CN101655468B - Method for identifying failure causes of secondary battery - Google Patents
Method for identifying failure causes of secondary battery Download PDFInfo
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- CN101655468B CN101655468B CN200810141991XA CN200810141991A CN101655468B CN 101655468 B CN101655468 B CN 101655468B CN 200810141991X A CN200810141991X A CN 200810141991XA CN 200810141991 A CN200810141991 A CN 200810141991A CN 101655468 B CN101655468 B CN 101655468B
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Abstract
The invention discloses a method for identifying the failure causes of a secondary battery, which comprises the following steps: sampling an electrode material of a failure battery; analyzing an electrode material sample by using an X-ray diffraction instrument to obtain an X-ray diffraction pattern of the electrode material sample; then performing crystal phase retrieval analysis on the diffraction pattern to obtain the crystal phase composition of the sample; and comparing the crystal phase composition of the sample with an identification standard to find a standard crystal phase corresponding to the crystal phase composition of the sample in the identification standard, wherein the failure causes corresponding to the standard crystal phase are the failure causes of the failure battery. Through the method disclosed by the invention, the failure secondary battery can be identified accurately, and even a failure battery due to an explosion can also be identified accurately.
Description
[technical field]
The present invention relates to a kind of method of identifying the battery failure reason, especially a kind of method of identifying the lithium rechargeable battery failure cause.
[background technology]
The lithium rechargeable battery of " lithium and cobalt oxides-barrier film and the non-aqueous eletrolyte-material with carbon element " system of employing has characteristics: because the restriction of system material (comprising: positive and negative pole material, electrolytic solution, diaphragm material etc.) self character, battery can not bear " overcharging ", otherwise can lose efficacy, serious meeting produces " blast ", this point clear and definite being labeled in the battery application notice usually.
Usually identify that " lithium and cobalt oxides-barrier film and non-aqueous eletrolyte-material with carbon element " is the method for lithium rechargeable battery inefficacy (particularly " blast ") reason of battery system, mainly contain visualization analytic approach, resistance method of temperature measurement, voltage measurement method etc., specifically comprise: the outward appearance of observation battery, deformation, internal gas pressure etc.; Check the voltage of dead battery, interior resistance, electric capacity etc.; Check whether inside battery exists short dot, trip point; Check whether " anti-overcharge " circuit board lost efficacy; Check whether " explosion-proof ball " lost efficacy etc.; Above method has suitable accuracy and reliability to the failure analysis of " non-blast " battery that profile is not damaged, but to producing the battery of " blast ", because of can there be in various degree destruction in its outward appearance, pattern and inner result, check and analysis conclusion error is big, often controversial, effect is bad.
[summary of the invention]
In order to overcome in the prior art to the inefficacy secondary cell, especially produce the big shortcoming of evaluation error of the failure cause of the secondary cell that explodes, the invention provides a kind of method of identifying the battery failure reason, can accurately identify the failure cause of battery by this method, even, also can accurately identify to producing the battery after exploding.
The invention provides a kind of method of identifying failure causes of secondary battery, comprise electrode material sampling to dead battery, analyze with X-ray diffractometer, obtain the X ray diffracting spectrum of electrode material sample, then diffracting spectrum is carried out the crystalline phase retrieval analysis and obtain sample crystalline phase composition, the sample crystalline phase is formed and the standard of perfection contrast, find in the standard of perfection and form corresponding standard crystalline phase with the sample crystalline phase, the pairing battery failure reason of this standard crystalline phase is the failure cause of described dead battery.
The failure cause of secondary cell can be divided into two big classes: non-overcharging lost efficacy and overcharged inefficacy, can be divided into explosive type and overcharged and lost efficacy and non-explosive type overcharges inefficacy and overcharge inefficacy.
