CN1704765A - Method for testing battery electrode material filling properties - Google Patents
Method for testing battery electrode material filling properties Download PDFInfo
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- CN1704765A CN1704765A CNA2004100273946A CN200410027394A CN1704765A CN 1704765 A CN1704765 A CN 1704765A CN A2004100273946 A CNA2004100273946 A CN A2004100273946A CN 200410027394 A CN200410027394 A CN 200410027394A CN 1704765 A CN1704765 A CN 1704765A
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- electrode material
- pole piece
- testing
- filling capacity
- battery electrode
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
This invention relates to a test method for filling performance of a cell pole material including the following steps: A, mixing uniformly a pole material containing an active material and an adhesive in terms of the formulation to turn it to a paste, B, coating the paste uniformly on said collection sheet to turn it to a pole plate, C, cutting said pole plate to multiple plates to be tested and weighing them accurately after drying the paste, D, accurately testing thickness of each plate to be tested and the length of the collecting sheet, E, rolling the pole plates one by one till severe deformation happens to some plates, F, measuring the thickness and length of the plates, G, computing the filling performance parameter of said pole material according to the weight of a same plate and thickness difference before and after the deformation.
Description
[technical field]
The present invention relates to the method for test battery electrode material, more particularly, the present invention relates to a kind of method of filling capacity of the electrode material of testing lithium ion battery.
[background technology]
At present, with the lithium ion battery be the novel battery that the secondary cell of representative belongs to high-energy-density.Along with battery capacity, cycle performance and security performance requirement are more and more higher, people are also more and more higher to the requirement of battery positive and negative electrode material.Because the requirement to electrical property improves day by day, the filling performance of material more and more receives publicity.Because electrode material unit volume fill-up height in the electrode of battery that filling performance is good, thereby can correspondingly promote the capacity of battery, that is to say: the high pack completeness of electrode material is one of the most direct effective method that improves battery capacity.Because main electrode material such as active matter, conductive agent are to be in the particle packing state when initial, then just bonded dose is bonded on the flow collection sheet, and therefore people are the filling performances of testing and estimate electrode material according to the tap density of general powder granule in the past.
The measurement of tap density is to make material granule tightly packed as much as possible with long-time physical vibration, calculates by the unit volume quality of measuring particulate material under the closest packing state.It is an overall target of material granule granularity, size matching degree, and the instrument of particle tested bulk density is various powders or pellet characteristic tester usually, and this quasi-instrument is easy to be obtained by commercially available.
The tap density energy measurement of material goes out the maximum of general particulate material and piles up degree.But the stacking states of general particulate material is also inequality with the state of aggregation of the electrode particle material in battery pole piece.Include active material particle, conductive agent particle and cementing agent etc. in the battery pole piece, and in battery pole piece, the notion of particle even also comprise bar shape, high molecular particle etc.In addition, pole piece also needs to carry out roll-in, and material granule in the roll-in process deformation can take place.Obviously, use tap density evaluating material filling performance insufficient inaccurate, be unfavorable for design, production and the technology controlling and process of battery.
About the problem of battery electrode material particle properties aspect, it is that 01123431.8 Chinese patent file discloses a kind of meso-position radius of cobalt acid lithium and method of tap density of improving that application number is arranged.With Li
2CO
3, LiOH or both potpourris, CoCO
3, Co
3O
4Or both potpourris, LiCoO
2, three kinds of materials mix in proportion; 300～1000 ℃ of following Synthetic 2～20 hour; With the aggregate fragmentation in the synthetic material.It is said: prepared in this way LiCoO
2Meso-position radius and tap density big, and overcome once-firing LiCoO
2Incomplete and the incomplete problem of crystal formation of the particle internal-response that macroparticle may cause has been avoided to improving LiCoO
2Meso-position radius and tap density and with LiCoO
2Repeatedly sintering causes the excessive volatilization of lithium and to problem such as the destruction of particle surface and energy consumption be huge.Can be used for the particularly manufacturing field of lithium ion battery of high capacity power source.This document does not relate to accurate to improve, the rational content of the particles filled property detection of improvement.
The problem of relevant test material particle properties aspect, it is that the Chinese patent file of 87210110.U discloses a kind of cylinder formula (or box) vacuum plant of measuring the powder real density that the patent No. is arranged, and mainly is made of a vacuum tank and the liquid reservoir that several pycnometers are housed.Liquid feeding can carry out in a vacuum.It is said that this device can once record several samples, obtain average, it is about 40% to save the test duration, can not splash at dry powder body situation lower pumping, and test result is accurate.Can be widely used in fire-resistant, cement, dedusting technology, the strength conveying waits in all industries that need measure the powder real density.
