphragm, a room-temperature liquid alloy cathode and a liquid polysulfide anode which are respectively arranged on two sides of the diaphragm, and a current collector connected with the liquid polysulfide anode; the room-temperature liquid alloy cathode is formed by reacting lithium and mercury according to a preset proportion, and the diaphragm is a lithium ion battery diaphragm with a boron nitride coating; the liquid polysulfide positive electrode is
(ii) a The current collector includes an aluminum foil coated with a conductive carbon material.
On the other hand, the invention also provides a preparation method of the room-temperature all-liquid-state lithium-sulfur battery, which comprises the following steps:
step S1: manufacturing a room-temperature liquid alloy cathode;
step S2: manufacturing a diaphragm;
step S3: manufacturing a liquid polysulfide positive electrode;
step S4: manufacturing a current collector;
step S5: and injecting the room-temperature liquid alloy cathode and the liquid polysulfide anode into an H-shaped electrolytic cell with a replaceable film, inserting a foil electrode into the room-temperature liquid alloy cathode, clamping a current collector on a lead clamp, immersing the current collector into the liquid polysulfide anode, clamping a diaphragm between the anode cell and the cathode cell, and sealing the H-shaped electrolytic cell integrally to form the room-temperature full-liquid lithium-sulfur battery.
Further, the step S1 specifically includes the following steps:
the room-temperature liquid-state alloy cathode adopts lithium and mercury with the oxide film removed, and the room-temperature liquid-state lithium-based alloy cathode can be prepared by controlling the content of the lithium in the liquid mercury according to a preset proportion.
Further, the mass ratio of lithium to mercury is (0.01-0.86): (99.14-99.99).
Further, the step S2 specifically includes the following steps:
step S21, ball-milling boron nitride and guanidine carbonate or guanidine nitrate, and dispersing into a solvent to obtain a uniform and stable dispersion liquid;
and step S22, carrying out suction filtration on the dispersion liquid to obtain the lithium ion battery diaphragm with the boron nitride coating after drying, and forming the diaphragm.
Further, the step S3 specifically includes the following steps:
and step S31, assembling a common lithium-sulfur battery by using an H-shaped electrolytic cell, short-circuiting the positive electrode and the negative electrode to discharge, diffusing polysulfide into the electrolyte, and changing the electrolyte into brown yellow.
And step S32, collecting the electrolyte, adding elemental sulfur into the electrolyte, taking supernate after full reaction, and obtaining the liquid polysulfide anode.
Further, step S4 specifically includes the following steps:
and coating a conductive carbon material on the aluminum foil to form the current collector.
Further, the conductive carbon material comprises one or more of graphite, graphene, carbon nanotubes and carbon nanofibers.
Further, steps S1 to S5 are all performed under normal temperature and pressure conditions.
Further, steps S1 to S5 are all completed in a glove box filled with argon gas.
The invention has the beneficial effects that: the invention solves the existing problems of the lithium-sulfur battery by utilizing the advantages of the liquid battery, can work at room temperature, does not need high-temperature heating, and saves energy. The liquid alloy is used for replacing metal lithium, so that the generation of lithium dendrite is inhibited, and the cycle life and the safety performance of the battery are improved; the liquid polysulfide replaces the elemental sulfur anode, so that the conductivity of the anode is greatly improved, and the problem of volume expansion in the charging and discharging process is effectively solved; by carrying out surface modification and structure improvement on the diaphragm, shuttling of polysulfide is effectively inhibited, loss of active substances and self-discharge are reduced, and the coulomb efficiency of the lithium-sulfur battery is improved.
Drawings
FIG. 1 is a symmetrical cell cycle voltage curve for a room temperature liquid alloy negative electrode with a current density of 2.84 mA cm-2.
Fig. 2 is a cyclic voltammogram of a room temperature fully liquid lithium sulfur battery.
Fig. 3 is an electrochemical test curve of a room temperature all-liquid lithium sulfur battery.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", and the like, indicate orientations and positional relationships based on those shown in the drawings, and are used only for convenience of description and simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be considered as limiting the present invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly stated or limited, "above" or "below" a first feature means that the first and second features are in direct contact, or that the first and second features are not in direct contact but are in contact with each other via another feature therebetween. Also, the first feature being "on," "above" and "over" the second feature includes the first feature being directly on and obliquely above the second feature, or merely indicating that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature includes the first feature being directly under and obliquely below the second feature, or simply meaning that the first feature is at a lesser elevation than the second feature.
The present invention will be described in further detail with reference to the following detailed description and accompanying drawings.
