CN100516820C - Method for detecting water content in lithium-ion cell pole piece or ploe core - Google Patents
Method for detecting water content in lithium-ion cell pole piece or ploe core Download PDFInfo
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- CN100516820C CN100516820C CNB2005101304081A CN200510130408A CN100516820C CN 100516820 C CN100516820 C CN 100516820C CN B2005101304081 A CNB2005101304081 A CN B2005101304081A CN 200510130408 A CN200510130408 A CN 200510130408A CN 100516820 C CN100516820 C CN 100516820C
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- pole piece
- moisture
- solvent
- pole
- lithium
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Abstract
The invention relates to a method to test humidity in lithium ion cell pole piece or pole piece. It adopts the solvent that would not react with water and could dissolve in water to contact the pole piece or pole piece to test water content. The method has little measuring error, good repeatability, and has wide using condition and range.
Description
Technical field
The invention relates to a kind of assay method of moisture, more particularly, the invention relates to the assay method of moisture in a kind of electrodes of lithium-ion batteries or the pole piece.
Background technology
Moisture in the lithium ion battery is the key factor that influences battery performance.Moisture in the battery is mainly from three aspects: the one, in battery manufacturing process, by the moisture of air introduction; The 2nd, the moisture that electrolytic solution self is brought into; The 3rd, inside battery has absorbed airborne moisture, after the immersion by electrolytic solution, is diffused into the moisture in the electrolytic solution.Wherein, introduce by air and can directly measure by pertinent instruments by the moisture that electrolytic solution self is brought into.
At present, the method that is applied to the solid sample determination of moisture has oven drying method and capacitance method.Oven drying method is by infrared or microwave heating, and the moisture evaporation in the solid sample is gone out, according to the quality that calculates moisture of poor quality before and after the heating.Capacitance method is by measuring the specific inductive capacity of aqueous specimen, the moisture of indirect determination sample.But these two kinds of methods have following shortcoming: (1) mainly is to measure constant moisture, cause than mistake if be used for measuring the minor amount of water branch of pole piece or pole piece, and poor repeatability; (2) the said determination method is to carry out in air, and airborne moisture can influence measurement result; (3) can not reflect the amount that is diffused into the moisture in the electrolytic solution by pole piece or pole piece intuitively; (4) measuring accuracy is subjected to the influence of sample kind, prescription, particle shape and sample bulk density.
Summary of the invention
The objective of the invention is to overcome the existing method of measuring the micro-moisture in pole piece or the pole piece with solid sample determination of moisture method can cause than mistake, and the defective of poor repeatability and provide a kind of can accurately measure and the mensuration electrodes of lithium-ion batteries of good reproducibility or pole piece in the method for moisture.
The invention provides a kind of method of measuring moisture in electrodes of lithium-ion batteries or the pole piece, wherein, this method comprises with not contacting with moisture pole piece or pole piece with water reaction and the solvent that can dissolve each other with water, and mensuration has absorbed the moisture in the solvent of moisture in pole piece or the pole piece then.
The determination of moisture method that the assay method of moisture will be used for liquid in electrodes of lithium-ion batteries provided by the invention or the pole piece is applied to solid sample, and can accurately directly determine by pole piece or pole piece and be diffused into micro-moisture in the electrolytic solution.The method can overcome existing defective in the existing solid moisture assay method, is not subjected to the influence of water in air branch, and is not subjected to the influence of sample kind, prescription, particle shape and sample bulk density, and the error of mensuration is little, but and replication.
Embodiment
According to method provided by the invention, described solvent carries out with contacting in closed container of pole piece or pole piece, and described contact is preferably carried out in battery container.Under the preferable case, the described solvent that does not react with water and can dissolve each other with water is to be injected in the battery container that is sealed with pole piece or pole piece by the liquid injection hole on the battery container, and sealing liquid injection hole, leave standstill contact, described solvent is fully contacted with moisture pole piece or pole piece, the solvent that will absorb moisture is then extracted out, and measures moisture wherein.
According to assay method provided by the invention, the described solvent that does not react with water and can dissolve each other with water is the polar organic solvent of moisture less than 20ppm, as being selected from the liquid carbonate solvent one or more, described liquid carbon acid esters can be dimethyl carbonate (DMC), ethylene carbonate (EC), the first and second basic carbonic esters (EMC), diethyl carbonate (DEC).
