CN102655250B - Solid electrolyte for lithium air cells and preparation method thereof - Google Patents
Solid electrolyte for lithium air cells and preparation method thereof Download PDFInfo
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- CN102655250B CN102655250B CN201210110017.3A CN201210110017A CN102655250B CN 102655250 B CN102655250 B CN 102655250B CN 201210110017 A CN201210110017 A CN 201210110017A CN 102655250 B CN102655250 B CN 102655250B
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- solid electrolyte
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- mixture
- electrolyte
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- 239000007784 solid electrolyte Substances 0.000 title claims abstract description 24
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims description 9
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 20
- 239000003792 electrolyte Substances 0.000 claims abstract description 18
- 239000002202 Polyethylene glycol Substances 0.000 claims description 14
- 229920001223 polyethylene glycol Polymers 0.000 claims description 14
- 238000007731 hot pressing Methods 0.000 claims description 13
- 229910003002 lithium salt Inorganic materials 0.000 claims description 12
- 159000000002 lithium salts Chemical class 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 8
- 229910052582 BN Inorganic materials 0.000 claims description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 5
- 229910005793 GeO 2 Inorganic materials 0.000 claims description 5
- 239000000428 dust Substances 0.000 claims description 4
- 229910015015 LiAsF 6 Inorganic materials 0.000 claims description 2
- 229910013063 LiBF 4 Inorganic materials 0.000 claims description 2
- 229910013684 LiClO 4 Inorganic materials 0.000 claims description 2
- 229910013398 LiN(SO2CF2CF3)2 Inorganic materials 0.000 claims description 2
- 229910013870 LiPF 6 Inorganic materials 0.000 claims description 2
- 230000000994 depressogenic effect Effects 0.000 claims description 2
- 230000004927 fusion Effects 0.000 claims description 2
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 7
- 239000001301 oxygen Substances 0.000 abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 abstract description 7
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 231100000331 toxic Toxicity 0.000 abstract description 2
- 230000002588 toxic effect Effects 0.000 abstract description 2
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 abstract 4
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 abstract 4
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 abstract 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 2
- 229910052593 corundum Inorganic materials 0.000 abstract 2
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 abstract 2
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 2
- 239000010409 thin film Substances 0.000 abstract 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 12
- 239000011888 foil Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910013872 LiPF Inorganic materials 0.000 description 2
- 101150058243 Lipf gene Proteins 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000005030 aluminium foil Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910052493 LiFePO4 Inorganic materials 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
The invention discloses a solid electrolyte for lithium air cells. The solid electrolyte comprises a thin film prepared from a mixture of Al2O3, Li2O, GeO2 and P2O5, wherein the molar ratio of Al2O3 to Li2O to GeO2 to P2O5 is 1: (2.5-3.5): (5.5-6.5): (5.5-6.5). According to the invention, because a solid electrolyte is adopted, and no organic solvent is used, an air positive electrode is not flooded by the electrolyte, thereby solving the problem that in the process of discharge, the oxygen supply is insufficient and the cycle performance of the cell is reduced; and the solid electrolyte is environment-friendly, so that the harms that an electrolyte for traditional lithium ion cells is toxic and volatile are avoided.
Description
Technical field
The present invention relates to solid electrolyte of a kind of lithium-air battery and preparation method thereof.
Background technology
Along with day by day consuming and energy demand growing of fossil energy, extremely urgent to the research and development of novel energy material.Electric energy is as far back as eighties of last century popularization and application, and battery is one of common tool using electric energy, and studying now and applying is lithium ion battery more widely.Because lithium ion battery energy density is high, long service life, the advantages such as the low and memory-less effect of self-discharge rate, lithium ion battery is just receiving World Science man's concern.But current business-like lithium ion battery is main still based on LiCoO
2deng the rocking chair mechanism of lithium ion inlay compound, positive electrode becomes the restriction of lithium ion battery energy density, and end-point energy density can only reach 400Wh/Kg, so the unbearable important task of lithium ion battery, finds new electrochemical power source approach imperative.