The inventor finds, secondary cell is owing to fall, collision, acupuncture or use in hot environment etc. that reason causes non-to overcharge the crystalline phase composition that lost efficacy with the electrode material that overcharges dead battery be different, and explosive type overcharges the crystalline phase of the electrode material of dead battery and forms with non-explosive type that to overcharge the crystalline phase composition of dead battery electrode material also different, be that the non-electrode material that overcharges dead battery does not have new material to generate basically, but not explosive type overcharges in the electrode material of dead battery owing to overcharge, broken the reversible electrochemical equilibrium system that normally discharges and recharges, produce new thing phase, explosive type overcharges the electrode material of dead battery owing to produced more violent reaction, has produced the new thing phase that is not used in above each material.
The present invention analyzes the electrode material of dead battery by X-ray diffraction (XRD), is non-ly to overcharge inefficacy, explosive type to overcharge inefficacy also be that non-explosive type overcharges inefficacy according to its its inefficacy of crystalline phase composition analysis.If analyze is the non-inefficacy that overcharges, and then can continue to adopt existing technology to analyze.Method disclosed by the invention can accurately identify the failure cause of battery, even to producing the battery after exploding, also can accurately identify.
[description of drawings]
Fig. 1 is the XRD diffractogram of the residual both positive and negative polarity active material of the dead battery that records in the embodiment of the invention 1;
Fig. 2 is the XRD diffractogram of the residual both positive and negative polarity active material of the dead battery that records in the embodiment of the invention 2;
Fig. 3 is the XRD diffractogram of the residual both positive and negative polarity active material of the dead battery that records in the embodiment of the invention 3;
Fig. 4 is the XRD diffractogram of the residual both positive and negative polarity active material of the dead battery that records in the embodiment of the invention 4;
Fig. 5 is the XRD diffractogram of the residual both positive and negative polarity active material of the dead battery that records in the embodiment of the invention 5.
[embodiment]
The invention discloses a kind of method of identifying failure causes of secondary battery, comprise electrode material sampling to dead battery, analyze with X-ray diffractometer, obtain the X ray diffracting spectrum of electrode material sample, then diffracting spectrum is carried out the crystalline phase retrieval analysis and obtain sample crystalline phase composition, the sample crystalline phase is formed and the standard of perfection contrast, find in the standard of perfection and form corresponding standard crystalline phase with the sample crystalline phase, the pairing battery failure reason of this standard crystalline phase is the failure cause of described dead battery.
The X-ray diffractometer of described employing can be this area X-ray diffractometer commonly used, as the D/MAX2200PC type X-ray powder diffraction instrument of Japan company of science production.
Described XRD diffraction approach is that conventional polycrystalline (powder) XRD diffraction approach gets final product, for example can comprise together dead battery both positive and negative polarity retained material sample collection, grind mixing, getting sample powder behind an amount of mixing inserts in the groove (groove size: 20 millimeters * 18 millimeters * 0.5 millimeter) on the glass sample framework, through arrangement, obtain being parallel to the smooth test surfaces on sample framework surface, put into polycrystalline (powder) XRD diffractometer then and carry out sweep test.
Test condition is: the copper X-ray source, and wavelength X=1.54056 dusts, Cu/K α 1, the power that uses of Cu target is 40-60 kilovolt, 20-40 milliampere; Use graphite monochromator; The sweep speed of angular instrument be the 1-8 degree/minute, sweep limit is 20=10 °-80 °, scan mode is θ/20 linked scans; Scanning step footpath was 0.02 degree/step; The light path divergent slit is that 1 °, anti-scatter slit are that 10 millimeters, variable gap are that to adjust, receive slit automatically be 0.3 person of outstanding talent's rice to instrument.。The instrument data process software is: MDI-JADE (5.0).
Before carrying out described crystalline phase retrieval analysis, also comprise XRD figure spectrum carried out following processing: 9 level and smooth, K α 1 separates with K α 2 and revises with influence, the button of eliminating K α 2 and carry on the back the end, peak-seeking, carries out the crystalline phase retrieval analysis then.Above-mentioned data and Flame Image Process and crystalline phase retrieval analysis all are directly to finish by data processing software MDI-JADE (5.0), and disposal route has been conventionally known to one of skill in the art.
