CN109244549A - Method for preparing garnet electrolyte sheet with high density and high conductivity by guiding crystal growth - Google Patents
Method for preparing garnet electrolyte sheet with high density and high conductivity by guiding crystal growth Download PDFInfo
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- CN109244549A CN109244549A CN201811016882.5A CN201811016882A CN109244549A CN 109244549 A CN109244549 A CN 109244549A CN 201811016882 A CN201811016882 A CN 201811016882A CN 109244549 A CN109244549 A CN 109244549A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0562—Solid materials
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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
- H01M6/00—Primary cells; Manufacture thereof
- H01M6/14—Cells with non-aqueous electrolyte
- H01M6/18—Cells with non-aqueous electrolyte with solid electrolyte
- H01M6/185—Cells with non-aqueous electrolyte with solid electrolyte with oxides, hydroxides or oxysalts as solid electrolytes
- H01M6/186—Only oxysalts-containing solid electrolytes
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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
- H01M6/00—Primary cells; Manufacture thereof
- H01M6/14—Cells with non-aqueous electrolyte
- H01M6/18—Cells with non-aqueous electrolyte with solid electrolyte
- H01M6/188—Processes of manufacture
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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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
- H01M2300/0068—Solid electrolytes inorganic
- H01M2300/0071—Oxides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention provides a method for preparing a high-density and high-conductivity electrolyte sheet by guiding crystal growth, which comprises the following steps: fully ball-milling and roasting the raw materials for synthesizing the solid electrolyte powder, fully ball-milling and drying again, and then pressing into tablets by isostatic pressing and roasting at the temperature of 1000-; grinding the roasted electrolyte sheet to obtain electrolyte particles with a certain particle size, adding the electrolyte particles into solid electrolyte powder, uniformly mixing and grinding the electrolyte particles, performing isostatic pressing again to obtain the compact high-conductivity solid electrolyte sheet, and roasting the compact high-conductivity solid electrolyte sheet. The invention induces the formation and growth of crystal grains in the solid electrolyte by introducing the solid electrolyte crystal seeds, reduces the energy required by nucleation and crystal nucleus growth of the material, and reduces the temperature required by the densification of the solid electrolyte sheet. The low-temperature densification effectively inhibits the volatilization of lithium element in the solid electrolyte, the composition of the synthesized solid electrolyte is accurately controlled, and the solid electrolyte sheet with low impedance and high conductivity is prepared.
Description
Technical field
The invention belongs to field of batteries, and in particular to one kind has high-compactness, high conductivity solid electrolyte.
Background technique
With high conductivity (~10-4S/cm Li)7La3Zr2O12Garnet-type solid electrolyte has phase with metal Li
To stable interface, and there is good chemical stability in air, in high-energy density and the good all-solid-state battery of safety
There is good application prospect in research and development.Li7La3Zr2O12There are tetragonal phases and cubic phase, research shows that under high temperature easily
The cubic phase with high conductivity is synthesized, but occurs a certain amount of tetragonal phase in temperature-fall period.To stablize Li7La3Zr2O12Object phase,
Using Al3+、B3+、Ga3+、Ta5+Equal elements are doped, and are compared by result of study, Ta5+The resistate that is entrained in of ion is mutually tied
While structure, be conducive to the conductivity for improving solid electrolyte.Research is found: in solid electrolyte sheet, low consistency and a large amount of
The presence of crystal boundary makes electrolyte sheet produce high Intergranular impedance.To improve the consistency of solid electrolyte sheet, reducing crystal boundary,
Frequently with the optimization (such as: hot pressed sintering, SPS sintering, isostatic cool pressing, high temperature sintering) of preparation process and low-melting component (such as:
LiBO3, LiF) introducing.Preparation process after optimization uses high temperature and pressure, is unfavorable for the mass production of solid electrolyte sheet；
And the part after low-melting component introducing in solid electrolyte sheet generates high impedance phase, affects solid electrolyte to a certain extent
Body impedance.