The injection rate IR of described solvent is pole piece or pole piece weight 0.25-2 a times, is preferably 0.3-1 doubly, and the weight of described pole piece is the general assembly (TW) of positive pole, negative pole and barrier film.
After being injected into described solvent in the battery container, the method that liquid injection hole is sealed can adopt the method for well known to a person skilled in the art, as adopting the steel ball sealing.
The temperature of described contact is 45-75 ℃, is preferably 60-75 ℃, and the time of contact is 24-48 hour, is preferably 24-30 hour.
According to the present invention, described mensuration has absorbed in the solvent of moisture in pole piece or the pole piece method of moisture and can adopt and well known to a person skilled in the art any means, as NEUTRON METHOD, spectral method, karl fischer titrimetry etc., these methods are the micro-moisture in the working sample accurately, can also avoid the influence of environment to the result.Under the preferable case, it is that the Karl fischer coulometric titration moisture teller of 10ppm-10000ppm is measured that the present invention adopts instrument journey scope.
Described fundamental reaction principle with moisture in Karl fischer coulometric titration moisture teller mensuration pole piece or the pole piece is I
2With quantitative H
2O reacts.Equation is as follows:
In the Karl fischer coulometric titration, the direct electrolysis of electrolyte electrochemical method generates required iodine (" electronics dropper ").Utilize two platinum electrodes to apply stable interchange, the potential method directing terminal.When a spot of free-iodine very, the voltage difference at platinum indicator electrode two ends sharply reduces.Utilize this variation to determine titration end-point.
According to the present invention, the computing method of moisture are in described pole piece or the pole piece:
Solvent quality (gram) * 10 behind the diffusing capacity of moisture (gram) in pole piece or the pole piece=moisture (ppm) * absorption moisture
-6Wherein said moisture is the content of having removed behind solvent self moisture.
Diffusing capacity (the gram) * η of moisture in moisture in pole piece or the pole piece (gram)=pole piece or the pole piece (in the formula, η is the coefficient of diffusion of hydrone, is test empirical constant, η=1.5);
Percent water content (the %)=pole piece in pole piece or the pole piece or the quality (gram) * 100% of moisture (gram)/pole piece in the pole piece or pole piece.
The computing formula of the relative standard deviation of the percent water content in pole piece or the pole piece is:
In the formula, standard deviation
Absolute deviation d
i=x
i-x.
According to method provided by the invention, described pole piece can be anode pole piece or cathode pole piece, and the anode pole piece of described lithium ion battery and the composition of cathode pole piece, content and preparation method are conventionally known to one of skill in the art.
For example, described positive pole comprises collector body and coating and/or is filled in positive electrode on the collector body that described positive electrode comprises positive active material, conductive agent and anodal bonding agent.Described positive active material is the positive active material of the embedded removal lithium embedded of this area routine, a kind of or its potpourri: the Li in the preferred following material
xNi
1-yCoO
2(wherein, 0.9≤x≤1.1,0≤y≤1.0), Li
1+aM
bMn
2-bO
4(wherein ,-0.1≤a≤0.2,0≤b≤1.0, M is a kind of in lithium, boron, magnesium, aluminium, titanium, chromium, iron, cobalt, nickel, copper, zinc, gallium, yttrium, fluorine, iodine, the element sulphur), Li
mMn
2-nB
nO
2(wherein, B is a transition metal, 0.9≤m≤1.1,0≤n≤1.0).
The kind of described anodal bonding agent and content are conventionally known to one of skill in the art, for example one or more in fluorine resin and polyolefin compound such as polyvinylidene fluoride (PVDF), polytetrafluoroethylene (PTFE), the styrene-butadiene rubber (SBR).In general, according to the difference of used anodal bonding agent kind, be benchmark with the weight of positive active material, the content of anodal bonding agent is 0.5-8 weight %, is preferably 1-5 weight %.
Described anodal conductive agent is not particularly limited, can be the anodal conductive agent of this area routine, such as the ketjen carbon black, acetylene black, furnace black, carbon fiber VGCF, in nano-graphite, graphite and the electrically conductive graphite one or more, weight with positive active material is benchmark, and the content of described conductive agent is 0.01-20 weight %, is preferably 0.5-10 weight %.
