CN104681870A - Method for treating microcrystal glass ceramic electrolyte surface - Google Patents
Method for treating microcrystal glass ceramic electrolyte surface Download PDFInfo
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- CN104681870A CN104681870A CN201310645621.0A CN201310645621A CN104681870A CN 104681870 A CN104681870 A CN 104681870A CN 201310645621 A CN201310645621 A CN 201310645621A CN 104681870 A CN104681870 A CN 104681870A
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- glass ceramics
- devitrified glass
- electrolyte sheet
- ceramics electrolyte
- intermediate metal
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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
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Abstract
The invention relates to a method for treating a microcrystal glass ceramic electrolyte surface. The method is characterized by comprising the following manufacturing steps: (1) polishing and pretreating the microcrystal glass ceramic electrolyte surface in sequence; and (2) manufacturing a metal transitional layer at a position, close to the periphery, of one surface of the pretreated microcrystal glass ceramic electrolyte surface to complete a manufacturing process of the microcrystal glass ceramic electrolyte sheet. According to the method disclosed by the invention, the microcrystal glass ceramic electrolyte surface is polished and pretreated to remove impurities and oil dirt which are attached to the surface, and surface unfavorable groups can be removed by washing liquid in the pretreatment process, so that the bonding strength with other substances is enhanced; with the adoption of a magnetron sputtering method, a layer of metal serving as the metal transitional layer is deposited around one surface of the microcrystal glass ceramic electrolyte sheet, so that a firm sealing effect is achieved after the microcrystal glass ceramic electrolyte sheet is sealed with other substances, and the microcrystal glass ceramic electrolyte sheet can be safely sealed and stored for a long time after being sealed with other substances.
Description
Technical field
The invention belongs to lithium battery material technical field, particularly relate to the method for devitrified glass ceramics bath surface process.
Background technology
Devitrified glass ceramics electrolyte sheet is as can laying in for a long time and having the electrochemical system of more high-energy-density and specific power potentiality and become an emerging important directions of lithium series battery research and development.The theoretical specific energy of devitrified glass ceramics electrolyte sheet, far above traditional chemical power source system, is more than ten times of conventional lithium battery energy.Because lithium metal is easy to by aqueous corrosion liberation of hydrogen, cause loss and the potential safety hazard of capacity, current devitrified glass ceramics electrolyte sheet mainly adopts devitrified glass ceramics electrolyte sheet to protect lithium metal.Devitrified glass ceramics electrolyte sheet is electronic body, but the conduction of lithium ion can be realized under electric field action, due to the compact structure of rete own, therefore it can the penetrating of block water molecule completely, and liberation of hydrogen exothermic reaction occurs on the surface avoiding water directly to touch lithium metal.
At present, the method of conventional encapsulation devitrified glass ceramics electrolyte sheet is mostly by PUR encapsulation devitrified glass ceramics electrolyte sheet, can depart from interface because devitrified glass ceramics electrolyte sheet and PUR are under organic electrolyte and aqueous electrolyte environment for a long time, such battery in long-time storage and discharge process from having the danger revealed inefficacy and even blast.
Summary of the invention
The present invention provides one to have secure seal effect for solving in known technology the technical problem that exists, and ensureing after sealing with other material can the method for the devitrified glass ceramics bath surface process of safe storage for a long time.
The present invention includes following technical scheme:
The method of devitrified glass ceramics bath surface process, is characterized in: comprise following making step:
(1) successively polishing, preliminary treatment are carried out to devitrified glass ceramics electrolyte sheet surface;
(2) devitrified glass ceramics electrolyte sheet one side is after the pre-treatment upper makes intermediate metal near surrounding place, completes the manufacturing process of devitrified glass ceramics electrolyte sheet of the present invention.
The present invention can also adopt following technical measures:
Described devitrified glass ceramics electrolyte sheet surface finish process comprises: with 5000 ~ 7000 object polishing sand papers, is carried out the polishing of rotating speed 80 ~ 150rpm, 10 ~ 30min by polisher lapper in devitrified glass ceramics electrolyte sheet one side.
Described devitrified glass ceramics electrolyte sheet preprocessing process comprises:
(1) in supersonic wave cleaning machine, with ethanol or acetone organic solvent to the ultrasonic immersion 5 ~ 30min of devitrified glass ceramics electrolyte sheet, the surface and oil contaminant of removing devitrified glass ceramics electrolyte sheet;
(2) by except the devitrified glass ceramics electrolyte sheet after degreasing is at dense H
2sO
4+ K
2cr
2o
71 ~ 20min is soaked in washing lotion;
(3) the devitrified glass ceramics electrolyte sheet ultrasonic cleaning after washing lotion being soaked with deionized water 3 ~ 6 times, the time of each ultrasonic cleaning is 5 ~ 15min;
(4) the devitrified glass ceramics electrolyte sheet after cleaning is placed in vacuum drying chamber, at 50 ~ 100 DEG C of temperature, dry 3 ~ 12h, completes the preprocessing process of devitrified glass ceramics electrolyte sheet.
