CN111525205B - Lithium ion battery containing lithium lanthanum zirconium oxygen three electrodes and preparation method thereof - Google Patents
Lithium ion battery containing lithium lanthanum zirconium oxygen three electrodes and preparation method thereof Download PDFInfo
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- CN111525205B CN111525205B CN202010350610.XA CN202010350610A CN111525205B CN 111525205 B CN111525205 B CN 111525205B CN 202010350610 A CN202010350610 A CN 202010350610A CN 111525205 B CN111525205 B CN 111525205B
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M10/05—Accumulators with non-aqueous electrolyte
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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
- H01M10/48—Accumulators combined with arrangements for measuring, testing or indicating the condition of cells, e.g. the level or density of the electrolyte
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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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
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Abstract
The invention relates to the field of lithium ion batteries, and discloses a lithium ion battery containing a lithium lanthanum zirconium oxygen three-electrode, which comprises an electric core and a shell, wherein the electric core comprises a negative plate, a negative pole lug, a diaphragm, a positive plate, a positive pole lug and a reference electrode, the reference electrode is arranged between the negative plate and the shell on the outermost side, and the reference electrode consists of a lithium lanthanum zirconium oxygen hollow shell, metal lithium and a leading-out electrode.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a lithium lanthanum zirconium oxygen three-electrode lithium ion battery and a preparation method thereof.
Background
A common three-electrode battery in the market is formed by embedding a lithium-melting metal wire (silver, gold, copper, etc.) in the battery. And a lithium melting metal wire is inserted between the diaphragm and the negative plate, and the other end of the metal wire is welded with a reference electrode tab.
The disadvantage of embedding the metal wire as the reference electrode is that the metal wire is arranged between the anode and the cathode and is inevitably subjected to Li in the charging and discharging process+The Li metal on the surface of the alloy is easy to consume and the service life of the alloy is short. And the pole piece near the embedded metal wire area is pressed and other areas are uneven, which easily causes the fluctuation of electrochemical performance. Therefore, the method can only be used for short-term research on the positive and negative electrode potentials and cannot be used for a long time in the whole life cycle of the battery.
Disclosure of Invention
In view of the above problems, the present invention provides a lithium ion battery containing three lithium lanthanum zirconium oxygen electrodes and a preparation method thereof, which can ensure the long-term stability of LLZO in the battery cell.
In order to achieve the purpose, the invention adopts a technical scheme that:
the utility model provides a lithium ion battery who contains lithium lanthanum zirconium oxygen three electrode, includes shell and electric core, electric core includes negative pole piece, negative pole utmost point ear, diaphragm, positive plate, anodal utmost point ear, reference electrode arranges in between the negative pole piece in the outside and the shell, its characterized in that reference electrode comprises lithium lanthanum zirconium oxygen hollow shell, lithium metal and the derivation utmost point.
Further, the lithium lanthanum zirconium oxygen hollow shell is wrapped with metal lithium.
Further onThe component of the lithium lanthanum zirconium oxygen hollow shell is Li7-xLa3Zr2-xMxO12Wherein M is one of Nb, Ta, Hf, Al, Si and Ga, and x is more than or equal to 0 and less than or equal to 2.
Further, the Li7-xLa3Zr2-xMxO12，According to the mol ratio of Li, La, Zr and M in the chemical formula, LiOH H is selected2O or Li2CO3、La2O3Or La (OH)3、ZrO2And M2O5As raw materials, wherein M is one of Nb, Ta, Hf, Al, Si and Ga, and x is more than or equal to 0 and less than or equal to 2.
Furthermore, the lithium lanthanum zirconium oxygen hollow shell has the size of 50-70mm in length, 30-50mm in width and 0.5-3mm in thickness.
Further, the lead-out electrode is at least one of a Cu sheet, an Al sheet, and a Ni sheet.