As shown in fig. 1 to 3, the present invention provides a room temperature all-liquid lithium sulfur battery, which includes a diaphragm, a room temperature liquid alloy cathode and a liquid polysulfide anode respectively installed at two sides of the diaphragm, and a current collector connected with the liquid polysulfide anode; the room-temperature liquid alloy cathode is formed by reacting lithium and mercury according to a preset proportion, and the diaphragm is a lithium ion battery diaphragm with a boron nitride coating; the liquid polysulfide positive electrode is
(ii) a The current collector includes an aluminum foil coated with a conductive carbon material.
The invention solves the existing problems of the lithium-sulfur battery by utilizing the advantages of the liquid battery, can work at room temperature, does not need high-temperature heating, and saves energy. The liquid alloy is used for replacing metal lithium, so that the generation of lithium dendrite is inhibited, and the cycle life and the safety performance of the battery are improved; the liquid polysulfide replaces the elemental sulfur anode, so that the conductivity of the anode is greatly improved, and the problem of volume expansion in the charging and discharging process is effectively solved; by carrying out surface modification and structure improvement on the diaphragm, shuttling of polysulfide is effectively inhibited, loss of active substances and self-discharge are reduced, and the coulomb efficiency of the lithium-sulfur battery is improved.
On the other hand, the invention also provides a preparation method of the room-temperature all-liquid-state lithium-sulfur battery, which comprises the following steps:
step S1: manufacturing a room-temperature liquid alloy cathode;
step S2: manufacturing a diaphragm;
step S3: manufacturing a liquid polysulfide positive electrode;
step S4: manufacturing a current collector;
step S5: and injecting the room-temperature liquid alloy cathode and the liquid polysulfide anode into an H-shaped electrolytic cell with a replaceable film, inserting a foil electrode into the room-temperature liquid alloy cathode, clamping a current collector on a lead clamp, immersing the current collector into the liquid polysulfide anode, clamping a diaphragm between the anode cell and the cathode cell, and sealing the H-shaped electrolytic cell integrally to form the room-temperature full-liquid lithium-sulfur battery.
The invention solves the existing problems of the lithium-sulfur battery by utilizing the advantages of the liquid battery, can work at room temperature, does not need high-temperature heating, and saves energy. The liquid alloy is used for replacing metal lithium, so that the generation of lithium dendrite is inhibited, and the cycle life and the safety performance of the battery are improved; the liquid polysulfide replaces the elemental sulfur anode, so that the conductivity of the anode is greatly improved, and the problem of volume expansion in the charging and discharging process is effectively solved; by carrying out surface modification and structure improvement on the diaphragm, shuttling of polysulfide is effectively inhibited, loss of active substances and self-discharge are reduced, and the coulomb efficiency of the lithium-sulfur battery is improved.
In an optional embodiment, the step S1 specifically includes the following steps:
the room-temperature liquid-state alloy cathode adopts lithium and mercury with the oxide film removed, and the room-temperature liquid-state lithium-based alloy cathode can be prepared by controlling the content of the lithium in the liquid mercury according to a preset proportion. The mass ratio of the lithium to the mercury is (0.01-0.86): (99.14-99.99).
Specifically, different types of liquid alkali metal alloy cathodes can also be prepared by adopting metal potassium and metal sodium instead of metal lithium.
In an optional embodiment, the step S2 specifically includes the following steps:
step S21, ball-milling boron nitride and guanidine carbonate or guanidine nitrate, and dispersing into a solvent to obtain a uniform and stable dispersion liquid;
and step S22, carrying out suction filtration on the dispersion liquid to obtain the lithium ion battery diaphragm with the boron nitride coating after drying, and forming the diaphragm.
In an optional embodiment, the step S3 specifically includes the following steps:
and step S31, assembling a common lithium-sulfur battery by using an H-shaped electrolytic cell, short-circuiting the positive electrode and the negative electrode to discharge, diffusing polysulfide into the electrolyte, and changing the electrolyte into brown yellow.
And step S32, collecting the electrolyte, adding elemental sulfur into the electrolyte, taking supernate after full reaction, and obtaining the liquid polysulfide anode.
In an alternative embodiment, step S4 specifically includes the following steps:
and coating a conductive carbon material on the aluminum foil to form the current collector.
In an alternative embodiment, the conductive carbon material comprises one or more of graphite, graphene, carbon nanotubes, carbon nanofibers.
In an alternative embodiment, steps S1 to S5 are all performed under normal temperature and pressure conditions.
In an alternative embodiment, steps S1 to S5 are all completed in a glove box filled with argon gas.