Described step (2) in the manufacturing process of intermediate metal comprise:
(1) adopt magnetron sputtering apparatus, in inert gas Ar environment, using with devitrified glass ceramics electrolyte sheet surface deposition one deck aluminium of aluminum plastic film bonding site, titanium or nickel dam as intermediate metal;
(2) respectively degreasing, bright dipping and Passivation Treatment are carried out to intermediate metal.
Described ungrease treatment be by intermediate metal in concentration be 1 ~ 5% C106 degreaser in soak 10 ~ 60s, with deionized water rinsing 30 ~ 180s after taking out; It is soak 5 ~ 30s in the light-emitting solution of 30 ~ 80%D140 in concentration that described bright dipping is treated to the intermediate metal after by ungrease treatment, with deionized water rinsing 30 ~ 180s after taking out; Described Passivation Treatment be by bright dipping process after intermediate metal soak 30 ~ 120s, with deionized water rinsing 30 ~ 180s after taking out at the B901 passivating solution that concentration is 1 ~ 10%.
The advantage that the present invention has and good effect:
The present invention, by carrying out polishing, preliminary treatment to devitrified glass ceramics electrolyte sheet surface, eliminates impurity and the greasy dirt of its surface attachment, and removes surperficial unfavorable group by washing lotion in preprocessing process, adds the adhesion with other material; Adopt magnetron sputtering mode deposition layer of metal around devitrified glass ceramics electrolyte sheet one side as intermediate metal, after sealing with other material, to have secure seal effect, can store by sealingly secure for a long time after guarantee and other material seal.
Accompanying drawing explanation
Fig. 1 is the devitrified glass ceramics electrolyte sheet that the present invention makes;
Fig. 2 is the structural representation adopting the water system lithium cell made.
In figure: 1-aluminum plastic film, 2-PUR, 3-intermediate metal, 4-devitrified glass ceramics electrolyte sheet, 5-lithium metal.
Embodiment
For summary of the invention of the present invention, Characteristic can be disclosed further, be also described in detail as follows by reference to the accompanying drawings especially exemplified by following instance.
The method of devitrified glass ceramics bath surface process, is characterized in: comprise following making step:
(1) successively polishing, preliminary treatment are carried out to devitrified glass ceramics electrolyte sheet surface;
(2) devitrified glass ceramics electrolyte sheet one side is after the pre-treatment upper makes intermediate metal near surrounding place, completes the manufacturing process of devitrified glass ceramics electrolyte sheet of the present invention.
Described devitrified glass ceramics electrolyte sheet surface finish process comprises: with 5000 ~ 7000 object polishing sand papers, is carried out the polishing of rotating speed 80 ~ 150rpm, 10 ~ 30min by polisher lapper in devitrified glass ceramics electrolyte sheet one side.
Described devitrified glass ceramics electrolyte sheet preprocessing process comprises:
(1) in supersonic wave cleaning machine, with ethanol or acetone organic solvent to the ultrasonic immersion 5 ~ 30min of devitrified glass ceramics electrolyte sheet, the surface and oil contaminant of removing devitrified glass ceramics electrolyte sheet;
(2) by except the devitrified glass ceramics electrolyte sheet after degreasing is at dense H
2sO
4+ K
2cr
2o
71 ~ 20min is soaked in washing lotion;
(3) the devitrified glass ceramics electrolyte sheet ultrasonic cleaning after washing lotion being soaked with deionized water 3 ~ 6 times, the time of each ultrasonic cleaning is 5 ~ 15min;
(4) the devitrified glass ceramics electrolyte sheet after cleaning is placed in vacuum drying chamber, at 50 ~ 100 DEG C of temperature, dry 3 ~ 12h, completes the preprocessing process of devitrified glass ceramics electrolyte sheet.
Described step (2) in the manufacturing process of intermediate metal comprise:
(1) adopt magnetron sputtering apparatus, in inert gas Ar environment, using with devitrified glass ceramics electrolyte sheet surface deposition one deck aluminium of aluminum plastic film bonding site, titanium or nickel dam as intermediate metal;
(2) respectively degreasing, bright dipping and Passivation Treatment are carried out to intermediate metal.