This document discloses it test process that comprises ten steps in embodiment:
1, gets 4 of clean pycnometers of drying, be taken at 110 ± 5 ℃ and dry experiment powder 40～80 grams that are cooled to room temperature down.
2, weighing pycnometer on ten thousand/balance. quality is with M
1Expression.
3, in each pycnometer, pack into 5～10 the gram dry powder, weighing on balance respectively.With M
2Expression: calculate M=M
2-M
1M is the quality of powder sample.
4, the pycnometer that powder is housed is placed on the carriage. put into vacuum reservoir again. cut-out tap valve 19,22,23, take off rubber plug 17, in reservoir, inject 900 milliliters of liquid liquid mediums, cover rubber plug, start vacuum pump and open cock, when surplus pressure in the vacuum tank reaches 20 mm Hg when following, continued again to bleed 30 minutes.
5, the cut-out tap valve 19, open stopcock 21, close vacuum pump.
6, open cock successively and hear 23, fluid injection is till be lower than bottleneck 12-15 millimeter in pycnometer. cover bottle stopper at leisure.Make in the bottle and the capillary of bottle stopper hairpin in do not have bubble.
7, pycnometer was put into water bath with thermostatic control constant temperature (20 ℃ ± 0.5 ℃) 30～40 minutes, take out, dry, weigh, quality is represented with R.
8, sample in the pycnometer and liquid are outwelled, peace and quiet, the liquid medium in the reservoir that reinjects.Take out, cover bottle cap, making does not have bubble in the bottle.
9, pycnometer was put into water bath with thermostatic control constant temperature (20 ℃ ± 0.5 ℃) 30～40 minutes, take out, dry, weigh.Quality is represented with W.
10, calculate the powder real density by certain formula.
Therefore what above-mentioned test process recorded is traditional bulk density, and is not suitable for the filling capacity test of electrode material.
[summary of the invention]
At the above-mentioned shortcoming of prior art, the technical purpose that the present invention will reach is a kind of state of aggregation that more meets battery electrode material will be provided, be more suitable for the filling performance in the test electrode material, simple and effective battery electrode material filling capacity method of testing.
For this reason, technical scheme of the present invention is a kind of battery electrode material filling capacity method of testing, described electrode comprises flow collection sheet and the electrode material that applies on flow collection sheet, described electrode material comprises active material, bonding agent, this method of testing comprises the steps: A) will comprise that the electrode material of active material and bonding agent mixes according to prescription, make lotion, B) the gained lotion is uniformly coated on the described flow collection sheet, make pole piece, C) make gained lotion drying after, cutting gained pole piece is made multi-disc pole piece to be checked and is accurately weighed, D) accurately measure every pole piece thickness to be checked and flow collection sheet length, E) pole piece to be measured of the isobaric roll-in gained in pressurization ground piecewise, until the tested pole piece that gross distortion occurs, F) measure the tested pole piece thickness and the length of being out of shape, G) according to same tested pole piece weight, the filling capacity parameter that thickness difference before and after the distortion and length difference are calculated described electrode material.Therefore, of the present invention improve one's methods complete reference electrode material in battery electrode state of aggregation, prepare print to be measured according to electrode material prescription and technology, then the simulation print under the state of aggregation of multiple electrode material is carried out the filling capacity test, therefore, method of the present invention more meets the state of aggregation of battery electrode material, the more reasonable science of electrode material filling performance that test obtains, and method of testing of the present invention is simply effective.
For further strengthening the above-mentioned principal advantages of the inventive method, the present invention takes following concrete measure: stronger for the specific aim that makes test, more reflect material filling capacity under the true state of aggregation, it is anode electrode material or negative electrode material that method of the present invention is further distinguished described electrode material.
Described filling capacity parameter comprises compacted density, this compacted density value is the weight of tested the above electrode material of pole piece of distortion and the ratio of volume, the weight of this electrode material equals at step D) in the weight of the pole piece to be checked that accurately records deduct the weight of flow collection sheet, perhaps also can adopt other method calculate the weight of electrode material.