In order to achieve the above object, the present invention further provides a method for preparing the lithium ion battery containing the lithium lanthanum zirconium oxygen triple electrode, comprising:
the method comprises the following steps:
s1 preparation of Li7-xLa3Zr2-xMxO12Ball milling lithium lanthanum zirconium oxygen solid electrolyte in alcohol medium for 24 hr;
s2, drying the ball-milled lithium lanthanum zirconium oxide solid electrolyte;
s3, calcining the dried lithium lanthanum zirconium oxygen solid electrolyte at the temperature of 900-1100 ℃ for 6-24 hours at the heating rate of 1-5 ℃/min to obtain Li7-xLa3Zr2-xMxO12(LLZO) ceramic powder;
s4, tabletting the LLZO ceramic powder to obtain a ceramic green body;
s5: and (3) vertically pressurizing the ceramic green body by 5-40MPa, heating up at the rate of 1-5 ℃/min, and keeping the temperature at the constant temperature of 1100 ℃ and 1250 ℃ for 1-3 hours to obtain the ceramic solid electrolyte with the density of 99%.
S6: the ceramic solid electrolyte is made into a lithium lanthanum zirconium oxygen hollow shell.
S7: lithium metal is plugged into the LLZO hollow shell and heated to 185-220 ℃ under an inert atmosphere to melt the Li. One end of the lead-out electrode is plugged into the molten Li, and the other end of the lead-out electrode is extended to the shell.
S8: after cooling to room temperature, the hollow shell opening was sealed to form LLZO @ Li.
Further, the metallic lithium can be replaced by at least one of alloy of Li, Sn and In or lithium-intercalated graphite, LiPO4, NMC and LTO.
Further, the number of layers of the LLZO @ Li may be one or more
Further, the inert gas is at least one of helium (He), neon (Ne), argon (Ar), krypton (Kr), and xenon (Xe).
Compared with the prior art, the invention has the beneficial effects that:
the lithium metal embedded in the high-density ceramic LLZO shell is used as the three electrodes, so that the long-term stability and reliability of the reference electrode are greatly improved. The potential change in the life cycle of the battery cell can be continuously monitored according to the potential difference between the electrode and the positive and negative electrodes, and important parameters such as the SOH of the battery cell can be analyzed according to the potential change. The shell size of the LLZO is consistent with that of the negative pole piece, so that the stress uniformity is ensured, and unnecessary performance attenuation caused by uneven stress is avoided. The electrochemical stability of the LLZO ensures that the LLZO can exist stably in the battery cell for a long time, and meanwhile, the high compactness of the LLZO prevents the electrolyte from being in direct contact with the metal lithium, so that the long-term stability of the metal lithium is ensured, and a long-term reliable reference potential is provided.
Drawings
One or more embodiments are illustrated by way of example in the accompanying drawings, which correspond to the figures in which like reference numerals refer to similar elements and which are not to scale unless otherwise specified.
FIG. 1 is a schematic structural view of the present invention;
fig. 2 is a schematic view of a tab position structure of the present invention;
FIG. 3 is a schematic structural diagram of a lithium lanthanum zirconium oxide solid electrolyte according to the present invention;
in the figure:
1. outer casing
2. Battery cell
21. Negative plate
22. Negative pole tab
41. Positive plate
42. Positive pole ear
5. A reference electrode is arranged on the substrate,
51. lithium lanthanum zirconium oxygen hollow shell
52. Metallic lithium
53. Lead-out pole
Detailed Description
The present invention is further illustrated by the following examples, it being understood that the specific embodiments described herein are merely illustrative and explanatory of the invention and are not restrictive thereof.
Example 1
Referring to fig. 1 to fig. 3, the lithium ion battery including the li-la-zr-o three-electrode in the present embodiment includes a housing 1 and a battery cell 2, wherein the battery cell 2 includes a negative electrode tab 21, a negative electrode tab 22, a separator (not shown), a positive electrode tab 41, a positive electrode tab 42, and a reference electrode 5, wherein the negative electrode tab 22 is at the rightmost side, the lead-out electrode 52 is in the middle, the positive electrode tab 42 is at the leftmost side, and three electrodes are on the same side. Wherein the reference electrode 5 is disposed between the outermost negative electrode tab 21 and the can 1. The reference electrode 5 is composed of a lithium lanthanum zirconium oxygen hollow shell 51, a metal lithium 52, and a lead-out electrode 53, and further, the lithium lanthanum zirconium oxygen hollow shell 51 is wrapped with the metal lithium 52.
