CN104089876A - Test method for bonding strength between battery current collector and binder - Google Patents
Test method for bonding strength between battery current collector and binder Download PDFInfo
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- CN104089876A CN104089876A CN201410284458.4A CN201410284458A CN104089876A CN 104089876 A CN104089876 A CN 104089876A CN 201410284458 A CN201410284458 A CN 201410284458A CN 104089876 A CN104089876 A CN 104089876A
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Abstract
The invention relates to a test method for bonding strength between a battery current collector and a binder. A bonding force between the battery current collector and the binder is obtained by using a multi-functional mechanical property tester to carry out a destructive test on a binder film on the surface of the current collector; and further the bonding strength between the battery current collector and the binder is obtained. The test method provided by the invention is suitable for a surface formed by coating a positive electrode binder on a positive electrode current collector, a surface formed by coating a negative electrode binder on a negative electrode current collector, and a surface formed on metal or alloy coated by a polymer. The test method provided by the invention is simple in operations, convenient for sample preparation and direct and accurate in test results, and can evaluate the bonding performance of the binder simply and accurately.
Description
Technical field
The present invention relates to a kind of bonding strength measuring technology, particularly the method for testing of bonding strength between a kind of battery afflux liquid and cementing agent.
Background technology
In recent years, lithium ion battery has become the most promising technology in the field such as electric motor car and hand portable equipment, and its energy density is the highest in known secondary cell.In order to improve the performance of lithium ion battery, Scientific Research Workers is attempted electrode material, electrolyte and the conductive agent that exploitation makes new advances.But battery efficiency largely depends on electrode engineering.Cementing agent is as the non-active ingredient in lithium ion cell electrode sheet, is to prepare one of important materials that lithium ion cell electrode sheet must use.The Main Function of cementing agent is connecting electrode active substance, conductive agent and electrode current collecting body, make between them, to there is overall connectivity, thereby reduce the impedance of electrode, bonding strength between stabilized electrodes chip architecture, thereby collector better and cementing agent has just become a critical index of Binder Properties.
In lithium ion battery charge and discharge process, can constantly there is volume change in active substance, its volume increases with the embedding of lithium ion, deviating from and reduce with lithium ion, this volume change can cause the variation that contacts between positive and negative electrode active substance and between active substance and collector, when serious, even can occur active substance from collector come off, the phenomenon of dry linting, thereby cause the internal resistance of cell to increase, battery capacity decay, the lost of life; And this volume change finally causes lithium ion battery volumetric expansion, battery distortion.In nowadays smart mobile phone and dull and stereotyped apparatus such as computer, size and safety requirements to lithium ion battery are strict, and therefore good cementing agent must have outstanding adhesive property, after the certain number of times of circulating battery, still active substance can be bonded on collector.
Through retrieval, publication number is the Chinese patent of CN 102323249 A, a kind of method for qualitative analysis of cementing agent adhesive property has been proposed, in this invention, be blended in the Raman shift size of a certain characteristic peak in the Raman spectrum with Raman-active species in cementing agent by measurement, the adhesive property of cementing agent is carried out to qualitative analysis, the method can not actually test out the adhesion between lithium ion battery cementing agent and collector, and the data that the method draws not are mechanical performance data, can not truly represent this performance of bonding strength of cementing agent.
Summary of the invention
The present invention be directed to now cannot actual test lithium ion battery cementing agent and collector between the problem of adhesion, the method of testing of bonding strength between a kind of battery afflux liquid and cementing agent has been proposed, utilize multi-functional mechanical test instrument (rubbing wear instrument) to do destructive testing to the adhesive film that is coated in collection liquid surface, obtain the adhesion of battery afflux liquid and cementing agent, and then obtain the bonding strength of collector and cementing agent, method of testing of the present invention is applicable to the surface that anodal adhesive coated forms on plus plate current-collecting body, the surface that negative pole adhesive coated forms on negative current collector, also be applicable to the surface forming on the metal or alloy of high molecular polymer coating simultaneously.