Summary of the invention
In view of the above-mentioned problems, the present invention provides one kind can prepare pure phase, high-densit and high conductivity solid at low temperature
The method of electrolyte sheet.This method passes through the introducing of solid electrolyte crystal seed, induces the formation and length of crystal grain in solid electrolyte
Greatly, so that energy needed for reducing material forming core and nucleus growth, reduces the required temperature of solid electrolyte sheet densification；
Meanwhile effectively inhibiting the volatilization of elemental lithium in solid electrolyte, the accurate composition for controlling synthesis of solid electrolyte has prepared tool
There is the solid electrolyte of Low ESR, high conductivity, provides good basis for the preparation of all-solid-state battery.
Present example provides and a kind of can prepare pure phase at low temperature, is high-densit with high conductivity solid electrolyte sheet
Method, it is characterised in that the following steps are included:
(1) raw material needed for weighing by the stoichiometric ratio of garnet solid electrolyte powder composition, is added in ball grinder, is added suitable
Ball milling 6-15h after the grinding aid of amount, in 50-95 DEG C of dry 12h.
(2) powder obtained after drying is in 800-950 DEG C of roasting 6-20h.
(3) ball milling 5-10h after grinding aid is added in the powder burnt down again, after dry in 50-95 DEG C, by equal static pressure with
50-400Mpa pressure is pressed into disk.
(4) solid electrolyte sheet is placed on the high-purity corundum ceramic wafer for being covered with step (2) synthesis of solid electrolyte powder,
And buried solid electrolyte sheet using electrolyte powder, it is warming up to 1000-1100 DEG C with 2-10 DEG C/min, keeps the temperature 6-15h, is obtained
Garnet-type solid electrolyte piece.
(5) after grinding the solid electrolyte sheet in step (4), the solid electrolyte particle that partial size is 10-80 μm is obtained.
(6) the solid electrolyte powder that step (2) obtain is added in the electrolyte granular for screening different-grain diameter, and grinding aid is added
Afterwards, ball milling 5-10h, after 50-95 DEG C dry, by waiting static pressure to be pressed into disk with 50-400Mpa pressure.
(7) solid electrolyte sheet is placed on the high-purity corundum ceramic wafer for being covered with step (2) synthesis of solid electrolyte powder,
And buried solid electrolyte sheet using electrolyte powder, it is warming up to 1100-1200 DEG C with 4-10 DEG C/min, keeps the temperature 2-5h, cooling
To 1000-1100,4-9h is kept the temperature, obtains the garnet-type solid electrolyte piece of fine and close, high conductivity.
Garnet-type solid electrolyte group in step 1 of the present invention becomes Li5+xLa5-y-z-z’ZryTazMz’O12, 0 < x
≤ 2,0 < y+z+z '≤4.5, wherein M can be independently selected from the one of Nb, W, Ti, Hf, Ru, Mo, Nd, Ba, Ga, In, Ge, Sn, Sb, Se
Kind is several.
For step 1 of the present invention in synthesis of solid electrolyte powder, lithium source selects lithium hydroxide, lithium carbonate, lithium sulfate, nitre
Sour lithium, lithium acetate, lithium borate, lithium niobate, lithium dihydrogen phosphate；Lanthanum source selects lanthanum hydroxide, lanthanum carbonate, lanthanum sulfate, lanthanum nitrate, oxygen
Change lanthanum, lanthanum chloride, lanthanum nitrate；Tantalum source selects tantalum pentoxide, tantalic chloride.
Grinding aid in step 1 of the present invention is ethyl alcohol, propyl alcohol, isopropanol, n-butanol, isobutanol, the tert-butyl alcohol.
Advantages of the present invention: (1) by the introducing of solid electrolyte crystal seed, induce in solid electrolyte the formation of crystal grain with
It grows up, energy needed for reducing material forming core and nucleus growth reduces the required temperature of solid electrolyte sheet densification.
(2) low temperature densification effectively inhibits the volatilization of elemental lithium in solid electrolyte, the accurate composition for controlling synthesis of solid electrolyte, system
It is standby gone out the solid electrolyte with Low ESR, high conductivity.
Detailed description of the invention
The object phasor of synthesis of solid electrolyte sheet under Fig. 1 different temperatures.
The object phasor of solid electrolyte powder after Fig. 2 Ta, Nb doping.
Solid electrolyte sheet Cross Section Morphology figure after crystal seed is added in Fig. 3.
