CN116864782A - Solid-state battery based on liquid gallium tin alloy negative electrode and preparation method thereof - Google Patents
Solid-state battery based on liquid gallium tin alloy negative electrode and preparation method thereof Download PDFInfo
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- CN116864782A CN116864782A CN202311043248.1A CN202311043248A CN116864782A CN 116864782 A CN116864782 A CN 116864782A CN 202311043248 A CN202311043248 A CN 202311043248A CN 116864782 A CN116864782 A CN 116864782A
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- 239000007788 liquid Substances 0.000 title claims abstract description 59
- 229910001128 Sn alloy Inorganic materials 0.000 title claims abstract description 42
- YZZNJYQZJKSEER-UHFFFAOYSA-N gallium tin Chemical compound [Ga].[Sn] YZZNJYQZJKSEER-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000007784 solid electrolyte Substances 0.000 claims abstract description 32
- 239000007787 solid Substances 0.000 claims abstract description 21
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims abstract description 12
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 12
- 229910018091 Li 2 S Inorganic materials 0.000 claims abstract description 11
- HFCVPDYCRZVZDF-UHFFFAOYSA-N [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O Chemical compound [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O HFCVPDYCRZVZDF-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 3
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 239000011572 manganese Substances 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 9
- 229910013716 LiNi Inorganic materials 0.000 claims description 8
- 239000006229 carbon black Substances 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 6
- GLNWILHOFOBOFD-UHFFFAOYSA-N lithium sulfide Chemical compound [Li+].[Li+].[S-2] GLNWILHOFOBOFD-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 229910000572 Lithium Nickel Cobalt Manganese Oxide (NCM) Inorganic materials 0.000 claims description 4
- FBDMTTNVIIVBKI-UHFFFAOYSA-N [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] Chemical compound [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] FBDMTTNVIIVBKI-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 4
- 239000003792 electrolyte Substances 0.000 claims description 3
- 229910003473 lithium bis(trifluoromethanesulfonyl)imide Inorganic materials 0.000 claims description 3
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 claims description 3
- 229910003055 Li0.33 La0.57 TiO3 Inorganic materials 0.000 claims description 2
- 229920001021 polysulfide Polymers 0.000 claims description 2
- 239000005077 polysulfide Substances 0.000 claims description 2
- 150000008117 polysulfides Polymers 0.000 claims description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 9
- 229910052744 lithium Inorganic materials 0.000 description 9
- 210000004027 cell Anatomy 0.000 description 4
- 210000001787 dendrite Anatomy 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910013553 LiNO Inorganic materials 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- H01M10/058—Construction or manufacture
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/134—Electrodes based on metals, Si or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a solid-state battery based on a liquid gallium tin alloy negative electrode and a preparation method thereof. A solid-state battery comprises a liquid gallium tin alloy negative electrode, a solid electrolyte, a nickel cobalt lithium manganate positive electrode or liquid Li 2 S 8 A positive electrode; the liquid gallium-tin alloy cathode contains gallium-tin alloy generated by the proportional reaction of metallic gallium and metallic tin; the mass ratio of the gallium metal to the tin metal is (3-11.5): 1. the invention provides good interface contact for the electrode/solid electrolyte interface by utilizing the liquid gallium tin alloy cathode, the liquid electrode and the solid electrolyte, solves the problems of low interface stability and large interface impedance of the electrode/solid electrolyte interface of the solid battery, and improves the solid stateCapacity and cycle life of the battery.
Description
Technical Field
The invention relates to the technical field of lithium batteries, in particular to a solid-state battery based on a liquid gallium-tin alloy negative electrode and a preparation method thereof.
Background
The rapid growth of social energy demands drives the explosive development of new energy battery industry, and solid-state lithium batteries with high mechanical strength and safety become research hotspots. However, the use of solid state lithium batteries faces multiple challenges including poor interfacial contact between the electrode and the electrode solid state electrolyte, large volume changes during cycling, and uncontrolled lithium dendrite growth, etc., rendering the solid state batteries incapable of exhibiting their excellent electrochemical performance. Therefore, developing a suitable strategy to solve the solid-solid contact problem is extremely necessary for practical all-solid batteries. The use of liquid electrodes instead of conventional solid electrode materials to construct the liquid-solid electrode/electrolyte interface may be one of the effective ways to improve the electrochemical performance of solid-state lithium batteries. The liquid-solid interface is used for replacing the traditional solid-solid interface, so that the contact area of an electrode/solid electrolyte can be effectively increased, the interface compatibility is enhanced, the interface impedance is reduced, lithium dendrites are inhibited, the influence of volume expansion is relieved, and the chemical and electrochemical stability of the interface is improved, thereby improving the electrochemical performance of the battery.
