CN107271317B - The method for testing rare earth new power negative electrode tab expansion rate - Google Patents
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Abstract
The invention belongs to water system power battery technology fields, and in particular to a method of test rare earth new power negative electrode tab expansion rate.Rare earth new power battery core is packed into battery case, after top seal is good, carry out normal pressure fluid injection, sealing, chemical conversion, activated battery is discharged, it shelves, rotary valve is opened under inert gas normal pressure atmosphere, the flowing electrolyte for pouring out the inside adds electrolyte, closes rotary valve, after carrying out charge and discharge five times, it shelves, opens rotary valve under inert gas normal pressure atmosphere, pour out the electrolyte that the inside is flowed, it weighs before and after each operation, the expansion rate of rare earth new power negative electrode tab in actual use can be obtained.There are two present invention results obtained, can carry out error calculation, improves accuracy rate, under conditions of not changing the process conditions and process of battery production, the real data for the measurement pole piece expansion rate that can be convenient, error is small, favorable repeatability, simple and easy, versatility is high, is convenient for practical operation.
Description
Technical field
The invention belongs to water system power battery technology fields, and in particular to a kind of test rare earth new power negative electrode tab expansion rate
Method.
Background technique
Rare earth new power is a kind of main novel water system power battery for applying feature with rare earth new material, as a kind of new
Type energy carrier becomes the hot spot of battery industry research, represents the developing direction of water system power battery.Due to rare earth new power
With high power, the long-life, the environmental-friendly temperature applicable range that can be recycled, have a wide reach, use safe, memory-less effect etc.
Advantage, therefore referred to as new generation of green battery.In energy shortage, today of environmental pollution, rare earth new power shows wide
Application prospect.
Important electrochmical power source of the rare earth new power as a kind of important automobile-used and other power and energy-storage system, rare earth are new
Power cathode piece expansion rate is the key parameter for influencing battery performance.In order to design high-performance rare-earth new power, it would be desirable to
The accurate expansion rate for knowing negative electrode tab is all the chief active indirectly to negative electrode tab so far according to traditional evaluation method
The measurement of material abundance rare earth alloy progress cubical expansivity；It is individually to carry out outside battery or estimate indirectly, this survey
Method for testing can measure to a certain extent the expansion rate of negative electrode tab, but the result tested in this way and they battery true work
Expansion rate under condition environment be it is differentiated, can not reflect influence of the true environment to negative electrode tab expansion rate.In addition, existing side
The deficiencies of there is also measurement data fluctuations for method greatly, and poor reproducibility, inconvenient or material consumption is more, easy cross contamination.
Summary of the invention
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of test rare earth new power negative electrode tab expansion rates
Method, under conditions of not changing the process conditions and process flow of battery manufacturing technology, convenient measurement pole piece expansion rate
Real data, error is small, favorable repeatability, simple and easy, versatility is high, is convenient for practical operation.
The method of test rare earth new power negative electrode tab expansion rate of the present invention, comprising the following steps:
(1) volume for measuring negative electrode tab, is denoted as V0, rare earth new power battery core is made, rare earth new power battery core is packed into electricity
Pond shell after top seal is good, installs safety valve additional；
(2) it opens the safety-valve, is sealed after carrying out normal pressure fluid injection, weigh, be denoted as M3；It is melted into according to existing chemical synthesis technology
It weighs after activation, is denoted as M4；
(3) it shelves, opens rotary valve under inert gas normal pressure atmosphere, after the flowing electrolyte for pouring out the inside, to battery
It weighs, is denoted as M5；It weighs to the electrolyte poured out, is denoted as M6；Electrolyte is added, after adding electrolyte, to pass
The completed cell for closing rotary valve is weighed, and M is denoted as8；
(4) it to battery charging and discharging five times, shelves, weighs to battery, be denoted as M9；Then in inert gas normal pressure atmosphere
Lower opening rotary valve pours out the electrolyte that the inside is flowed, weighs to the electrolyte poured out, be denoted as M10；After pouring out electrolysis
Battery is also weighed, and M is denoted as11, calculate rare earth new power negative electrode tab expansion rate.
