CN105576276A - Vacuum liquid injection device - Google Patents

Vacuum liquid injection device Download PDF

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Publication number
CN105576276A
CN105576276A CN201410542481.9A CN201410542481A CN105576276A CN 105576276 A CN105576276 A CN 105576276A CN 201410542481 A CN201410542481 A CN 201410542481A CN 105576276 A CN105576276 A CN 105576276A
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China
Prior art keywords
vacuum
connector
electrolyte
connecting tube
clave
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CN201410542481.9A
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CN105576276B (en
Inventor
王可
杜兆龙
马万顺
卢威
陈立桅
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Suzhou Institute of Nano Tech and Nano Bionics of CAS
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Suzhou Institute of Nano Tech and Nano Bionics of CAS
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

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  • Secondary Cells (AREA)
  • Filling, Topping-Up Batteries (AREA)

Abstract

The invention relates to a vacuum liquid injection device. The vacuum liquid injection device comprises a vacuum chamber, Kolafu joints, a vacuum-pumping part and an injection device with an electrolyte. A base, side walls and a top cover form the vacuum chamber. The Kolafu joint is inserted into an opening of the top cover. The vacuum-pumping part comprises a connection pipe, a flexible pipe and a vacuum pump. Two ends of the flexible pipe are respectively connected to the vacuum pump and the connection pipe. The Kolafu joints comprise a first Kolafu joint for connecting the connection pipe and the vacuum chamber and a second Kolafu joint for connecting the injection device with the electrolyte and the vacuum chamber. Each one of the Kolafu joints comprises a housing, a sealing cover and a communication duct, has good leakproofness and realizes vacuum-pumping and liquid injection functions through cooperating with the vacuum-pumping part and the injection device with the electrolyte. The vacuum liquid injection device has a simple structure, a small volume and good liquid injection effects, realizes accurate liquid injection, has a fast liquid injection rate and satisfies injection demands of different electrolytes.

Description

A kind of vacuum electrolyte filling device
Technical field
The present invention relates to battery production equipment field, in particular for the vacuum electrolyte filling device of battery.
Background technology
Along with the fast development of mechanics of communication and intelligent system, people for the battery of various equipment or the energy storage demand of ultracapacitor more and more higher, such as mobile phone, notebook computer or palmtop PC etc.
In actual applications, button cell and ultracapacitor, all gradually towards the future development using thick electrode sheet, by the surface density using thick electrode sheet to improve active material on electrode slice, thus improve energy storage capacity.But, use thick electrode sheet will inevitably face electrolyte and infiltrate insufficient problem in thick electrode sheet, the active material in electrode is caused to be difficult to obtain effective performance, the energy storage capacity of battery still cannot improve, so one of problem of solution of having to when the infiltration problem of electrode slice is and studies button cell and ultracapacitor.
Patent CN201562708U discloses a kind of device for filling lithium battery with electrolyte in vacuuming manner, comprises frame, battery positioning and driving mechanism, battery vacuum liquid injection controlling organization, electrolyte filling mechanism, the exquisite mechanism of electrolyte, battery charging and discharging mechanism.Realized the automatic job of battery by battery charging and discharging mechanism, inject electrolyte by battery vacuum liquid injection controlling organization.
Patent CN202662706U discloses a kind of vacuum liquid injection machine for lithium ion battery, comprises frame, vacuum liquid filling mechanism, battery main body heating pressing mechanism and feedback control system.This filling machine can heating battery main body while vacuum liquid filling, improves electrolyte to the effect of impregnation of electrode.
Although in prior art, to some extent solved the infiltration problem of electrode slice by vacuum liquid filling technology, but still there are some defects:
(1) complex structure of vacuum electrolyte filling device, volume are larger.Operation and the control of this kind of vacuum electrolyte filling device are often comparatively loaded down with trivial details, and equipment is expensive.Its huge volume also cannot carry out fluid injection by the button cell less to size in addition.