Positive electrode collector can be positive electrode collector conventional in the lithium ion battery, uses aluminium foil as positive electrode collector in specific embodiments of the present invention.
The preparation method of described positive pole can adopt conventional preparation method.For example, the slurry of described positive active material, conductive agent and bonding agent and solvent is applied and/or is filled on the collector body, drying, calendering or do not roll can obtain described positive pole.Wherein, described solvent can be selected from one or more in N-Methyl pyrrolidone (NMP), dimethyl formamide (DMF), diethylformamide (DEF), dimethyl sulfoxide (DMSO) (DMSO), tetrahydrofuran (THF) and water and the alcohols; The consumption of solvent can make described pastel have viscosity and flowability, can be coated on the described collector body to get final product.In general the weight with positive active material is benchmark, and the content 20-70 weight % of described solvent is preferably 30-60 weight %.Wherein, drying, the method for calendering and condition are conventionally known to one of skill in the art.
Described negative pole comprises collector body and coating and/or is filled in negative material on the collector body that described negative material comprises negative electrode active material and negative pole bonding agent.
Described negative electrode active material is not particularly limited, can use embedding of this area routine to disengage the negative electrode active material of lithium, such as in native graphite, Delanium, petroleum coke, organic cracking carbon, carbonaceous mesophase spherules, carbon fiber, ashbury metal, the silicon alloy one or more, preferred electrographite.
The kind of described negative pole bonding agent and content are conventionally known to one of skill in the art, for example one or more in fluorine resin and polyolefin compound such as polyvinylidene fluoride (PVDF), polytetrafluoroethylene (PTFE), the styrene-butadiene rubber (SBR); In general, according to the difference of adhesive therefor kind, be benchmark with the weight of negative electrode active material, the content of negative pole bonding agent is 0.01-8 weight %, is preferably 0.02-5 weight %.
Described negative material can also comprise conductive agent, and described conductive agent is not particularly limited, and can be the cathode conductive agent of this area routine, such as in ketjen carbon black, acetylene black, furnace black, carbon fiber VGCF, conductive carbon black and the electrically conductive graphite one or more.Weight with negative electrode active material is benchmark, and the content of described conductive agent is 1-15 weight %, is preferably 2-10 weight %.
Negative electrode collector can be for negative electrode collector conventional in the lithium ion battery, as stamped metal, and metal forming, net metal, foamed metal uses Copper Foil as negative electrode collector in specific embodiments of the present invention.
The preparation method of described negative pole can adopt conventional preparation method.For example, with negative electrode active material, conductive agent and negative pole bonding agent and solvent, apply and/or be filled on the described collector body, drying is rolled or is not rolled, and can obtain described negative pole.Wherein, described solvent can be selected from one or more in N-Methyl pyrrolidone (NMP), dimethyl formamide (DMF), diethylformamide (DEF), dimethyl sulfoxide (DMSO) (DMSO), tetrahydrofuran (THF) and water and the alcohols.The consumption of solvent can make described pastel have viscosity and flowability, can be coated on the described collector body to get final product.In general, be benchmark with the weight of negative electrode active material, the consumption of described solvent is 100-150%.Wherein, drying, the method for calendering and condition are conventionally known to one of skill in the art.
According to the present invention, the pole piece of described lithium ion battery comprises positive pole, negative pole and barrier film, described barrier film is arranged between positive pole and the negative pole, described barrier film can be selected from various barrier films used in the lithium ion battery, as the high molecular polymer microporous membrane, comprise polypropylene microporous membrane and polypropylene and poly MULTILAYER COMPOSITE microporous membrane.The position of described barrier film, character and kind are conventionally known to one of skill in the art.Described pole piece is by positive pole, barrier film, the negative pole of battery being reeled successively, stackedly constitute, and described coiling, stacked method are conventionally known to one of skill in the art.When according to the method described in the present invention the moisture in the pole piece being measured, described pole piece can reel according to coiling, the overlapping method of pole piece, measure after being sealed in the battery container after stacked.
Below will the invention will be further described by embodiment.
Embodiment 1
Present embodiment illustrates the preparation of electrodes of lithium-ion batteries provided by the invention.
