CN109616691A - A kind of test method for the assembling equipment and the solid electrolyte conductivity being assembled into solid state battery using solid electrolyte - Google Patents
A kind of test method for the assembling equipment and the solid electrolyte conductivity being assembled into solid state battery using solid electrolyte Download PDFInfo
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- CN109616691A CN109616691A CN201811331079.0A CN201811331079A CN109616691A CN 109616691 A CN109616691 A CN 109616691A CN 201811331079 A CN201811331079 A CN 201811331079A CN 109616691 A CN109616691 A CN 109616691A
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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
- H01M10/04—Construction or manufacture in general
- H01M10/0404—Machines for assembling batteries
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/4166—Systems measuring a particular property of an electrolyte
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R27/00—Arrangements for measuring resistance, reactance, impedance, or electric characteristics derived therefrom
- G01R27/02—Measuring real or complex resistance, reactance, impedance, or other two-pole characteristics derived therefrom, e.g. time constant
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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
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- 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 discloses a kind of test methods of assembling equipment and the solid electrolyte conductivity that solid state battery is assembled into using solid electrolyte.The test method includes: step a, and solid electrolyte powder is fabricated to solid electrolyte sheet;Solid electrolyte sheet is assembled into solid state battery using the assembling equipment of solid state battery, and applies pressure for a period of time to solid state battery by step b;Step c carries out ac impedance measurement to the solid state battery under different temperatures, obtains the EIS curve of the solid electrolyte of different temperatures, the impedance value of solid electrolyte is read from EIS curve;Step d passes through formula according to the impedance value of solid electrolyte:The conductivity of solid electrolyte is calculated.The present invention, which assembles equipment and press merely with solid state battery, can measure the conductivity of solid electrolyte, and acquired results are suitable with traditional metal spraying test method, but involved material is cheap, and sample preparation procedure is simple.
Description
Technical field
The present invention relates to battery apparatus production technical fields, and in particular to a kind of to be assembled into solid-state electricity using solid electrolyte
The assembling equipment in pond and the test method of the solid electrolyte conductivity.
Background technique
Demand sustainable growth of the current social to lithium ion battery, and conventional lithium ion battery is there are more problem,
Energy density is lower, and security performance is poor, and multiple cells burst explosion reminds the security performance of people's lithium ion battery to need
It improves, and conventional lithium ion battery uses liquid electrolyte, electrolyte therein is organic solvent, and it is inflammable and explosive, therefore want
Think the safety issue for thoroughly solving lithium ion battery, all-solid lithium-ion battery research and development are extremely urgent, and preparing has high electricity
The solid electrolyte of conductance high electrochemical stability becomes key, at present by Japanese Scientists Yuki Kato [1] et al. preparation
Li9.54Si1.74P1.44S11.7Cl0.3, have with the comparable ionic conductivity of liquid electrolyte, reach 2.5X10-2S/
Cm, the complex valuableness of solid electrolyte conductivity test method, specific steps are as follows: first under high pressure by solid electrolyte powder
The electrolyte sheet for being jetted through gold is finally placed in obstruction electricity by last tabletting, the solid electrolyte sheet surface metal spraying that will be obtained later
In extremely, ac impedance measurement is carried out, the ionic conductivity of the electrolyte is calculated according to impedance value.This solid electrolyte conductance
Rate test method process is complicated, and noble metal bronze is needed to be sputtered onto electrolyte surface, higher cost.
Summary of the invention
To solve the above problems, the present invention provides a kind of assembling equipment for being assembled into solid state battery using solid electrolyte
And the test method of the solid electrolyte conductivity, structure is simple, electrolyte impedance value and true value low in cost, and measuring
Between deviation it is smaller.
To achieve the above object, the technical scheme adopted by the invention is as follows: it is a kind of using solid electrolyte be assembled into solid-state electricity
The assembling equipment in pond is used for stationary electrolyte piece and conduction including the hollow shell for placing solid electrolyte sheet
Blocking electrode, lower blocking electrode on alternating current, the upper blocking electrode are flexibly connected by sealing bolt with shell, the lower obstruction
Electrode is flexibly connected with shell;The upper blocking electrode, lower blocking electrode end be provided with the gasket for insulation.