(2) directly electrolyte poor effect is dripped.Generally pass through directly to drip electrolyte on electrode slice for the battery that size is less, liquid to be electrolysed infiltrates naturally to electrode slice.But for thick electrode sheet, this natural pattern of invasion is not enough to realize the complete wetting of electrolyte to thick electrode sheet.
(3) reservoir quantity precision is difficult to control, and fluid injection speed is slow.Existing vacuum electrolyte filling device often accurately cannot control reservoir quantity, or in order to regulate reservoir quantity to affect fluid injection speed, this wastes electrolyte on the one hand, causes the reservoir quantity of every block battery inconsistent on the other hand, affects product quality.
(4), when injecting different electrolytes, easily cross pollution is produced.To in the development process of battery, frequent needs inject different electrolyte to test effect on electrode slice, fluid injection parts in existing vacuum electrolyte filling device are often all fixedly installed, be difficult to change, or replacement cost is higher, so inject with same fluid injection parts the problem that different electrolyte will inevitably bring cross pollution.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of vacuum electrolyte filling device, has that volume is little simultaneously, fluid injection is fast and reservoir quantity can accurately control, fluid injection parts are easy to the multiple beneficial effects such as replacing.
The invention provides a kind of vacuum electrolyte filling device, comprise vacuum chamber, Clave connector, vacuumizing part and the syringe of electrolyte is housed, described vacuum chamber is enclosed by base, sidewall and top cover and forms, some perforates for plugging described Clave connector are provided with in described top cover, described vacuumizing part comprises tube connector, flexible pipe and vacuum pump, described flexible pipe one end connects described vacuum pump, and the other end connects described tube connector;
Described Clave connector comprises shell, seal cover and connecting tube, the inside up/down perforation of described shell, the inside of described connecting tube is a cavity, and the top of described connecting tube is a sharp-pointed portion of taper, the sidewall in described sharp-pointed portion is provided with at least one through hole, and described through hole is communicated in the internal cavities of described connecting tube, and described seal cover is set in the outside of described connecting tube, the sharp-pointed portion of described connecting tube and described shell are isolated, and described casing is located at the outside of described seal cover;
Described Clave connector is plugged in the perforate of described top cover, and described Clave connector comprises the first Clave connector for vacuumizing and the second Clave connector for fluid injection, described first Clave connector upper end is mated with the tube connector of described vacuumizing part and is connected, and described second Clave connector upper end is mated with the described syringe that electrolyte is housed and is connected.
Wherein, described Clave connector is the conventional joint in medical transfusion field, buys obtain by business, such as American I CU medical company produce and sell Clave connector, the quantity of described first Clave connector at least one, the quantity of described second Clave connector at least one;
Wherein, described syringe is common fluid injection instrument, comprises syringe shell and is arranged on syringe shell inside and the piston rod that mate airtight with syringe shell, but do not comprise syringe needle;
Wherein, described electrolyte is be injected into the liquid medium in battery or capacitor, such as, can be any one in potassium hydroxide (KOH) electrolyte, two trifluoromethanesulfonimide lithium (LiTFSI) electrolyte, ethylene carbonate electrolyte or lithium hexafluorophosphate electrolyte solution.
Further, in vacuum electrolyte filling device of the present invention, the seal cover of described Clave connector is made by having elastically-deformable material, and such as seal cover can be silicon matter cap, when described seal cover is not stressed, the through hole in the sharp-pointed portion of described connecting tube is sealed in described seal cover; During the stressed downward compression of described seal cover, described seal cover is punctured by the sharp-pointed portion of described connecting tube, and the through hole of described sharp-pointed portion sidewall is exposed in the outside of described seal cover.
Alternatively, in vacuum electrolyte filling device of the present invention, the base of described vacuum chamber can be the one in circle, ellipse, triangle, rectangle, pentagon or hexagon.