The calculation formula of rare earth new power negative electrode tab expansion rate is one of following two:
Expansion rate μ1=[M6+(M3-M4)+(M4-M5-M6)]/ρV0* 100%；
Or expansion rate μ2=[M10+(M8-M9)+(M9-M10-M11)]/ρV0* 100%；
Wherein, ρ is electrolyte density.
Electrolyte is preferably the KOH solution of 6mol/L, specific gravity 1.2900g/L.The expansion rate data of acquisition can anti-mistake
The process conditions and process flow of battery manufacturing technology are further instructed, in design brand new cells, which can
Verified again in practice as design considerations.
The calculation formula of expansion rate error are as follows:
Expansion rate error: Δ μ=| (μ1-μ2)|/μ1* 100%.
Each monomer is tested there are two the same data of expansion rate obtained, and front and back can directly carry out error calculation, I
Using it as internal longitudinal index, and compared with the lateral scale error of multiple batteries, to obtain very objective
Data.
Production rare earth new power battery core described in step (1) are as follows: by negative electrode tab according to the technique of existing battery manufacturing technology
Condition and the condition of process flow make rare earth new power battery core.
Battery case is the square cell that transparent, bottom has rotary valve.Rare earth new power is square lamination, because
This, using square cell, the battery case of test be transparent organic glass (organic glass pull with a thickness of 10mm, using ABS
Glue carries out bubble-free bonding), this is because can intuitively see internal-response situation in test process.Not special
Under explanation, all test environment temperatures are 20 ± 5 DEG C.Furthermore battery case size can be with according to the battery core capacity and size of test
Processing and fabricating, the rare earth new power for being very suitable to all kinds of capacity carry out 1:1 actual test.
Preferably, the structure of battery case is as follows: battery case includes battery case shell, and battery case upper part of the housing is equipped with top cover,
Top cover is equipped with safety valve, there is rare earth new power battery core in battery case shell, and battery case housing bottom is equipped with rotary valve, and rare earth is new
It include negative electrode tab in power supply battery core.Negative electrode tab is preferably 30.
When being weighed in operating process, it is accurate to 0.0001g.Weighing uses the balance of a ten thousandth precision, tests
Cheng Zhong, rotary valve need to open it is primary, the gas that the inside is run out may be it is micro, during chemical conversion and charge and discharge five times
Gas can be generated, in the case that air pressure is excessively high, may be run out of from safety valve, the gas flow run out of is seldom, and the present invention uses
Accuracy of balance is a ten thousandth, can control weight error within 0.1%.
Shelving in step (3) and step (4) is to shelve 48~72h.The reaction of rare earth new power negative electrode tab is catalysis
Mechanism, in charge and discharge process, inside battery can generate bulk gas, mainly hydrogen, after stopping charge or discharge, certain
Time in, the rare earth alloy of negative electrode tab can hydrogen that gradually catalytic adsorption generates, the air pressure of inside battery can gradually decrease
It is balanced to external atmosphere pressure, this process needs 48~72h of time, and the time is too short, and internal pressure fully ensures that be reduced to not yet
It is consistent with ambient pressure, rotary valve is opened too early, and the gas run out will cause that electrolyte weight is relatively low, and the time is too long, battery
Increase tendency can be presented in self-discharge rate, and this can also generate gas, and internal pressure is caused to go up not down, and opening rotary valve will also result in
Internal gas loss, it is relatively low to also result in electrolyte weight.
The flowing electrolyte that the inside is poured out described in step (3) pours out time 0.5~1h of needs.Rotary valve is opened, is inclined
Electrolyte needs the time, because being all to be coated with diaphragm inside battery pole piece, diaphragm is nonwoven cloth material, has three-dimensional apertures
Diameter has capillarity to liquid, so if the time is too short, battery core bottom hanging drop is unable to come down, and the time is too long, suspends
Drop may be adsorbed to again above；At the right time, shaking appropriate can be fallen with power-assisted hanging drop.
