CN107271317A - The method for testing rare earth new power negative plate expansion rate - Google Patents
The method for testing rare earth new power negative plate expansion rate Download PDFInfo
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- CN107271317A CN107271317A CN201710500642.1A CN201710500642A CN107271317A CN 107271317 A CN107271317 A CN 107271317A CN 201710500642 A CN201710500642 A CN 201710500642A CN 107271317 A CN107271317 A CN 107271317A
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- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/02—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content
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Abstract
The invention belongs to water system power battery technology field, and in particular to a kind of method of test rare earth new power negative plate expansion rate.Rare earth new power battery core loads in battery case, after top seal is good, carry out normal pressure fluid injection, sealing, chemical conversion, the battery activated is discharged, shelve, rotary valve is opened under inert gas normal pressure atmosphere, the flowing electrolyte of the inside is poured out, electrolyte is added, rotary valve is closed, after progress discharge and recharge five times, shelve, rotary valve is opened under inert gas normal pressure atmosphere, pour out the electrolyte of the inside flowing, weighed before and after each operation, the expansion rate of rare earth new power negative plate in actual use can be obtained.The result that the present invention is obtained has two, can carry out error calculation, improves accuracy rate, under conditions of the process conditions and flow of battery making are not changed, the real data of pole piece expansion rate can be easily measured, error is small, favorable repeatability, simple and easy to apply, versatility is high, is easy to practical operation.
Description
Technical field
The invention belongs to water system power battery technology field, and in particular to one kind test rare earth new power negative plate expansion rate
Method.
Background technology
A kind of new water system electrokinetic cell of the rare earth new power using rare earth new material as main application feature, as a kind of new
Type energy carrier turns into the focus that battery industry is studied, and represents the developing direction of water system electrokinetic cell.Due to rare earth new power
With high power, the long-life, the environment-friendly recyclable, temperature applicable range that haves a wide reach, using safety, memory-less effect etc.
Advantage, therefore it is referred to as new generation of green battery.In energy shortage, today of environmental pollution, rare earth new power shows wide
Application prospect.
Rare earth new power is as a kind of important automobile-used and other power and the important electrochmical power source of energy-storage system, and rare earth is new
Power cathode piece expansion rate is to influence the key parameter of battery performance.In order to design high-performance rare-earth new power, it would be desirable to
The accurate expansion rate for knowing negative plate, is all the chief active indirectly to negative plate so far according to traditional evaluation method
Material abundance rare earth alloy carries out the measure of cubical expansivity；Individually carry out or estimate indirectly outside battery, it is this to survey
Method for testing can measure the expansion rate of negative plate to a certain extent, but the result so tested with they battery true work
Expansion rate under condition environment is differentiated, can not reflect influence of the true environment to negative plate expansion rate.In addition, existing side
Also there is measurement data fluctuation greatly in method, poor reproducibility, and operation inconvenience, or material consumption are more, the deficiency such as easy cross pollution.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of test rare earth new power negative plate expansion rate
Method, under conditions of the process conditions of battery manufacturing technology and technological process is not changed, convenient measurement pole piece expansion rate
Real data, error is small, favorable repeatability, and simple and easy to apply, versatility is high, is easy to practical operation.
The method of test rare earth new power negative plate expansion rate of the present invention, comprises the following steps：
(1) volume of negative plate is determined, V is designated as0, rare earth new power battery core is made, rare earth new power battery core is loaded into electricity
Pond shell, after top seal is good, installs safety valve additional；
(2) open the safety-valve, sealed after normal pressure fluid injection, weigh, be designated as M3；It is melted into according to existing chemical synthesis technology
Weighed after activation, be designated as M4；
(3) shelve, rotary valve is opened under inert gas normal pressure atmosphere, after the flowing electrolyte for pouring out the inside, to battery
Weighed, be designated as M5；The electrolyte poured out is weighed, M is designated as6；Electrolyte is added, is added after electrolyte, to closing
The completed cell for closing rotary valve is weighed, and is designated as M8；
(4) to battery charging and discharging five times, shelve, battery is weighed, be designated as M9；Then in inert gas normal pressure atmosphere
Lower opening rotary valve, pours out the electrolyte of the inside flowing, the electrolyte poured out is weighed, M is designated as10；Pour out after electrolysis
Battery is also weighed, and is designated as M11, calculate rare earth new power negative plate expansion rate.