Further, the composition of the lithium lanthanum zirconium oxygen hollow shell 51 is Li7-xLa3Zr2-xMxO12， Li7-xLa3Zr2-xMxO12，According to the mol ratio of Li, La, Zr and M in the chemical formula, LiOH H is selected2O or Li2CO3、La2O3Or La (OH)3、ZrO2And M2O5As raw materials, wherein M is one of Nb, Ta, Hf, Al, Si and Ga, and x is more than or equal to 0 and less than or equal to 2. In this example, M is specifically selected to be Nb, X is 1, the molar ratio of Li, La, Zr and M in the formula is 6:3:1:1:12, LiOH. H is selected2O、La2O33、ZrO2And Nb2O5As a raw material, wherein LiOH. H2Excess of O was 15%, and the mixture was put into a container, mixed, heated and dried.
Mixing Li6La3ZrNbO12Ball milling in alcohol medium for 24 hr, stoving the ball milled Li-La-Zr-O, calcining at 900-1100 deg.c for 6-24 hr at 1-5 deg.c/min to obtain Li7-xLa3Zr2-xMxO12(LLZO) ceramic powder; in this example, Li La Zr O was calcined at 1000 deg.C for 20 hours at a heating rate of 3 deg.C/min to obtain Li6La3ZrNbO12(LLZO) ceramic powder, tabletting the LLZO ceramic powder to obtain a ceramic green compact; then vertically pressurizing the ceramic green body for 5-40MPa, heating up at a rate of 1-5 ℃/min, and keeping the temperature at a constant temperature of 1100 ℃ and 1250 ℃ for 1-3 hours to obtain a ceramic solid electrolyte with the density of 99%; in this embodiment, specifically, a ceramic green body is vertically pressurized at 35MPa, the heating rate is 3 ℃/min, and the temperature is maintained at 1200 ℃ for 2 hours, so as to obtain a ceramic solid electrolyte with a density of 99%.
Further, the lithium lanthanum zirconium oxygen hollow shell with the size of 50-70mm in length, 30-50mm in width and 0.5-3mm in thickness, in the embodiment, the specific size of 60mm in length, 40mm in width and 2.5mm in thickness is plugged with metal lithium in the LLZO hollow shell, and the lithium is heated to 185-220 ℃ in the atmosphere of inert argon gas to melt the Li; in this example, Li was melted by heating to 210 ℃. One end of the lead-out electrode is plugged into the molten Li, and the other end of the lead-out electrode is extended to the shell. After cooling to room temperature, the hollow shell opening was sealed to form LLZO @ Li. In another embodiment, the metal lithium may be replaced by at least one of Li, Sn and In, or lithium intercalation graphite, LiPO4, NMC, LTO, which is not limited In this embodiment.
Further, the lead-out electrode is at least one of a Cu sheet, an Al sheet, and a Ni sheet, which is not limited in this embodiment.
Further, the inert gas is at least one of helium (He), neon (Ne), argon (Ar), krypton (Kr), and xenon (Xe), which is not limited in this embodiment.
In the embodiment, the lithium metal is embedded in the high-density ceramic LLZO shell to serve as the three electrodes, so that the long-term stability and reliability of the reference electrode are greatly improved. The shell size of the LLZO is consistent with that of the negative pole piece, so that the stress uniformity is ensured, and unnecessary performance attenuation caused by uneven stress is avoided. The electrochemical stability of the LLZO ensures that the LLZO can exist stably in the battery cell for a long time, and meanwhile, the high compactness of the LLZO prevents the electrolyte from being in direct contact with the metal lithium, so that the long-term stability of the metal lithium is ensured, and a long-term reliable reference potential is provided.
