CN105914396A - Preparation method of ultrathin nano-lithium lanthanum zirconium oxygen all-solid-state electrolyte layer - Google Patents
Preparation method of ultrathin nano-lithium lanthanum zirconium oxygen all-solid-state electrolyte layer Download PDFInfo
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- CN105914396A CN105914396A CN201610376884.XA CN201610376884A CN105914396A CN 105914396 A CN105914396 A CN 105914396A CN 201610376884 A CN201610376884 A CN 201610376884A CN 105914396 A CN105914396 A CN 105914396A
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- lanthanum zirconium
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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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- 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
Abstract
The invention discloses a preparation method of an ultrathin nano-lithium lanthanum zirconium oxygen all-solid-state electrolyte layer. The method includes: preparation of a nano-lithium lanthanum zirconium oxygen slurry; and film formation from the nano-lithium lanthanum zirconium oxygen slurry. The preparation process is simple, the preparation process has no need for a mold and pressure, the electrolyte layer shapes naturally, the operation is convenient, and the energy consumption is low. The raw materials are wide and easily available, the preparation process is controllable, and the repeatability is high. The solid electrolyte film prepared by the method has thickness up to 1 micrometer.
Description
Technical field
The present invention relates to all-solid-state battery field, especially relate to the preparation method of a kind of ultra-thin lithium lanthanum zirconium oxygen all solid state electrolyte layer.
Background technology
Since lithium ion battery commercialization, it is widely used in every field.But currently used organic electrolyte is the potential safety hazard place of lithium ion battery.Inorganic solid electrolyte has the advantages such as safety is good, energy density is high, good cycle, thermal adaptability are good, it is possible to fundamentally solve the safety problem of liquid electrolyte.
Lithium lanthanum zirconium oxygen is the one of solid oxide electrolyte, has good stability in atmosphere, and ionic conductivity is high, synthesizes the advantages such as simple.Lithium lanthanum titanium oxide chemical formula is Li7La3Zr2O12, current all-solid-state battery, the main method using powder compacting.Powder compression process needs, with fixing mould, to apply the biggest impressed pressure, and the solid electrolyte layer that the method obtains is relatively thick.
Summary of the invention
Because above-mentioned, it is an object of the invention to provide a kind of simple process, the preparation method preparing ultrathin nanometer lithium lanthanum zirconium oxygen all solid state electrolyte layer that energy consumption is low.
The preparation method of ultrathin nanometer lithium lanthanum zirconium oxygen all solid state electrolyte layer of the present invention, comprises the steps:
1) the lithium lanthanum zirconium oxygen of 1 weight portion is joined in the solvent of 5~100 weight portions, add 0.5~2 weight portion lithium salts, 0.01~0.2 parts per weight dispersing agent and 0.01~0.2 parts by weight binder, after stirring 1~12 hour, it is transferred in zirconia ball grinding jar, carry out ball milling, obtain nanometer lithium lanthanum zirconium oxygen slurry;
2) by slurry good for ball milling with becoming membranization method to be uniformly coated on electrode material surface, make annealing treatment 6~120 hours at 50~600 DEG C, naturally cool to room temperature, obtain ultrathin nanometer lithium lanthanum zirconium oxygen all solid state electrolyte layer.
In preparation process of the present invention, described solvent can be one or more mixing in ethanol, isopropanol, n-butyl alcohol, toluene, acetaldehyde, N-Methyl pyrrolidone (NMP), propylene carbonate ester (PC), ethylene carbonate (EC), dimethyl carbonate (DMC) and fluorinated ethylene carbonate (FEC).
In preparation process of the present invention, described dispersant can be one or more in ethyl acetate, acetylacetone,2,4-pentanedione, ethyl acetoacetate Tween-80, FC4430, sodium lauryl sulphate (SDS), dodecylbenzene sodium sulfonate (SDBS), cetyl trimethylammonium bromide (CTAB), EO-PO type polyethers (F127) and polyoxyethylene-poly-oxypropylene polyoxyethylene (P123).
In preparation process of the present invention, described binding agent can be Kynoar (PVDF), carboxymethyl cellulose (CMC), sulfonated polyether-ether-ketone and one or more in pendant lithiumation fluosulfonic acid (SPEEK-PSI-Li), styrene butadiene lactoprene (SBR) and Brown algae (Brown Algae).
In preparation process of the present invention, described lithium salts can be LiPF6、LiClO4, one or more mixing in LiTFSI and LiBoB.
In preparation process of the present invention, the rotating speed of described ball milling is generally 500~1500
Rev/min.
In preparation process of the present invention, described one-tenth membranization method may is that wet coating is covered or silk screen printing or inkjet printing or 3D print.