Technical scheme of the present invention is: the method for testing of bonding strength between a kind of battery afflux liquid and cementing agent, specifically comprises the steps:
1) binder solution preparing is evenly coated in to collection liquid surface, puts into air dry oven and dry 3～24h at 80 DEG C, after bonding rear taking-up, at room temperature leave standstill 0.5～2h completely, make the sample that specification is 1cm × 2cm;
2) select multi-functional mechanical testing instrument and friction pair, on sample, install power sensor, connect friction pair and multi-functional mechanical testing instrument, power sensor connects computing machine, sample is fixed on objective table, then sample is moved under needle point friction pair;
3) multi-functional mechanical testing instrument is carried out to setting parameter, precompression, squeeze time, linear loading force scope, range ability, working time are set, start multi-functional mechanical testing instrument, friction pair does to load feed motion to the sample on objective table, the linear friction force that increases, sample is done to destructive testing, make that film starts to break, partial rupture is until break completely;
4) loading force and frictional force data are real-time transmitted to computing machine by power sensor, computing machine is to the data obtained curve plotting, from figure, show when friction force Fx and friction factor COF simultaneous mutation are the most violent that the corresponding time is the complete rupture time of film, corresponding loading force Fz is the adhesion of collector and cementing agent.
Described step 1) configuration sample concrete steps: take the cementing agent of mass ratio and the solvent of mass ratio, cementing agent gradation is added and in solvent, stirs 3～24h, be configured to massfraction and be 1%～5% sticky binder solution, the solution that takes a morsel after stirring is placed on collector after treatment, binder solution is evenly coated in to collection liquid surface with scraper, wet film thickness can be controlled in 100～200um, collector after coating is positioned in air dry oven, after drying 3～24h at 80 DEG C, take out, at room temperature leave standstill 0.5～2h, make the sample that specification is 1cm × 2cm, and sample is carried out to mark.
Described sample be lithium battery anode adhesive coated on corresponding plus plate current-collecting body, can be also that cathode of lithium battery adhesive coated is in corresponding negative pole currect collecting surface.
Beneficial effect of the present invention is: the method for testing of bonding strength between battery afflux liquid of the present invention and cementing agent, and the bonding strength that solving China not yet has pair affluxion body in lithium ion batteries and cementing agent is tested and the method for analyzing; Used test instrument is Multifunctional display micro mechanics tester (rubbing wear instrument), and what friction pair was selected is Diamond tip, can realize the adhesion test accurately of film and matrix, and to material and roughness thereof all without particular/special requirement; The inventive method is simple to operate, sample preparation is easy, test result is directly accurate, can evaluate cementing agent adhesive property simply exactly.
Brief description of the drawings
Fig. 1 be in the embodiment of the present invention 1 loading force, friction force, friction factor, working time be related to schematic diagram;
Fig. 2 be in the embodiment of the present invention 2 loading force, friction force, friction factor, working time be related to schematic diagram;
Fig. 3 be in the embodiment of the present invention 3 loading force, friction force, friction factor, working time be related to schematic diagram;
Fig. 4 be in the embodiment of the present invention 4 loading force, friction force, friction factor, working time be related to schematic diagram;
Fig. 5 is the scanning electron microscope (SEM) photograph of cementing agent PVDF film breaks in the embodiment of the present invention 1;
Fig. 6 is the scanning electron microscope (SEM) photograph of cementing agent PI film breaks in the embodiment of the present invention 2;
Fig. 7 is the scanning electron microscope (SEM) photograph of cementing agent PVDF film breaks in the embodiment of the present invention 3;
Fig. 8 is the scanning electron microscope (SEM) photograph of cementing agent xanthans film breaks in the embodiment of the present invention 4.
Embodiment
Set forth the method for testing of bonding strength between battery afflux liquid of the present invention and cementing agent below by 4 embodiment.
Embodiment 1:
1) take the PVDF(polyvinylidene fluoride of 0.2g) 900, the NMP(N-methyl pyrrolidone of 4g), PVDF gradation is added in nmp solution and stirs 3h with magnetic stirrer, be configured to massfraction and be 5% PVDF900 solution, the solution that takes a morsel after stirring is placed on Cu paper tinsel after treatment (selecting Cu paper tinsel thickness is 14um), binder solution is evenly coated in to Cu paper tinsel surface with scraper, wet film thickness is 100um;
2) the Cu paper tinsel after applying is positioned in air dry oven, dries at 80 DEG C after 3h and takes out and leave standstill 0.5h, makes the sample that specification is 1cm × 2cm, and sample is carried out to mark;
3) use multi-functional mechanical testing instrument (rubbing wear instrument) and Diamond tip, select to install the mechanics sensor of 20N, select Diamond tip as friction pair, first sample is fixed on objective table, then sample is moved under needle point;
4) precompression Fz=-0.05N, squeeze time t are set
1for 5s, loading force Fz from-0.05N to-12N is linear to be increased, range ability d is 8mm, working time t
2for 200s, after start-up routine, friction pair is done to load feed motion to sample on objective table, and the PVDF film that is coated in Cu paper tinsel surface is done to destructive testing, makes that film starts to break, partial rupture is until break completely.