Disclosure of Invention
In order to solve the interface problem of the solid-state battery, the invention provides a solid-state battery based on a liquid gallium tin alloy anode and a preparation method thereof.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the first aspect of the invention provides a solid-state battery comprising a liquid gallium tin alloy anode, a solid electrolyte, a nickel cobalt lithium manganate anode or a liquid Li 2 S 8 A positive electrode;
the liquid gallium-tin alloy cathode contains gallium-tin alloy generated by the proportional reaction of metallic gallium and metallic tin; the mass ratio of the gallium metal to the tin metal is (3-11.5): 1.
preferably, the solid electrolyte comprises Li 10 GeP 2 S 12 、Li 0.33 La 0.57 TiO 3 、Li 7 La 3 Zr 2 O 12 At least one of (a) and (b); further preferably, the solid electrolyte is Li 10 GeP 2 S 12 。
Preferably, the lithium nickel cobalt manganese oxide positive electrode comprises LiNi 8 Co 1 Mn 1 O 2 。
Preferably, the liquid Li 2 S 8 The anode is polysulfide synthesized by lithium sulfide and elemental sulfur.
The second aspect of the present invention provides a method for preparing the solid-state battery, comprising the steps of:
(1) Manufacturing a liquid gallium-tin alloy cathode;
(2) Manufacturing a solid electrolyte sheet;
(3) Manufacturing an anode;
(4) The liquid gallium tin alloy is pressed on one side of the solid electrolyte sheet, and the nickel cobalt lithium manganate anode or liquid Li 2 S 8 And the positive electrode is added on the other side of the solid electrolyte sheet to assemble the solid battery.
Preferably, the step (1) specifically includes the following steps: mixing gallium and tin, heating to obtain liquid gallium-tin alloy, putting a base material into a mould, adding the liquid gallium-tin alloy, and pressing into a tablet to obtain the liquid gallium-tin alloy cathode.
Further preferably, in the step (1), the temperature at which the gallium metal and the tin metal are heated is 200-250 ℃; further preferably, the temperature at which gallium and tin are heated is 210-230 ℃.
Further preferably, in the step (1), the pressure for compression into tablets is 80-300MPa and the dwell time is 2-10min.
Preferably, the step (2) specifically includes the following steps: placing the solid electrolyte powder into a die and pressing the solid electrolyte powder into a tablet; further preferably, the pressure for compression into tablets is 80-300MPa and the dwell time is 2-10min.
Preferably, when the positive electrode is a lithium nickel cobalt manganese oxide positive electrode, the step (3) specifically includes the following steps: liNi is added to 8 Co 1 Mn 1 O 2 、Li 10 GeP 2 S 12 And mixing and ball milling with carbon black to obtain the nickel cobalt lithium manganate anode.
Preferably, the LiNi 8 Co 1 Mn 1 O 2 、Li 10 GeP 2 S 12 And carbon black in a mass ratio of (2-4): (3-5): 1, a step of; further preferably, the LiNi 8 Co 1 Mn 1 O 2 、Li 10 GeP 2 S 12 And the mass ratio of the carbon black is (2.5-3.5): (3.5-4.5): 1, a step of; still further preferably, the LiNi 8 Co 1 Mn 1 O 2 、Li 10 GeP 2 S 12 And the mass ratio of the carbon black is 3:4:1.
further preferably, the ball milling time is 4.5-5.5 hours; still further preferably, the ball milling time is 5 hours.
Preferably, when the positive electrode is liquid Li 2 S 8 In the positive electrode, the step (3) specifically includes the following steps: adding LiTFSI solution into lithium sulfide and elemental sulfur, and stirring until the solution is completely dissolved after ultrasonic dispersion to obtain the liquid Li 2 S 8 And a positive electrode.
Preferably, all of the steps (1) - (4) are carried out under normal temperature and pressure conditions.