Preferably, described vacuum chamber is cylindrical chamber, and described base is cup dolly, described top cover is circular top cover, and the diameter of described base is 40-160mm, and described Sidewall Height is 50-200mm, the diameter of described top cover is 30-150mm, and the width of described groove is 4-6mm.
More preferably, the diameter of described base is 80-120mm, and described Sidewall Height is 50-100mm, and the diameter of described top cover is 70-110mm, and the width of described groove is 4.5-5.5mm.
Further, in vacuum electrolyte filling device of the present invention, the base of described vacuum chamber is provided with at least one battery case and a groove, described battery case is used for placing battery shell, or for placing ultracapacitor, be provided with packing ring in described groove, described vacuum chamber is enclosed by the packing ring arranged in described base, described base groove, described sidewall and described top cover and forms.
Should be understood that, the quantity of described battery case is determined according to the specification of the number of battery cells that need prepare and described vacuum electrolyte filling device.
Further, in vacuum electrolyte filling device of the present invention, the diameter of described battery case is 18-25mm, is preferably 20.5-21mm, is more preferably 20.5mm.
Further, in vacuum electrolyte filling device of the present invention, the below correspondence of described second Clave connector arranges described battery case, and described battery case is identical with the quantity of described second Clave connector.
Further, in vacuum electrolyte filling device of the present invention, the tube connector of described vacuumizing part is syringe shell.
Further, in vacuum electrolyte filling device of the present invention, in the process vacuumized, the described syringe that electrolyte is housed by described second Clave connector to described battery case fluid injection, or after completing and vacuumizing, described in electrolyte is housed syringe by described second Clave connector to described battery case fluid injection.
Further, the present invention also provides a kind of Clave connector, comprise shell, seal cover and connecting tube, the inside up/down perforation of described shell, the inside of described connecting tube is a cavity, and the top of described connecting tube is a sharp-pointed portion of taper, the sidewall in described sharp-pointed portion is provided with at least one through hole, described through hole is communicated in the internal cavities of described connecting tube, described seal cover is set in the outside of described connecting tube, the sharp-pointed portion of described connecting tube and described shell are isolated, and described casing is located at the outside of described seal cover.
Beneficial effect of the present invention is as follows:
(1) fluid injection is effective, structure is simple, volume is little.
In vacuum electrolyte filling device of the present invention, have employed the special Clave connector of structure and realize vacuumizing and liquid injecting function.Electrode slice to be infiltrated is put into battery case, and when vacuumizing, the air in electrode slice hole is discharged, and during fluid injection, electrolyte can enter in the hole of electrode slice smoothly, realizes good effect of impregnation.
In the present invention, when not working, the sharp-pointed portion of inner connecting tube is sealed in sealing lid by the seal cover of Clave connector.
In the present invention, first Clave connector upper end is mated with the tube connector of vacuumizing part and is connected, during vacuum pump work, the tube connector of vacuumizing part is pressed downward to the enclosure of the first Clave connector, the seal cover of the first Clave connector is forced to compress downwards, the be connected sharp-pointed portion of conduit of seal cover punctures, through hole on sharp-pointed portion sidewall is exposed at seal cover outside, now the air in vacuum chamber is extracted out by the cavity of the through hole in flexible pipe, tube connector, connecting tube and connecting tube inside by vacuum pump successively, thus realizes vacuumizing function.
In the present invention, second Clave connector upper end is connected with the syringe that electrolyte is housed, during fluid injection, syringe is pressed downward to the enclosure of the second Clave connector, the seal cover of the second Clave connector is forced to compress downwards, the be connected sharp-pointed portion of conduit of seal cover punctures, through hole on sharp-pointed portion sidewall is exposed at seal cover outside, electrolyte now in syringe flows into the cavity of connecting tube inside by the through hole on sharp-pointed portion sidewall, and then the described battery case that instillation the second Clave connector lower end is corresponding, complete liquid injecting function.