Described ungrease treatment be by intermediate metal in concentration be 1 ~ 5% C106 degreaser in soak 10 ~ 60s, with deionized water rinsing 30 ~ 180s after taking out; It is soak 5 ~ 30s in the light-emitting solution of 30 ~ 80%D140 in concentration that described bright dipping is treated to the intermediate metal after by ungrease treatment, with deionized water rinsing 30 ~ 180s after taking out; Described Passivation Treatment be by bright dipping process after intermediate metal soak 30 ~ 120s, with deionized water rinsing 30 ~ 180s after taking out at the B901 passivating solution that concentration is 1 ~ 10%.
Embodiment:
1. take and be of a size of 20 × 20mm, the devitrified glass ceramics electrolyte sheet 4 of thick 0.5mm, use precise grinding polisher, polishing sand paper 7000 order, polishing rotating speed 110rpm, polishing time 20min, carry out polishing to devitrified glass ceramics electrolyte sheet;
2. after polishing completes, devitrified glass ceramics electrolyte sheet is placed in the ultrasonic immersion treatment 20min of supersonic wave cleaning machine acetone, the surface and oil contaminant of removing devitrified glass ceramics electrolyte sheet; Taking-up puts into dense H after drying
2sO
4+ K
2cr
2o
7soak 10min in washing lotion, use deionized water ultrasonic cleaning 5 times after completing, the time of each ultrasonic cleaning is 10min; Devitrified glass ceramics electrolyte sheet after cleaning is put into vacuum drying chamber 70 DEG C of dry 10h, completes the preprocessing process of devitrified glass ceramics electrolyte sheet;
3. adopt SP-3 magnetron sputtering apparatus, base vacuum is evacuated to 3 × 10
-3, sputtering pressure 1pa, sputtering power 2w/cm
2, the devitrified glass ceramics electrolyte sheet one side place of the keeping to the side deposition one deck completed in preliminary treatment is wide is about the Titanium making intermediate metal 3 of 500nm for 2mm thickness;
4. be soak 20s in 3% degreaser by intermediate metal in C106 concentration, use deionized water rinsing 120s after taking out, complete the ungrease treatment of intermediate metal;
5. be soak 10s in the light-emitting solution of 50% in D140 concentration by the intermediate metal after ungrease treatment, use deionized water rinsing 120s after taking out, complete the bright dipping process of intermediate metal;
6. the intermediate metal after bright dipping process is soaked 60s at the passivating solution that B901 concentration is 3%, use deionized water rinsing 120s after taking out, complete the manufacturing process of devitrified glass ceramics electrolyte sheet as shown in Figure 1.
The devitrified glass ceramics electrolyte sheet adopting the present invention to make makes aqueous systems lithium metal battery:
As shown in Figure 2, PUR 2 is placed between the intermediate metal 3 on the devitrified glass ceramics electrolyte sheet 4 of the aluminum plastic film 1 that lithium metal 5 is housed and the present invention's making, adopts hot press that aluminum plastic film and intermediate metal sealing are hot pressed into one; Bet into PC+EC+DMC=1:1:1,1M LiPF in dry atmosphere
6electrolyte, completes the manufacturing process of aqueous systems lithium metal battery as shown in Figure 2.
Seal tightness test is carried out to aqueous systems lithium metal battery in Fig. 2: the aqueous systems lithium metal battery after having encapsulated is immersed NH
4in the 4Mol/L LiCl that Cl is saturated, after placing 30 days, disassemble under dry atmosphere, interior metal lithium has no corrosion.Test proves, devitrified glass ceramics electrolyte sheet prepared by the present invention is by the devitrified glass ceramics electrolyte sheet after surface processes makes intermediate metal, there is not leakage problem being in for a long time under organic and aqueous electrolyte environment in the lithium metal of encapsulation, greatly improves the stability of aqueous systems lithium metal battery in discharge process and fail safe.
Although be described the preferred embodiments of the present invention by reference to the accompanying drawings above; but the present invention is not limited to above-mentioned embodiment; above-mentioned embodiment is only schematic; be not restrictive; those of ordinary skill in the art is under enlightenment of the present invention; not departing under the ambit that present inventive concept and claim protect, a lot of form can also be made.These all belong within protection scope of the present invention.
Claims (5)
1. the method for devitrified glass ceramics bath surface process, is characterized in that: comprise following making step:
(1) successively polishing, preliminary treatment are carried out to devitrified glass ceramics electrolyte sheet surface;
(2) devitrified glass ceramics electrolyte sheet one side is after the pre-treatment upper makes intermediate metal near surrounding place, completes the manufacturing process of devitrified glass ceramics electrolyte sheet of the present invention.
2. the method for devitrified glass ceramics bath surface according to claim 1 process, it is characterized in that: described devitrified glass ceramics electrolyte sheet surface finish process comprises: with 5000 ~ 7000 object polishing sand papers, carried out the polishing of rotating speed 80 ~ 150rpm, 10 ~ 30min by polisher lapper in devitrified glass ceramics electrolyte sheet one side.
