CN106329002A - Method for efficiently preparing and collecting chalcogenide solid electrolyte - Google Patents
Method for efficiently preparing and collecting chalcogenide solid electrolyte Download PDFInfo
- Publication number
- CN106329002A CN106329002A CN201610865804.7A CN201610865804A CN106329002A CN 106329002 A CN106329002 A CN 106329002A CN 201610865804 A CN201610865804 A CN 201610865804A CN 106329002 A CN106329002 A CN 106329002A
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- solid electrolyte
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- sulfur system
- system solid
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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
- H01M2300/00—Electrolytes
- H01M2300/0085—Immobilising or gelification of electrolyte
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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 discloses a method for efficiently preparing and collecting chalcogenide solid electrolyte. The method comprises the following steps of 1, performing dry milling: putting lithium sulfide and phosphorus pentasulfide into a ball mill container to be subjected to ball milling mixing for preparing Li3PS4; 2, performing wet milling: adding a proton inert organic solvent into the ball mill container; performing ball milling stirring to realize the dissolution of the Li3PS4 for obtaining an Li3PS4 solution; 3, transferring the Li3PS4 solution in the ball mill container into a collecting container; performing drying to remove organic solvents. The efficient preparation and collection of the chalcogenide solid electrolyte is realized. Through the continuous ball milling, solution and deposition paths, the adhesion and residue of powdery products on the inner wall of a ball mill tank and the surface of a grinding ball in the collecting process are greatly reduced; the purity and the collection efficiency of the solid electrolyte are improved; meanwhile, the method is also suitable for being used for realizing continuous in-situ coverage on the solid electrolyte layer on the surface of active materials.
Description
Technical field
The invention belongs to solid lithium ion battery field, relate to a kind of sulfur system solid electrolyte, be specifically related to a kind of efficient
Preparation and the process of collection sulfur system solid electrolyte.
Background technology
All-solid lithium-ion battery be the problem for liquid electrolyte lithium ion battery poor safety performance put forward new
One of type lithium-ion battery system.By replacing barrier film and organic electrolysis with the higher solid electrolyte material of heat stability
Liquid, fundamentally improves the safety problem of lithium ion battery.Solid electrolyte leads lithium layer as solid-state, it is possible to give full play to solid-state
The advantage that planform is flexible and changeable, is expected to change the conventional preparation techniques of lithium ion battery, obtain the lithium of various shapes from
Sub-battery.Solid electrolyte material also is able to play suppression Li dendrite life while replacement electrolyte is transmitted leading lithium simultaneously
The long effect preventing both positive and negative polarity short circuit.
As the Typical Representative in inorganic electrolyte material, sulfur system solid electrolyte material is owing at room temperature having excellence
Ionic conductivity (~ 10-2S/cm) and the chemical property such as stable electrochemical window (5 ~ 10V), can be with the sulfur system of high power capacity
Positive pole is combined into high specific energy, the high security solid lithium battery of wide temperature range application.At present, multiple sulfide solid-state has been developed
Electrolyte, such as, Publication No. CN201180040786, the Chinese patent of CN20130535524.6 individually disclose tool
Standby macroion conductance and the sulfide solid electrolyte to air stability excellence.Sulfur system solid electrolyte is mainly with mechanical ball
Prepared by mill method, but the solid electrolyte prepared of dry ball milling still exists ball milling and the low problem of collection efficiency, such as,
Need ball milling 20-40h just can obtain the solid-state of glassy state under 370rpm rotating speed；Not only consume additionally, traditional mistake sieve method collects powder body
Time effort, and major part powder body still can residue in grinding pot, mill ball (when mill ball granule less (≤5mm) consumption is many
Become apparent from) and screen surface, add due to expensive raw material price, test feeds intake general only between 1 ~ 2g every time, therefore real
The collectable powder body in border is the most less.The efficiently preparation and collection of sulfur system solid electrolyte powder body still have to be solved.
Summary of the invention
The present invention is directed to chalcogenide glass ceramic solid electrolyte Mechano-chemical Synthesizing and the highest problem of collection efficiency, purport
Efficiently prepare providing a kind of new method and collect sulfur system solid electrolyte powder body.