In view of the special construction of Clave connector, vacuum electrolyte filling device of the present invention does not need complicated fluid injection control system, the parts such as Clave connector, syringe by means of only small volume just can realize vacuum liquid filling, make vacuum electrolyte filling device designs simplification, easy and simple to handle, simultaneously according to the volume of the number of batteries and volume size design vacuum chamber that need fluid injection, therefore, vacuum electrolyte filling device of the present invention is used in the assembling carrying out button cell and ultracapacitor in glove box.
(2) reservoir quantity can accurately control, and fluid injection speed is fast.
In vacuum electrolyte filling device of the present invention, all corresponding second connector in top of each battery case, the syringe of electrolyte is equipped with in the upper end coupling connection one of each second Clave connector, namely each syringe that electrolyte is housed all can control the reservoir quantity that it injects corresponding battery case independently, Infiltrating according to electrode slice accurately regulates fluid injection speed and consumption, the pollution that when avoiding electrolyte to inject too much, electrolyte causes device.
In addition, in vacuum electrolyte filling device of the present invention, owing to adopting the direct fluid injection of syringe, syringe can quick adjustment its inject the reservoir quantity of battery case, therefore, the fluid injection speed of syringe can be very fast, avoids electrolyte to expose for a long time and cause volatilization in a vacuum, ensure that electrolyte under vacuum to the effect of impregnation of electrode slice.
(3) conveniently meet the injection demand of different electrolytes, and can not cross pollution be produced.Clave connector in the present invention is commercially produced product, and cheap, easily changes.Therefore, when needs inject different electrolytes, only need change Clave connector and need not change the miscellaneous part of vacuum electrolyte filling device of the present invention, such be easy to operate, and can not use different electrolyte because of certain parts in vacuum electrolyte filling device with and cause cross pollution.
Accompanying drawing explanation
Fig. 1 is the structural representation of embodiment 1 vacuum electrolyte filling device.
Fig. 2 is the exploded view of device in Fig. 1.
Fig. 3 is the structure chart (vacuum electrolyte filling device does not work) of embodiment 1 Clave connector.
Fig. 4 is the structure chart (when vacuumizing work) of embodiment 1 first Clave connector.
Fig. 5 is the structure chart (during fluid injection work) of embodiment 1 second Clave connector.
Fig. 6 is the cyclic voltammetry curve of capacitor performance test.
Fig. 7 is the cycle performance resolution chart of battery performance test.
Embodiment
Below by specific embodiment, the present invention is described in detail, should be understood that, these embodiments are only used for exemplifying the present invention, not forms any type of any restriction to real protection scope of the present invention.
Embodiment 1
Consult Fig. 1 to Fig. 2, the present embodiment provides a kind of vacuum electrolyte filling device, comprise vacuum chamber 1, Clave connector 2, vacuumizing part 3 and the syringe (not shown) of electrolyte is housed, vacuum chamber 1 is enclosed by base 11, sidewall 12 and top cover 13 and forms, Clave connector 2 is arranged in the top cover 13 of vacuum chamber 1, for vacuumizing part 3, syringe that electrolyte is housed being connected with vacuum chamber 1 respectively.
Vacuum chamber 1 is cylindrical chamber, and base 11 is cup dolly, and its diameter is 105mm, and the height of sidewall 12 is 80mm, and top cover 13 is circular top cover, and its diameter is 95mm, and is provided with seven in this top cover 13 for plugging the perforate of Clave connector 2.
Six battery cases 14 and a groove 15 is provided with in base 11, this battery case 14 is the battery case of button cell, its diameter is 20.5mm, and the diameter of this battery case 14, slightly larger than the diameter of button cell shell, contributes to improving the steadiness vacuumized with button cell shell in injection process; This groove 15 is the annular groove of width 5.5mm, and the outer ledge of this groove 15 is apart from the outer ledge 5mm of this base 11, and be provided with the packing ring 16 of one and matching grooves in this groove 15, packing ring 16 is for improving the seal degree of vacuum chamber 1.