Form through the crystalline phase that can obtain tested electrode material sample behind the described crystalline phase retrieval analysis, then described sample crystalline phase composition is analyzed with standard of perfection.
Described standard of perfection be in the electrode material certain special thing mutually and with the mutually corresponding battery of this thing in the reason of this thing phase appears, and then provide the reason of battery failure.
Under the preferable case, described standard of perfection can obtain in the following way: the battery non-defective unit is destroyed, cause dissimilar inefficacies, then the electrode material of dead battery is taken a sample, analyze with X-ray diffractometer, obtain the X ray diffracting spectrum of electrode material sample, then diffracting spectrum is carried out the crystalline phase retrieval analysis and obtain the standard crystalline phase, the failure mode of again that each standard crystalline phase is corresponding with it battery connects, and can obtain described standard of perfection.
For making qualification result more accurate, described standard of perfection more preferably obtains in the following way: the mode that repeats 2-6 above-mentioned acquisition standard of perfection, the crystalline phase of the battery of the same failure type that obtains of contrast is formed, with the crystalline phase that contains the jointly standard crystalline phase as this battery failure reason correspondence.
The described method of standard crystalline phase corresponding with sample crystalline phase composition in the standard of perfection that finds is: the standard of respectively the organizing crystalline phase in sample crystalline phase composition and the standard of perfection is compared, the sample crystalline phase is formed when all comprising one group of standard crystalline phase, this standard crystalline phase is with this sample crystalline phase forms corresponding standard crystalline phase, and the pairing battery failure reason of this standard crystalline phase is the failure cause of the pairing battery of this sample.
The failure cause of secondary cell can be divided into two big classes: non-overcharging lost efficacy and overcharged inefficacy, can be divided into explosive type and overcharged and lost efficacy and non-explosive type overcharges inefficacy and overcharge inefficacy.
Described " the non-inefficacy of overcharging " battery includes but not limited to following situation: use in the hot environment and lost efficacy; The inefficacy that fall, reason such as collision and acupuncture causes.Described " inefficacy of overcharging " includes but not limited to following situation: charging current surpasses specialized range, charging voltage and surpasses specialized range, charging current voltage and all surpass specialized range, rate of charge above specialized range etc.; According to different battery sizes, its scope has nothing in common with each other, and can be labeled in the battery operation instructions usually described " specialized range ".
To containing lithium and cobalt oxides at positive electrode, the lithium rechargeable battery that negative pole contains material with carbon element carries out destructive test, be about to the battery non-defective unit and carry out non-ly overcharging inefficacys, explosive type and overcharging and lost efficacy and non-explosive type overcharges the destruction of the three kinds of modes that lost efficacy, then the battery after the destruction is prepared standard of perfection according to the method described above.Described destruction methods is conventionally known to one of skill in the art.The battery of described battery non-defective unit for normally discharging and recharging, more accurate for making qualification result, preferred above-mentioned battery non-defective unit is same batch battery, the i.e. battery of charge-discharge performance unanimity when making standard of perfection.