The bottom surface shape appearance figure of solid electrolyte sheet after crystal seed is added in Fig. 4, and scratch is sand polishing trace in figure.
The impedance spectrum of solid electrolyte sheet after Fig. 5 is adulterated by the difference that pre- kind of crystal seed obtains.
Specific embodiment
The technical solution in embodiment of the present invention will be clearly and completely described, but is not limited to following below
Embodiment.Based on the embodiment in the present invention, those skilled in the art are obtained without creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Embodiment 1
(1) garnet solid electrolyte powder Li is pressed6.4La3Zr1.4Ta0.6O12Raw material needed for the stoichiometric ratio of composition is weighed is added
Into ball grinder, ball milling 8h after suitable isopropanol is added, in 75 DEG C of dry 12h.
(2) powder obtained after drying is in 850 DEG C of roasting 10h.
(3) ball milling 5h after isopropanol is added in the powder burnt down again, after 75 DEG C dry, by waiting static pressure to press with 100Mpa
It forces and disk is made.
(4) solid electrolyte sheet is placed on the high-purity corundum ceramic wafer for being covered with step (2) synthesis of solid electrolyte powder,
And buried solid electrolyte sheet using electrolyte powder, 1000 DEG C are warming up to 2 DEG C/min, keeps the temperature 10h, it is solid to obtain carbuncle type
Body electrolyte sheet.
(5) after grinding the solid electrolyte sheet in step (4), partial size D is obtained50For 60 μm of solid electrolyte particle.
(6) the solid electrolyte powder that step (2) obtain is added in the electrolyte granular in (5), after isopropanol is added, ball milling
6h, after 75 DEG C dry, by waiting static pressure to be pressed into disk with 200Mpa pressure.
(7) solid electrolyte sheet is placed on the high-purity corundum ceramic wafer for being covered with step (2) synthesis of solid electrolyte powder,
And buried solid electrolyte sheet using electrolyte powder, 1200 DEG C are warming up to 5 DEG C/min, keeps the temperature 2h, is cooled to 1000 DEG C, is protected
Warm 4h obtains the garnet-type solid electrolyte piece of fine and close, high conductivity.
Embodiment 2
(1) garnet solid electrolyte powder Li is pressed6.4La3Zr1.4Ta0.3Nb0.3O12Raw material needed for the stoichiometric ratio of composition is weighed,
It is added in ball grinder, ball milling 10h after suitable grinding aid n-butanol is added, in 80 DEG C of dry 10h.
(2) powder obtained after drying is in 900 DEG C of roasting 10h.
(3) ball milling 6h after n-butanol is added in the powder burnt down again, after 80 DEG C dry, static pressure 100Mpa is waited to be pressed into circle
Piece.
(4) solid electrolyte sheet is placed on the high-purity corundum ceramic wafer for being covered with step (2) synthesis of solid electrolyte powder,
And buried solid electrolyte sheet using electrolyte powder, 1000 DEG C are warming up to 3 DEG C/min, keeps the temperature 10h, it is solid to obtain carbuncle type
Body electrolyte sheet.
(5) after grinding the solid electrolyte sheet in step (4), partial size D is obtained50For 60 μm of solid electrolyte particle.
(6) the solid electrolyte powder that step (2) obtain is added in the electrolyte granular for screening different-grain diameter, and n-butanol is added
Afterwards, ball milling 12h, after 80 DEG C dry, by waiting static pressure to be pressed into disk with 300Mpa pressure.
(7) solid electrolyte sheet is placed on the high-purity corundum ceramic wafer for being covered with step (2) synthesis of solid electrolyte powder,
And buried solid electrolyte sheet using electrolyte powder, 1200 DEG C are warming up to 5 DEG C/min, keeps the temperature 3h, is cooled to 1000 DEG C, is protected
Warm 6h obtains the garnet-type solid electrolyte piece of fine and close, high conductivity.
Embodiment 3
(1) garnet solid electrolyte powder Li is pressed6.8La3Zr1.4Ta0.2Ge0.4O12Raw material needed for the stoichiometric ratio of composition is weighed,
It is added in ball grinder, ball milling 12h after suitable grinding aid ethyl alcohol is added, in 60 DEG C of dry 8h.
(2) powder obtained after drying is in 900 DEG C of roasting 12h.