As a preferred technical solution of the invention: the upper blocking electrode and lower blocking electrode are by stainless steel material
It is made, and is provided with screw on the outside of end, the screw is used to connect with external alternating current circuit;Above the interior of shell
O-ring seal is provided with above lower blocking electrode;The shell is made of PEEK material, and the gasket, sealing bolt are by poly- four
Fluoride material is made.
The present invention also provides a kind of test methods of solid electrolyte conductivity, comprising the following steps: step a, in nothing
Solid electrolyte powder is fabricated to solid electrolyte sheet in the environment of water anaerobic;Step b, using described in above-mentioned technical proposal
The assembling equipment of solid state battery the solid electrolyte sheet in step a is assembled into solid state battery, and solid state battery is applied
Pressure is for a period of time;Step c carries out ac impedance measurement to the solid state battery under different temperatures with electrochemical workstation, obtains
The EIS curve of the solid electrolyte of different temperatures reads the impedance value of solid electrolyte from EIS curve;Step d, according to solid
The impedance value of state electrolyte, passes through formula:
The conductivity of solid electrolyte is calculated;
Wherein, σ is the conductivity (S/cm) of electrolyte,
S is the area (cm2) of electrolyte sheet,
L is the thickness (cm) of electrolyte sheet,
R is the electrolyte impedance value (Ω) obtained from AC impedance figure.
As a preferred technical solution of the invention: solid electrolyte sheet manufacturing process in the step a are as follows: will
Solid electrolyte powder is placed into compression mold, and to after compression mold application pressure and after pressure maintaining for a period of time, demoulding is obtained
Solid electrolyte sheet;The manufacturing process carries out in the closed container full of inert gas.
As a preferred technical solution of the invention: the compression mold by the 40Mpa pressure provided by press,
The dwell time is 30min;The compression mold is infrared test stainless steel mould, a diameter of 12mm;It is described closed
Container is glove box.
As a preferred technical solution of the invention: the press includes pedestal, is provided with above the pedestal more
Root support column, the support column top are provided with screw rod, the nut being threadedly coupled with it are provided on the screw rod, is covered on screw rod
Equipped with pressing plate, the pressing plate is located at the lower section of multiple nuts.
As a preferred technical solution of the invention: in the step c solid state battery between 20 DEG C -80 DEG C into
The ac impedance measurement of row different temperatures, the EIS curve of the solid electrolyte under obtaining between 20 DEG C -80 DEG C.
As a preferred technical solution of the invention: the ac impedance measurement process of the different temperatures are as follows: will consolidate
After state battery is put into baking oven, oven temperature is adjusted to 80 DEG C, is stood 1h in carrying out ac impedance measurement at this temperature and is obtained EIS
Curve;Oven temperature is then down to 70 DEG C, then stands 1h, and in carrying out ac impedance measurement at this temperature, obtains EIS song
Line;60 DEG C are then cooled to, operation identical with above-mentioned steps is carried out, finally obtains at 20-80 DEG C, fixed electricity under different temperatures
Solve the EIS curve of matter;The electrochemical workstation is ten thousand energization chem workstation of Switzerland.
As a preferred technical solution of the invention: it further include step e, it will not homogeneity in the environment of anhydrous and oxygen-free
The solid electrolyte powder of amount is fabricated to the solid electrolyte sheet of different-thickness, and repeats step b, c, d.
As a preferred technical solution of the invention: the mass range of the solid electrolyte powder is
0.0500g -0.0700g, the thickness range of the solid electrolyte sheet are 350um -490um.
The invention has the following advantages:
1, the conductivity of solid electrolyte, gained knot can be measured merely with the assembling equipment and press of solid state battery
Fruit is suitable with the AC impedance that traditional use is tested to electrolyte sheet metal spraying, but the equal price of involved material is low
It is honest and clean, and sample preparation procedure is simple.
2, the assembling equipment of solid state battery and the use of press substantially reduce electrolyte sheet and the direct boundary of blocking electrode
Face impedance.And the process that metal spraying handles this time-consuming consumption cost is eliminated, so that solid electrolyte conductivity of the present invention is tested
Method has repeatability well.
