CN105633479A - Preparation method of all-solid-state lithium-sulfur battery - Google Patents
Preparation method of all-solid-state lithium-sulfur battery Download PDFInfo
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- CN105633479A CN105633479A CN201610142043.2A CN201610142043A CN105633479A CN 105633479 A CN105633479 A CN 105633479A CN 201610142043 A CN201610142043 A CN 201610142043A CN 105633479 A CN105633479 A CN 105633479A
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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
- H01M2220/00—Batteries for particular applications
- H01M2220/30—Batteries in portable systems, e.g. mobile phone, laptop
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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 preparation method of an all-solid-state lithium-sulfur battery. The method comprises the following steps: carrying out high-temperature sintering on raw materials of Li<2>CO<3> and the like by a solid-phase method to obtain an all-solid-state electrolyte; evaporating a metal lithium layer on one surface of an all-solid-state electrolyte flake as a negative electrode; coating the other surface with a sulfur-carbon composite material as a positive electrode and dropwise adding an ionic liquid to strengthen the conductivity; and finally encapsulating the battery with an aluminum-plastic package, so as to obtain a rechargeable and dischargeable all-solid-state lithium-sulfur battery. The all-solid-state lithium-sulfur battery prepared by the method has relatively good electrochemical properties and practicability and good medium-high temperature safety.
Description
Technical field
The present invention relates to a kind of can the preparation method of charge and discharge all solid lithium sulphur battery, specifically relate to the preparation method that a kind of positive and negative electrode active substance has the good all solid lithium sulphur battery contacting, having good electrical chemical property with all solid state electrolyte sheet.
Background technology
Along with the development of social science and technology, mobile phone, the portable type electronic products such as notebook computer obtain and apply more and more widely, and for the lithium cell of these electronic products offer electric energy is due to its high energy storage density, the features such as high output voltage and well received, secondary lithium battery commercial at present generally uses organic electrolyte, be short-circuited or excessively the abnormal conditions such as charging time organic electrolyte can be made to heat up, thus cause the hazardous conditions such as battery spontaneous combustion or blast, in order to improve the safety and reliability of battery, an effective method is exactly that the organic electrolyte of easily combustion is replaced the material for having excellent heat stability, in all-solid-state battery, solid electrolyte instead of tradition organic electrolyte, have nonflammable, the feature of good stability, can significantly improve the safety of battery.
In secondary lithium battery, lithium-sulfur cell gathers around grow a lot potentiality and application prospect, its active substance sulphur has extremely high energy density, and at cost, the aspects such as environmental friendliness embody bigger advantage, for organic system lithium-sulfur cell conventional at present, its greatest drawback is difficult to solve " effect of shuttling back and forth ", namely sulphur can be dissolved in electrolytic solution at the intermediate product of charge and discharge process, with the problem of negative pole metallic lithium direct reaction, once there is " effect of shuttling back and forth ", the negative pole of lithium-sulfur cell can be corroded, the serious coulomb efficiency reducing battery makes it cannot normal operation, and potential safety hazard may be caused.
All solid lithium sulphur battery can solve " effect of shuttling back and forth " problem completely; so obtaining a large amount of concerns and research; because after using all solid state electrolyte sheet; the polysulfide that positive discharge produces cannot arrive negative pole through electrolyte sheet; thus protect negative pole metallic lithium; extending the working life of lithium-sulfur cell, all solid state electrolyte sheet has good high-temperature stability compared with organic electrolyte, so the security of all solid lithium sulphur battery is very good.