In described step e) in, the length elongation of anodal tested pole piece is not less than 2%, and the length elongation of the tested pole piece of negative pole is not less than 1%.Experiment confirm: positive electrode is after elongation is greater than 2%, and the compacted density of positive electrode material tends towards stability, and negative material is after elongation is greater than 1%, and the compacted density of negative electrode material also tends towards stability.Compacted density when therefore tending towards stability with the compacted density of electrode material is as the key index of electrode material filling capacity.
In order to improve the precision of follow-up measurement, press close to the actual state of aggregation of electrode material in the electrode, at described step D) in, the measuring accuracy of described pole piece to be checked is: thickness is accurate to 0.1 μ m, and length is accurate to 0.1mm.At described step C) in, described pole piece to be checked is of a size of 10cm * 0.5cm, weighs to be accurate to 1 μ g.In described steps A) in, also be added with solvent in the described bonding agent.At described step B) in, coating density and/or the consistency of thickness of described lotion on described flow collection sheet.Described electrode material also comprises conductive agent.Described flow collection sheet is metal forming or wire netting.
The electrode used therein material is selected for use according to actual prescription in the general battery electrode and is got final product in the inventive method test:
The positive electrode active materials material is selected from the composite oxides of cobalt acid lithium, lithium nickelate, ferrous acid lithium, LiMn2O4 or cobalt, nickel;
Negative active core-shell material is selected from acticarbon, graphite, modified artificial graphite, carbon particulate, carbon coated, carbon nanomaterial and carbon alloy material.
Conductive agent is selected from acetylene black, carbon fiber, graphite, carbon nanomaterial.
Cementing agent is selected from teflon, Kynoar, alkyd resin, modified starch, modified fibre.
Solvent is selected from N-Methyl pyrrolidone hereinafter to be referred as NMP, dimethyl formamide, dimethyl acetamide, pure water.
The metal flow collection sheet is selected from aluminium foil, Copper Foil.
In a word, method improvement of the present invention have be easy to implement, effectively, the advantage of closing to reality.
Below, with accompanying drawing technical solution of the present invention is described further in conjunction with specific embodiments.
[description of drawings]
Fig. 1 is the anode electrode material filling capacity curve map that the inventive method records.
Fig. 2 is the negative electrode material filling capacity curve map that the inventive method records.
[embodiment]
Embodiment 1
Anode electrode material filling capacity curve map shown in Figure 1 is to record through following concrete steps: 1) by weight percentage, and with a certain amount of different positive electrode active materials (seeing Table 1) and conductive agent acetylene black, polyfluortetraethylene of binding element, solvent NMP furnishing lotion; 2) make flow collection sheet with density and the uniform aluminium foil of thickness, lotion is coated on the flow collection sheet with uniform coating density, drying cuts into the pole piece of 10cm * 0.5cm, weighs, and weight is accurate to 1 ‰ of general assembly (TW); 3) thickness and the flow collection sheet length of every pole piece of measurement, thickness is accurate to 0.1um, and length is accurate to 0.1mm; 4) pole piece is put into isobaric roll squeezer roll-in, roll-in pressure is 1500Kpa; 5) pole piece thickness and the flow collection sheet length after the measurement roll-in, precision is the same; 6) repeated for 3～5 steps repeatedly, until the pole piece gross distortion; 7) calculate pole piece thickness deformation quantity and length deformation quantity: calculate elongation promptly with the length deformation quantity, elongation=(distortion back length-original length)/original length * 100%; Calculate compacted density promptly with the thickness deformation quantity, compacted density=electrode material weight/distortion rear electrode material coating volume; Make the curve map of anode pole piece compacted density and elongation according to actual test data.
Utilization said determination method is measured positive electrode active materials (sequence number A, B, C, D, E) respectively, and it is 53g/m that flow collection sheet is selected density for use
2, thickness is the aluminium foil of 20um, the result is referring to Fig. 1 and table 1.
Table 1
| Anodal sample | A (cobalt acid lithium) | B (lithium nickelate) | C (ferrous acid lithium) | D (LiMn2O4) | E (lithium nickel cobalt dioxide) |
| Compacted density g/cm 3 | ???3.615 | ???3.555 | ?3.682 | ?3.81 | ?3.66 |
Test result shows: the anode electrode material that method of the present invention records is after elongation is greater than 2%, and its compacted density tends towards stability, and this shows the filling performance when method of the present invention can reflect the electrode material practical application accurately.
Embodiment 2
Negative electrode material filling capacity curve map shown in Figure 2 is to record through similar above-mentioned test concrete steps: negative active core-shell material comprises that (sequence number A, B, C, D) is several, and it is 48g/m that flow collection sheet is selected density for use
2, thickness is the Copper Foil of 12um, result such as Fig. 2, table 2.