(1) Zheng Ji preparation
With the anodal active component LiCoO of 100 grams
2, 2 gram bonding agent teflon and 3.2 gram conductive agent acetylene blacks join among the 40 gram NMP, mix, in de-airing mixer, stir then and form uniform anode sizing agent.This slurry is coated on the aluminium foil equably, 150 ℃ of following oven dry, roll-ins then, cuts to make and be of a size of 540 * 43.5 millimeters positive pole, wherein contain 5.8 gram active component LiCoO
2
(2) preparation of negative pole
100 gram negative electrode active composition native graphites, 1 gram bonding agent teflon and 4 gram conductive agent carbon blacks are joined among the 120 gram NMP, in de-airing mixer, stir then and form uniform cathode size.This slurry is coated on the Copper Foil equably, then in 90 ℃ of following oven dry, roll-in, cut to make and be of a size of 500 * 44 millimeters negative pole, wherein contain 2.6 gram active component native graphites.
Embodiment 2
Present embodiment illustrates the assay method of moisture in the electrodes of lithium-ion batteries provided by the invention.
The weight that embodiment 1 is obtained is that 4.6 cathode pole pieces that restrain are wound into the pole piece shape, be inserted in the battery aluminum hull, the laser bonding cover plate, vacuum high-temperature baking 14 hours, inject the 4.2 gram DMC that moisture is 11ppm by the fluid injection machine, the employing diameter is 1.4 millimeters a steel ball sealing liquid injection hole, places 24 hours in 75 ℃ of baking boxs.From 5 samples that obtain according to the method described above, extract DMC respectively with 5 milliliters of syringes then, the DMC that at every turn extracts is about 1 milliliter, be injected into the moisture of measuring in the Karl fischer coulometric titration moisture teller wherein successively, the result is as shown in table 1, and the percent water content in the calculating pole piece, the result is as shown in table 2.
Embodiment 3
Present embodiment illustrates the assay method of moisture in the electrodes of lithium-ion batteries provided by the invention.
With the weight that obtains among the embodiment 1 is that 4.6 cathode pole pieces that restrain place 25 ℃, humidity is under 54% the environment, placed 24 hours, reel, be stacked to the pole piece shape again, be inserted in the battery aluminum hull laser bonding cover plate, vacuum high-temperature baking 14 hours, injecting 4.2 gram moistures by the fluid injection machine is the EC of 13.5ppm and the mixed solvent of DEC (weight ratio of EC and DEC is 7: 3), and the employing diameter is 1.4 millimeters a steel ball sealing liquid injection hole, places 24 hours in 75 ℃ of baking boxs.From 5 samples that obtain according to the method described above, extract DMC respectively with 5 milliliters of syringes then, the DMC that at every turn extracts is about 1 milliliter, be injected into the moisture of measuring in the Karl fischer coulometric titration moisture teller wherein successively, the result is as shown in table 1, and the percent water content in the calculating pole piece, the result is as shown in table 2.
Embodiment 4
Present embodiment illustrates the assay method of moisture in the Lithium-Ion Battery Core provided by the invention.
Measure moisture according to the method for embodiment 2, different is, mensuration be the positive and negative electrode pole piece that will obtain among the embodiment 1 and polypropylene screen is wound into moisture in the pole pieces that weight is 12 grams, and the injection rate IR of DMC is 4.7 to restrain.The result is as shown in table 1, and calculates the percent water content in the pole piece, and the result is as shown in table 2.
Comparative Examples 1
The reference assay method of moisture in this Comparative Examples explanation electrodes of lithium-ion batteries.
This Comparative Examples adopts the moisture in infrared moisture tester (model SARTORIUS AG MA50) the mensuration pole piece of the same race.Infrared method is for earlier being that the cathode pole pieces of 4.6 grams place 25 ℃ with the weight that obtains among the embodiment 1, and humidity is under 54% the environment, to place 24 hours, and then be wound into the pole piece shape, be inserted in the battery aluminum hull laser bonding cover plate, vacuum high-temperature baking 14 hours, take out pole piece, after shredding pole piece is put into the infrared moisture tester, be heated to 130 ℃, be 2 minutes heat time heating time, mensuration obtains percent water content value wherein, and the result is as shown in table 2.
Comparative Examples 2
The reference assay method of moisture in this Comparative Examples explanation Lithium-Ion Battery Core.