For reaching above-mentioned purpose, the invention provides a kind of efficient preparation and the method collecting sulfur system solid electrolyte, should
Method comprises the steps of
Step 1, dry grinding: lithium sulfide, phosphorus pentasulfide are placed in ball milling mixing in ball mill container, prepare Li3PS4；
Step 2, wet grinding: add proton-inert organic solvent in ball mill container, ball grinding stirring, to realize the dissolving of Li3PS4, obtains
To Li3PS4 solution；
Step 3, by the Li in ball mill container3PS4Solution is transferred to collect container, is dried to remove organic solvent, it is achieved sulfur system
The efficiently preparation of solid electrolyte and collection.
Preferably, described lithium sulfide, the mol ratio of phosphorus pentasulfide are 3:1.
Preferably, the purity of described lithium sulfide is 99.9%, and the purity of described phosphorus pentasulfide is 99%.
Preferably, the rotational speed of ball-mill of step 1 is 500～1000rpm, and Ball-milling Time is 5h ~ 10h.
Preferably, the ball milling of step 1 uses ZrO2Mill ball.
Preferably, described proton-inert organic solvent is N-METHYLFORMAMIDE, N-Methyl pyrrolidone and dehydrated alcohol
In any one.
Preferably, in step 3, drying condition is under inert atmosphere, and temperature is 80 ~ 120 DEG C.
Step 3 also comprises: dried, carries out heat treatment being not less than 200 DEG C so that Li3PS4Powder is converted into glass pottery
Porcelain solid electrolyte Li3PS4。
Preferably, described heat treatment temperature is 200-300 DEG C.
In step 3, also comprise: to Li3PS4Solution adds after active material, after mix homogeneously, then is dried and has to remove
Machine solvent, it is thus achieved that be coated on the solid-state electrolyte layer of surface of active material.
The present invention combines high-energy ball milling and dissolves the method separated out again, makes each reactant phase uniform contact highly effective reaction,
And the loss of product is significantly reduced by liquid phase deposition method, it is achieved the efficiently synthesizing and collecting of sulfur system solid electrolyte.
Sulfur system solid electrolyte prepared by the present invention, has higher purity；With under suitable ratio of grinding media to material and rotating speed to former
Material carries out high-energy ball milling, improves the extent of reaction between two kinds of reactants and speed, and finally improves generated product
Purity；Utilize the approach dissolving-evaporating to collect the solid electrolyte product generated, be greatly improved the collection efficiency of product；
Meanwhile, the method also can realize solid electrolyte and is coated with continuously on the surface of electrolysis material granule.
Accompanying drawing explanation
Fig. 1 is sulfur system solid electrolyte (Li prepared by the present invention3PS4) XRD(X x ray diffraction) spectrogram.
Fig. 2 is sulfur system solid electrolyte (Li prepared by the present invention3PS4) SEM(scanning electron microscope) shape appearance figure.
Fig. 3 is the schematic diagram that different approaches forms solid/liquid/solid interface: (a) mechanical ball milling mixes；(b) liquid phase coating.
Detailed description of the invention
Below in conjunction with accompanying drawing, by specific embodiment, the invention will be further described, and these embodiments are merely to illustrate this
Bright, it is not limiting the scope of the invention.
Embodiment 1:
0.4738g lithium sulfide (99.9%) powder, 1.5262g phosphorus pentasulfide is weighed in the glove box of inert protective atmosphere
(99%), first grind uniformly in agate mortar, be subsequently adding the ZrO that volume is 50ml2In ball grinder, a diameter of by 120
The ZrO of a diameter of 2mm of 5mm and 3mL2Mill ball is placed in ball grinder, is first set in ball milling 0.5h under the rotating speed of 200rpm, so
After switch to ball milling 10h under the rotating speed of 1000rpm.After ball milling, ball grinder is placed in glove box, by 20mL proton inertia
Organic solvent (e.g., NMF) instills in ball grinder, with the rotating speed ball grinding stirring 30min of 100rpm after sealing.Again in glove box
Solution in grinding pot is collected in specific glass container, at a temperature of 80 DEG C, glass container is carried out heated and stirred 1h, molten
After agent volatilization, the powder body of solid electrolyte separates out.This powder body is amorphous state, and its XRD spectra is not as it is shown in figure 1, have characteristic peak with just
Beginning raw material is corresponding, therefore conclude that there occurs and meet the reaction of stoichiometric proportion and define sulfur system solid electrolyte Li3PS4.Separate out
Powder drying after, be placed in Ar atmosphere and can obtain glass ceramics solid electrolyte through 300 DEG C of heat treatment certain times
Li3PS4, its pattern is as shown in Figure 2.