The calculation formula of rare earth new power negative plate expansion rate is one kind in following two：
Expansion rate μ1=[M6+(M4-M3)+(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 6mol/L KOH solution, and proportion is 1.2900g/L.The expansion rate data of acquisition can anti-mistake
Further to instruct process conditions and the technological process of battery manufacturing technology, in design brand new cells, the expansion rate data can
As design considerations, to be verified again in practice.
The calculation formula of expansion rate error is：
Expansion rate error：Δ μ=| (μ1-μ2)|/μ1* 100%.
Each monomer, which tests the obtained same data of expansion rate, two, front and rear directly to carry out error calculation, I
Using it as internal longitudinal index, and contrasted with the horizontal scale error of multiple batteries, so as to obtain very objective
Data.
Making rare earth new power battery core described in step (1) is：By technique of the negative plate according to existing battery manufacturing technology
Condition and the condition of technological process make rare earth new power battery core.
Battery case is the square cell that transparent, bottom carries rotary valve.Rare earth new power is square lamination, because
This, using square cell, for transparent lucite, (thickness that lucite is pulled is 10mm to the battery case of test, using ABS
Glue carries out bubble-free bonding) because in test process, can intuitively see internal-response situation.Not special
Under explanation, all test environment temperature are 20 ± 5 DEG C.In addition 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 especially suitable for all kinds of capacity carries out 1:1 actual test.
Preferably, the structure of battery case is as follows：Battery case includes battery case housing, and battery case housing upper is provided with top cover,
Top cover, which is provided with safety valve, battery case housing, rare earth new power battery core, and battery case housing bottom is provided with rotary valve, and rare earth is new
Negative plate is included in power supply battery core.Negative plate is preferably 30.
When being weighed in operating process, 0.0001g is accurate to.The balance weighed using a ten thousandth precision, was tested
Cheng Zhong, rotary valve needs to open once, and the gas that the inside is run out is probably micro, during chemical conversion and discharge and recharge five times
Gas can be produced, in the case that air pressure is too high, may be run out of from safety valve, seldom, the present invention is used the gas flow run out of
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 plate is catalysis
Mechanism, in charge and discharge process, inside battery can produce a large amount of gases, mainly hydrogen, stop after charge or discharge, certain
Time in, the rare earth alloy of negative plate can hydrogen that gradually catalytic adsorption is produced, the air pressure of inside battery can reduce gradually
Balanced to external atmosphere pressure, this process needs 48~72h of time, the time is too short, and internal pressure is not fully ensured that also and is reduced to
It is consistent with ambient pressure, rotary valve is opened too early, and the gas run out can cause electrolyte weight relatively low, and the time is oversize, battery
Increase tendency can be presented in self-discharge rate, and this can also produce gas, cause internal pressure to go up not down, and open rotary valve and will also result in
Internal gas loses, and also results in electrolyte weight relatively low.
The flowing electrolyte for pouring out the inside described in step (3), the time of pouring out needs 0.5~1h.Rotary valve is opened, is inclined
Electrolyte needs the time, because being all to be coated with barrier film inside battery pole piece, barrier film is nonwoven cloth material, with three-dimensional apertures
Footpath, 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 oversize, suspends
Drop may be adsorbed to above again；At the right time, it is appropriate to rock, it 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 run into, easily oxidation, influence the catalytic performance of rare earth alloy, operated in inert gas atmosphere, completely cut off air
In oxygen, do not influence battery performance, it is ensured that chemical property is consistent before and after test, the influence that control influence factor is caused is by mistake
In poor scope.
Refer to for five times chargeability change from 0~100% to battery charging and discharging.Chargeability change refers to filling from 0~100%
Electricity is just full of, and electric discharge uniformly discharges into 1.0V, just discharge off, and charging and discharging currents are 0.2C；If electric current is too small, need
Overlong time is wanted, if electric current is too big, the rise of inside battery internal pressure can be caused soon, the chemical property difference of front and rear five times is higher than
The error amount of permission.
The present invention carries the square cell of rotary valve by transparent, bottom, in the technique of existing battery manufacturing technology
Under conditions of condition and technological process, rare earth new power battery core is loaded in battery case with complete structure, is carried out according to set flow
Operation, carries out being weighed, is volume by electrolyte weight differential conversion, with rare earth new power negative plate before and after each operation
Volume is compared, it is hereby achieved that the expansion rate data of rare earth new power negative plate in actual use, also simultaneously
Battery core pick up data can be obtained.