Table 2
| The negative pole sample | A (acticarbon) | B (Delanium) | C (carbon coated) | D (carbon particulate) |
| Compacted density g/cm 3 | ?1.613 | ?1.674 | 1.760 | ???1.881 |
Test result shows: the negative electrode material that method of the present invention records is after elongation is greater than 1%, and its compacted density tends towards stability, and this shows the filling performance when method of the present invention can reflect the electrode material practical application accurately.
Therefore, method of testing of the present invention is simple, is fit to commercial production and uses.
Claims (10)
1, a kind of battery electrode material filling capacity method of testing, described electrode comprises flow collection sheet and the electrode material that applies on flow collection sheet, described electrode material comprises active material, bonding agent, described method of testing comprises the steps: A) will comprise that the electrode material of active material and bonding agent mixes according to prescription, make lotion, B) the gained lotion is uniformly coated on the described flow collection sheet, make pole piece, C) make gained lotion drying after, cutting gained pole piece is made multi-disc pole piece to be checked and is accurately weighed, D) accurately measure every pole piece thickness to be checked and flow collection sheet length, E) pole piece to be measured of the isobaric roll-in gained in pressurization ground piecewise, until the tested pole piece that gross distortion occurs, F) measure the tested pole piece thickness and the length of being out of shape, G) according to same tested pole piece weight, the filling capacity parameter that thickness difference before and after the distortion and length difference are calculated described electrode material.
2, battery electrode material filling capacity method of testing as claimed in claim 1, it is characterized in that: described electrode material is anode electrode material or negative electrode material.
3, battery electrode material filling capacity method of testing as claimed in claim 1 or 2, it is characterized in that: described filling capacity parameter comprises compacted density, this compacted density value is the weight of tested the above electrode material of pole piece of distortion and the ratio of volume.
4, battery electrode material filling capacity method of testing as claimed in claim 3 is characterized in that: in described step e) in, the length elongation of anodal tested pole piece is not less than 2%, and the length elongation of the tested pole piece of negative pole is not less than 1%.
5, battery electrode material filling capacity method of testing as claimed in claim 3 is characterized in that: at described step D) in, the measuring accuracy of described pole piece to be checked is: thickness is accurate to 0.1 μ m, and length is accurate to 0.1mm.
6, battery electrode material filling capacity method of testing as claimed in claim 3 is characterized in that: at described step C) in, weighing is accurate to 1 μ g.
7, battery electrode material filling capacity method of testing as claimed in claim 3 is characterized in that: in described steps A) in, also be added with solvent in the described bonding agent.
8, battery electrode material filling capacity method of testing as claimed in claim 3 is characterized in that: at described step B) in, coating density and/or the consistency of thickness of described lotion on described flow collection sheet.
9, battery electrode material filling capacity method of testing as claimed in claim 3, it is characterized in that: described electrode material also comprises conductive agent.
9, battery electrode material filling capacity method of testing as claimed in claim 3, it is characterized in that: described flow collection sheet is metal forming or wire netting.