Owing to general all solid lithium sulphur battery does not use electrolytic solution, for solid-solid phase contacts between positive and negative electrode with all solid state electrolyte sheet, Gu the contact of-solid phase can cause bigger interface impedance, affect the performance of battery, positive pole at all solid lithium sulphur battery adds the electroconductibility that ionic liquid can improve battery effectively, reduces impedance. And the high-temperature stability of ionic liquid is equally very good, the security of all solid lithium sulphur battery can not be affected, on the other hand, if the contact of positive and negative electrode and all solid state electrolyte sheet does not closely even come off, battery generation open circuit can be made to work, improve contact between the two as much as possible, be the key factor improving all solid lithium sulphur battery performance, evaporation coating method is adopted to be deposited on all solid state electrolyte sheet by metallic lithium, it is possible to obtain one layer of battery lithium negative pole that can not come off.
In sum, all solid lithium sulphur battery, compared with tradition organic system serondary lithium battery, possesses the features such as No leakage, use temperature scope are wide, security height, has great research and probe and value of exploiting and utilizing.
Summary of the invention
1. goal of the invention
It is an object of the invention to provide the preparation method of a kind of all solid lithium sulphur battery, this preparation method can be applied in preparation technology's flow process of lithium cell, has the features such as positive and negative electrode active substance contacts, chemical property height with all solid state electrolyte sheet.
2. technical scheme
The present invention gives a kind of employing solid phase method high temperature sintering and prepare solid state electrolyte sheet, at an evaporation metal lithium of electrolyte sheet as negative pole, the matrix material coating sulphur and carbon to the another side of electrolyte sheet again, as positive pole, finally drips and adds ionic liquid and use aluminum-plastic packaged universal method cell package got up.
The principle of work of the present invention is: take Li by a certain percentage2CO3��Al2O3��GeO2��NH4H2PO4Deng material, through a series of ball milling and heat-processed, then compressing tablet sintering obtains all solid state electrolyte sheet LAGP; The another side making metallic lithium deposit to LAGP sheet by steaming the method for plating is as negative pole; The mixture of sulphur and multi-walled carbon nano-tubes is heated in argon hydrogen environment and obtains matrix material, be then coated onto LAGP sheet one side as positive pole with PVDF as binding agent; Drip at positive pole and add a small amount of ionic liquid; After collector is put on positive and negative electrode surface, use aluminum-plastic packaged encapsulation respectively, obtain all solid lithium sulphur battery that can use.
A preparation method for all solid lithium sulphur battery, its preparation process is as follows:
(1) according to weight ratio Li2CO3: Al2O3: GeO2: NH4H2PO4=3:1:9:20 takes various material, puts into ball grinder with the rotating speed ball milling 4 hours of 300rpm;
(2) being transferred in retort furnace by the mixed powder that step 1 obtains, in air atmosphere, 600 DEG C are heated 1 hour;
(3) mixed powder that step 2 obtains is transferred in ball grinder, with the rotating speed ball milling 4 hours of 300rpm;
(4) being transferred in retort furnace by the mixed powder that step 3 obtains, in air atmosphere, 900 DEG C are heated 10 hours;
(5) mixed powder that step 4 obtains is transferred in ball grinder, with the rotating speed ball milling 4 hours of 300rpm;
(6) mixed powder that step 5 obtains is transferred in mould, press 10 minutes with the pressure of 30MPa, obtain circular electrolyte sheet;
(7) circular electrolyte sheet step 6 obtained, its diameter is 12mm, and thickness is 1mm, is transferred in retort furnace, and in air atmosphere, 900 DEG C are heated 10 hours, obtain target product solid state electrolyte sheet;
(8) solid state electrolyte sheet step 7 obtained is put into and is steamed plating instrument, and in argon gas atmosphere, heating is placed with the evaporation boat of metal lithium sheet, makes the metallic lithium of evaporation deposit on the another side of solid state electrolyte sheet;
(9) sulphur and multi-walled carbon nano-tubes are mixed according to mass ratio 4:1 and grind so that it is mix;
(10) put into tube furnace by step 9 obtains mixed powder, heat 10 hours with 165 DEG C in argon gas atmosphere, naturally cooling;
(11) mixed powder binding agent step 10 obtained mixes according to mass ratio 85:15, it may also be useful to magnetic agitation and add 5ml NMP dispersion become uniform sizing material;
(12) slurry that step 11 obtains is evenly coated in the one side of the solid state electrolyte sheet that step 8 obtains and dries;
(13) ionic liquid two (trimethyl fluoride sulfonyl) 1-ethyl-3-Methylimidazole is dripped it is added in the solid state electrolyte sheet that step 12 obtains and scribbles in the one side of slurry;
(14) solid state electrolyte sheet step 13 obtained is transferred in argon gas atmosphere glove box, with aluminum-plastic packaged coated for solid state electrolyte sheet and seal get up.