Clave connector 2 comprises the first identical Clave connector 21 and the second Clave connector 22 of structure, this first Clave connector 21 is for connecting vacuumizing part 2 and vacuum chamber 1, and this second Clave connector 22 is for connecting syringe and vacuum chamber 1 that electrolyte is housed.
First Clave connector 21 is identical with the structure of the second Clave connector 22, and therefore illustrate the structure of the first Clave connector 21 and all may be used in the second Clave connector 22, this should not cause the disturbance of understanding to the second Clave connector 22.Consult Fig. 3 to Fig. 5, first Clave connector 21 comprises shell 211, seal cover 212 and connecting tube 213, the inside up/down perforation of this shell 211, sealing lid 212 is silicon matter cap, this connecting tube 213 inside is a cavity, and the top of this connecting tube 213 is a sharp-pointed portion of taper, the sidewall in this sharp-pointed portion is provided with two through holes 2131, and these two through holes 2131 are communicated in the cavity of this connecting tube 213 inside.
Sealing lid 212 is set in the outside of this connecting tube 213, for the sharp-pointed portion of this connecting tube 213 is sealed in sealing lid 212, especially the through hole 2131 on the sharp-pointed portion sidewall of connecting tube 213 is sealed in sealing lid 212, to make the sharp-pointed portion of whole connecting tube 213 and shell 211 and outside air isolate, this shell 211 is set in the outside of sealing lid 212.
Consult Fig. 1 and Fig. 2, vacuumizing part 3 comprises tube connector 31, flexible pipe 32 and vacuum pump 33, this flexible pipe 32 one end connects this vacuum pump 33, the other end connects this tube connector 31, this tube connector 31 is for taking out the syringe shell of piston rod, and this tube connector 31 lower end is mated with the first Clave connector 21 and is connected.
The syringe of electrolyte is housed for injecting electrolyte in battery case, and this syringe is provided with six altogether, often prop up the syringe lower end that electrolyte is housed to mate with one second Clave connector 22 respectively and be connected, the corresponding battery case 14 in lower end of each the second Clave connector 22.
Consult Fig. 3, vacuum electrolyte filling device of the present invention is not when working, tube connector 31 lower end of vacuumizing part 3 and the syringe lower end that electrolyte is housed all are not inserted in Clave connector 2, now, the sharp-pointed portion of connecting tube is sealed in sealing lid by the seal cover of Clave connector 2, isolates with shell and outside air.
Consult Fig. 4, the vacuum electrolyte filling device of embodiment is when carrying out vacuumizing work, first the shell 211 tube connector 31 of vacuumizing part 3 being pressed downward to the first Clave connector 21 is inner, and open vacuum pump 33, due to the pressure that tube connector 31 is downward, the seal cover 212 of the first Clave connector 21 is forced to compress downwards, the be connected sharp-pointed portion of conduit 213 of sealing lid 212 punctures, through hole 2131 on sharp-pointed portion sidewall is exposed, now vacuum pump 33 is successively by flexible pipe 32, tube connector 31, air in vacuum chamber is extracted out by the cavity of the through hole 2131 in connecting tube and connecting tube 213 inside, thus complete the work of vacuumizing.
Consult Fig. 5, after completing the work of vacuumizing, the shell 221 syringe that electrolyte is housed being pressed downward to the second Clave connector 22 is inner, the seal cover 222 of the second Clave connector 22 is forced to compress downwards, the be connected sharp-pointed portion of conduit 223 of sealing lid 222 punctures, through hole 2231 on sharp-pointed portion sidewall is exposed, the electrolyte be now equipped with in the syringe of electrolyte flows in the cavity of connecting tube 223 inside by the through hole 2231 on sharp-pointed portion sidewall, and then the battery case 14 that instillation the second Clave connector 22 lower end is corresponding, complete fluid injection work.