Detailed description of the invention
Fig. 1 is the AC impedance figure of 350um thickness electrolyte at different temperatures;
Fig. 2 is the AC impedance figure of 420um thickness electrolyte at different temperatures;
Fig. 3 is the AC impedance figure of 490um thickness electrolyte at different temperatures;
Fig. 4 is the assembling device structure schematic diagram of solid state battery;
Fig. 5 is press structure schematic diagram;
In Fig. 1-Fig. 5,1, shell, 2, upper blocking electrode, 3, lower blocking electrode, 4, sealing bolt, 5, gasket, 6, screw, 7, O
Type sealing ring, 8, pedestal, 9, support column, 10, screw rod, 11, nut, 12, pressing plate.
Specific embodiment
In order to which objects and advantages of the present invention are more clearly understood, the present invention is carried out with reference to embodiments further
It is described in detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to limit this hair
It is bright.
As shown in figure 4, the embodiment of the invention provides a kind of group installings for being assembled into solid state battery using solid electrolyte
It is standby, including the hollow shell 1 for placing solid electrolyte sheet, it is used for stationary electrolyte piece and alternating current, on
Blocking electrode 2, lower blocking electrode 3, upper blocking electrode 2 are flexibly connected by sealing bolt 4 with shell 1, lower blocking electrode 3 and shell
1 is flexibly connected, and sealing bolt 4 plays the role of sealing, prevent electrolyte during the test with moisture in air;Upper obstruction
Electrode 2, lower blocking electrode 3 end be provided with the gasket 5 for insulation;Upper blocking electrode 2 and lower blocking electrode 3 are by stainless steel
Material is made, and screw 6 is provided on the outside of end, and screw 6 is used to connect with external alternating current circuit;1 inner upper of shell
O-ring seal 7 is provided with above lower blocking electrode 3;Shell 1 is made of PEEK material, and gasket 5, sealing bolt 4 are by polytetrafluoroethyl-ne
Alkene material is made.
The embodiment of the present invention also provides a kind of test method of solid electrolyte conductivity, including step a, by solid state electrolysis
Matter powder is placed into compression mold, and compression mold is infrared test stainless steel mould, a diameter of 12mm;With press to pressure
After sheet mold application pressure and after pressure maintaining for a period of time, demoulding obtains solid electrolyte sheet;Solid electrolyte sheet made
Cheng Jun is carried out in the closed container full of inert gas, and closed container is preferably glove box;Compression mold is mentioned by by press
The 40Mpa pressure of confession, dwell time 30min increase electrolyte sheet consistency to reach, and reduce between electrolyte granular
Interface impedance purpose, keep the electrolyte impedance value measured as suitable with electrolyte ontology impedance value as possible;As shown in figure 5,
Press includes pedestal 8, and more support columns 9 are provided with above pedestal 8, screw rod 10 is provided with above support column 9, is arranged on screw rod 10
There is the nut 11 being threadedly coupled with it, pressing plate 12 is arranged on screw rod 10, pressing plate 12 is located at the lower section of multiple nuts 11.
Solid electrolyte sheet in step a is assembled into solid state battery using the assembling equipment of solid state battery by step b,
And pressure is applied for a period of time to solid state battery;The pressure certain to press apparatus of nut 11 is turned with spanner, passes through press pair
Electrolyte sheet in solid state battery applies pressure, can substantially improve the interface problem between electrolyte and electrode, reach
Effect is identical to two surface metal spraying effects achieved of electrolyte with conventional test methodologies;The assembling equipment of solid state battery with
And press can substantially reduce the testing cost of electrolytic conductivity.
Step c will take out in the slave glove box of good solid state battery made above, with electrochemical workstation to different temperatures
Under solid state battery carry out ac impedance measurement, obtain the EIS curve of the solid electrolyte of different temperatures, read from EIS curve
Take the impedance value of solid electrolyte;The preferred ten thousand energization chem workstation of Switzerland of electrochemical workstation, measuring accuracy is high, error
It is small, the impedance value Ω of electrolyte sheet can be read directly from test curve;Solid state battery carries out not between 20 DEG C -80 DEG C
Synthermal ac impedance measurement, the EIS curve of the solid electrolyte under obtaining between 20 DEG C -80 DEG C.