Step 2 of the present invention) in, preferably heat treatment temperature is 80~200 DEG C, and the time is 12~24 hours.
In the present invention, described lithium lanthanum zirconium oxygen can use " Fast
Lithium Ion Conduction in Garnet-Type Li7La3Zr2O12" (DOI:10.1002/anie.200701144), " Synthesis of garnet-type
Li7-xLa3Zr2O12-1/2x and its stability in aqueous solutions " method described in the document such as (DOI:10.1016/j.ssi.2010.12.010) prepares.
Other raw material of the present invention and reagent are the most commercially.
The beneficial effects of the present invention is:
Preparation technology of the present invention is simple, need not mould, need not pressure in preparation process, and natural molding, easy to operate, energy consumption is low;Raw material extensively and is easy to get, and preparation process is controlled, repeatable high;The thickness of the solid electrolyte film prepared by the method can reach 1 micron.
Detailed description of the invention
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1
1) the lithium lanthanum zirconium oxygen of 1 weight portion, the LiPF of 0.5 weight portion are taken6As lithium salts, the PVDF of 0.1 weight portion is as binding agent, and the FC4430 of 0.1 weight portion joins as dispersant in the solvent isopropanol of 10 weight portions.After stirring 10 hours, being transferred in zirconia ball grinding jar, ball milling 1h, rotational speed of ball-mill is 800
R/min, obtains nanometer lithium lanthanum zirconium oxygen slurry.
2) by nanometer lithium lanthanum zirconium oxygen slurry screen-printing deposition in electrode material surface, anneal 12 hours at 200 DEG C, obtain the nanometer lithium lanthanum zirconium oxygen all solid state electrolyte layer that thickness is about 1 micron.
Embodiment 2
1) the lithium lanthanum zirconium oxygen of 1 weight portion, the LiPF of 1 weight portion are taken6As lithium salts, the PVDF of 0.1 weight portion is as binding agent, and the Tween 80 of 0.1 weight portion joins as dispersant in the solvent isopropanol of 10 weight portions.After stirring 1 hour, being transferred in zirconia ball grinding jar, ball milling 3h, rotational speed of ball-mill is 1000
R/min, obtains nanometer lithium lanthanum zirconium oxygen slurry.
2) nanometer lithium lanthanum zirconium oxygen slurry inkjet printing is coated in electrode material surface, anneals 24 hours at 100 DEG C, obtain the nanometer lithium lanthanum zirconium oxygen all solid state electrolyte layer that thickness is about 5 microns.
Embodiment 3
1) taking the lithium lanthanum zirconium oxygen of 1 weight portion, the LiTFSI of 1 weight portion joins in solvent PC, EC mixed solution of 5 weight portions (volume ratio of PC Yu EC is 1:3) as dispersant as binding agent, the SDS of 0.05 weight portion as lithium salts, the CMC of 0.1 weight portion.After stirring 12 hours, being transferred in zirconia ball grinding jar, ball milling 12h, rotational speed of ball-mill is 1200 r/min, obtains nanometer lithium lanthanum zirconium oxygen slurry.
2) by nanometer lithium lanthanum zirconium oxygen slurry screen-printing deposition in electrode material surface, anneal 12 hours at 60 DEG C, obtain the nanometer lithium lanthanum zirconium oxygen all solid state electrolyte layer that thickness is about 1 micron.
Embodiment 4
1) the lithium lanthanum zirconium oxygen of 1 weight portion is taken, the LiBOB of 0.5 weight portion is as lithium salts, the SBR of 0.1 weight portion joins in solvent PC, EC, FEC mixed solution of 10 weight portions (volume ratio of PC:EC:FEC is 1:2:1) as dispersant as binding agent, the SDBS of 0.1 weight portion.After stirring 2 hours, being transferred in zirconia ball grinding jar, ball milling 1h, rotational speed of ball-mill is 1200 r/min, obtains nanometer lithium lanthanum zirconium oxygen slurry.
2) by nanometer lithium lanthanum zirconium oxygen slurry screen-printing deposition in electrode material surface, anneal 12 hours at 300 DEG C, obtain the nanometer lithium lanthanum zirconium oxygen all solid state electrolyte layer that thickness is about 2 microns.
Embodiment 5
Take the lithium lanthanum zirconium oxygen of 1 weight portion, the LiClO of 0.5 weight portion4As lithium salts, the CMC of 0.1 weight portion joins in solvent NMP, PC mixed solution of 10 weight portions (volume ratio of NMP Yu PC is 2:1) as dispersant as binding agent, the SDBS of 0.1 weight portion.After stirring 8 hours, being transferred in zirconia ball grinding jar, ball milling 1h, rotational speed of ball-mill is 1500 r/min, obtains nanometer lithium lanthanum zirconium oxygen slurry.