(3) ball milling 6h after ethyl alcohol is added in the powder burnt down again, after 60 DEG C dry, static pressure 100Mpa is waited to be pressed into circle
Piece.
(4) solid electrolyte sheet is placed on the high-purity corundum ceramic wafer for being covered with step (2) synthesis of solid electrolyte powder,
And buried solid electrolyte sheet using electrolyte powder, 1200 DEG C are warming up to 5 DEG C/min, keeps the temperature 2h, fast cooling to 1050
DEG C, 10h is kept the temperature, garnet-type solid electrolyte piece is obtained.
(5) after grinding the solid electrolyte sheet in step (4), partial size D is obtained50For 40 μm of solid electrolyte particle.
(6) the solid electrolyte powder that step (2) obtain is added in electrolyte granular, after ethyl alcohol is added, ball milling 12h, in 60
After DEG C dry, disk is pressed into 300Mpa pressure by equal static pressure.
(7) solid electrolyte sheet is placed on the high-purity corundum ceramic wafer for being covered with step (2) synthesis of solid electrolyte powder,
And buried solid electrolyte sheet using electrolyte powder, 1100 DEG C are warming up to 5 DEG C/min, keeps the temperature 10h, obtains fine and close, high electricity
The garnet-type solid electrolyte piece of conductance.
Embodiment 4
(1) garnet solid electrolyte powder Li is pressed6.5La3Zr1.4Ta0.2Ge0.1Nb0.3O12Needed for the stoichiometric ratio weighing of composition
Raw material is added in ball grinder, and ball milling 12h after suitable isobutanol is added, in 80 DEG C of dry 10h.
(2) powder obtained after drying is in 850 DEG C of roasting 10h.
(3) ball milling 8h after isobutanol is added in the powder burnt down again, after 60 DEG C dry, static pressure 200Mpa is waited to be pressed into circle
Piece.
(4) solid electrolyte sheet is placed on the high-purity corundum ceramic wafer for being covered with step (2) synthesis of solid electrolyte powder,
And buried solid electrolyte sheet using electrolyte powder, 1150 DEG C are warming up to 5 DEG C/min, keeps the temperature 2h, fast cooling to 1050
DEG C, 10h is kept the temperature, solid electrolyte sheet is obtained.
(5) after grinding the solid electrolyte sheet in step (4), partial size D is obtained50For 40 μm of solid electrolyte particle.
(6) the solid electrolyte powder that step (2) obtain is added in electrolyte granular, after isobutanol is added, ball milling 12h, in
After 60 DEG C of dryings, disk is pressed into 300Mpa pressure by equal static pressure.
(7) solid electrolyte sheet is placed on the high-purity corundum ceramic wafer for being covered with step (2) synthesis of solid electrolyte powder,
And buried solid electrolyte sheet using electrolyte powder, 1050 DEG C are warming up to 5 DEG C/min, keeps the temperature 10h, obtains fine and close, high electricity
The garnet-type solid electrolyte piece of conductance.
Embodiment 5
(1) garnet solid electrolyte powder Li is pressed6.4La3Zr1.4Ta0.3W0.3O12Raw material needed for the stoichiometric ratio of composition is weighed,
It is added in ball grinder, ball milling 12h after suitable isopropanol is added, in 80 DEG C of dry 10h.
(2) powder obtained after drying is in 900 DEG C of roasting 15h.
(3) ball milling 8h after isopropanol is added in the powder burnt down again, after 80 DEG C dry, static pressure 300Mpa is waited to be pressed into circle
Piece.
(4) solid electrolyte sheet is placed on the high-purity corundum ceramic wafer for being covered with step (2) synthesis of solid electrolyte powder,
And buried solid electrolyte sheet using electrolyte powder, 1200 DEG C are warming up to 5 DEG C/min, keeps the temperature 1h, fast cooling to 1050
DEG C, 10h is kept the temperature, solid electrolyte sheet is obtained.
(5) after grinding the solid electrolyte sheet in step (4), partial size D is obtained50For 10 μm of solid electrolyte particle.
(6) the solid electrolyte powder that step (2) obtain is added in electrolyte granular, after isopropanol is added, ball milling 15h, in
After 60 DEG C of dryings, disk is pressed into 200Mpa pressure by equal static pressure.
