CN114678510A - Selenium-coated disordered lithium-rich material and preparation method thereof - Google Patents
Selenium-coated disordered lithium-rich material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 73
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 63
- 239000011669 selenium Substances 0.000 title claims abstract description 49
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910052711 selenium Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 6
- 239000011247 coating layer Substances 0.000 claims abstract description 5
- 238000001354 calcination Methods 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 12
- 229910052593 corundum Inorganic materials 0.000 claims description 12
- 239000010431 corundum Substances 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- 229910003002 lithium salt Inorganic materials 0.000 claims description 5
- 159000000002 lithium salts Chemical class 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 150000002751 molybdenum Chemical class 0.000 claims description 5
- 150000002815 nickel Chemical class 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000003837 high-temperature calcination Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000010405 anode material Substances 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- 229910001416 lithium ion Inorganic materials 0.000 description 7
- 239000003792 electrolyte Substances 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000010406 cathode material Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 2
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 229910003208 (NH4)6Mo7O24·4H2O Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910001290 LiPF6 Inorganic materials 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000006183 anode active material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 101150047356 dec-1 gene Proteins 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000006864 oxidative decomposition reaction Methods 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
Abstract
The invention discloses a selenium-coated disordered lithium-rich material and a preparation method thereof, wherein the disordered lithium-rich material is arranged inside the material, a selenium coating layer is arranged outside the material, and the chemical formula of the disordered lithium-rich material is Li1.2Ni1/ 3Ti1/3Mo2/15O2The mass fraction of Se in the selenium-coated disordered lithium-rich material is 0.5-5% of that of the disordered lithium-rich material. The selenium surface is coated and modified by the disordered lithium-rich anode material, so that the capacity attenuation and the voltage attenuation in the circulation process of the disordered lithium-rich anode can be effectively inhibited, and the preparation process is simple and easy to popularize.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to a selenium-coated disordered lithium-rich material and a preparation method thereof.
Background
Lithium ion batteries have high energy density and long cycle life and are considered to be an effective energy storage device. Nowadays, under the background of the vigorous promotion of new energy sources and the vigorous development of consumer electronics market in China, the development of novel positive electrode materials for creating lithium ion batteries with higher energy density is urgently needed. Among the anode materials meeting the conditions, the lithium-rich anode material is made out of the advantages of higher specific discharge capacity, low cost, high working voltage and the like.
Despite the outstanding energy density of lithium-rich cathode materials, their poor cycling stability and gas evolution at high voltages have limited their commercial application. Firstly, in a long-term circulation process, the surface structure of the lithium-rich cathode material is easy to deteriorate and is gradually changed into an inert rock salt phase from the surface to the inside, the discharge capacity is gradually reduced, and the circulation stability of the battery is seriously damaged. Secondly, under a higher working voltage of more than 4.5V, the interface side reaction of the electrolyte and the lithium-rich anode material is intensified, the problem of gas generation is particularly prominent at the moment, and the main components of the gas are oxygen and carbon dioxide which are respectively released from the surface lattice oxygen of the lithium-rich anode material and the oxidative decomposition of an ester solvent in the electrolyte, so that the safety performance of the battery is seriously damaged.
The preparation of novel disordered lithium-rich materials is an effective way to solve the above problems. At present, the preparation of disordered lithium-rich materials usually adopts a ball milling method, but the mixing uniformity is limited, the particle size is not uniform, and the material performance is influenced. Therefore, the method for preparing the disordered lithium-rich material with uniform particles and good performance is researched to have important significance.
Disclosure of Invention
Based on the problems in the prior art, the invention provides a selenium-coated disordered lithium-rich material and a preparation method thereof, aiming at realizing the uniformity of particle size by a sol-gel method, and simultaneously slowing down the corrosion of electrolyte to the surface of the material by a coating strategy, and reducing the degradation speed of the surface structure and the dissolution of surface ions.