The inventor finds by a large amount of tests, described " the non-inefficacy of overcharging " battery, and relative gentle reversible electrochemical reaction takes place with negative material in the positive electrode in the battery.In the crystalline phase of positive electrode is formed, will contain LiCoO
2Or Li
1-xCoO
2(x≤0.6) can also contain or not contain C; The crystalline phase of negative material will contain C or C in forming
yLi (6≤y≤24) can also contain in addition owing to dissect suction in the back placement air, inhale CO at battery
2LiOH or Li that the back produces
2CO
3
Described " non-explosive type overcharges inefficacy ", positive electrode in the battery and negative material generation decomposition reaction in the crystalline phase of positive electrode is formed, will contain Co
3O
4The crystalline phase of negative material will contain C or C in forming
yLi (6≤y≤24) can also contain in addition owing to dissect suction in the back placement air, inhale CO at battery
2LiOH or Li that the back produces
2CO
3
Described " explosive type overcharges inefficacy ", decomposition reaction not only takes place in positive electrode in the battery and negative material, owing to produce blast, complicated chemical oxidation-reduction reaction can take place also.In the crystalline phase of positive electrode is formed, will contain non-material, CoO or the Co that decides crystal formation, can also contain or not contain Co
3O
4The crystalline phase of negative material will contain C in forming
yLi (6≤y≤24) can also contain in addition owing to dissect suction in the back placement air, inhale CO at battery
2LiOH or Li that the back produces
2CO
3
Preferably, repeat the mode of 3 above-mentioned acquisition standards of perfection, the crystalline phase of the battery of the same failure type that contrast obtains is formed, with the crystalline phase that contains the jointly standard crystalline phase as this battery failure reason correspondence.It is as follows to obtain in the described standard of perfection standard crystalline phase and its pairing battery failure reason:
A, crystalline phase contain CoO or Co in forming, and described battery failure is former because explosive type overcharges inefficacy;
B, crystalline phase contain Co in forming
3O
4, no CoO or Co, described battery failure is former because non-explosive type overcharges inefficacy;
C, crystalline phase do not have Co in forming
3O
4, CoO or Co, described battery failure is former because non-ly overcharge inefficacy.
Positive electrode is contained lithium and cobalt oxides, the electrode material (containing positive electrode) that negative pole contains the inefficacy secondary cell of material with carbon element adopts said method to carry out XRD analysis, the sample crystalline phase composition that obtains is analyzed with above-mentioned standard of perfection, rule according to standard of perfection is judged, can obtain the failure cause of this inefficacy secondary cell.
Can accurately identify the inefficacy secondary cell by method disclosed by the invention, even owing to the dead battery that produces blast also can accurately be identified.
The present invention is further illustrated below by embodiment.
Positive electrode to 5 same batch contains lithium and cobalt oxides, and lithium rechargeable battery A, B, C, D, E that negative pole contains material with carbon element carry out destructive test.
Embodiment 1
Present embodiment is used to illustrate authentication method provided by the invention.
1, destroys battery and cause its inefficacy
The above-mentioned battery A of acupuncture lost efficacy until it.
2, preparation testing sample
Dissect battery A, powdered rubber residual on the positive plate is collected in together, grind mixing, getting sample powder behind an amount of mixing inserts in the groove (groove size: 20 millimeters * 18 millimeters * 0.5 millimeter) on the glass sample framework, through arrangement, obtain being parallel to the smooth test surfaces on sample framework surface, be numbered A1, standby.
3, carry out XRD analysis
Open X-ray powder diffraction instrument (the D/MAX2200PC type X-ray powder diffraction instrument that Japanese company of science produces), test condition is set is: the copper X-ray source, wavelength X=1.54056 dusts, Cu/K α 1, the use power of Cu target are 40 kilovolts, 20 milliamperes; Use graphite monochromator; The sweep speed of angular instrument be 4 degree/minute, sweep limit is 2 θ=15 °-65 °, scan mode is θ/2 θ linked scans; Scanning step footpath was 0.02 degree/step; The light path divergent slit is that 1 °, anti-scatter slit are that 10 millimeters, variable gap are that to adjust, receive slit automatically be 0.3 millimeter to instrument.
Ready A1 is placed on the sample stage.(XRD) carries out sweep test to A1 under above-mentioned test condition with x-ray powder diffraction instrument, obtains the X-ray powder diffraction figure of A1, as shown in Figure 1; Then resulting X-ray powder diffraction figure is carried out the processing of following order: 9 level and smooth; K α 1 separates with K α 2 and revises to eliminate the influence of K α 2; Instrument broadens at correction, the button back of the body end; Peak-seeking; With MDI-JADE (5.0) data processing software diffraction pattern is carried out the crystalline phase retrieval analysis, obtain the sample crystalline phase and consist of A2:CoLiO
2, Li
0.4CoO
2
Present embodiment is used to illustrate authentication method provided by the invention.