The ac impedance measurement process of different temperatures are as follows: after solid state battery is put into baking oven, adjust oven temperature to 80 DEG C,
It stands 1h and obtains EIS curve in carrying out ac impedance measurement at this temperature;Oven temperature is then down to 70 DEG C, then is stood
1h, and in carrying out ac impedance measurement at this temperature, obtain EIS curve;60 DEG C are then cooled to, is carried out identical as above-mentioned steps
Operation, finally obtain the EIS curve of stationary electrolyte under different temperatures at 20-80 DEG C.
Step d passes through formula according to the impedance value of solid electrolyte:
The conductivity of solid electrolyte is calculated;
Wherein, σ is the conductivity (S/cm) of electrolyte, and S is the area (cm2) of electrolyte sheet, and L is the thickness of electrolyte sheet
(cm), R is the electrolyte impedance value (Ω) obtained from AC impedance figure.
The solid electrolyte powder of different quality is fabricated to consolidating for different-thickness in the environment of anhydrous and oxygen-free by step e
State electrolyte sheet, and repeat step b, c, d;The mass range of solid electrolyte powder is 0.0500g -0.0700g, solid-state
The thickness range of electrolyte sheet is 350um -490um;Such as 0.0500g electrolyte powder is put into tabletting in glove box
In mold, after taking-up under 40Mp pressure pressure maintaining 30min, obtain diameter 12mm, the electrolyte sheet with a thickness of 350um, according to
Fig. 1 reads the impedance value R of electrolyte sheet under different temperatures, and the ionic conductance of electrolyte under different temperatures can be calculated according to formula
Rate;0.0600g electrolyte powder is put into compression mold in glove box, after taking-up under 40Mp pressure pressure maintaining 30min, obtain
To diameter 12mm, with a thickness of the electrolyte sheet of 420um, read the impedance value R of electrolyte sheet under different temperatures, root according to fig. 2
The ionic conductivity of electrolyte under different temperatures can be calculated according to formula;0.0700g electrolyte powder is put into glove box
In compression mold, after taking-up under 40Mp pressure pressure maintaining 30min, obtain diameter 12mm, the electrolyte sheet with a thickness of 490um,
The impedance value R that electrolyte sheet under different temperatures is read according to Fig. 3, the ion of electrolyte under different temperatures can be calculated according to formula
Conductivity.
The present invention can measure the conductivity of solid electrolyte, institute merely with the assembling equipment and press of solid state battery
It is suitable with the AC impedance that traditional use is tested to electrolyte sheet metal spraying to obtain result, but the equal price of involved material
It is cheap, and sample preparation procedure is simple.The assembling equipment of solid state battery and the use of press substantially reduce electrolyte sheet and resistance
The direct interface impedance of electrode is filled in, and eliminates the process that metal spraying handles this time-consuming consumption cost, so that solid-state of the present invention is electric
Solving matter conductivity test method has repeatability well.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the principle of the present invention, it can also make several improvements and retouch, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of assembling equipment for being assembled into solid state battery using solid electrolyte, which is characterized in that including for placing solid-state
The hollow shell of electrolyte sheet, blocking electrode, lower blocking electrode on stationary electrolyte piece and alternating current, institute
It states blocking electrode to be flexibly connected by sealing bolt with shell, the lower blocking electrode is flexibly connected with shell;The upper obstruction
Electrode, lower blocking electrode end be provided with the gasket for insulation.
2. a kind of assembling equipment for being assembled into solid state battery using solid electrolyte according to claim 1, feature are existed
In the upper blocking electrode is made with lower blocking electrode of stainless steel material, and is provided with screw on the outside of end, the screw
For being connect with external alternating current circuit;O-ring seal is provided with above the interior of shell and above lower blocking electrode;It is described
Shell is made of PEEK material, and the gasket, sealing bolt are made of polytetrafluoroethylene material.