3. the method for devitrified glass ceramics bath surface according to claim 1 process, is characterized in that: described devitrified glass ceramics electrolyte sheet preprocessing process comprises:
(1) in supersonic wave cleaning machine, with ethanol or acetone organic solvent to the ultrasonic immersion 5 ~ 30min of devitrified glass ceramics electrolyte sheet, the surface and oil contaminant of removing devitrified glass ceramics electrolyte sheet;
(2) by except the devitrified glass ceramics electrolyte sheet after degreasing is at dense H
2sO
4+ K
2cr
2o
71 ~ 20min is soaked in washing lotion;
(3) the devitrified glass ceramics electrolyte sheet ultrasonic cleaning after washing lotion being soaked with deionized water 3 ~ 6 times, the time of each ultrasonic cleaning is 5 ~ 15min;
(4) the devitrified glass ceramics electrolyte sheet after cleaning is placed in vacuum drying chamber, at 50 ~ 100 DEG C of temperature, dry 3 ~ 12h, completes the preprocessing process of devitrified glass ceramics electrolyte sheet.
4. the method for devitrified glass ceramics bath surface according to claim 1 process, is characterized in that: described step (2) in the manufacturing process of intermediate metal comprise:
(1) adopt magnetron sputtering apparatus, in inert gas Ar environment, using with devitrified glass ceramics electrolyte sheet surface deposition one deck aluminium of aluminum plastic film bonding site, titanium or nickel dam as intermediate metal;
(2) respectively degreasing, bright dipping and Passivation Treatment are carried out to intermediate metal.
5. the method for devitrified glass ceramics bath surface according to claim 4 process, it is characterized in that: described ungrease treatment be by intermediate metal in concentration be 1 ~ 5% C106 degreaser in soak 10 ~ 60s, with deionized water rinsing 30 ~ 180s after taking out; It is soak 5 ~ 30s in the light-emitting solution of 30 ~ 80%D140 in concentration that described bright dipping is treated to the intermediate metal after by ungrease treatment, with deionized water rinsing 30 ~ 180s after taking out; Described Passivation Treatment be by bright dipping process after intermediate metal soak 30 ~ 120s, with deionized water rinsing 30 ~ 180s after taking out at the B901 passivating solution that concentration is 1 ~ 10%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310645621.0A CN104681870A (en) | 2013-12-03 | 2013-12-03 | Method for treating microcrystal glass ceramic electrolyte surface |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310645621.0A CN104681870A (en) | 2013-12-03 | 2013-12-03 | Method for treating microcrystal glass ceramic electrolyte surface |
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| Publication Number | Publication Date |
|---|---|
| CN104681870A true CN104681870A (en) | 2015-06-03 |
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|---|---|---|---|
| CN201310645621.0A Pending CN104681870A (en) | 2013-12-03 | 2013-12-03 | Method for treating microcrystal glass ceramic electrolyte surface |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109719081A (en) * | 2018-12-29 | 2019-05-07 | 华中光电技术研究所（中国船舶重工集团有限公司第七一七研究所） | A kind of cleaning method of devitrified glass |
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| 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 |
| CN101702444A (en) * | 2004-02-06 | 2010-05-05 | 波利普拉斯电池有限公司 | Protected active metal electrode and battery cell structures with non-aqueous interplayer architecture |
| CN102354735A (en) * | 2011-08-29 | 2012-02-15 | 能一郎科技股份有限公司 | Method for preparing aluminum, nickel and copper tabs for flexibly packaged or polymer lithium ion power battery |
-
2013
- 2013-12-03 CN CN201310645621.0A patent/CN104681870A/en active Pending
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 |
| CN101702444A (en) * | 2004-02-06 | 2010-05-05 | 波利普拉斯电池有限公司 | Protected active metal electrode and battery cell structures with non-aqueous interplayer architecture |
| CN102354735A (en) * | 2011-08-29 | 2012-02-15 | 能一郎科技股份有限公司 | Method for preparing aluminum, nickel and copper tabs for flexibly packaged or polymer lithium ion power battery |
Non-Patent Citations (1)
| Title |
|---|
| 杜国华: "《实用工程材料焊接手册》", 31 August 2004, 机械工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109719081A (en) * | 2018-12-29 | 2019-05-07 | 华中光电技术研究所（中国船舶重工集团有限公司第七一七研究所） | A kind of cleaning method of devitrified glass |
| CN109719081B (en) * | 2018-12-29 | 2021-07-06 | 华中光电技术研究所（中国船舶重工集团有限公司第七一七研究所） | Method for cleaning microcrystalline glass |
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Application publication date: 20150603 |