Analytical approach is with embodiment 1, and different is: battery B was dried by the fire 2 hours in 120 ℃ of high temperature ovens, its bulging was lost efficacy.Obtain the sample crystalline phase and consist of B2:LiCoO
2, C.
Present embodiment is used to illustrate authentication method provided by the invention.
Analytical approach is with embodiment 1, and different is: battery C in high magnification (5C) charging down, is made its inefficacy and not blast.Obtain the sample crystalline phase and consist of C2:Co
3O
4, LiCoO2, C.
Embodiment 4
Present embodiment is used to illustrate authentication method provided by the invention.
Analytical approach is with embodiment 1, and different is: battery D in high magnification (5C) charging down, is made it produce blast and lost efficacy.
Get its positive and negative pole material potpourri and prepare sample D1, ultimate analysis obtains the sample crystalline phase and consists of D2:Co, Co
3O
4, Li
2CO
3, C, CoO, LiAlO
2
Embodiment 5
Present embodiment is used to illustrate authentication method provided by the invention.
Analytical approach is with embodiment 4, and different is: destroy earlier battery E holding circuit plate, charge normal then to E and explode.Ultimate analysis obtains the sample crystalline phase and consists of E2:CoO, Co, Li
2CO
3, C.
Above-mentioned sample crystalline phase is formed the following standard of perfection of employing to be analyzed:
A, crystalline phase contain CoO or Co in forming, and described battery failure is former because explosive type overcharges inefficacy;
B, crystalline phase contain Co in forming
3O
4, no CoO or Co, described battery failure is former because non-explosive type overcharges inefficacy;
C, crystalline phase do not have Co in forming
3O
4, CoO or Co, described battery failure is former because non-ly overcharge inefficacy.
The sample crystalline phase of sample A1 consists of among the A2, and the crystalline phase material of existence is: CoLiO
2And Li
0.4CoO
2,, judge that the failure cause of this battery is " the non-inefficacy of overcharging " according to standard of perfection of the present invention;
The sample crystalline phase of sample B1 consists of among the B2, and the crystalline phase material of existence is: LiCoO
2And C, according to standard of perfection of the present invention, the failure cause of judging this battery is " the non-inefficacy of overcharging ";
The sample crystalline phase of sample C1 consists of among the C2, and the crystalline phase material of existence is: Co
3O
4, LiCoO
2And C, according to standard of perfection of the present invention, judge that the failure cause of this battery is " non-explosive type overcharges inefficacy ";
The sample crystalline phase of sample D1 consists of among the D2, and the crystalline phase material of existence is: Co, Co
3O
4, Li
2CO
3, C, CoO and LiAlO
2,, judge that the failure cause of this battery is " explosive type overcharges inefficacy " according to standard of perfection of the present invention;
The sample crystalline phase of sample E1 consists of among the E2, and the crystalline phase material of existence is: CoO, Co, Li2CO3 and C, according to standard of perfection of the present invention, judge that the failure cause of this battery is " explosive type overcharges inefficacy ".
The analysis result that obtains is as shown in table 1.
Table 1
| Sample | The crystalline phase result for retrieval | Analyze failure cause | The considered repealed reason |
| ?A | CoLiO 2、 Li 0.4CoO 2 | Non-overcharging | The acupuncture short circuit |
| ?B | LiCoO 2、C | Non-overcharging | Baking is after 2 hours in 120 ℃ of high temperature ovens, and bulging lost efficacy |
| ?C | Co 3O 4、 LiCoO2、C | Non-explosive type overcharges | High magnification (5C) charging was lost efficacy, not blast |
| ?D | Co、Co 3O 4、Li 2CO 3、C、CoO、LiAlO 2 | Explosive type overcharges | High magnification (5C) charging was lost efficacy, blast |
| ?E | CoO、Co、 Li 2CO 3、C | Explosive type overcharges | The holding circuit plate lost efficacy and charged normal blast |
From the result of table 1 as can be seen, adopt method disclosed by the invention that sample is analyzed, the conclusion that obtains, be that battery failure reason and actual cause are in full accord, illustrate and adopt method disclosed by the invention to identify that the battery failure reason is very accurately, also can accurately identify its failure cause even produce the battery of blast.