The preparation method of described a kind of all solid lithium sulphur battery, in step 1, the ball matter of ball milling is than being 4:1.
The preparation method of described a kind of all solid lithium sulphur battery, in step 2,4,7, temperature rise rate is 2 DEG C/min.
The preparation method of described a kind of all solid lithium sulphur battery, in step 3,5, the ball matter of ball milling is than being 2:1.
The preparation method of described a kind of all solid lithium sulphur battery, in step 11, binding agent is PVDF.
The preparation method of described a kind of all solid lithium sulphur battery, the oven dry Heating temperature in step 12 is 80 DEG C.
The preparation method of described a kind of all solid lithium sulphur battery, the steaming plating time in step 8 is 1 hour.
The preparation method of described a kind of all solid lithium sulphur battery, dripping, in step 13, the ionic liquid added is 0.05ml.
3. useful effect
The present invention uses the method for high temperature solid-phase sintering to prepare all solid state electrolyte sheet, then at the another side evaporation metal lithium of electrolyte sheet as negative pole, the matrix material coating sulphur and carbon nanotube to the one side of electrolyte sheet again is as positive pole, finally positive pole drip add ionic liquid and use aluminum-plastic packaged cell package got up obtain can be practical all solid lithium sulphur battery, its advantage shows: first, the intermediate product that all solid state electrolyte sheet blocks positive discharge contacts with negative pole, protects negative pole metallic lithium; 2nd, the metallic lithium that the sulphur carbon composite being coated on all solid state electrolyte sheet and steaming are plated on all solid state electrolyte sheet all has extraordinary contact with all solid state electrolyte sheet, can not come off; 3rd, all solid state electrolyte sheet and ionic liquid all have good high-temperature stability, so battery system has extraordinary security, it may also be useful to the preparation method of this kind of originality can obtain can practical, security is good, all solid lithium sulphur battery of excellent electrochemical performance.
Four, accompanying drawing explanation
Fig. 1: all solid state electrolyte LAGP SEM Electronic Speculum figure under 5 ��m of resolving power;
Fig. 2: the SEM Electronic Speculum figure of sulphur carbon nano tube compound material under 500nm resolving power;
Fig. 3: steam the SEM Electronic Speculum figure of the metal lithium layer plated under 10 ��m of resolving power;
Fig. 4: all solid state electrolyte LAGP impedance chart;
Fig. 5: impedance chart before and after all solid lithium sulphur battery charging and discharging;
Fig. 6: all solid lithium sulphur battery discharge product X RD;
Fig. 7: all solid lithium sulphur battery is at room temperature chemical property;
Fig. 8: the chemical property of all solid lithium sulphur battery under differing temps and electric current.