Inert gas is nitrogen or argon gas, and purity is not less than 99.9%.Battery material rare earth alloy used in rare earth new power
The oxygen in air is encountered, it is easy to oxidize, the catalytic performance of rare earth alloy is influenced, is operated in inert gas atmosphere, air is completely cut off
In oxygen, do not influence battery performance, it is ensured that test front and back chemical property it is consistent, control influence factor caused by influence accidentally
In poor range.
Refer to chargeability variation from 0~100% to battery charging and discharging five times.Chargeability variation refers to filling from 0~100%
Electricity is just full of, and electric discharge uniformly discharges into 1.0V, and just discharge off, charging and discharging currents are 0.2C；If electric current is too small, need
Overlong time is wanted, if electric current is too big, inside battery internal pressure is will lead to and increases fastly, the chemical property difference that front and back is five times is higher than
The error amount of permission.
The present invention has the square cell of rotary valve by transparent, bottom, in the technique of existing battery manufacturing technology
Under conditions of condition and process flow, rare earth new power battery core is packed into battery case with complete structure, is carried out according to set process
Operation is weighed before and after each operation, is volume by electrolyte weight differential conversion, with rare earth new power negative electrode tab
Volume is compared, it is hereby achieved that the expansion rate data of rare earth new power negative electrode tab in actual use, simultaneously also
Battery core imbibition rate data can be obtained.
As a kind of perferred technical scheme, the present invention may be used also while testing rare earth new power negative electrode tab expansion rate
To test rare earth new power battery core imbibition, comprising the following steps:
(1) volume for measuring negative electrode tab, is denoted as V0, the weight of rare earth new power battery core is measured, M is denoted as1, rare earth is newly electric
Source battery core is packed into battery case, after top seal is good, installs safety valve additional and weighs together, be denoted as M2；
(2) it opens the safety-valve, is sealed after carrying out normal pressure fluid injection, weigh, be denoted as M3；It is melted into according to existing chemical synthesis technology
It weighs after activation, is denoted as M4；
(3) it shelves after a certain period of time, opens rotary valve under inert gas normal pressure atmosphere, pour out the flowing electrolyte of the inside
Afterwards, it weighs to battery, is denoted as M5；It weighs to the electrolyte poured out, is denoted as M6；Add electrolyte, the electricity of addition
Solution liquid measure is weighed, and M is denoted as7；After adding electrolyte, weighs to the completed cell for closing rotary valve, be denoted as M8；
(4) it to battery charging and discharging five times, shelves after a certain period of time, weighs to battery, be denoted as M9；Then in indifferent gas
Rotary valve is opened under body normal pressure atmosphere, the electrolyte that the inside is flowed is poured out, weighs to the electrolyte poured out, be denoted as M10；?
Battery after being electrolysed out is also weighed, and M is denoted as11。
The calculation formula of imbibition rate is one of following two:
Rare earth new power battery core imbibition: imbibition rate ν1=[(M3-M4)+(M3-M2)]/M1* 100%
Imbibition rate ν2=[| (M7-M6)|+(M3-M4)+(M3-M2)]/M1* 100%
Each monomer is tested there are two the same data of expansion rate obtained, and front and back can directly carry out error calculation, I
Using it as internal longitudinal index, and compared with the lateral scale error of multiple batteries, to obtain very objective
Data.
The calculation formula of imbibition rate error are as follows:
Imbibition rate error: Δ ν=| (ν1-ν2)|/ν1* 100%.
Each monomer is tested there are two the same data of imbibition rate obtained, and front and back can directly carry out error calculation, I
Using it as internal longitudinal index, and compared with the lateral scale error of multiple batteries, to obtain very objective
Data.