(7) solid electrolyte sheet is placed on the high-purity corundum ceramic wafer for being covered with step (2) synthesis of solid electrolyte powder,
And buried solid electrolyte sheet using electrolyte powder, 1050 DEG C are warming up to 5 DEG C/min, keeps the temperature 6h, obtains fine and close, high conductance
The garnet-type solid electrolyte piece of rate.
Claims (4)
1. a kind of method that guidance crystal growth prepares high-compactness, high conductivity Garnet-type electrolyte piece, it is characterised in that
The following steps are included:
(1) raw material needed for weighing by the stoichiometric ratio of garnet solid electrolyte powder composition, is added in ball grinder, is added suitable
Ball milling 6-15h after the grinding aid of amount, in 50-95 DEG C of dry 12h；
(2) powder obtained after drying is in 800-950 DEG C of roasting 6-20h；
(3) ball milling 5-10h after grinding aid is added in the powder burnt down again, after 50-95 DEG C dry, by waiting static pressure with 50-
400Mpa pressure is pressed into disk；
(4) solid electrolyte sheet is placed on the high-purity corundum ceramic wafer for being covered with step (2) synthesis of solid electrolyte powder, and adopted
Solid electrolyte sheet is buried with electrolyte powder, 1000-1200 DEG C is warming up to 2-10 DEG C/min, keeps the temperature 6-15h, obtain pomegranate
Stone-type solid electrolyte sheet；
(5) after grinding the solid electrolyte sheet in step (4), the solid electrolyte particle that partial size is 10-80 μm is obtained；
(6) the solid electrolyte powder that step (2) obtain is added in the electrolyte granular for screening different-grain diameter, after grinding aid is added, ball
5-10h is ground, after 50-95 DEG C dry, by waiting static pressure to be pressed into disk with 50-400Mpa pressure；
(7) solid electrolyte sheet is placed on the high-purity corundum ceramic wafer for being covered with step (2) synthesis of solid electrolyte powder, and adopted
Solid electrolyte sheet is buried with electrolyte powder, 1000-1200 DEG C is warming up to 4-10 DEG C/min, keeps the temperature 2-5h, be cooled to
1000-1100 keeps the temperature 4-9h, obtains the garnet-type solid electrolyte piece of fine and close, high conductivity.
2. according to the method described in claim 1, it is characterized in that the garnet-type solid electrolyte group in step 1 becomes
Li5+xLa5-y-z-zZryTazMz’O12, 0 < x≤2,0 < y+z+z '≤4.5, wherein M can be independently selected from Nb, W, Ti, Hf, Ru,
The one or more of Mo, Nd, Ba, Ga, In, Ge, Sn, Sb, Se.
3. according to the method described in claim 1, lithium source selects hydrogen it is characterized in that step 1 is in synthesis of solid electrolyte powder
Lithia, lithium carbonate, lithium sulfate, lithium nitrate, lithium acetate, lithium borate, lithium niobate, lithium dihydrogen phosphate；Lanthanum source selection lanthanum hydroxide,
Lanthanum carbonate, lanthanum sulfate, lanthanum nitrate, lanthana, lanthanum chloride, lanthanum nitrate；Tantalum source selects tantalum pentoxide, tantalic chloride.
4. according to the method described in claim 1, it is characterized in that grinding aid in step 1 is ethyl alcohol, propyl alcohol, isopropanol, just
Butanol, isobutanol, the tert-butyl alcohol.
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| CN110137567A (en) * | 2019-06-03 | 2019-08-16 | 哈尔滨工业大学 | The preparation method and applications of high-compactness carbuncle type all solid state electrolyte under a kind of low temperature |
| CN110311172A (en) * | 2019-06-04 | 2019-10-08 | 上海应用技术大学 | A kind of LiCuLaZrO method for preparing solid electrolyte and application |
| CN111786014A (en) * | 2020-08-05 | 2020-10-16 | 长沙理工大学 | Garnet type solid electrolyte powder with superfine particle size and preparation method thereof |
| CN113614038A (en) * | 2019-03-29 | 2021-11-05 | 古河机械金属株式会社 | Method for producing sulfide-based inorganic solid electrolyte material |
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