Five, embodiment
The preparation method of a kind of all solid lithium sulphur battery, it is characterised in that the step of this preparation method is as follows:
(1) according to weight ratio Li2CO3: Al2O3: GeO2: NH4H2PO4=3:1:9:20 takes various material, puts into ball grinder with the rotating speed ball milling 4 hours of 300rpm, and ball milling ball matter is than being 2:1;
(2) being transferred in retort furnace by the mixed powder that step 1 obtains, in air atmosphere, 600 DEG C are heated 1 hour, and temperature rise rate is 2 DEG C/min;
(3) being transferred in ball grinder by the mixed powder that step 2 obtains, with the rotating speed ball milling 4 hours of 300rpm, ball milling ball matter is than being 2:1;
(4) being transferred in retort furnace by the mixed powder that step 3 obtains, in air atmosphere, 900 DEG C are heated 10 hours, and temperature rise rate is 2 DEG C/min;
(5) being transferred in ball grinder by the mixed powder that step 4 obtains, with the rotating speed ball milling 4 hours of 300rpm, ball milling ball matter is than being 2:1;
(6) mixed powder that step 5 obtains is transferred in mould, press 10 minutes with the pressure of 30MPa, obtain circular electrolyte sheet;
(7) circular electrolyte sheet step 6 obtained, its diameter is 12mm, and thickness is 1mm, is transferred in retort furnace, and in air atmosphere, 900 DEG C are heated 10 hours, and temperature rise rate is 2 DEG C/min, obtains target product solid state electrolyte sheet;
(8) solid state electrolyte sheet step 7 obtained is put into and is steamed plating instrument, and in argon gas atmosphere, heating is placed with the evaporation boat of metal lithium sheet, makes the metallic lithium of evaporation deposit on the another side of solid state electrolyte sheet, and steaming the plating time is 1 hour;
(9) sulphur and multi-walled carbon nano-tubes are mixed according to mass ratio 4:1 and grind so that it is mix;
(10) tube furnace is put into by step 9 obtains mixed powder, with 165 DEG C of heating in argon gas atmosphere
10 hours, naturally cooling;
(11) mixed powder binding agent step 10 obtained mixes according to mass ratio 85:15, it may also be useful to magnetic agitation and add 5ml NMP dispersion become uniform sizing material;
(12) being evenly coated in by the slurry that step 11 obtains in the one side of the solid state electrolyte sheet that step 8 obtains and dry, Heating temperature is 80 degree;
(13) 0.05ml ionic liquid two (trimethyl fluoride sulfonyl) 1-ethyl-3-Methylimidazole is dripped it is added in the solid state electrolyte sheet that step 12 obtains and scribbles in the one side of slurry;
(14) solid state electrolyte sheet step 13 obtained is transferred in argon gas atmosphere glove box, with aluminum-plastic packaged coated for solid state electrolyte sheet and seal get up.
The SEM Electronic Speculum figure of all solid state electrolyte LAGP under 5 ��m of resolving power is as shown in Figure 1, the SEM Electronic Speculum figure of sulphur carbon nano tube compound material under 500nm resolving power is as shown in Figure 2, the SEM Electronic Speculum figure of the metal lithium layer of steaming plating under 10 ��m of resolving power is as shown in Figure 3, all solid state electrolyte LAGP impedance chart is as shown in Figure 4, before and after all solid lithium sulphur battery charging and discharging, impedance chart is as shown in Figure 5, all solid lithium sulphur battery discharge product X RD is as shown in Figure 6, all solid lithium sulphur battery is at room temperature chemical property as shown in Figure 7, the chemical property of all solid lithium sulphur battery under differing temps and electric current is as shown in Figure 8. visible, the intermediate product that all solid state electrolyte sheet blocks positive discharge contacts with negative pole, protects negative pole metallic lithium, the metallic lithium that the sulphur carbon composite being coated on all solid state electrolyte sheet and steaming are plated on all solid state electrolyte sheet all has extraordinary contact with all solid state electrolyte sheet, can not come off, all solid state electrolyte sheet and ionic liquid all have good high-temperature stability, so battery system has extraordinary security, it may also be useful to the preparation method of this kind of originality can obtain can practical, security is good, all solid lithium sulphur battery of excellent electrochemical performance.