As a kind of perferred technical scheme, the present invention may be used also while rare earth new power negative plate expansion rate is tested
To test rare earth new power battery core imbibition, comprise the following steps：
(1) volume of negative plate is determined, V is designated as0, the weight of rare earth new power battery core is determined, M is designated as1, rare earth is newly electric
Source battery core loads battery case, after top seal is good, installs safety valve additional and weighs together, be designated as M2；
(2) open the safety-valve, sealed after normal pressure fluid injection, weigh, be designated as M3；It is melted into according to existing chemical synthesis technology
Weighed after activation, be designated as M4；
(3) shelve after certain time, rotary valve is opened under inert gas normal pressure atmosphere, pour out the flowing electrolyte of the inside
Afterwards, battery is weighed, is designated as M5；The electrolyte poured out is weighed, M is designated as6；Add electrolyte, the electricity of addition
Solution liquid measure is weighed, and is designated as M7；Add after electrolyte, the completed cell for closing rotary valve is weighed, M is designated as8；
(4) to battery charging and discharging five times, shelve after certain time, battery is weighed, be designated as M9；Then in indifferent gas
Rotary valve is opened under body normal pressure atmosphere, the electrolyte of the inside flowing is poured out, the electrolyte poured out is weighed, M is designated as10；
The battery gone out after electrolysis is also weighed, and is designated as M11。
The calculation formula of pick up is one kind in following two：
Rare earth new power battery core imbibition：Pick up ν1=[(M3-M4)+(M3-M2)]/M1* 100%
Pick up ν2=[| (M7-M6)|+(M3-M4)+(M3-M2)]/M1* 100%
Each monomer, which tests the obtained same data of expansion rate, two, front and rear directly to carry out error calculation, I
Using it as internal longitudinal index, and contrasted with the horizontal scale error of multiple batteries, so as to obtain very objective
Data.
The calculation formula of pick up error is：
Pick up error：Δ ν=| (ν1-ν2)|/ν1* 100%.
Each monomer, which tests the obtained same data of pick up, two, front and rear directly to carry out error calculation, I
Using it as internal longitudinal index, and contrasted with the horizontal scale error of multiple batteries, so as to obtain very objective
Data.
In summary, the present invention has advantages below：
(1) the present invention is especially suitable for test negative plate expansion rate, weighed before and after each operation, by electrolyte weight
Amount differential conversion is volume, is compared with rare earth new power negative plate volume, it is hereby achieved that rare earth new power negative plate exists
Expansion rate data in actual use.With traditional negative plate battery material abundance rare earth alloy expansion rate method of testing
Compare, this method of testing is not under conditions of the process conditions of battery manufacturing technology and technological process is changed, in that context 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 plate
Rate.
(2) present invention, which tests each monomer obtained negative plate expansion rate, two, front and rear directly to be missed
Difference is calculated, and improves accuracy rate, and we are carried out it pair as internal longitudinal index, and with the horizontal scale errors of multiple batteries
Than so as to obtain very objective data, in design brand new cells, the expansion rate data can be as design considerations, in reality
Trample it is middle verified again, reduce R＆D costs and shorten the R＆D cycle.
(3) simple and easy to apply, versatility of the invention is high, is easy to practical operation.
(4) accurately and reliably, the repetition uniformity of test result is fine for the method for present invention test negative plate expansion rate.
(5) the data M in present invention test7If more than M10+(M9-M10-M11), show that cell activation system is unreasonable, need
Further to improve, if M7Equal to M10+(M9-M10-M11), then show that chemical synthesis technology is very reasonable, the result that the present invention is measured can
Direct practical manifestation of the reflection test object in battery, with actual directive significance, test result thus can be used for improving
Chemical synthesis technology.
Brief description of the drawings
Fig. 1 is the structural representation for the battery case that the embodiment of the present invention is used；
In figure：1- battery case housings, 2- rare earth new power battery cores, 3- top covers, 4- safety valves, 5- rotary valves.
Embodiment
With reference to embodiment, the present invention will be further described.