Claims (5)
1. method of identifying failure causes of secondary battery, comprise electrode material sampling to dead battery, analyze with X-ray diffractometer, obtain the X ray diffracting spectrum of electrode material sample, then diffracting spectrum is carried out the crystalline phase retrieval analysis and obtain sample crystalline phase composition, the sample crystalline phase is formed and the standard of perfection contrast, found in the standard of perfection and form corresponding standard crystalline phase with the sample crystalline phase, the pairing battery failure reason of this standard crystalline phase is the failure cause of described dead battery; Described standard of perfection can obtain in the following way: the battery non-defective unit is destroyed, cause dissimilar inefficacies, then the electrode material of dead battery is taken a sample, analyze with X-ray diffractometer, obtain the X ray diffracting spectrum of electrode material sample, then diffracting spectrum is carried out the crystalline phase retrieval analysis and obtain the standard crystalline phase, the failure mode of again that each standard crystalline phase is corresponding with it battery connects, and can obtain described standard of perfection.
2. method according to claim 1 is characterized in that, repeats the mode of 2-6 described acquisition standard of perfection, and the crystalline phase of the battery of the same failure type that obtains of contrast is formed, with the crystalline phase that contains the jointly standard crystalline phase as this battery failure reason correspondence.
3. method according to claim 1, it is characterized in that, the described method of standard crystalline phase corresponding with sample crystalline phase composition in the standard of perfection that finds is: the standard of respectively the organizing crystalline phase in sample crystalline phase composition and the standard of perfection is compared, the sample crystalline phase is formed when all comprising one group of standard crystalline phase, and this standard crystalline phase is with this sample crystalline phase forms corresponding standard crystalline phase.
4. according to any described method among the claim 1-3, the positive electrode of described battery contains lithium and cobalt oxides, negative pole contains material with carbon element, and described electrode material sample is the electrode material that contains positive electrode, and standard crystalline phase and its pairing battery failure reason are as follows in the described standard of perfection:
A, crystalline phase contain CoO or Co in forming, and described battery failure is former because explosive type overcharges inefficacy;
B, crystalline phase contain Co in forming
3O
4, no CoO or Co, described battery failure is former because non-explosive type overcharges inefficacy;
C, crystalline phase do not have Co in forming
3O
4, CoO or Co, described battery failure is former because non-ly overcharge inefficacy.
5. method according to claim 4, wherein, the described condition of analyzing with X-ray diffractometer is: the copper X-ray source, wavelength X=1.54056 dusts, Cu/K α 1, the power that uses of Cu target is 40-60 kilovolt, 20-40 milliampere; Use graphite monochromator; The sweep speed of angular instrument be the 1-8 degree/minute, sweep limit is 2 θ=10 °-80 °, scan mode is θ/2 θ linked scans; Scanning step footpath was 0.02 degree/step; The light path divergent slit is that 1 °, anti-scatter slit are that 10 millimeters, variable gap are that to adjust, receive slit automatically be 0.3 millimeter to instrument.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1862252A (en) * | 2005-05-11 | 2006-11-15 | 公安部第三研究所 | X-ray human body safety check apparatus |
| WO2006119995A1 (en) * | 2005-05-13 | 2006-11-16 | Süd-Chemie AG | Lithium secondary battery and electrodes for use therein |
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2008
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1862252A (en) * | 2005-05-11 | 2006-11-15 | 公安部第三研究所 | X-ray human body safety check apparatus |
| WO2006119995A1 (en) * | 2005-05-13 | 2006-11-16 | Süd-Chemie AG | Lithium secondary battery and electrodes for use therein |
Non-Patent Citations (1)
| Title |
|---|
| 吴贤章等.循环用阀控电池失效模式的研究.<蓄电池>.2002,(第4期),第151-154页. * |
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