Example 2
Referring to fig. 1 to fig. 3, the lithium ion battery including three lithium lanthanum zirconium oxygen electrodes in the present embodiment includes a housing 1 and a battery cell 2, wherein the battery cell 2 includes a negative electrode tab 21, a negative electrode tab 22, a separator (not shown), a positive electrode tab 41, a positive electrode tab 42, and a reference electrode 5, wherein the negative electrode tab 22 is at the rightmost side, a lead-out electrode 52 is in the middle, the positive electrode tab 42 is at the leftmost side, and three electrodes are on the same side. Wherein the reference electrode 5 is disposed between the outermost negative electrode tab 21 and the can 1. The reference electrode 5 is composed of a lithium lanthanum zirconium oxygen hollow shell 51, a metal lithium 52, and a lead-out electrode 53, and further, the lithium lanthanum zirconium oxygen hollow shell 51 is wrapped with the metal lithium 52.
Further, the composition of the lithium lanthanum zirconium oxygen hollow shell 51 is Li7-xLa3Zr2-xMxO12， Li7-xLa3Zr2-xMxO12，According to the mol ratio of Li, La, Zr and M in the chemical formula, LiOH H is selected2O or Li2CO3、La2O3Or La (OH)3、ZrO2And M2O5As raw materials, wherein M is one of Nb, Ta, Hf, Al, Si and Ga, and x is more than or equal to 0 and less than or equal to 2. In this example, M is Nb, X is 0.5, the molar ratio of Li, La, Zr and M in the formula is 5.5:3:0.5:1.5:12, LiOH. H is selected2O、La2O3、ZrO2And Nb2O5As a raw material, wherein LiOH. H2O is excessive by 13%, and the mixture is put into a container to be mixed, heated and dried.
Mixing Li5.5La3Zr0.5Nb1.5O12，Ball milling in alcohol medium for 24 hr, stoving the ball milled Li-La-Zr-O, calcining at 900-1100 deg.c for 6-24 hr at 1-5 deg.c/min to obtain Li7-xLa3Zr2-xMxO12(LLZO) ceramic powder; in this example, Li La Zr O was calcined at 1000 deg.C for 20 hours at a heating rate of 3 deg.C/min to obtain Li5.5La3Zr0.5Nb1.5O12(LLZO) ceramic powder, tabletting the LLZO ceramic powder to obtain a ceramic green compact; then vertically pressurizing the ceramic green body for 5-40MPa, heating up at a rate of 1-5 ℃/min, and keeping the temperature at a constant temperature of 1100 ℃ and 1250 ℃ for 1-3 hours to obtain a ceramic solid electrolyte with the density of 99%; in this embodiment, specifically, a ceramic green body is vertically pressurized at 35MPa, the heating rate is 3 ℃/min, and the temperature is maintained at 1200 ℃ for 2 hours, so as to obtain a ceramic solid electrolyte with a density of 99%.
The length and width of the lithium lanthanum zirconium oxygen hollow shell are determined according to the size of the pole piece of the matched battery core.
Further, the lithium lanthanum zirconium oxygen hollow shell with the size of 50-70mm in length, 30-50mm in width and 0.5-3mm in thickness, in the embodiment, the specific size of the lithium lanthanum zirconium oxygen hollow shell with the length of 55mm, 45mm in width and 3mm in thickness is plugged with an alloy sheet of Li and Sn in the LLZO hollow shell, and is heated to 185-220 ℃ in the atmosphere of inert argon gas to melt the Li and Sn; in this example, the alloy is melted by heating to 210 ℃. One end of the lead-out pole is plugged into the molten alloy, and the other end is extended to the shell. After cooling to room temperature, the hollow shell opening was sealed to form the LLZO @ alloy. In another embodiment, the metallic lithium may be replaced by at least one of Li, Sn and In, or an alloy of Li, Sn and In, or embedded lithium graphite, LiPO4, NMC, LTO, which have a potential different from that of the lithium metal, but are placed inside the LLZO to ensure a stable potential, which also can serve as a reference electrode, and this embodiment is not limited. Furthermore, the placement position of LLZO @ Li can replace any pole piece position in the battery cell, and the function performance of the battery cell is not influenced.