3. a kind of test method of solid electrolyte conductivity, which comprises the following steps:
Solid electrolyte powder is fabricated to solid electrolyte sheet in the environment of anhydrous and oxygen-free by step a;
Step b, using the assembling equipment of the described in any item solid state batteries of claims 1 or 22 by the solid electrolyte in step a
Thin slice is assembled into solid state battery, and applies pressure for a period of time to solid state battery;
Step c carries out ac impedance measurement to the solid state battery under different temperatures with electrochemical workstation, obtains different temperatures
The EIS curve of solid electrolyte reads the impedance value of solid electrolyte from EIS curve;
Step d passes through formula according to the impedance value of solid electrolyte:
The conductivity of solid electrolyte is calculated;
Wherein, σ is the conductivity (S/cm) of electrolyte;
S is the area (cm2) of electrolyte sheet;
L is the thickness (cm) of electrolyte sheet;
R is the electrolyte impedance value (Ω) obtained from AC impedance figure.
4. a kind of test method of solid electrolyte conductivity according to claim 3, which is characterized in that the step a
Middle solid electrolyte sheet manufacturing process are as follows: solid electrolyte powder is placed into compression mold, compression mold is applied and is pressed
After power and after pressure maintaining for a period of time, demoulding obtains solid electrolyte sheet;The manufacturing process is close full of inert gas
It closes in container and carries out.
5. a kind of test method of solid electrolyte conductivity according to claim 4, which is characterized in that the tabletting mould
For tool by the 40Mpa pressure provided by press, the dwell time is 30min;The compression mold is infrared test with stainless
Steel mold, a diameter of 12mm;The closed container is glove box.
6. a kind of test method of solid electrolyte conductivity according to claim 5, which is characterized in that the press packet
Pedestal is included, more support columns are provided with above the pedestal, screw rod is provided with above the support column, is provided on the screw rod
The nut being threadedly coupled with it is arranged with pressing plate on screw rod, and the pressing plate is located at the lower section of multiple nuts.
7. a kind of test method of solid electrolyte conductivity according to claim 3, which is characterized in that the step c
Middle solid state battery carries out the ac impedance measurement of different temperatures, consolidating under obtaining between 20 DEG C -80 DEG C between 20 DEG C -80 DEG C
The EIS curve of state electrolyte.
8. a kind of test method of solid electrolyte conductivity according to claim 3, which is characterized in that the not equality of temperature
The ac impedance measurement process of degree are as follows: after solid state battery is put into baking oven, adjusts oven temperature to 80 DEG C, 1h is stood, in the temperature
Degree is lower to carry out ac impedance measurement, obtains EIS curve;Oven temperature is then down to 70 DEG C, then stands 1h, and at this temperature
Ac impedance measurement is carried out, EIS curve is obtained;60 DEG C are then cooled to, operation identical with above-mentioned steps is carried out, finally obtains
At 20-80 DEG C, the EIS curve of stationary electrolyte under different temperatures;The electrochemical workstation is ten thousand energization chemical work of Switzerland
It stands.
9. according to a kind of described in any item test methods of solid electrolyte conductivity of claim 3-8, which is characterized in that also
Including step e, the solid electrolyte powder of different quality is fabricated to the solid-state electricity of different-thickness in the environment of anhydrous and oxygen-free
Matter thin slice is solved, and repeats step b, c, d.
10. a kind of test method of solid electrolyte conductivity according to claim 9, which is characterized in that the solid-state
The mass range of electrolyte powder is 0.0500g -0.0700g, and the thickness range of the solid electrolyte sheet is 350um -
490um。
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CN110146821A (en) * | 2019-05-27 | 2019-08-20 | 清华大学深圳研究生院 | Battery tester and its application method |
CN111443243A (en) * | 2020-03-17 | 2020-07-24 | 合肥国轩高科动力能源有限公司 | Detection method for conductivity of lithium ion battery binder |
CN113687144A (en) * | 2021-07-30 | 2021-11-23 | 蜂巢能源科技有限公司 | Testing device and testing method for diaphragm ionic conductivity |
CN113804926A (en) * | 2021-09-13 | 2021-12-17 | 中汽创智科技有限公司 | Battery clamp device, preparation and test method and application |
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CN113687144A (en) * | 2021-07-30 | 2021-11-23 | 蜂巢能源科技有限公司 | Testing device and testing method for diaphragm ionic conductivity |
CN113804926A (en) * | 2021-09-13 | 2021-12-17 | 中汽创智科技有限公司 | Battery clamp device, preparation and test method and application |
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