In conclusion the invention has the following advantages that
(1) it the present invention is especially suitable for test negative electrode tab expansion rate, weighs before and after each operation, by electrolyte weight
Amount differential conversion is volume, is compared with rare earth new power negative electrode tab volume, it is hereby achieved that rare earth new power negative electrode tab exists
Expansion rate data in actual use.With traditional negative electrode tab battery material abundance rare earth alloy expansion rate test method
It compares, this test method is not under conditions of changing the process conditions and process flow of battery manufacturing technology, it may be convenient to survey
The real data of pole piece expansion rate is measured, and error is small, favorable repeatability, can accurately test the expansion of rare earth new power negative electrode tab
Rate.
(2) present invention tests there are two negative electrode tab expansion rates obtained each monomer, and front and back can directly be missed
Difference calculates, and improves accuracy rate, we carry out pair using it as internal longitudinal direction index with the lateral scale error of multiple batteries
Than to obtain very objective data, in design brand new cells, which can be used as design considerations, in reality
Trample it is middle verified again, reduce research and development cost and shorten the R&D cycle.
(3) the invention is simple and feasible, versatility is high, is convenient for practical operation.
(4) method of present invention test negative electrode tab expansion rate is accurate and reliable, and the repetition consistency of test result is fine.
(5) the data M in present invention test7If more than M10+(M9-M10-M11), show that cell activation system is unreasonable, needs
It is further improved, if M7Equal to M10+(M9-M10-M11), then show that chemical synthesis technology is very reasonable, the result that the present invention measures can
Directly practical manifestation of the reflection test object in battery, has a practical directive significance, test result thus can be used for improving
Chemical synthesis technology.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of battery case used by the embodiment of the present invention；
In figure: 1- battery case shell, 2- rare earth new power battery core, 3- top cover, 4- safety valve, 5- rotary valve.
Specific embodiment
Below with reference to embodiment, the present invention will be further described.
Embodiment 1
A method of test rare earth new power negative electrode tab expansion rate and battery core imbibition:
(1) volume for measuring negative electrode tab, is denoted as V0, the weight of rare earth new power battery core is measured, M is denoted as1, with complete structure
It is packed into the square cell that transparent, bottom has rotary valve, after top seal is good, safety valve is installed additional and weighs together, be denoted as M2；
(2) it opens the safety-valve, is sealed after carrying out normal pressure fluid injection, weigh, be denoted as M3；It is melted into according to existing chemical synthesis technology
It weighs after activation, is denoted as M4；
(3) after shelving 60h, rotary valve is opened under inert gas normal pressure nitrogen atmosphere, pours out the flowing electrolyte of the inside,
After continuing 0.8h, weighs to battery, be denoted as M5；It weighs to the electrolyte poured out, is denoted as M6；Electrolyte is added,
The electrolyte content of addition is weighed, and M is denoted as7；It after adding electrolyte, weighs, remembers to the completed cell for closing rotary valve
For M8；
(4) to battery charging and discharging five times, chargeability changes from 0~100%, after shelving 60h, weighs to battery, remembers
For M9；Then rotary valve is opened under inert gas normal pressure nitrogen atmosphere, pours out the electrolyte that the inside is flowed, after continuing 0.8h,
It weighs to the electrolyte poured out, is denoted as M10；Battery after pouring out electrolysis is also weighed, and M is denoted as11。
As shown in Figure 1, battery case includes battery case shell 1,1 top of battery case shell is equipped with the structure of battery case used
Top cover 3, top cover 3 are equipped with safety valve 4, there is rare earth new power battery core 2 in battery case shell 1, and 1 bottom of battery case shell is equipped with rotation
Rotary valve 5, interior rare earth new power battery core 2 includes negative electrode tab, and negative electrode tab is 30.
The data tested out calculate negative electrode tab expansion rate μ by the calculation formula of expansion rate1With expansion rate μ2Respectively
For 2.1017% and 2.0964%；Imbibition rate ν is calculated by the calculation formula of battery core imbibition rate1And ν2It is 14.4709% respectively
With 14.4688%.Error is respectively 0.25% and 0.015%, respectively less than 0.3% allowable error, and measuring accuracy is met the requirements.