Preferably, all of the steps (1) - (4) are performed in a glove box filled with argon.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides good interface contact for the electrode/solid electrolyte interface by utilizing the liquid gallium tin alloy cathode, the liquid electrode and the solid electrolyte, solves the problems of low interface stability and large interface impedance of the electrode/solid electrolyte interface of the solid battery, and improves the capacity and the cycle life of the solid battery. The liquid gallium tin alloy cathode is used for replacing metal lithium, so that the generation of lithium dendrite is inhibited, the safety and the cycle life of the battery are improved, the liquid gallium tin alloy cathode is in good interface contact with solid electrolyte, and a liquid-solid interface is used for replacing a traditional solid-solid interface, so that the contact area of the electrode/solid electrolyte can be effectively increased, the interface compatibility is enhanced, the interface impedance is reduced, the lithium dendrite is inhibited, the influence of volume expansion is relieved, the chemical and electrochemical stability of the interface is improved, and the electrochemical performance of the battery is improved.
Drawings
Fig. 1 is a cyclic voltammogram of a solid state battery based on a liquid gallium tin alloy anode of example 1;
fig. 2 is an ac impedance curve of the solid-state battery based on the liquid gallium-tin alloy anode of example 1;
fig. 3 is a charge-discharge curve of the solid-state battery based on the liquid gallium-tin alloy anode of example 1;
fig. 4 is a cycle performance curve of the solid-state battery based on the liquid gallium tin alloy anode of example 1.
Detailed Description
The following describes the invention in more detail. The description of these embodiments is provided to assist understanding of the present invention, but is not intended to limit the present invention. In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
The experimental methods in the following examples, unless otherwise specified, are conventional, and the experimental materials used in the following examples, unless otherwise specified, are commercially available.
Example 1
The embodiment provides a preparation method of a solid-state battery based on a liquid gallium tin alloy negative electrode, which specifically comprises the following steps:
(1) Taking 75mg of metallic gallium, removing an oxide film, adding 25mg of metallic tin, and heating to 220 ℃ to obtain 100mg of liquid gallium-tin alloy. And (3) placing a base material into a die with the diameter of 15mm, adding liquid gallium-tin alloy, pressing into a tablet, keeping the pressure at 200MPa, and maintaining the pressure for 3 minutes to obtain the liquid gallium-tin alloy cathode.
(2) 70mg Li is taken 10 GeP 2 S 12 The powder was pressed with a die having a diameter of 15mm under a pressure of 80MPa for 2 minutes to obtain a solid electrolyte sheet.
(3) 30mg of LiNi is taken 8 Co 1 Mn 1 O 2 Positive electrode material, 40mg Li 10 GeP 2 S 12 Mixing the solid electrolyte with 10mg of carbon black, and ball milling for 5 hours to obtain the nickel cobalt lithium manganate anode.
114.8mg of lithium sulfide and 560mg of elemental sulfur were taken and 10mL of 1M L was addediTFSI(DME:DOL＝1:1,with 1wt％LiNO 3 ) After ultrasonic dispersion for 30 minutes, magnetically stirring for 48 hours to obtain a liquid positive electrode.
(4) And pressing the liquid gallium tin alloy cathode on one side of the solid electrolyte sheet, wherein the pressure is 80MPa, and maintaining the pressure for 2 minutes. And pressing 10mg of nickel cobalt lithium manganate anode on the other side of the solid electrolyte sheet, wherein the pressure is 80MPa, and the pressure is maintained for 2 minutes. Or 20 mu L of liquid positive electrode is dripped on the other side of the solid electrolyte sheet, a current collector is covered on the liquid positive electrode, the button cell is assembled, and the electrochemical performance of the button cell is tested.
Example 2
The embodiment provides a preparation method of a solid-state battery based on a liquid gallium tin alloy negative electrode, which specifically comprises the following steps:
(1) Taking 92mg of metallic gallium, removing an oxide film, adding 8mg of metallic tin, and heating to 220 ℃ to obtain 100mg of liquid gallium-tin alloy. And (3) placing a base material into a die with the diameter of 15mm, adding liquid gallium-tin alloy, pressing into a tablet, keeping the pressure at 200MPa, and maintaining the pressure for 3 minutes to obtain the liquid gallium-tin alloy cathode.
(2) 70mg Li is taken 10 GeP 2 S 12 The powder was pressed with a die having a diameter of 15mm under a pressure of 80MPa for 2 minutes to obtain a solid electrolyte sheet.
(3) 60mg of LiNi is taken 8 Co 1 Mn 1 O 2 Positive electrode material, 80mg Li 10 GeP 2 S 12 Mixing the solid electrolyte with 20mg of carbon black, and ball milling for 5 hours to obtain the nickel cobalt lithium manganate anode.
114.8mg of lithium sulfide and 560mg of elemental sulfur were taken and 10mL of 1M LiTFSI (DME: DOL= 1:1,with 1wt%LiNO) was added 3 ) After ultrasonic dispersion for 30 minutes, magnetically stirring for 48 hours to obtain a liquid positive electrode.