Claims (8)
1. the preparation method of an all solid lithium sulphur battery, it is characterised in that the step of this preparation method is as follows:
(1) according to weight ratio Li2CO3: Al2O3: GeO2: NH4H2PO4=3:1:9:20 takes various material, puts into ball grinder with the rotating speed ball milling 4 hours of 300rpm;
(2) being transferred in retort furnace by the mixed powder that step (1) obtains, in air atmosphere, 600 DEG C are heated 1 hour;
(3) mixed powder that step (2) obtains is transferred in ball grinder, with the rotating speed ball milling 4 hours of 300rpm;
(4) being transferred in retort furnace by the mixed powder that step (3) obtains, in air atmosphere, 900 DEG C are heated 10 hours;
(5) mixed powder that step (4) obtains is transferred in ball grinder, with the rotating speed ball milling 4 hours of 300rpm;
(6) mixed powder that step (5) obtains is transferred in mould, press 10 minutes with the pressure of 30MPa, obtain circular electrolyte sheet;
(7) circular electrolyte sheet step (6) obtained, its diameter is 12mm, and thickness is 1mm, is transferred in retort furnace, and in air atmosphere, 900 DEG C are heated 10 hours, obtain target product solid state electrolyte sheet;
(8) the solid state electrolyte sheet that step (7) obtains is put into steaming plating instrument, and in argon gas atmosphere, heating is placed with the evaporation boat of metal lithium sheet, makes the metallic lithium of evaporation deposit on the another side of solid state electrolyte sheet;
(9) sulphur and multi-walled carbon nano-tubes are mixed according to mass ratio 4:1 and grind so that it is mix;
(10) put into tube furnace by step (9) obtains mixed powder, heat 10 hours with 165 DEG C in argon gas atmosphere, naturally cooling;
(11) the mixed powder binding agent that step (10) obtains is mixed according to mass ratio 85:15, it may also be useful to magnetic agitation and add 5ml NMP dispersion become uniform sizing material;
(12) slurry that step (11) obtains is evenly coated in the one side of the solid state electrolyte sheet that step (8) obtains and dries;
(13) ionic liquid two (trimethyl fluoride sulfonyl) 1-ethyl-3-Methylimidazole is dripped it is added in the solid state electrolyte sheet that step (12) obtains and scribbles in the one side of slurry;
(14) the solid state electrolyte sheet that step (13) obtains is transferred in argon gas atmosphere glove box, with aluminum-plastic packaged coated for solid state electrolyte sheet and seal get up.
2. the preparation method of a kind of all solid lithium sulphur battery according to claim 1, it is characterised in that in step (1), the ball matter of ball milling is than being 4:1.
3. the preparation method of a kind of all solid lithium sulphur battery according to claim 1, it is characterised in that in step (2), (4), (7), temperature rise rate is 2 DEG C/min.
4. the preparation method of a kind of all solid lithium sulphur battery according to claim 1, it is characterised in that in step (3), (5), the ball matter of ball milling is than being 2:1.
5. the preparation method of a kind of all solid lithium sulphur battery according to claim 1, it is characterised in that in step (11), binding agent is PVDF.
6. the preparation method of a kind of all solid lithium sulphur battery according to claim 1, it is characterised in that the oven dry Heating temperature in step (12) is 80 DEG C.
7. the preparation method of a kind of all solid lithium sulphur battery according to claim 1, it is characterised in that the steaming plating time in step (8) is 1 hour.
8. the preparation method of a kind of all solid lithium sulphur battery according to claim 1, it is characterised in that dripping, in step (13), the ionic liquid added is 0.05ml.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106784623A (en) * | 2017-01-20 | 2017-05-31 | 江南山 | A kind of multitube lithium-sulfur cell |
| CN108110217A (en) * | 2017-12-19 | 2018-06-01 | 成都亦道科技合伙企业（有限合伙） | A kind of solid state lithium battery composite negative pole and preparation method thereof |
| CN110265723A (en) * | 2018-03-12 | 2019-09-20 | 深圳先进技术研究院 | A kind of preparation method of all-solid-state battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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