Embodiment 2
A method of test rare earth new power negative electrode tab expansion rate and battery core imbibition:
(1) volume for measuring negative electrode tab, is denoted as V0, the weight of rare earth new power battery core is measured, M is denoted as1, with complete structure
It is packed into the square cell that transparent, bottom has rotary valve, after top seal is good, safety valve is installed additional and weighs together, be denoted as M2；
(2) it opens the safety-valve, is sealed after carrying out normal pressure fluid injection, weigh, be denoted as M3；It is melted into according to existing chemical synthesis technology
It weighs after activation, is denoted as M4；
(3) after shelving 48h, rotary valve is opened under inert gas normal pressure argon atmosphere, pours out the flowing electrolyte of the inside,
After continuing 0.5h, weighs to battery, be denoted as M5；It weighs to the electrolyte poured out, is denoted as M6；Electrolyte is added,
The electrolyte content of addition is weighed, and M is denoted as7；It after adding electrolyte, weighs, remembers to the completed cell for closing rotary valve
For M8；
(4) to battery charging and discharging five times, chargeability changes from 0~100%, after shelving 48h, weighs to battery, remembers
For M9；Then rotary valve is opened under inert gas normal pressure argon atmosphere, pours out the electrolyte that the inside is flowed, after continuing 0.5h,
It weighs to the electrolyte poured out, is denoted as M10；Battery after pouring out electrolysis is also weighed, and M is denoted as11。
The structure of battery case used is same as Example 1.
The data tested out calculate negative electrode tab expansion rate μ by the calculation formula of expansion rate1With expansion rate μ2Respectively
For 2.1003% and 2.0994%；Imbibition rate ν is calculated by the calculation formula of battery core imbibition rate1And ν2It is 14.4698% respectively
With 14.4683%.Error is respectively 0.05% and 0.01%, respectively less than 0.3% allowable error, and measuring accuracy is met the requirements.
Embodiment 3
A method of test rare earth new power negative electrode tab expansion rate and battery core imbibition:
(1) volume for measuring negative electrode tab, is denoted as V0, the weight of rare earth new power battery core is measured, M is denoted as1, with complete structure
It is packed into the square cell that transparent, bottom has rotary valve, after top seal is good, safety valve is installed additional and weighs together, be denoted as M2；
(2) it opens the safety-valve, is sealed after carrying out normal pressure fluid injection, weigh, be denoted as M3；It is melted into according to existing chemical synthesis technology
It weighs after activation, is denoted as M4；
(3) after shelving 72h, rotary valve is opened under inert gas normal pressure nitrogen atmosphere, pours out the flowing electrolyte of the inside,
After continuing 1h, weighs to battery, be denoted as M5；It weighs to the electrolyte poured out, is denoted as M6；Electrolyte is added, is added
The electrolyte content entered is weighed, and M is denoted as7；After adding electrolyte, weighs, be denoted as to the completed cell for closing rotary valve
M8；
(4) to battery charging and discharging five times, chargeability changes from 0~100%, after shelving 72h, weighs to battery, remembers
For M9；Then rotary valve is opened under inert gas normal pressure nitrogen atmosphere, pours out the electrolyte that the inside is flowed, it is right after continuing 1h
The electrolyte poured out is weighed, and M is denoted as10；Battery after pouring out electrolysis is also weighed, and M is denoted as11。
The structure of battery case used is same as Example 1.
The data tested out calculate negative electrode tab expansion rate μ by the calculation formula of expansion rate1With expansion rate μ2Respectively
For 2.0998% and 2.0959%；Imbibition rate ν is calculated by the calculation formula of battery core imbibition rate1And ν2It is 14.4703% respectively
With 14.4619%.Error is respectively 0.19% and 0.06%, respectively less than 0.3% allowable error, and measuring accuracy is met the requirements.