After the tube connector of vacuumizing part is pressed into the first Clave connector and after the syringe that electrolyte is housed is pressed into the second Clave connector, Clave connector and the external world remain isolation, namely vacuum chamber remains air-tight state, only have Clave connector inner with vacuumizing part and/or the syringe that electrolyte is housed carry out the motion of gas or liquid, so fluid injection work both can be carried out after the work of vacuumizing completes, also can carry out in the process vacuumized, because vacuum chamber is in the state of vacuumizing all the time, therefore in vacuum, carry out the vacuum degree that fluid injection work can not affect vacuum chamber.
In vacuum electrolyte filling device of the present invention, electrode slice to be infiltrated is put into battery case, the air in electrode slice space can be discharged during owing to vacuumizing, therefore make in injection process, electrolyte can enter in the space of electrode slice smoothly, realizes good effect of impregnation.
Embodiment 2
The difference of the present embodiment and embodiment 1 is only that the specification of vacuum chamber varies in size.
In the present embodiment, vacuum chamber 1 is cylindrical chamber, and base 11 is cup dolly, and its diameter is 80mm, and the height of sidewall 12 is 50mm, and top cover 13 is circular top cover, and its diameter is 70mm.
Embodiment 3
The difference of the present embodiment and embodiment 1 is only that the specification of vacuum chamber varies in size.
In the present embodiment, vacuum chamber 1 is cylindrical chamber, and base 11 is cup dolly, and its diameter is 120mm, and the height of sidewall 12 is 100mm, and top cover 13 is circular top cover, and its diameter is 110mm.
Embodiment 4
The difference of the present embodiment and embodiment 1 is only, in the present embodiment, does not arrange battery case in the base of vacuum chamber 1.
Embodiment 5
The present embodiment provides a kind of Clave connector, and its structure is identical with the Clave connector structure in embodiment 1.
In order to verify the fluid injection effect of vacuum electrolyte filling device of the present invention, inventor has also carried out capacitor and battery performance test.
Capacitor preparation example
(1) prepare electrode slice: utilize the mode of superposition to be pressed in nickel foam by carbon nano-tube film, obtained electrode slice, electrode slice surface density reaches 7.17mg/cm 2.
(2) electrode slice is infiltrated: the vacuum electrolyte filling device using the embodiment of the present invention 1, the battery case of specification 2025 is put into the battery case of base, electrode slice obtained in (1) is put into battery case, in the groove of base, puts into packing ring, top cover, makes vacuum chamber seal;
Be connected with tube connector by first Clave connector, flexible pipe two ends are connected tube connector and vacuum pump respectively, open vacuum pump and carry out bleeding operation, bleed 30min;
The syringe lower end that 6mol/LKOH electrolyte is housed is connected the second Clave connector, and in the battery case of correspondence position, injects 0.5mL electrolyte by the second Clave connector, continue the 10min that bleeds.
Wherein, the battery case of specification 2025 is bought by business and is obtained, and the source battery Materials Co., Ltd of such as Shanxi power produces and 2025 battery cases sold.
(3) assemble ultracapacitor: prepare according to the step of (1) and (2) and infiltrate two electrode slices, two electrode slices after infiltrating are taken out, is assembled into ultracapacitor, called after DRQ-1.
Battery preparation example
(1) prepare electrode slice: utilize infrared tablet press machine to suppress carbon pipe that sulphur load capacity is 70%, obtained electrode slice, electrode slice surface density reaches 7.0mg/cm 2.
(2) electrode slice is infiltrated: the vacuum electrolyte filling device using the embodiment of the present invention 1, and this vacuum electrolyte filling device is put into glove box, the battery case of specification 2025 is put into the battery case of base, electrode slice obtained in (1) is put into battery case, packing ring is put in the groove of base, top cover, makes vacuum chamber seal;
Be connected with tube connector by first Clave connector, flexible pipe two ends are connected tube connector and vacuum pump respectively, open vacuum pump and carry out bleeding operation, bleed 30min;
The syringe lower end of the LiTFSI electrolyte that 1mol/L is housed is connected the second Clave connector, and in the battery case of correspondence position, injects 0.4mL electrolyte by the second Clave connector, continue the 10min that bleeds.