Embodiment 1
It is a kind of to test rare earth new power negative plate expansion rate and the method for battery core imbibition：
(1) volume of negative plate is determined, V is designated as0, the weight of rare earth new power battery core is determined, M is designated as1, with complete structure
Load the square cell that transparent, bottom carries rotary valve, after top seal is good, installs safety valve additional and weigh together, be designated as M2；
(2) open the safety-valve, sealed after normal pressure fluid injection, weigh, be designated as M3；It is melted into according to existing chemical synthesis technology
Weighed after activation, be designated as M4；
(3) shelve after 60h, rotary valve opened under inert gas normal pressure nitrogen atmosphere, pour out the flowing electrolyte of the inside,
Continue after 0.8h, battery is weighed, M is designated as5；The electrolyte poured out is weighed, M is designated as6；Add electrolyte,
The electrolyte content of addition is weighed, and is designated as M7；Add after electrolyte, the completed cell for closing rotary valve is weighed, remember
For M8；
(4) to battery charging and discharging five times, chargeability changes from 0~100%, shelves after 60h, battery is weighed, note
For M9；Then rotary valve is opened under inert gas normal pressure nitrogen atmosphere, pours out the electrolyte of the inside flowing, continued after 0.8h,
The electrolyte poured out is weighed, M is designated as10；Pour out the battery after electrolysis also to be weighed, be designated as M11。
The structure of battery case used is as shown in figure 1, battery case includes battery case housing 1, and the top of battery case housing 1 is provided with
Top cover 3, top cover 3, which is provided with safety valve 4, battery case housing 1, rare earth new power battery core 2, and the bottom of battery case housing 1 is provided with rotation
Negative plate is included in rotary valve 5, rare earth new power battery core 2, negative plate is 30.
The data tested out, negative plate expansion rate μ is calculated by the calculation formula of expansion rate1With expansion rate μ2Respectively
For 2.1017% and 2.0964%；Pick up ν is calculated by the calculation formula of battery core pick up1And ν2It is 14.4709% respectively
With 14.4688%.Error is respectively 0.25% and 0.015%, and respectively less than 0.3% allowable error, measuring accuracy meets requirement.
Embodiment 2
It is a kind of to test rare earth new power negative plate expansion rate and the method for battery core imbibition：
(1) volume of negative plate is determined, V is designated as0, the weight of rare earth new power battery core is determined, M is designated as1, with complete structure
Load the square cell that transparent, bottom carries rotary valve, after top seal is good, installs safety valve additional and weigh together, be designated as M2；
(2) open the safety-valve, sealed after normal pressure fluid injection, weigh, be designated as M3；It is melted into according to existing chemical synthesis technology
Weighed after activation, be designated as M4；
(3) shelve after 48h, rotary valve opened under inert gas normal pressure argon gas atmosphere, pour out the flowing electrolyte of the inside,
Continue after 0.5h, battery is weighed, M is designated as5；The electrolyte poured out is weighed, M is designated as6；Add electrolyte,
The electrolyte content of addition is weighed, and is designated as M7；Add after electrolyte, the completed cell for closing rotary valve is weighed, remember
For M8；
(4) to battery charging and discharging five times, chargeability changes from 0~100%, shelves after 48h, battery is weighed, note
For M9；Then rotary valve is opened under inert gas normal pressure argon gas atmosphere, pours out the electrolyte of the inside flowing, continued after 0.5h,
The electrolyte poured out is weighed, M is designated as10；Pour out the battery after electrolysis also to be weighed, be designated as M11。
The structure of battery case used is same as Example 1.
The data tested out, negative plate expansion rate μ is calculated by the calculation formula of expansion rate1With expansion rate μ2Respectively
For 2.1003% and 2.0994%；Pick up ν is calculated by the calculation formula of battery core pick up1And ν2It is 14.4698% respectively
With 14.4683%.Error is respectively 0.05% and 0.01%, and respectively less than 0.3% allowable error, measuring accuracy meets requirement.
Embodiment 3
It is a kind of to test rare earth new power negative plate expansion rate and the method for battery core imbibition：
(1) volume of negative plate is determined, V is designated as0, the weight of rare earth new power battery core is determined, M is designated as1, with complete structure
Load the square cell that transparent, bottom carries rotary valve, after top seal is good, installs safety valve additional and weigh together, be designated as M2；
(2) open the safety-valve, sealed after normal pressure fluid injection, weigh, be designated as M3；It is melted into according to existing chemical synthesis technology
Weighed after activation, be designated as M4；
(3) shelve after 72h, rotary valve opened under inert gas normal pressure nitrogen atmosphere, pour out the flowing electrolyte of the inside,
Continue after 1h, battery is weighed, M is designated as5；The electrolyte poured out is weighed, M is designated as6；Electrolyte is added, plus
The electrolyte content entered is weighed, and is designated as M7；Add after electrolyte, the completed cell for closing rotary valve is weighed, is designated as
M8；
(4) to battery charging and discharging five times, chargeability changes from 0~100%, shelves after 72h, battery is weighed, note
For M9；Then rotary valve is opened under inert gas normal pressure nitrogen atmosphere, pours out the electrolyte of the inside flowing, continued after 1h, it is right
The electrolyte poured out is weighed, and is designated as M10；Pour out the battery after electrolysis also to be weighed, be designated as M11。
The structure of battery case used is same as Example 1.