Further, the lead-out electrode is at least one of a Cu sheet, an Al sheet, and a Ni sheet, which is not limited in this embodiment.
Further, the inert gas is at least one of helium (He), neon (Ne), argon (Ar), krypton (Kr), and xenon (Xe), which is not limited in this embodiment.
In the embodiment, the alloy sheet embedded with Li and Sn in the high-density ceramic LLZO shell is used as the three electrodes, so that the long-term stability and reliability of the reference electrode are greatly improved. The shell size of the LLZO is consistent with that of the negative pole piece, so that the stress uniformity is ensured, and unnecessary performance attenuation caused by uneven stress is avoided. The electrochemical stability of the LLZO ensures that the LLZO can exist stably in the battery cell for a long time, and meanwhile, the high compactness of the LLZO prevents the electrolyte from being in direct contact with the metal lithium, so that the long-term stability of the metal lithium is ensured, and a long-term reliable reference potential is provided.
Li of the invention7-xLa3Zr2-xMxO12(LLZO) is an ion conductor of garnet structure due to its high ionic conductance (about 10 at room temperature)-3S/cm), high lithium ion mobility coefficient, high electrochemical stability, and good chemical stability for the positive electrode material and the lithium metal negative electrode.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention is subject to the protection scope of the claims.
Claims (5)
1. The lithium ion battery containing the lithium lanthanum zirconium oxygen three electrodes is characterized by comprising a shell and an electric core, wherein the electric core comprises a negative plate, a negative electrode tab, a diaphragm, a positive plate, a positive electrode tab and a reference electrode, the reference electrode is arranged between the negative plate on the outermost side and the shell and consists of a lithium lanthanum zirconium oxygen hollow shell, metal lithium and a leading-out electrode, the lithium lanthanum zirconium oxygen hollow shell wraps the metal lithium, and the lithium lanthanum zirconium oxygen hollow shell is 50-70mm long, 30-50mm wide and 0.5-3mm thick; of said lithium lanthanum zirconium oxygen hollow shellThe component is Li7-xLa3Zr2-xMxO12The Li7-xLa3Zr2-xMxO12According to the mol ratio of Li, La, Zr and M in the chemical formula, LiOH H is selected2O or Li2CO3、La2O3Or La (OH)3、ZrO2And M2O5As raw materials, wherein M is one of Nb, Ta, Hf, Al, Si and Ga, and x is more than or equal to 0 and less than or equal to 2.
2. A method of making a lithium lanthanum zirconium oxygen triple electrode-containing lithium ion battery as claimed in claim 1, comprising the steps of:
s1: mixing Li7-xLa3Zr2-xMxO12Ball milling lithium lanthanum zirconium oxide in alcohol medium for 24 hr;
s2: drying the ball-milled lithium lanthanum zirconium oxide;
s3: calcining the dried lithium lanthanum zirconium oxygen at the temperature of 900-7- xLa3Zr2-xMxO12(LLZO) ceramic powder;
s4: tabletting the LLZO ceramic powder to obtain a ceramic green body;
s5: vertically pressurizing the ceramic green body at 5-40MPa, heating up at a rate of 1-5 ℃/min, and keeping the temperature at 1100 ℃ and 1250 ℃ for 1-3 hours to obtain a ceramic solid electrolyte with the density of 99%;
s6: manufacturing a ceramic solid electrolyte into a lithium lanthanum zirconium oxygen hollow shell;
s7: filling metal lithium into the LLZO hollow shell, heating to 185-220 ℃ under inert gas to melt the Li, filling one end of a lead-out electrode into the molten Li, and extending the other end of the lead-out electrode to the shell;
s8: after cooling to room temperature, the hollow shell opening was sealed to form LLZO @ Li.
3. The method of claim 2, wherein the metallic lithium is replaced with an alloy of at least one of Li, Sn and In, or lithium-intercalated graphite, LiPO4、NMC、LTO。
4. The method of claim 3, wherein the LLZO @ Li is in one or more layers.
5. The method of claim 4, wherein the inert gas is at least one of helium (He), neon (Ne), argon (Ar), krypton (Kr), and xenon (Xe).
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