5) power sensor is transferred to the continuous data of loading force Fz, friction force Fx in computing machine, obtains friction factor, the polishing scratch degree of depth, the loading force when obtaining PVDF film and breaking completely, i.e. and adhesion between PVDF and Cu paper tinsel, and then obtain bonding strength.
6) data that obtain are carried out to mapping analysis, its schematic diagram as shown in Figure 1, simultaneously with reference to film breaks situation in accompanying drawing 5, the complete rent of film obtains working time apart from the distance of friction pair section start divided by operating rate, it is the complete rupture time of film, now friction force Fx and friction factor COF simultaneous mutation is the most violent, and corresponding loading force Fz is the adhesion between collector and cementing agent.And there is again violent sudden change along with increasing working time in friction factor COF, because can friction pair still can continue to do feed motion on Cu paper tinsel surface according to program after the complete breakage of film, friction factor COF is now relevant to the roughness of Cu paper tinsel, and and cohesive force between film and Cu paper tinsel irrelevant, so time friction factor COF do not do to consider; Start again to decline along with increasing friction factor COF working time, because friction pair can continue again to move on objective table after scratching Cu paper tinsel, friction factor COF is now relevant to the roughness of objective table, and and cohesive force between film and Cu paper tinsel irrelevant, so time friction factor COF do not do to consider yet.From figure, analyze and draw: t
2=78.5s, Fx=-2.568N, Fz=-3.954N, now, PVDF film breaks completely on Cu paper tinsel surface, and as shown in Figure 5, Fz is the adhesion of collector Cu paper tinsel and cementing agent PVDF900 to the scanning electron microscope (SEM) photograph of film breaks.
Embodiment 2:
1) take the PI(polyamide of 0.2g), the NMP(N-methyl pyrrolidone of 4g), PI gradation is added in nmp solution and stirs 3h with magnetic stirrer, be configured to massfraction and be 5% PI solution, the solution that takes a morsel after stirring is placed in (selecting Cu paper tinsel thickness is 14um) on Cu paper tinsel after treatment, binder solution is evenly coated in to Cu paper tinsel surface with scraper, wet film thickness is 100um;
2) the Cu paper tinsel after applying is positioned in air dry oven, dries at 80 DEG C after 3h and takes out and leave standstill 0.5h, makes the sample that specification is 1cm × 2cm, and sample is carried out to mark;
3) use multi-functional mechanical testing instrument (rubbing wear instrument) and Diamond tip, select to install the mechanics sensor of 20N, select Diamond tip as friction pair, first sample is fixed on objective table, then sample is moved under needle point;
4) precompression Fz=-0.05N, squeeze time t are set
1for 5s, loading force Fz from-0.05N to-12N is linear to be increased, range ability d is 6mm, working time t
2for 100s, after start-up routine, friction pair is done to load feed motion to sample on objective table, and the PI film that is coated in Cu paper tinsel surface is done to destructive testing, makes that film starts to break, partial rupture is until break completely.
5) power sensor is transferred to the continuous data of loading force Fz, friction force Fx in computing machine, obtains friction factor, the polishing scratch degree of depth, the loading force when obtaining PI film and breaking completely, i.e. and adhesion between PI film and Cu paper tinsel, and then obtain bonding strength.
6) data that obtain are carried out to mapping analysis, its schematic diagram as shown in Figure 2, simultaneously with reference to film breaks situation in accompanying drawing 6, the complete rent of film obtains working time apart from the distance of friction pair section start divided by operating rate, it is the complete rupture time of film, now friction force Fx and friction factor COF simultaneous mutation is the most violent, and corresponding loading force Fz is the adhesion between collector and cementing agent.And friction factor COF is along with increase working time can be fluctuateed, because can friction pair still can continue to do feed motion on Cu paper tinsel surface according to program after the complete breakage of film, friction factor COF is now relevant to Cu paper tinsel roughness, and and cohesive force between film and Cu paper tinsel irrelevant, so time friction factor COF do not do to consider.From figure, analyze and draw: t
2=57.4s, Fx=-1.94N, Fz=-2.996N, now, PI film breaks completely on Cu paper tinsel surface, and as shown in Figure 6, Fz is the adhesion of collector Cu paper tinsel and cementing agent PI to the scanning electron microscope (SEM) photograph of film breaks.