(4) And pressing the liquid gallium tin alloy cathode on one side of the solid electrolyte sheet, wherein the pressure is 80MPa, and maintaining the pressure for 2 minutes. And pressing 10mg of nickel cobalt lithium manganate anode on the other side of the solid electrolyte sheet, wherein the pressure is 80MPa, and the pressure is maintained for 2 minutes. Or 20 mu L of liquid positive electrode is dripped on the other side of the solid electrolyte sheet, a current collector is covered on the liquid positive electrode, the button cell is assembled, and the electrochemical performance of the button cell is tested.
The embodiments of the present invention have been described in detail above, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, and yet fall within the scope of the invention.
Claims (10)
1. A solid-state battery is characterized by comprising a liquid gallium tin alloy anode, a solid electrolyte, a nickel cobalt lithium manganate anode or a liquid Li 2 S 8 A positive electrode;
the liquid gallium-tin alloy cathode contains gallium-tin alloy generated by the proportional reaction of metallic gallium and metallic tin; the mass ratio of the gallium metal to the tin metal is (3-11.5): 1.
2. the solid state battery of claim 1, wherein the solid state electrolyte comprises Li 10 GeP 2 S 12 、Li 0.33 La 0.57 TiO 3 、Li 7 La 3 Zr 2 O 12 At least one of them.
3. The solid state battery of claim 1, wherein the lithium nickel cobalt manganese oxide positive electrode comprises LiNi 8 Co 1 Mn 1 O 2 。
4. The solid-state battery according to claim 1, wherein the liquid Li 2 S 8 The anode is polysulfide synthesized by lithium sulfide and elemental sulfur.
5. A method of manufacturing a solid-state battery according to any one of claims 1 to 4, comprising the steps of:
(1) Manufacturing a liquid gallium-tin alloy cathode;
(2) Manufacturing a solid electrolyte sheet;
(3) Manufacturing an anode;
(4) Liquid stateThe gallium-tin alloy anode is pressed at one side of a solid electrolyte sheet, and nickel cobalt lithium manganate anode or liquid Li 2 S 8 And the positive electrode is added on the other side of the solid electrolyte sheet to assemble the solid battery.
6. The method for manufacturing a solid-state battery according to claim 5, wherein the step (1) specifically comprises the steps of: mixing gallium and tin, heating to obtain liquid gallium-tin alloy, putting a base material into a mould, adding the liquid gallium-tin alloy, and pressing into a tablet to obtain the liquid gallium-tin alloy cathode.
7. The method of manufacturing a solid-state battery according to claim 5, wherein when the positive electrode is a lithium nickel cobalt manganese oxide positive electrode, the step (3) specifically comprises the steps of: liNi is added to 8 Co 1 Mn 1 O 2 、Li 10 GeP 2 S 12 And mixing and ball milling with carbon black to obtain the nickel cobalt lithium manganate anode.
8. The method for manufacturing a solid-state battery according to claim 7, wherein the LiNi 8 Co 1 Mn 1 O 2 、Li 10 GeP 2 S 12 And the mass ratio of the carbon black is (2-4): (3-5): 1.
9. the method for producing a solid-state battery according to claim 7, wherein the time of ball milling is 4.5 to 5.5 hours.
10. The method for manufacturing a solid-state battery according to claim 5, wherein when the positive electrode is liquid Li 2 S 8 In the positive electrode, the step (3) specifically includes the following steps: adding LiTFSI solution into lithium sulfide and elemental sulfur, and stirring until the solution is completely dissolved after ultrasonic dispersion to obtain the liquid Li 2 S 8 And a positive electrode.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311043248.1A CN116864782A (en) | 2023-08-18 | 2023-08-18 | Solid-state battery based on liquid gallium tin alloy negative electrode and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311043248.1A CN116864782A (en) | 2023-08-18 | 2023-08-18 | Solid-state battery based on liquid gallium tin alloy negative electrode and preparation method thereof |
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| Publication Number | Publication Date |
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| CN116864782A true CN116864782A (en) | 2023-10-10 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202311043248.1A Pending CN116864782A (en) | 2023-08-18 | 2023-08-18 | Solid-state battery based on liquid gallium tin alloy negative electrode and preparation method thereof |
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| Country | Link |
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| CN (1) | CN116864782A (en) |
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2023
- 2023-08-18 CN CN202311043248.1A patent/CN116864782A/en active Pending
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