The research of lithium-air battery is arisen at the historic moment, it is taking lithium metal as negative pole, the porous electrode being made up of carbon-based material is anodal, in discharge process, lithium metal loses battery at negative pole becomes lithium ion, and electronics arrives porous anode by external circuit, by airborne oxygen reduction, this reaction continues to carry out, and battery just can provide energy to load.Charging process is just in time contrary, and under the effect of charging voltage, the discharging product producing in discharge process is first oxidized at porous anode, again emit oxygen, lithium ion is reduced into lithium metal at negative pole, treats that this process carries out completely, and battery can provide energy to load again again.As can be seen here, lithium-air battery can not produce environmentally harmful material in whole charge and discharge process, is the green process of zero pollution completely.
Another significant advantage of lithium-air battery be exactly anodal active material oxygen be to be directed to surrounding air, because of but inexhaustible, and do not need to be stored in inside battery, so not only reduced cost but also alleviated the weight of battery, so the energy density of battery depends on lithium metal one side completely.Calculated and can be drawn by theory, the energy density of lithium-air battery can reach the superelevation theoretical energy density of 13200Wh/Kg, and this energy density is enough to compare favourably with gasoline, thereby is expected to replace completely gasoline, really realizes pure electric automobile.
Lithium-air battery has huge application potential, but at present research is not yet ripe, still has the solution that requires study of many key technology points.For example, using airborne oxygen as positive active material, inevitable requirement positive electrode can be conducive to oxygen molecule rapid diffusion, with the electronics fast reaction of battery.And for example, traditional lithium ion battery adopts organic electrolyte, and surface tension can make oil loving air electrode be flooded by electrolyte, is unfavorable for forming diffusion electrode, and oxygen supply deficiency when guiding discharge reduces cycle performance of battery.
Summary of the invention
The object of this invention is to provide solid electrolyte of a kind of lithium-air battery and preparation method thereof.
The technical solution used in the present invention is:
A solid electrolyte for lithium-air battery, comprises that by mol ratio be 1:(2.5-3.5): (5.5-6.5): Al (5.5-6.5)
2o
3, Li
2o, GeO
2, P
2o
5the film made of mixture.
Also comprise the film of being made up of the mixture of polyethylene glycol oxide, lithium salts electrolyte, boron nitride, taking three's quality sum as 100% calculating, lithium salts electrolyte is 18-25wt%, and boron nitride is 8-16wt%, and surplus is polyethylene glycol oxide.
Also comprise by polyethylene glycol oxide, lithium salts electrolyte, Li
2the film that the mixture of O is made, taking three's quality sum as 100% calculating, lithium salts electrolyte is 18-25wt%, Li
2o is 8-16wt%, and surplus is polyethylene glycol oxide.
Described lithium salts electrolyte is LiPF
6, LiClO
4, LiAsF
6, LiBF
4, LiN (SO
2cF
2cF
3)
2in one.
The preparation method of the solid electrolyte of lithium-air battery, comprises the following steps:
1) by mixture melt, abrasive dust, flattens, and sintering, obtains the first film;
2) mixture is mixed, ball milling, hot pressing, to 200-400 μ m, obtains the second film;
3) mixture is mixed, ball milling, hot pressing, to 200-400 μ m, obtains the 3rd film;
4) the first film is clipped between B and C, is depressed into 800-1000 μ m, obtain solid electrolyte.
In step 1), fusion temperature is 1200-1400 DEG C.
In step 1), sintering temperature is 800-1000 DEG C.
In step 1), sintering time is 1-2h.
The invention has the beneficial effects as follows: the present invention adopts solid electrolyte, there is no organic solvent, air positive pole can not flooded by electrolyte, oxygen supply deficiency while solving electric discharge, the problem of reduction cycle performance of battery.And environmentally friendly, the harm that solves the electrolyte toxic and volatile of traditional lithium ion battery.
Brief description of the drawings
Fig. 1 is battery structure schematic diagram.
Fig. 2 is specific capacity-cycle-index curve chart of the battery that contains solid electrolyte of the present invention.