Measure according to the method for Comparative Examples 1 that the positive and negative electrode pole piece coiling that obtains among the embodiment 1 is become weight is moisture in the pole pieces of 12 grams, different is, directly will obtain putting into the infrared moisture tester after pole piece shreds, be heated to 130 ℃, be 2 minutes heat time heating time, mensuration obtains percent water content value wherein, and the result is as shown in table 2.
Table 1
Annotate: the moisture that records in table 1 data is for removing the moisture that carries in the solvent behind the moisture.
Table 2
Data from table 2 as can be seen, 1-2 compares with Comparative Examples, identical pole piece and the pole piece that under identical condition, obtains respectively, owing to the infrared analysis method that adopts among the Comparative Examples 1-2 is subjected to the influence that water in air is divided for measuring under explorative environment, and in the process of heating, bonding agent in the pole piece material, thereby materials such as solvent evaporate the accuracy that has influence on the result easily, the numerical error that obtains is bigger, and method provided by the invention is for to carry out under airtight condition, and be not subjected to the interference of other factors, therefore can determine the micro-moisture in pole piece or the pole piece more accurately, error at measurment is little, favorable repeatability.
Claims (7)
1, a kind of method of measuring moisture in electrodes of lithium-ion batteries or the pole piece, it is characterized in that, this method comprises with not contacting with moisture pole piece or pole piece with water reaction and the solvent that can dissolve each other with water, and mensuration has absorbed the moisture in the solvent of moisture in pole piece or the pole piece then; Described contact is carried out in closed container.
2, method according to claim 1, wherein, described closed container is a battery container.
3, method according to claim 1, wherein, described solvent is the polar organic solvent of moisture less than 20ppm.
4, method according to claim 3, wherein, described polar organic solvent is selected from one or more in dimethyl carbonate, ethylene carbonate, the first and second basic carbonic esters, the diethyl carbonate.
5, method according to claim 1, wherein, the injection rate IR of described solvent is pole piece or pole piece weight 0.25-2 a times, the weight of described pole piece is the general assembly (TW) of positive pole, negative pole and barrier film.
6, method according to claim 1, wherein, the time of described contact is 24-48 hour, the temperature of contact is 45-75 ℃.
7, method according to claim 1 wherein, is that the Karl fischer coulometric titration moisture teller of 10ppm-10000ppm is measured the moisture in the solvent absorbed moisture in pole piece or the pole piece with instrument journey scope.
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|---|---|---|---|
| CNB2005101304081A CN100516820C (en) | 2005-12-09 | 2005-12-09 | Method for detecting water content in lithium-ion cell pole piece or ploe core |
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|---|---|---|---|
| CNB2005101304081A CN100516820C (en) | 2005-12-09 | 2005-12-09 | Method for detecting water content in lithium-ion cell pole piece or ploe core |
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| CN100516820C true CN100516820C (en) | 2009-07-22 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101377459B (en) * | 2007-08-29 | 2012-05-23 | 深圳市比克电池有限公司 | Method for measuring penetrating capability of electrolytic solution to electrode material |
| CN109406713A (en) * | 2018-11-22 | 2019-03-01 | 东莞市杉杉电池材料有限公司 | A kind of karl Fischer volumetric method reagent and its preparation method and application |
| CN110514724B (en) * | 2019-08-22 | 2022-04-12 | 中车青岛四方车辆研究所有限公司 | Method for detecting micro-water content in soft package lithium ion capacitor core |
| CN117214112A (en) * | 2023-09-07 | 2023-12-12 | 深圳埃克森新能源科技有限公司 | Online consistency monitoring method for battery baking pole piece based on laser moisture tester |
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2005
- 2005-12-09 CN CNB2005101304081A patent/CN100516820C/en not_active Expired - Fee Related
Non-Patent Citations (4)
| Title |
|---|
| 六氟磷酸锂的水分测定. 李雯，凌宝萍，杜秀月.盐湖研究，第12卷第3期. 2004 |
| 六氟磷酸锂的水分测定. 李雯，凌宝萍，杜秀月.盐湖研究，第12卷第3期. 2004 * |
| 锂电池用有机溶剂的纯化与效果. 丁运长，王中锋.高等学校化学学报，第7卷第12期. 1986 |
| 锂电池用有机溶剂的纯化与效果. 丁运长，王中锋.高等学校化学学报，第7卷第12期. 1986 * |
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