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| CNB2004100273946A CN100385248C (en) | 2004-06-01 | 2004-06-01 | Method for testing battery electrode material filling properties |
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|---|---|---|---|
| CNB2004100273946A CN100385248C (en) | 2004-06-01 | 2004-06-01 | Method for testing battery electrode material filling properties |
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| CN1704765A true CN1704765A (en) | 2005-12-07 |
| CN100385248C CN100385248C (en) | 2008-04-30 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010111851A1 (en) * | 2009-03-31 | 2010-10-07 | 深圳市吉阳自动化科技有限公司 | Electrode plate processing method |
| CN101992174A (en) * | 2010-09-14 | 2011-03-30 | 天津力神电池股份有限公司 | Method for monitoring surface density of coating quantity of lithium ion battery pole piece |
| CN102916175A (en) * | 2012-10-25 | 2013-02-06 | 湖南长远锂科有限公司 | Lithium manganese oxide spinel of anode materials of lithium ion batteries and method for manufacturing lithium manganese oxide spinel |
| CN107925130A (en) * | 2015-10-08 | 2018-04-17 | 株式会社Lg化学 | The method of adhesive distribution in measuring electrode |
| CN108226641A (en) * | 2017-12-30 | 2018-06-29 | 湖北金泉新材料有限责任公司 | A kind of test method of anode material for lithium-ion batteries conductivity |
| CN108895945A (en) * | 2018-05-15 | 2018-11-27 | 首钢集团有限公司 | A kind of measuring device and method of converter bottom seam refractory material pack uniformity |
| CN109802091A (en) * | 2018-12-29 | 2019-05-24 | 深圳市豪鹏科技有限公司 | A kind of preparation method of nickel electrode |
| CN115343175A (en) * | 2022-07-19 | 2022-11-15 | 岳阳耀宁新能源科技有限公司 | Method for measuring elongation of rolled pole piece |
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| CN87210110U (en) * | 1987-07-10 | 1988-06-08 | 西安冶金建筑学院 | Jar (or case) type vaccum device for measuring real density of powder substance |
| CN1052578C (en) * | 1994-06-15 | 2000-05-17 | 国营第七五五厂 | Preparation method of slurry-pulling type metal hydride electrode |
| KR100231525B1 (en) * | 1996-12-13 | 1999-11-15 | 손욱 | Cathode active material of nickel-type battery and its manufacturing method |
| JP4612132B2 (en) * | 1999-05-20 | 2011-01-12 | 大日本印刷株式会社 | Non-aqueous electrolyte secondary battery electrode plate, intermediate product of the electrode plate, and manufacturing method thereof |
| JP4644899B2 (en) * | 2000-02-23 | 2011-03-09 | ソニー株式会社 | Electrode and battery, and manufacturing method thereof |
| JP4848577B2 (en) * | 2000-05-25 | 2011-12-28 | ソニー株式会社 | Non-aqueous electrolyte battery |
| JP4945029B2 (en) * | 2001-03-06 | 2012-06-06 | 新日鐵化学株式会社 | Material for negative electrode of lithium secondary battery, method for producing the same, and lithium secondary battery |
| CN1147951C (en) * | 2001-07-23 | 2004-04-28 | 北大先行科技产业有限公司 | Method for increasing meso-position radius and jolt density of lithium cobaltate |
| CN1482697A (en) * | 2002-09-09 | 2004-03-17 | 三河动力电池有限公司 | Electrode plate for alkaline storage battery and processing method thereof |
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| WO2010111851A1 (en) * | 2009-03-31 | 2010-10-07 | 深圳市吉阳自动化科技有限公司 | Electrode plate processing method |
| CN101992174A (en) * | 2010-09-14 | 2011-03-30 | 天津力神电池股份有限公司 | Method for monitoring surface density of coating quantity of lithium ion battery pole piece |
| CN101992174B (en) * | 2010-09-14 | 2012-12-05 | 天津力神电池股份有限公司 | Method for monitoring surface density of coating quantity of lithium ion battery pole piece |
| CN102916175A (en) * | 2012-10-25 | 2013-02-06 | 湖南长远锂科有限公司 | Lithium manganese oxide spinel of anode materials of lithium ion batteries and method for manufacturing lithium manganese oxide spinel |
| CN107925130B (en) * | 2015-10-08 | 2020-07-31 | 株式会社Lg化学 | Method for measuring binder distribution in electrode |
| CN107925130A (en) * | 2015-10-08 | 2018-04-17 | 株式会社Lg化学 | The method of adhesive distribution in measuring electrode |
| US10663528B2 (en) | 2015-10-08 | 2020-05-26 | Lg Chem, Ltd. | Method of measuring distribution of binder in electrode |
| CN108226641A (en) * | 2017-12-30 | 2018-06-29 | 湖北金泉新材料有限责任公司 | A kind of test method of anode material for lithium-ion batteries conductivity |
| CN108226641B (en) * | 2017-12-30 | 2020-08-11 | 湖北亿纬动力有限公司 | Method for testing conductivity of lithium ion battery anode material |
| CN108895945A (en) * | 2018-05-15 | 2018-11-27 | 首钢集团有限公司 | A kind of measuring device and method of converter bottom seam refractory material pack uniformity |
| CN108895945B (en) * | 2018-05-15 | 2020-06-19 | 首钢集团有限公司 | Device and method for measuring filling uniformity of refractory material of converter bottom joint |
| CN109802091A (en) * | 2018-12-29 | 2019-05-24 | 深圳市豪鹏科技有限公司 | A kind of preparation method of nickel electrode |
| CN115343175A (en) * | 2022-07-19 | 2022-11-15 | 岳阳耀宁新能源科技有限公司 | Method for measuring elongation of rolled pole piece |
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