Embodiment
Below in conjunction with specific embodiment, the present invention is described further:
Below relate to the step 2 of hot pressing), 3) in, hot pressing pressure is 25-30MPa, hot pressing time is 0.5-1h.
embodiment 1:
1) by Al
2o
3, Li
2o, GeO
2, P
2o
5press the mixed in molar ratio of 1:3:6:6, fusing at 1400 DEG C, abrasive dust, then flattens, and at 1000 DEG C, sintering 1h, obtains the first film, and the thickness of film is 400 μ m;
2) by the LiPF of the polyethylene glycol oxide of 60wt%, 25wt%
6mix with the BN of 15wt%, ball milling, hot pressing to 400 μ m at 1000 DEG C, obtains the second film;
3) by the LiPF of the polyethylene glycol oxide of 60wt%, 25wt%
6li with 15wt%
2o mixes, ball milling, and hot pressing to 400 μ m at 1000 DEG C, obtains the 3rd film;
4) the first film is clipped in respectively between the second film and the 3rd film, hot pressing to 1000 μ m at 1000 DEG C, obtains solid electrolyte.
embodiment 2:
1) by Al
2o
3, Li
2o, GeO
2, P
2o
5press the mixed in molar ratio of 1:2.5:5.5:5.5, fusing at 1200 DEG C, abrasive dust, then flattens, and at 800 DEG C, sintering 2h, obtains the first film, and the thickness of film is 400 μ m;
2) by the LiClO of the polyethylene glycol oxide of 70wt%, 18wt%
4mix with the BN of 12wt%, ball milling, hot pressing to 400 μ m at 1000 DEG C, obtains the second film;
3) by the LiClO of the polyethylene glycol oxide of 70wt%, 18wt%
4li with 12wt%
2o mixes, ball milling, and hot pressing to 400 μ m at 1000 DEG C, obtains the 3rd film;
4) the first film is clipped in respectively between the second film and the 3rd film, hot pressing to 1000 μ m at 1000 DEG C, obtains solid electrolyte.
By LiFePO4, acetylene black, PVDF, mass ratio taking mass ratio as 7:2:1 is dissolved in NMP, make slurry, be coated on again on aluminium foil, oven dry, compacting, be cut to the disk of 1 cm, make anodal layer, taking metallic lithium foil as negative electrode layer, electrolyte adopts the solid electrolyte of embodiment 1, composition battery, further, in conjunction with Fig. 1, battery structure of the present invention is described, this lithium-air battery has anode coat 4(plastic housing), in the inside bottom surface of anode coat 4, form aluminium foil 6 as negative current collector, with cathode conductor 2(1mm diameter steel bar) be connected; On negative current collector, form metallic lithium foil 5 as negative electrode layer; The copper bar of anodal layer 9 and positive wire 1(1mm diameter) be connected; Between negative electrode layer and anodal layer, configure three layers of solid electrolyte; Metallic lithium foil 5 and the 3rd film 7 are fitted, anodal layer 9 and the second film 13 are fitted, the first film 8 is between the second film 13 and the 3rd film 7, outside the anode coat 4 of this battery, be also provided with anodal shell 3(steel casing), between anode coat 4 and anodal shell 3, being provided with sealing ring 12(sealing ring material is the M-11 lithium ion battery fluid sealant that Harbin Jingcheng Battery Sealant Co., Ltd produces).
Being assembled in the anhydrous glove box of anaerobic (MBRAUN, LabMater100, Germany) that is full of argon gas of battery carried out.
Above-mentioned sample is carried out to constant current charge-discharge test with electrochemical workstation, current density is 40mA/cm
2, voltage range is controlled between 2.0-4.8 V, circulates 50 times, and the specific capacity-cycle-index curve obtaining is as Fig. 2.As can be seen from Figure 2, the battery taking solid electrolyte as part of the present invention has good cycle charge discharge electrical property.
Claims (5)
1. a solid electrolyte for lithium-air battery, is characterized in that: comprise that by mol ratio be 1:(2.5-3.5): (5.5-6.5): Al (5.5-6.5)
2o
3, Li
2o, GeO
2, P
2o
5the film made of mixture; Also comprise the film of being made up of the mixture of polyethylene glycol oxide, lithium salts electrolyte, boron nitride, taking three's quality sum as 100% calculating, lithium salts electrolyte is 18-25wt%, and boron nitride is 8-16wt%, and surplus is polyethylene glycol oxide; Also comprise by polyethylene glycol oxide, lithium salts electrolyte, Li
2the film that the mixture of O is made, taking three's quality sum as 100% calculating, lithium salts electrolyte is 18-25wt%, Li
2o is 8-16wt%, and surplus is polyethylene glycol oxide; Described lithium salts electrolyte is LiPF
6, LiClO
4, LiAsF
6, LiBF
4, LiN (SO
2cF
2cF
3)
2in one.