2) by nanometer lithium lanthanum zirconium oxygen slurry screen-printing deposition in electrode material surface, anneal 12 hours at 150 DEG C, obtain the nanometer lithium lanthanum zirconium oxygen all solid state electrolyte layer that thickness is about 1 micron.
Embodiment 6
1) taking the lithium lanthanum zirconium oxygen of 1 weight portion, the LiTFSI of 0.5 weight portion is as lithium salts, and the Brown Algae of 0.1 weight portion is as binding agent, and the F127 of 0.1 weight portion joins as dispersant in the solvent NMP of 10 weight portions.After stirring 3 hours, being transferred in zirconia ball grinding jar, ball milling 1h, rotational speed of ball-mill is 1500 r/min, obtains nanometer lithium lanthanum zirconium oxygen slurry.
2) nanometer lithium lanthanum zirconium oxygen slurry wet coating is covered it is coated in electrode material surface, anneal 12 hours at 100 DEG C, obtain the nanometer lithium lanthanum zirconium oxygen all solid state electrolyte layer that thickness is about 2 microns.
Below it is only several embodiments of the present invention; it should be pointed out that, for those skilled in the art, on the premise of without departing from embodiment of the present invention principle; can also make some improvements and modifications, these improvements and modifications are also considered as the protection domain of the embodiment of the present invention.
Claims (8)
1. the preparation method of a ultrathin nanometer lithium lanthanum zirconium oxygen all solid state electrolyte layer, it is characterised in that comprise the steps:
1) the lithium lanthanum zirconium oxygen of 1 weight portion is joined in the solvent of 5~100 weight portions, add 0.5~2 weight portion lithium salts, 0.01~0.2 parts per weight dispersing agent and 0.01~0.2 parts by weight binder, after stirring 1~12 hour, it is transferred in zirconia ball grinding jar, carry out ball milling, obtain nanometer lithium lanthanum zirconium oxygen slurry;
2) by slurry good for ball milling with becoming membranization method to be uniformly coated on electrode material surface, make annealing treatment 6~120 hours at 50~600 DEG C, naturally cool to room temperature, obtain ultrathin nanometer lithium lanthanum zirconium oxygen all solid state electrolyte layer.
2. the preparation method of ultrathin nanometer lithium lanthanum zirconium oxygen all solid state electrolyte layer as claimed in claim 1, it is characterised in that step 1) described in solvent be one or more mixing in ethanol, isopropanol, n-butyl alcohol, toluene, acetaldehyde, N-Methyl pyrrolidone, propylene carbonate ester, ethylene carbonate, dimethyl carbonate and fluorinated ethylene carbonate.
3. the preparation method of ultrathin nanometer lithium lanthanum zirconium oxygen all solid state electrolyte layer as claimed in claim 1, it is characterised in that step 1) described in dispersant be one or more in ethyl acetate, acetylacetone,2,4-pentanedione, ethyl acetoacetate, Tween-80, FC4430, sodium lauryl sulphate, dodecylbenzene sodium sulfonate, cetyl trimethylammonium bromide, EO-PO type polyethers and polyoxyethylene-poly-oxypropylene polyoxyethylene.
4. the preparation method of ultrathin nanometer lithium lanthanum zirconium oxygen all solid state electrolyte layer as claimed in claim 1, it is characterised in that step 1) described in binding agent be Kynoar, carboxymethyl cellulose, sulfonated polyether-ether-ketone and one or more in pendant lithiumation fluosulfonic acid, styrene butadiene lactoprene and Brown algae.
5. the preparation method of ultrathin nanometer lithium lanthanum zirconium oxygen all solid state electrolyte layer as claimed in claim 1, it is characterised in that step 1) described in lithium salts be LiPF6、LiClO4, one or more mixing in LiTFSI and LiBoB.
6. the preparation method of ultrathin nanometer lithium lanthanum zirconium oxygen all solid state electrolyte layer as claimed in claim 1, it is characterised in that step 1) described in rotational speed of ball-mill be 500~1500
Rev/min.
7. the preparation method of ultrathin nanometer lithium lanthanum zirconium oxygen all solid state electrolyte layer as claimed in claim 1, it is characterised in that step 2) described in one-tenth membranization method be: wet coating is covered or silk screen printing or inkjet printing or 3D print.
8. the preparation method of ultrathin nanometer lithium lanthanum zirconium oxygen all solid state electrolyte layer as claimed in claim 1, it is characterised in that step 2) described in annealing temperature be 80~200 DEG C, the time is 12~24 hours.
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