The data tested out, negative plate expansion rate μ is calculated by the calculation formula of expansion rate1With expansion rate μ2Respectively
For 2.0998% and 2.0959%；Pick up ν is calculated by the calculation formula of battery core pick up1And ν2It is 14.4703% respectively
With 14.4619%.Error is respectively 0.19% and 0.06%, and respectively less than 0.3% allowable error, measuring accuracy meets requirement.
Claims (10)
1. a kind of method for testing rare earth new power negative plate expansion rate, it is characterised in that：Comprise the following steps：
(1) volume of negative plate is determined, V is designated as0, rare earth new power battery core is made, rare earth new power battery core is loaded into battery case,
After top seal is good, safety valve is installed additional；
(2) open the safety-valve, sealed after normal pressure fluid injection, weigh, be designated as M3；Chemical conversion activation is carried out according to existing chemical synthesis technology
After weigh, be designated as M4；
(3) shelve, rotary valve is opened under inert gas normal pressure atmosphere, after the flowing electrolyte for pouring out the inside, battery is carried out
Weigh, be designated as M5；The electrolyte poured out is weighed, M is designated as6；Electrolyte is added, is added after electrolyte, is revolved to closing
The completed cell of rotary valve is weighed, and is designated as M8；
(4) to battery charging and discharging five times, shelve, battery is weighed, be designated as M9；Then beaten under inert gas normal pressure atmosphere
Rotary valve is driven, the electrolyte of the inside flowing is poured out, the electrolyte poured out is weighed, M is designated as10；Pour out the battery after electrolysis
Also weighed, be designated as M11, calculate rare earth new power negative plate expansion rate.
2. the method for test rare earth new power negative plate expansion rate according to claim 1, it is characterised in that：
The calculation formula of rare earth new power negative plate expansion rate is one kind in following two：
Expansion rate μ1=[M6+(M4-M3)+(M4-M5-M6)]/ρV0* 100%；
Or expansion rate μ2=[M10+(M8-M9)+(M9-M10-M11)]/ρV0* 100%；
Wherein, ρ is electrolyte density.
3. the method for test rare earth new power negative plate expansion rate according to claim 2, it is characterised in that：
The calculation formula of expansion rate error is：
Expansion rate error：Δ μ=| (μ1-μ2)|/μ1* 100%.
4. the method for test rare earth new power negative plate expansion rate according to claim 1, it is characterised in that：Battery case is
Transparent, bottom carries the square cell of rotary valve.
5. the method for test rare earth new power negative plate expansion rate according to claim 4, it is characterised in that：Battery case bag
Battery case housing is included, battery case housing upper is provided with top cover, and top cover, which is provided with safety valve, battery case housing, rare earth new power
Battery core, battery case bottom, which is provided with rotary valve, rare earth new power battery core, includes negative plate.
6. the method for test rare earth new power negative plate expansion rate according to claim 1, it is characterised in that：When weighing,
It is accurate to 0.0001g.
7. the method for test rare earth new power negative plate expansion rate according to claim 1, it is characterised in that：Step (3)
It is to shelve 48~72h with shelving in step (4).
8. the method for test rare earth new power negative plate 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%.
9. the method for test rare earth new power negative plate 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.
10. the method for test rare earth new power negative plate expansion rate according to claim 1, it is characterised in that：To battery
Discharge and recharge refers to for five times chargeability change from 0~100%.
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| CN109696111A (en) * | 2018-12-27 | 2019-04-30 | 蜂巢能源科技有限公司 | Test the method and its application of the expansion rate of electrode active material |
| CN110108591A (en) * | 2019-03-28 | 2019-08-09 | 合肥国轩高科动力能源有限公司 | Evaluation method for SBR liquid absorption performance of lithium battery negative electrode |
| 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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| 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 |
| CN109696111A (en) * | 2018-12-27 | 2019-04-30 | 蜂巢能源科技有限公司 | Test the method and its application of the expansion rate of electrode active material |
| CN110108591A (en) * | 2019-03-28 | 2019-08-09 | 合肥国轩高科动力能源有限公司 | Evaluation method for SBR liquid absorption performance of lithium battery negative electrode |
| 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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| CN107271317B (en) | 2019-10-18 |
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