2. the preparation method of the solid electrolyte of lithium-air battery claimed in claim 1, is characterized in that: comprise the following steps:
1) be 1:(2.5-3.5 by mol ratio): (5.5-6.5): Al (5.5-6.5)
2o
3, Li
2o, GeO
2, P
2o
5mixture melt, abrasive dust, flatten, sintering, obtains the first film;
2) mixture is mixed, ball milling, hot pressing, to 200-400 μ m, obtains the second film; Described mixture is the mixture of the polyethylene glycol oxide described in claim 1, lithium salts electrolyte, boron nitride;
3) mixture is mixed, ball milling, hot pressing, to 200-400 μ m, obtains the 3rd film; Described mixture is the polyethylene glycol oxide described in claim 1, lithium salts electrolyte, Li
2the mixture of O;
4) the first film is clipped between the second film and the 3rd film, is depressed into 800-1000 μ m, obtain solid electrolyte.
3. the preparation method of the solid electrolyte of a kind of lithium-air battery according to claim 2, is characterized in that: in step 1), fusion temperature is 1200-1400 DEG C.
4. the preparation method of the solid electrolyte of a kind of lithium-air battery according to claim 2, is characterized in that: in step 1), sintering temperature is 800-1000 DEG C.
5. the preparation method of the solid electrolyte of a kind of lithium-air battery according to claim 2, is characterized in that: in step 1), sintering time is 1-2h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210110017.3A CN102655250B (en) | 2012-04-16 | 2012-04-16 | Solid electrolyte for lithium air cells and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210110017.3A CN102655250B (en) | 2012-04-16 | 2012-04-16 | Solid electrolyte for lithium air cells and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN102655250A CN102655250A (en) | 2012-09-05 |
| CN102655250B true CN102655250B (en) | 2014-09-17 |
Family
ID=46730830
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|---|---|---|---|
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108011078B (en) * | 2016-11-01 | 2020-02-14 | 中山大学 | Flexible substrate-based electrode assembly and preparation method of lithium-oxygen thin film battery |
| CN108023145B (en) * | 2016-11-01 | 2019-11-19 | 中山大学 | Electrode assembly, lithium-oxygen thin film battery and preparation method |
| CN111446490B (en) * | 2019-04-10 | 2021-09-17 | 西安瑞智材料科技有限公司 | Single-layer boron nitride modified PEO polymer electrolyte and preparation method thereof |
| CN114478328A (en) * | 2020-10-27 | 2022-05-13 | 上海漫关越水处理有限公司 | Ionic membrane compound of lithium air battery tert-aryl ether diene difluoromethyl sulfonate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1726608A (en) * | 2002-10-15 | 2006-01-25 | 波利普拉斯电池有限公司 | Ionically conductive membranes for protection of active metal anodes |
| CN1925203A (en) * | 2005-08-31 | 2007-03-07 | 株式会社小原 | Lithium ion secondary battery and solid electrolyte therefor |
| CN1938895A (en) * | 2004-02-06 | 2007-03-28 | 波利普拉斯电池有限公司 | Protected active metal electrode and battery cell structures with non-aqueous interlayer architecture |
-
2012
- 2012-04-16 CN CN201210110017.3A patent/CN102655250B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1726608A (en) * | 2002-10-15 | 2006-01-25 | 波利普拉斯电池有限公司 | Ionically conductive membranes for protection of active metal anodes |
| CN1938895A (en) * | 2004-02-06 | 2007-03-28 | 波利普拉斯电池有限公司 | Protected active metal electrode and battery cell structures with non-aqueous interlayer architecture |
| CN1925203A (en) * | 2005-08-31 | 2007-03-07 | 株式会社小原 | Lithium ion secondary battery and solid electrolyte therefor |
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| CN102655250A (en) | 2012-09-05 |
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