The invention adopts the following technical scheme for realizing the purpose:
a selenium-coated disordered lithium-rich material is characterized in that: the disordered lithium-rich material coated by the selenium is internally provided with a disordered lithium-rich material, the outer coating layer is provided with the selenium, and the chemical formula of the disordered lithium-rich material is Li1.2Ni1/3Ti1/3Mo2/15O2And the mass fraction of Se in the selenium-coated disordered lithium-rich material is 0.5-5% of that of the disordered lithium-rich material.
The preparation method of the selenium-coated disordered lithium-rich material comprises the following steps:
step 1, adding lithium salt, nickel salt and molybdenum salt into ethanol, stirring for 0.5-1h to obtain a green transparent solution, and slowly dropwise adding C16H36O4Ti, performing constant-temperature oil bath reaction to form green gel, and performing vacuum drying to obtain precursor powder;
step 2, pouring the precursor powder into a corundum ark, placing the corundum ark in a tubular furnace, calcining at high temperature in air atmosphere, and cooling to room temperature to obtain black disordered lithium-rich material powder;
and 3, mixing the disordered lithium-rich material powder with selenium powder, ball-milling, pouring the mixture into a corundum ark, placing the corundum ark into a tubular furnace, calcining the mixture at a high temperature in an air atmosphere, and cooling the calcined mixture to room temperature to obtain the selenium-coated disordered lithium-rich material.
Further, lithium salt, nickel salt, C in step 116H36O4The molar ratio of Ti to molybdenum salt is 20-25:6:6: 2-5.
Further, in the step 1, the constant-temperature oil bath reaction is carried out by stirring for 10-24h in a constant-temperature oil bath at 70-90 ℃.
Further, in the step 1, the temperature of the vacuum drying is 70-90 ℃ and the time is 10-24 h.
Further, in step 2, the temperature rise rate of the high-temperature calcination is 2-10 ℃/min, the calcination temperature is 500-900 ℃, and the calcination time is 3-10 h.
Further, in step 3, the ball milling method comprises the following steps: according to the mass ratio of ball materials of 5-15: 1, placing the mixture in a zirconia ball milling tank for ball milling for 1-6 h.
Further, in step 3, the temperature rise rate of the high-temperature calcination is 2-10 ℃/min, the calcination temperature is 200-400 ℃, and the calcination time is 2-8 h.
Further, in step 1: the lithium salt may be CH3COOLi·2H2O; the nickel salt can be selected from (CH)3COO)2Ni·4H2O; the molybdenum salt can be selected from (NH)4)6Mo7O24·4H2O。
The selenium-coated disordered lithium-rich material obtained by the invention can be used as a battery anode material to be applied to a lithium ion battery.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention adopts selenium surface coating modified disordered lithium-rich cathode material: on one hand, the coating layer can play a physical shielding role to block the direct action of the disordered lithium-rich material and the electrolyte; on the other hand, the coating layer can eliminate free radicals generated under high pressure, and inhibit side reactions at an electrode/electrolyte interface from the aspects of physical shielding and chemical blocking. Therefore, after the selenium coating is carried out, the capacity attenuation and the voltage attenuation in the cycle process of the disordered lithium-rich anode can be effectively inhibited. The electrochemical test of the lithium ion battery is carried out on the selenium-coated disordered lithium-rich material, and the result shows that the selenium-coated disordered lithium-rich material is 1.5-4.8V and 20mA g-1After the current density of the lithium ion battery is cycled for 50 times, the specific discharge capacity of the lithium ion battery is 169.1mAh g-1While the uncoated disordered lithium-rich positive electrode has only 43.2mAh g-1The capacity retention rate is improved by 291.4%.
2. The invention prepares the disordered lithium-rich material by a sol-gel method, and the particle size is uniform.
3. The preparation process is simple and easy to popularize.
Drawings
FIG. 1 shows the Se-coated disordered Li-rich material and uncoated material obtained in example 1 (i.e., Li obtained in step 2)1.2Ni1/ 3Ti1/3Mo2/15O2) X-ray diffraction pattern of (a).