Embodiment 2:
Weighing 0.2369g lithium sulfide powder in the glove box of inert protective atmosphere, 0.7631g phosphorus pentasulfide, first at agate
Nao mortar grinds uniformly, is subsequently adding the ZrO of 50ml2In grinding pot, by the ZrO of a diameter of for 30mL 1mm2Mill ball is placed in ball
In grinding jar, ball milling 10h under the rotating speed of 1000rpm.After ball milling, ball grinder is placed in glove box, by anhydrous for 20mL second
Alcohol instills in ball grinder, with the rotating speed ball grinding stirring 30min of 100rpm after sealing.Molten by grinding pot in glove box again
Liquid (and with the solution after dehydrated alcohol bulb syringe grinding jar) is collected in specific glass container, by a certain amount of LiCoO2(make
For active material) it is placed in the solid electrolyte solution of dilution (by the mass ratio 95:5 of active material Yu solid electrolyte), will
Mixture carries out heated and stirred 3h at a temperature of 80 DEG C, i.e. obtains, after solvent volatilization, the LiCoO that solid electrolyte is coated with continuously2Material
Material (liquid phase coating).As it is shown on figure 3, the liquid phase coating method ((b) of Fig. 3) of the present invention is mixed relative to the mechanical ball milling of prior art
Closing ((a) of Fig. 3), solid electrolyte contacts interface with active material will be continuous and big many, advantageously in lithium ion
Efficiently transport, it is achieved the utilization rate of active material and the lifting of electrode cycle performance.Visible, the liquid phase coating method of the present invention can be real
Existing solid-state electrolyte layer is tight and continuous print in-stiu coating in surface of active material.
In sum, first the present invention improves high-energy ball milling parameter to shorten the response time, to improve output efficiency；Next to that
Select be suitable for sprotic organic solvent by ball grinder and mill ball surface adhesion solid electrolyte dissolve, collect
Solvent is volatilized after specific container by solution again, can realize the efficient collection to solid electrolyte；It addition, the method also may be used
It is applicable to electrode active material surface is realized the in-stiu coating of continuous print solid-state electrolyte layer.
Although present disclosure has been made to be discussed in detail by above preferred embodiment, but it should be appreciated that above-mentioned
Description is not considered as limitation of the present invention.After those skilled in the art have read foregoing, for the present invention's
Multiple amendment and replacement all will be apparent from.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (10)
1. an efficient preparation and the method for collection sulfur system solid electrolyte, it is characterised in that the method includes the steps of:
Step 1, dry grinding: lithium sulfide, phosphorus pentasulfide are placed in ball milling mixing in ball mill container, prepare Li3PS4；
Step 2, wet grinding: adding proton-inert organic solvent in ball mill container, ball grinding stirring is to realize Li3PS4Dissolving,
To Li3PS4Solution；
Step 3, by the Li in ball mill container3PS4Solution is transferred to collect container, is dried to remove organic solvent, it is achieved sulfur system is solid
The efficiently preparation of state electrolyte and collection.
2. efficiently preparation as claimed in claim 1 and the method for collection sulfur system solid electrolyte, it is characterised in that described sulfur
Change lithium, the mol ratio of phosphorus pentasulfide is 3:1.
3. efficiently preparation as claimed in claim 1 and the method for collection sulfur system solid electrolyte, it is characterised in that described sulfur
The purity changing lithium is 99.9%, and the purity of described phosphorus pentasulfide is 99%.
4. efficiently preparation as claimed in claim 1 and the method for collection sulfur system solid electrolyte, it is characterised in that step 1
Rotational speed of ball-mill is 500～1000rpm, and Ball-milling Time is 5h ~ 10h.
5. efficiently preparation as claimed in claim 1 and the method for collection sulfur system solid electrolyte, it is characterised in that step 1
Ball milling uses ZrO2Mill ball.
6. efficiently preparation as claimed in claim 1 and the method for collection sulfur system solid electrolyte, it is characterised in that described matter
Sub-inert organic solvents is any one in N-METHYLFORMAMIDE, N-Methyl pyrrolidone and dehydrated alcohol.