The specific embodiment is as follows:
example one
(1) Taking 15 mg of metal lithium with an oxidation film removed, adding the metal lithium into 0.733 g of metal mercury, and standing for 24 hours to obtain a room-temperature liquid alloy cathode;
(2) mixing 1 g of boron nitride and 1 g of guanidine carbonate, performing ball milling for 48 h to obtain uniformly mixed powder, adding 20 mg of the mixed powder into 20 ml of NMP, and mechanically stirring for 12 h to obtain stable and uniform dispersion liquid A; taking a lithium ion battery diaphragm as filter paper, carrying out suction filtration on the dispersion liquid A, washing off NMP on the diaphragm by using deionized water, and drying the diaphragm to obtain the lithium ion battery diaphragm with the boron nitride coating;
(3) the H-shaped electrolytic cell is used for assembling a common lithium-sulfur battery, the anode and the cathode are in short circuit discharge, polysulfide can be diffused into electrolyte, and the electrolyte becomes brown yellow. Collecting electrolyte, adding 10 mg of elemental sulfur into the electrolyte, reacting for 24 hours, and taking supernatant to obtain the liquid polysulfide anode.
(4) Adding 90 mg of graphene and 10 mg of PVDF into 2 ml of NMP, magnetically stirring for 12 h, coating the obtained slurry on an aluminum foil by using a 200-micron scraper, drying, and cutting into circular sheets with the diameter of 15 mm to obtain the positive current collector.
(5) The liquid alloy negative electrode and the liquid polysulfide positive electrode are injected into the replaceable film H-shaped electrolytic cell, the foil electrode is inserted into the liquid alloy negative electrode, the current collector is clamped on the lead clamp and immersed into the liquid polysulfide positive electrode, the diaphragm is clamped between the positive electrode cell and the negative electrode cell, the whole cell is sealed, and the electrochemical performance of the cell is tested.
Example two
(1) Adding 90 mg of metal lithium with the oxide film removed into 4.398 g of metal mercury, and standing for 24h to obtain a room-temperature liquid alloy cathode;
(2) mixing 2 g of boron nitride and 2 g of guanidine carbonate, performing ball milling for 48 h to obtain uniform mixed powder, adding 50 mg of mixed powder into 50 ml of NMP, and mechanically stirring for 12 h to obtain stable and uniform dispersion A; taking a lithium ion battery diaphragm as filter paper, carrying out suction filtration on the dispersion liquid A, washing away NMP (N-methyl pyrrolidone) by using deionized water, and drying the diaphragm to obtain the lithium ion battery diaphragm with the boron nitride coating;
(3) the H-shaped electrolytic cell is used for assembling a common lithium-sulfur battery, the anode and the cathode are in short circuit discharge, polysulfide can be diffused into electrolyte, and the electrolyte becomes brown yellow. And collecting the electrolyte, adding 20 mg of elemental sulfur into the electrolyte, reacting for 24 hours, and taking supernatant to obtain the liquid polysulfide anode.
The current collector is a conductive carbon material coated on the aluminum foil, and the conductive carbon material is one or more of graphite, graphene, carbon nanotubes, carbon nanofibers and the like.
(4) Adding 180 mg of graphene and 20 mg of PVDF into 4 ml of NMP, magnetically stirring for 12 hours, coating the obtained slurry on an aluminum foil by using a 200-micron scraper, drying, and cutting into circular sheets with the diameter of 15 mm to obtain the positive current collector.
(5) The liquid alloy cathode and the liquid polysulfide anode are injected into an H-shaped electrolytic cell with a replaceable film, a foil electrode is inserted into the liquid lithium amalgam cathode, a current collector is clamped on a lead clamp and is immersed into the liquid polysulfide anode, a diaphragm is clamped between the cathode cell and the anode cell, the whole cell is sealed, and the electrochemical performance of the cell is tested.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" or the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is a more detailed description of the present invention that is presented in conjunction with specific embodiments, and the practice of the invention is not to be considered limited to those descriptions. It will be apparent to those skilled in the art that a number of simple derivations or substitutions can be made without departing from the inventive concept.
Claims (10)
1. The room-temperature full-liquid lithium-sulfur battery is characterized by comprising a diaphragm, a room-temperature liquid alloy cathode and a liquid polysulfide anode which are respectively arranged on two sides of the diaphragm, and a current collector connected with the liquid polysulfide anode; the room-temperature liquid alloy cathode is formed by reacting lithium and mercury according to a preset proportion, and the diaphragm is a lithium ion battery diaphragm with a boron nitride coating; the liquid polysulfide positive electrode is
(ii) a What is needed isThe current collector includes an aluminum foil coated with a conductive carbon material.