Embodiment 3:
1) take the PVDF(polyvinylidene fluoride of 0.2g) 900, the NMP(N-methyl pyrrolidone of 4g), PVDF900 gradation is added in nmp solution and stirs 4h with magnetic stirrer, be configured to massfraction and be 5% PVDF900 solution, the solution that takes a morsel after stirring is placed on Cu paper tinsel after treatment, binder solution is evenly coated in to Cu paper tinsel surface with scraper, wet film thickness is 200um;
2) the Cu paper tinsel after applying is positioned in air dry oven, dries at 80 DEG C after 5h and takes out and leave standstill 1h, makes the sample that specification is 1cm × 2cm, and sample is carried out to mark;
3) use multi-functional mechanical testing instrument (rubbing wear instrument) and Diamond tip, select to install the mechanics sensor of 20N, select Diamond tip as friction pair, first sample is fixed on objective table, then sample is moved under needle point;
4) precompression Fz=-0.05N, squeeze time t are set
1for 5s, loading force Fz from-0.05N to-12N is linear to be increased, range ability d is 8mm, working time t
2for 200s, after start-up routine, friction pair is done to load feed motion to sample on objective table, and the PVDF film that is coated in Cu paper tinsel surface is done to destructive testing, makes that film starts to break, partial rupture is until break completely.
5) power sensor is transferred to the continuous data of loading force Fz, friction force Fx in computing machine, obtains friction factor, the polishing scratch degree of depth, the loading force when obtaining PVDF film and breaking completely, i.e. and adhesion between PVDF and Cu paper tinsel, and then obtain bonding strength.
6) data that obtain are carried out to mapping analysis, its schematic diagram as shown in Figure 3, simultaneously with reference to film breaks situation in accompanying drawing 7, the complete rent of film obtains working time apart from the distance of friction pair section start divided by operating rate, it is the complete rupture time of film, now friction force Fx and friction factor COF simultaneous mutation is the most violent, and corresponding loading force Fz is the adhesion between collector and cementing agent.And in accompanying drawing 3 there is violent sudden change in friction factor COF first, that while doing feed motion because of friction pair on film, partial rupture can occur film, there is not the most violent sudden change in the friction force Fx that now friction factor COF is corresponding, power when the loading force Fz that now friction factor COF is corresponding is film generation partial rupture, and power when not film breaks completely.From figure, analyze and draw: t
2=179.9s, Fx=-3.72N, Fz=-10.989N, now, PVDF film breaks completely on Cu paper tinsel surface, and as shown in Figure 7, Fz is the adhesion of collector Cu paper tinsel and cementing agent PVDF900 to the scanning electron microscope (SEM) photograph of film breaks.
Embodiment 4:
1) take the xanthans of 1g, the deionized water of 99g, xanthans gradation is added to the water and stirs 24h with magnetic stirrer, be configured to massfraction and be 1% xanthan gum solution, the solution that takes a morsel after stirring is placed in (selecting Cu paper tinsel thickness is 14um) on Cu paper tinsel after treatment, binder solution is evenly coated in to Cu paper tinsel surface with scraper, wet film thickness is 200um;
2) the Cu paper tinsel after applying is positioned in air dry oven, dries at 80 DEG C after 12h and takes out and leave standstill 2h, makes the sample that specification is 1cm × 2cm, and sample is carried out to mark;
3) use multi-functional mechanical testing instrument (rubbing wear instrument) and Diamond tip, select to install the mechanics sensor of 20N, select Diamond tip as friction pair, first sample is fixed on objective table, then sample is moved under needle point;
4) precompression Fz=-0.05N, squeeze time t are set
1for 5s, loading force Fz from-0.05N to-12N is linear to be increased, range ability d is 8mm, working time t
2for 100s, after start-up routine, friction pair is done to load feed motion to sample on objective table, and the xanthans film that is coated in Cu paper tinsel surface is done to destructive testing, makes that film starts to break, partial rupture is until break completely.
5) power sensor is transferred to the continuous data of loading force Fz, friction force Fx in computing machine, obtains friction factor, the polishing scratch degree of depth, the loading force when obtaining xanthans film and breaking completely, i.e. and adhesion between xanthans and Cu paper tinsel, and then obtain bonding strength.