7. efficiently preparation as claimed in claim 1 and the method for collection sulfur system solid electrolyte, it is characterised in that in step 3,
Drying condition is under inert atmosphere, and temperature is 80 ~ 120 DEG C.
8. efficiently preparation as claimed in claim 1 and the method for collection sulfur system solid electrolyte, it is characterised in that step 3 is also
Comprise: dried, carry out heat treatment being not less than 200 DEG C so that Li3PS4Powder is converted into glass ceramics solid electrolyte
Li3PS4。
9. efficiently preparation as claimed in claim 8 and the method for collection sulfur system solid electrolyte, it is characterised in that in step 3,
Described heat treatment temperature is 200-300 DEG C.
10. efficiently preparation as claimed in claim 1 and the method for collection sulfur system solid electrolyte, it is characterised in that step 3
In, also comprise: to Li3PS4After solution adds active material, after mix homogeneously, then it is dried to remove organic solvent, it is thus achieved that bag
Overlay on the solid-state electrolyte layer of surface of active material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610865804.7A CN106329002A (en) | 2016-09-30 | 2016-09-30 | Method for efficiently preparing and collecting chalcogenide solid electrolyte |
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| CN201610865804.7A CN106329002A (en) | 2016-09-30 | 2016-09-30 | Method for efficiently preparing and collecting chalcogenide solid electrolyte |
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| CN201610865804.7A Pending CN106329002A (en) | 2016-09-30 | 2016-09-30 | Method for efficiently preparing and collecting chalcogenide solid electrolyte |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107910530A (en) * | 2017-11-18 | 2018-04-13 | 哈尔滨工业大学 | A kind of preparation method and applications of combination electrode material |
| CN108539178A (en) * | 2018-04-25 | 2018-09-14 | 广东工业大学 | Ion battery novel phosphorus and sulphur selenium composite negative pole material and preparation method thereof |
| CN108878962A (en) * | 2018-07-11 | 2018-11-23 | 桑德集团有限公司 | A kind of sulfide solid electrolyte and preparation method thereof |
| CN109604607A (en) * | 2018-12-19 | 2019-04-12 | 技锋精密刀具（马鞍山）有限公司 | A kind of production technology effectively improving hard alloy dise knife blank qualification rate |
| CN109888378A (en) * | 2019-04-17 | 2019-06-14 | 宁波容百新能源科技股份有限公司 | A kind of high ionic conductivity sulfide solid electrolyte and preparation method thereof based on liquid phase method |
| CN110526224A (en) * | 2019-08-26 | 2019-12-03 | 浙江工业大学 | A kind of mechanical ball mill synthetic method of phosphorus pentasulfide powder |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107910530A (en) * | 2017-11-18 | 2018-04-13 | 哈尔滨工业大学 | A kind of preparation method and applications of combination electrode material |
| CN108539178A (en) * | 2018-04-25 | 2018-09-14 | 广东工业大学 | Ion battery novel phosphorus and sulphur selenium composite negative pole material and preparation method thereof |
| CN108539178B (en) * | 2018-04-25 | 2020-11-13 | 广东工业大学 | Novel phosphorus-sulfur-selenium composite negative electrode material for ion battery and preparation method thereof |
| CN108878962A (en) * | 2018-07-11 | 2018-11-23 | 桑德集团有限公司 | A kind of sulfide solid electrolyte and preparation method thereof |
| CN109604607A (en) * | 2018-12-19 | 2019-04-12 | 技锋精密刀具（马鞍山）有限公司 | A kind of production technology effectively improving hard alloy dise knife blank qualification rate |
| CN109604607B (en) * | 2018-12-19 | 2020-12-29 | 技锋精密刀具（马鞍山）有限公司 | Production process for effectively improving qualified rate of hard alloy circular cutter blank |
| CN109888378A (en) * | 2019-04-17 | 2019-06-14 | 宁波容百新能源科技股份有限公司 | A kind of high ionic conductivity sulfide solid electrolyte and preparation method thereof based on liquid phase method |
| CN110526224A (en) * | 2019-08-26 | 2019-12-03 | 浙江工业大学 | A kind of mechanical ball mill synthetic method of phosphorus pentasulfide powder |
| CN110526224B (en) * | 2019-08-26 | 2021-07-09 | 浙江工业大学 | Mechanical ball milling synthesis method of phosphorus pentasulfide powder |
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Application publication date: 20170111 |