Wherein, the battery case of specification 2025 is bought by business and is obtained, and the source battery Materials Co., Ltd of such as Shanxi power produces and 2025 battery cases sold.
Wherein, LiTFSI electrolyte refers to two trifluoromethanesulfonimide lithium electrolyte.
(3) assembled battery: the electrode slice after infiltrating is taken out and as positive pole, with lithium sheet as negative pole, is assembled into battery in glove box, called after DC-1.
Comparative example 1
Comparative example 1 is only with the difference of capacitor preparation example, and two electrode slices in comparative example 1 do not use vacuum electrolyte filling device of the present invention to infiltrate, and the mode only taking nature dropping infiltration infiltrates electrode slice, the ultracapacitor called after D1 that comparative example 1 is finally assembled.
Comparative example 2
Comparative example 2 is only with the difference of battery preparation example, and the electrode slice in comparative example 2 does not use vacuum electrolyte filling device of the present invention to infiltrate, and the mode only taking nature dropping infiltration infiltrates electrode slice, the battery called after D2 that comparative example 2 is finally assembled.
Capacitor and battery performance test
1, cyclic voltammetric (cyclicvoltammetry, CV) curve test
After DRQ-1 and D1 is shelved 360min, test loop volt-ampere (CV) curve respectively.
Instrument: RST5000 type electrochemical workstation; Conditional parameter: the 1st potential setting of turning back is 1V, the 2nd potential setting of turning back is 0V, and sweep speed is set as 0.025V/s, and the sampling interval is 0.001V.
According to formula: c = ∫ 0 1 I ( U ) dU / mυ Wherein c is specific capacity, ∫ 0 1 I ( U ) dU It is the half of the area that cyclic voltammetric (CV) curve surrounds, m is the gross mass of the active electrode material of two electrode slices, and υ is sweep speed, known, when electrode slice quality is identical with sweep speed, the area of cyclic voltammetric (CV) curve reflects the size of specific capacity.
Active electrode material can be the electrode materials such as active carbon, carbon nano-tube or Graphene.In this experiment, active electrode material is carbon nano-tube.
The result of this experiment is see Fig. 6, because the electrode slice quality of DRQ-1 with D1 is the same, sweep speed is the same, the area that cyclic voltammetric (CV) curve that the area that in Fig. 6, cyclic voltammetric (CV) curve of DRQ-1 surrounds is greater than D-1 surrounds, so DRQ-1 is higher than the specific capacity of D1, prove that vacuum electrolyte filling device of the present invention contributes to promoting electrolyte to the effect of impregnation of electrode slice, the energy storage capacity of ultracapacitor is had a certain upgrade.
2, cycle performance test
After DC-1 and D2 is shelved 360min, test loop performance respectively.
Instrument: new prestige battery performance testing system; Conditional parameter: charge cutoff voltage is set as 2.8V, discharge cut-off voltage is set as 1.5V, and the charge-discharge magnification of battery is set as 0.33mAh/cm 2.
The result of this experiment is see Fig. 7, as can be seen from Figure 7 DC-1 is higher than the specific capacity of D2, prove that vacuum electrolyte filling device of the present invention contributes to promoting electrolyte to the effect of impregnation of electrode slice, make the active electrode material in electrode slice play a role more efficiently and then improve specific capacity, the energy storage capacity of battery is had a certain upgrade.
Active electrode material can be the electrode materials such as active carbon, carbon nano-tube or Graphene.In this experiment, active electrode material is carbon pipe.
The above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all execution modes.All any amendments done within the spirit and principles in the present invention, equivalent to replace and improvement etc., within the protection range that all should be included in the claims in the present invention.