FIG. 2 shows the Se-coated disordered Li-rich material obtained in example 1 at 20mA g-1And (3) a charge-discharge specific capacity curve of 50 times of circulation under the current density.
FIG. 3 shows the uncoated material obtained in example 1 at 20mA g-1And (3) a charge-discharge specific capacity curve of 50 times of circulation under the current density.
FIG. 4 shows the Se-coated disordered Li-rich material and uncoated material obtained in example 1 at 20mA g-1Discharge specific capacity curve of 50 cycles at current density.
Detailed Description
The following examples are given to illustrate the present invention, and the following examples are carried out on the premise of the technical solution of the present invention, and give detailed embodiments and specific procedures, but the scope of the present invention is not limited to the following examples.
The raw materials and instruments used in the following examples are commercially available.
Example 1
This example prepared a selenium-coated disordered lithium rich material (LiTiNiMoO @ 1% wt Se) with a disordered lithium rich material inside and selenium as the outer coating, where the disordered lithium rich material has the chemical formula Li1.2Ni1/3Ti1/3Mo2/15O2The selenium-coated disordered lithium-rich material comprises 1% of Se by mass and comprises the following specific steps:
step 1, respectively weighing chemically pure 3.222g CH3COOLi·2H2O、2.080g(CH3COO)2Ni·4H2O、0.589g(NH4)6Mo7O24·4H2O, adding 50mL of ethanol, stirring for 0.5h to obtain a green transparent solution, and slowly adding 2.906mL of C dropwise16H36O4And (3) Ti, stirring in a constant-temperature oil bath at 80 ℃ for 12h to form green gel, and vacuum drying at 80 ℃ for 12h to obtain precursor powder.
Step 2, pouring precursor powder into a corundum ark, placing the corundum ark in a tube furnace, controlling the heating rate to be 2 ℃/min under the air atmosphere, heating to 600 ℃, calcining for 5h, and cooling to room temperature to obtain the disordered lithium-rich material (Li)1.2Ni1/3Ti1/3Mo2/ 15O2) And (3) powder.
And 3, mixing and ball-milling 1g of disordered lithium-rich material powder and 0.01g of selenium powder (the mass ratio of ball materials is 15: 1, placing the mixture in a zirconia ball-milling tank for ball milling for 4 hours), then pouring the mixture into a corundum ark, placing the corundum ark in a tubular furnace, controlling the heating rate to be 2 ℃/min under the air atmosphere, heating to 280 ℃, calcining for 4 hours, and cooling to room temperature to obtain the selenium-coated disordered lithium-rich material, which is recorded as LiTiNiMoO @ 1% wt Se.
The LiTiNiMoO @1 wt% Se material obtained in the embodiment is used as a lithium ion battery anode active material, and the specific mode is as follows: mixing an active material with acetylene black and polyvinylidene fluoride (PVDF) according to a mass ratio of 8:1:1, adding N-methylpyrrolidone (NMP) as a solvent, stirring for 12 hours to form slurry, then uniformly coating the slurry on an aluminum foil, and drying in a drying box at 80 ℃ for 12 hours to obtain the positive plate. In a glove box filled with argon, the cut pole piece is a positive pole, the metal lithium piece is a negative pole, and 1.0M LiPF6DMC DEC 1:1:1 as electrolyte, assembled into button cells in an argon filled glove box. The charge and discharge test is carried out on a Land test system, all test voltages range from 1.5V to 4.8V, and the cycle performance adopts 20mA g-1The current density of (3) was charged and discharged 50 times.
Example 2
This example prepared a selenium-coated disordered lithium rich material (LiTiNiMoO @ 5% wt Se) having an interior of disordered lithium rich material and an outer coating of selenium, wherein the disordered lithium rich material has the chemical formula Li1.2Ni1/3Ti1/3Mo2/15O2The mass fraction of Se in the selenium-coated disordered lithium-rich material is 5% of that of the disordered lithium-rich material, and the specific steps are the same as those in example 1, except that the mass of the selenium powder in step 3 is 0.05 g.