2. The method for preparing the room-temperature all-liquid-state lithium-sulfur battery as claimed in claim 1, comprising the following steps:
step S1: manufacturing a room-temperature liquid alloy cathode;
step S2: manufacturing a diaphragm;
step S3: manufacturing a liquid polysulfide positive electrode;
step S4: manufacturing a current collector;
step S5: and injecting the room-temperature liquid alloy cathode and the liquid polysulfide anode into an H-shaped electrolytic cell with a replaceable film, inserting a foil electrode into the room-temperature liquid alloy cathode, clamping a current collector on a lead clamp, immersing the current collector into the liquid polysulfide anode, clamping a diaphragm between the anode cell and the cathode cell, and sealing the H-shaped electrolytic cell integrally to form the room-temperature full-liquid lithium-sulfur battery.
3. The method for preparing the room-temperature all-liquid-state lithium-sulfur battery according to claim 2, wherein the step S1 specifically comprises the following steps:
the room-temperature liquid-state alloy cathode adopts lithium and mercury with the oxide film removed, and the room-temperature liquid-state lithium-based alloy cathode can be prepared by controlling the content of the lithium in the liquid mercury according to a preset proportion.
4. The method for preparing the room-temperature all-liquid-state lithium-sulfur battery as claimed in claim 3, wherein the mass ratio of the lithium to the mercury is (0.01-0.86): (99.14-99.99).
5. The method for preparing the room-temperature all-liquid-state lithium-sulfur battery according to claim 2, wherein the step S2 specifically comprises the following steps:
step S21, ball-milling boron nitride and guanidine carbonate or guanidine nitrate, and dispersing into a solvent to obtain a uniform and stable dispersion liquid;
and step S22, carrying out suction filtration on the dispersion liquid to obtain the lithium ion battery diaphragm with the boron nitride coating after drying, and forming the diaphragm.
6. The method for preparing the room-temperature all-liquid-state lithium-sulfur battery according to claim 2, wherein the step S3 specifically comprises the following steps:
step S31, assembling a common lithium-sulfur battery by using an H-shaped electrolytic cell, and performing short-circuit discharge on the positive electrode and the negative electrode, wherein polysulfide can diffuse into electrolyte and the electrolyte becomes brown yellow;
and step S32, collecting the electrolyte, adding elemental sulfur into the electrolyte, taking supernate after full reaction, and obtaining the liquid polysulfide anode.
7. The method for preparing the room-temperature full-liquid lithium-sulfur battery as claimed in claim 2, wherein the step S4 comprises the following steps:
and coating a conductive carbon material on the aluminum foil to form the current collector.
8. The method of claim 7, wherein the conductive carbon material comprises one or more of graphite, graphene, carbon nanotubes, and carbon nanofibers.
9. The method of claim 2, wherein the steps S1 to S5 are performed under normal temperature and pressure conditions.
10. The method of claim 2, wherein steps S1 to S5 are performed in a glove box filled with argon gas.
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| CN106169586A (en) * | 2016-08-12 | 2016-11-30 | 洁能电投（北京）新能源科技有限公司 | A kind of flow battery system and the preparation method of positive electrode thereof |
| CN109309205A (en) * | 2017-07-26 | 2019-02-05 | 中能中科（天津）新能源科技有限公司 | Lithium-sulfur cell cathode, preparation method and lithium-sulfur cell |
| CN108565485A (en) * | 2018-04-04 | 2018-09-21 | 东华大学 | A kind of sulphur based on liquid electrode-bromine rechargeable battery and its application |
| CN108963349A (en) * | 2018-06-05 | 2018-12-07 | 燕山大学 | A kind of preparation method of the full liquid metal cell of room temperature |
| CN109167104A (en) * | 2018-09-12 | 2019-01-08 | 力信（江苏）能源科技有限责任公司 | A kind of room temperature sodium-sulphur battery and preparation method thereof |
| CN109888182A (en) * | 2019-01-25 | 2019-06-14 | 天津理工大学 | A kind of alkali metal electrode of in-situ conservation, preparation method and application |
| CN111564602A (en) * | 2020-05-23 | 2020-08-21 | 江西理工大学 | Method for directly preparing liquid positive electrode of lithium-sulfur battery by potential control |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113764718A (en) * | 2021-09-10 | 2021-12-07 | 广东工业大学 | Novel lithium-sulfur battery and preparation method thereof |
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