Claims (8)
1. a kind of method for testing rare earth new power negative electrode tab expansion rate, it is characterised in that: the following steps are included:
(1) volume for measuring negative electrode tab, is denoted as V0, rare earth new power battery core is made, rare earth new power battery core is packed into battery case,
After top seal is good, safety valve is installed additional；
(2) it opens the safety-valve, is sealed after carrying out normal pressure fluid injection, weigh, be denoted as M3；Chemical conversion activation is carried out according to existing chemical synthesis technology
After weigh, be denoted as M4；
(3) it shelves, opens rotary valve under inert gas normal pressure atmosphere, after the flowing electrolyte for pouring out the inside, battery is carried out
Weighing, is denoted as M5；It weighs to the electrolyte poured out, is denoted as M6；Electrolyte is added, after adding electrolyte, is revolved to closing
The completed cell of rotary valve is weighed, and M is denoted as8；
(4) it to battery charging and discharging five times, shelves, weighs to battery, be denoted as M9；Then it is beaten under inert gas normal pressure atmosphere
Rotary valve is opened, the electrolyte that the inside is flowed is poured out, weighs to the electrolyte poured out, be denoted as M10；Battery after pouring out electrolysis
Also it weighs, is denoted as M11, calculate rare earth new power negative electrode tab expansion rate；
The calculation formula of rare earth new power negative electrode tab expansion rate is one of following two:
Expansion rate μ1=[M6+(M3-M4)+(M4-M5-M6)]/ρV0* 100%；
Or expansion rate μ2=[M10+(M8-M9)+(M9-M10-M11)]/ρV0* 100%；
Wherein, ρ is electrolyte density；
The calculation formula of expansion rate error are as follows:
Expansion rate error: Δ μ=| (μ1-μ2)|/μ1* 100%.
2. the method for test rare earth new power negative electrode tab expansion rate according to claim 1, it is characterised in that: battery case is
Transparent, bottom has the square cell of rotary valve.
3. the method for test rare earth new power negative electrode tab expansion rate according to claim 2, it is characterised in that: battery case packet
Battery case shell is included, battery case upper part of the housing is equipped with top cover, and top cover is equipped with safety valve, has rare earth new power in battery case shell
Battery core, battery case bottom are equipped with rotary valve, include negative electrode tab in rare earth new power battery core.
4. the method for test rare earth new power negative electrode tab expansion rate according to claim 1, it is characterised in that: when weighing,
It is accurate to 0.0001g.
5. the method for test rare earth new power negative electrode tab expansion rate according to claim 1, it is characterised in that: step (3)
It is to shelve 48~72h with shelving in step (4).
6. the method for test rare earth new power negative electrode tab expansion rate according to claim 1, it is characterised in that: inert gas
For nitrogen or argon gas, purity is not less than 99.9%.
7. the method for test rare earth new power negative electrode tab expansion rate according to claim 1, it is characterised in that: step (3)
Described in pour out the inside flowing electrolyte, pour out the time need 0.5~1h.
8. the method for test rare earth new power negative electrode tab expansion rate according to claim 1, it is characterised in that: filled to battery
It discharges five times and refers to chargeability variation from 0~100%.
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| CN109100252B (en) * | 2018-06-29 | 2022-08-30 | 广东天劲新能源科技股份有限公司 | Equipment and method capable of accurately detecting liquid absorption performance of lithium ion battery pole piece and diaphragm |
| CN109696111B (en) * | 2018-12-27 | 2020-12-22 | 蜂巢能源科技有限公司 | Method for testing expansion rate of electrode active material and application thereof |
| CN110108591A (en) * | 2019-03-28 | 2019-08-09 | 合肥国轩高科动力能源有限公司 | A kind of evaluation method of cathode of lithium battery SBR absorbent |
| CN111928805A (en) * | 2020-07-31 | 2020-11-13 | 中国科学院宁波材料技术与工程研究所 | Method for testing and analyzing expansion rate of silicon-based negative electrode material |
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| US8631686B2 (en) * | 2011-10-17 | 2014-01-21 | Vineel Chakradhar | System to measure the absorptive capabilities of porous materials used in oil spill remediation |
| CN202735188U (en) * | 2011-12-27 | 2013-02-13 | 江门市本和机车配件实业有限公司 | Determination device for oil absorption expansion rate of sealing element |
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