Claims (10)

1. a vacuum electrolyte filling device, it is characterized in that comprising: vacuum chamber, Clave connector, vacuumizing part and the syringe of electrolyte is housed, described vacuum chamber is enclosed by base, sidewall and top cover and forms, some perforates for plugging described Clave connector are provided with in described top cover, described vacuumizing part comprises tube connector, flexible pipe and vacuum pump, described flexible pipe one end connects described vacuum pump, and the other end connects described tube connector;
Described Clave connector comprises shell, seal cover and connecting tube, the inside up/down perforation of described shell, the inside of described connecting tube is a cavity, and the top of described connecting tube is a sharp-pointed portion of taper, the sidewall in described sharp-pointed portion is provided with at least one through hole, and described through hole is communicated in the internal cavities of described connecting tube, and described seal cover is set in the outside of described connecting tube, the sharp-pointed portion of described connecting tube and described shell are isolated, and described casing is located at the outside of described seal cover;
Described Clave connector is plugged in the perforate of described top cover, and described Clave connector comprises the first Clave connector for vacuumizing and the second Clave connector for fluid injection, described first Clave connector upper end is mated with the tube connector of described vacuumizing part and is connected, and described second Clave connector upper end is mated with the described syringe that electrolyte is housed and is connected.
2. vacuum electrolyte filling device according to claim 1, it is characterized in that: the seal cover of described Clave connector is made by having elastically-deformable material, when described seal cover is not stressed, the through hole of the sharp-pointed portion sidewall of described connecting tube is sealed in described seal cover; During the stressed downward compression of described seal cover, described seal cover is punctured by the sharp-pointed portion of described connecting tube, the through hole of described sharp-pointed portion sidewall is exposed at described seal cover outside.
3. vacuum electrolyte filling device according to claim 1, it is characterized in that: described vacuum chamber is cylindrical chamber, described base is cup dolly, described top cover is circular top cover, the diameter of described base is 40-160mm, described Sidewall Height is 50-200mm, and the diameter of described top cover is 30-150mm.
4. vacuum electrolyte filling device according to claim 3, is characterized in that: the diameter of described base is 80-120mm, and described Sidewall Height is 50-100mm, and the diameter of described top cover is 70-110mm.
5. vacuum electrolyte filling device according to claim 1 and 2, it is characterized in that: the base of described vacuum chamber is provided with at least one battery case and a groove, described battery case is used for placing battery shell, or for placing ultracapacitor shell, be provided with packing ring in described groove, described vacuum chamber is enclosed by the packing ring arranged in described base, described base groove, described sidewall and described top cover and forms.
6. vacuum electrolyte filling device according to claim 5, is characterized in that: the diameter of described battery case is 18mm-25mm.
7. vacuum electrolyte filling device according to claim 6, is characterized in that: the diameter of described battery case is 20.5mm-21mm.
8. vacuum electrolyte filling device according to claim 5, is characterized in that: the below correspondence of described second Clave connector arranges described battery case, and the tube connector of described vacuumizing part is syringe shell.
9. vacuum electrolyte filling device according to claim 5, it is characterized in that: in the process vacuumized, the described syringe that electrolyte is housed by described second Clave connector to described battery case fluid injection, or after completing and vacuumizing, described in electrolyte is housed syringe by described second Clave connector to described battery case fluid injection.
10. a Clave connector, it is characterized in that, comprise shell, seal cover and connecting tube, the inside up/down perforation of described shell, the inside of described connecting tube is a cavity, and the top of described connecting tube is a sharp-pointed portion of taper, the sidewall in described sharp-pointed portion is provided with at least one through hole, described through hole is communicated in the internal cavities of described connecting tube, described seal cover is set in the outside of described connecting tube, the sharp-pointed portion of described connecting tube and described shell are isolated, and described casing is located at the outside of described seal cover.
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CN102319706A (en) * 2011-05-07 2012-01-18 李林风 Indwelling catheter embolism clearing device based on negative pressure suction principle
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