FIG. 1 shows the Se-coated disordered Li-rich material and uncoated material obtained in example 1 (i.e., Li obtained in step 2)1.2Ni1/ 3Ti1/3Mo2/15O2) X-ray diffraction pattern of (a).
FIG. 2 shows the Se-coated disordered Li-rich material obtained in example 1 at 20mA g-1The charge-discharge specific capacity curve of 50 cycles under the current density is shown in FIG. 3, which is the uncoated material at 20mA g-1Charging and discharging under current density for 50 timesFIG. 4 shows the specific capacity curves of the Se-coated disordered Li-rich material and the uncoated material obtained in example 1 at 20mA g-1Discharge specific capacity curve of 50 cycles under current density. As can be seen from the figure: at 1.5-4.8V and 20mA g-1After the current density of the material is cycled for 50 times, the specific discharge capacity of the selenium-coated disordered lithium-rich material is 169.1mAh g-1While the uncoated disordered lithium-rich material had only 43.2mAh g-1The capacity retention rate is improved by 291.4%. The result shows that the selenium coating strategy can obviously inhibit the problems of capacity attenuation and voltage attenuation of the disordered lithium-rich anode in the circulating process, and effectively improve the circulating performance of the material.
The above-described examples are merely illustrative of several embodiments of the present invention and are not intended to be limiting thereof. It should be noted that, for those skilled in the art, various modifications and alterations can be made to the present invention without departing from the concept of the technical principle of the present invention, and these modifications and alterations belong to the protection scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (8)
1. A selenium-coated disordered lithium-rich material, characterized in that: the disordered lithium-rich material coated by the selenium is internally provided with a disordered lithium-rich material, the outer coating layer is provided with the selenium, and the chemical formula of the disordered lithium-rich material is Li1.2Ni1/3Ti1/3Mo2/15O2And the mass fraction of Se in the selenium-coated disordered lithium-rich material is 0.5-5% of that of the disordered lithium-rich material.
2. The method for preparing the selenium-coated disordered lithium-rich material of claim 1, comprising the following steps:
step 1, adding lithium salt, nickel salt and molybdenum salt into ethanol, stirring for 0.5-1h to obtain transparent solution, and then dropwise adding C16H36O4Ti, performing oil bath reaction at constant temperature to form gel, and performing vacuum drying to obtain precursor powder;
step 2, pouring the precursor powder into a corundum ark, placing the corundum ark into a tube furnace, calcining at high temperature in air atmosphere, and cooling to room temperature to obtain disordered lithium-rich material powder;
and 3, mixing the disordered lithium-rich material powder with selenium powder, ball-milling, pouring the mixture into a corundum ark, placing the corundum ark into a tubular furnace, calcining the mixture at a high temperature in an air atmosphere, and cooling the calcined mixture to room temperature to obtain the selenium-coated disordered lithium-rich material.
3. The method of claim 2, wherein: in step 1, lithium salt, nickel salt, C16H36O4The molar ratio of Ti to molybdenum salt is 20-25:6:6: 2-5.
4. The method of claim 2, wherein: in the step 1, the constant-temperature oil bath reaction is carried out by stirring for 10-24h in a constant-temperature oil bath at 70-90 ℃.
5. The method of claim 2, wherein: in the step 1, the temperature of the vacuum drying is 70-90 ℃ and the time is 10-24 h.
6. The method of claim 2, wherein: in the step 2, the heating rate of the high-temperature calcination is 2-10 ℃/min, the calcination temperature is 500-900 ℃, and the calcination time is 3-10 h.
7. The method of claim 2, wherein: in step 3, the ball milling method comprises the following steps: according to the mass ratio of ball materials of 5-15: 1, placing the mixture in a zirconia ball milling tank for ball milling for 1-6 h.
8. The production method according to claim 2, characterized in that: in step 3, the heating rate of the high-temperature calcination is 2-10 ℃/min, the calcination temperature is 200-400 ℃, and the calcination time is 2-8 h.
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