6) data that obtain are carried out to mapping analysis, its schematic diagram as shown in Figure 4, simultaneously with reference to film breaks situation in accompanying drawing 8, the complete rent of film obtains working time apart from the distance of friction pair section start divided by operating rate, it is the complete rupture time of film, now friction force Fx and friction factor COF simultaneous mutation is the most violent, and corresponding loading force Fz is the adhesion between collector and cementing agent.And in accompanying drawing 4 there is violent sudden change in friction factor COF first, because friction pair is when touching first film and do feed motion on film, film can start to break, there is not the most violent sudden change in the friction force Fx that now friction factor COF is corresponding, the loading force Fz that now friction factor COF is corresponding is the power of film while starting to break, and power when not film breaks completely.From figure, analyze and draw: t
2=95.7s, Fx=-3.65N, Fz=-11.462N, now, xanthans film breaks completely on Cu paper tinsel surface, and as shown in Figure 8, Fz is the adhesion of collector Cu paper tinsel and cementing agent xanthans to the scanning electron microscope (SEM) photograph of film breaks.
Described test material surface comprise lithium battery anode adhesive coated in anode collection surface, negative pole adhesive coated is in negative pole currect collecting surface.
Described test material comprises that collector is as each metalloid and alloys thereof such as Cu, Al, Zn, Ni, and stainless steel etc. are nonmetal; Oiliness cementing agent is as Kynoar and modifier etc. thereof, aqueous binders is as xanthans, carboxymethyl cellulose and derivant thereof, polyacrylic, polyacrylate, polyoxyethylene class, polyamine class, sodium alginate, Arabic gum, gelatin, the natural glues such as xanthans etc., emulsion-type cementing agent is as teflon, styrene-butadiene rubber etc.
Claims (3)
1. a method of testing for bonding strength between battery afflux liquid and cementing agent, is characterized in that, specifically comprises the steps:
1) binder solution preparing is evenly coated in to collection liquid surface, puts into air dry oven and dry 3～24h at 80 DEG C, after bonding rear taking-up, at room temperature leave standstill 0.5～2h completely, make the sample that specification is 1cm × 2cm;
2) select multi-functional mechanical testing instrument and friction pair, on sample, install power sensor, connect friction pair and multi-functional mechanical testing instrument, power sensor connects computing machine, sample is fixed on objective table, then sample is moved under needle point friction pair;
3) multi-functional mechanical testing instrument is carried out to setting parameter, precompression, squeeze time, linear loading force scope, range ability, working time are set, start multi-functional mechanical testing instrument, friction pair does to load feed motion to the sample on objective table, the linear friction force that increases, sample is done to destructive testing, make that film starts to break, partial rupture is until break completely;
4) loading force and frictional force data are real-time transmitted to computing machine by power sensor, computing machine is to the data obtained curve plotting, from figure, show when friction force Fx and friction factor COF simultaneous mutation are the most violent that the corresponding time is the complete rupture time of film, corresponding loading force Fz is the adhesion of collector and cementing agent.
2. the method for testing of bonding strength between battery afflux liquid and cementing agent according to claim 1, it is characterized in that, described step 1) configuration sample concrete steps: take the cementing agent of mass ratio and the solvent of mass ratio, cementing agent gradation is added and in solvent, stirs 3～24h, be configured to massfraction and be 1%～5% sticky binder solution, the solution that takes a morsel after stirring is placed on collector after treatment, binder solution is evenly coated in to collection liquid surface with scraper, wet film thickness can be controlled in 100～200um, collector after coating is positioned in air dry oven, after drying 3～24h at 80 DEG C, take out, at room temperature leave standstill 0.5～2h, make the sample that specification is 1cm × 2cm, and sample is carried out to mark.
3. the method for testing of bonding strength between battery afflux liquid and cementing agent according to claim 2, it is characterized in that, described sample be lithium battery anode adhesive coated on corresponding plus plate current-collecting body, can be also that cathode of lithium battery adhesive coated is in corresponding negative pole currect collecting surface.
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| CN106644935A (en) * | 2017-03-02 | 2017-05-10 | 天津市捷威动力工业有限公司 | Method and apparatus for measuring bonding force between graphite and binder of negative electrode of lithium battery |
| CN106990036A (en) * | 2017-04-25 | 2017-07-28 | 天能电池集团有限公司 | A kind of device and detection method for Detection electrode active material softening degree |
| CN107017408A (en) * | 2017-04-01 | 2017-08-04 | 陕西科技大学 | Trigonella bean gum water-based binder and its application in negative electrode of lithium ion battery |
| CN109632630A (en) * | 2017-10-09 | 2019-04-16 | 深圳先进技术研究院 | The test method and test equipment of battery pole piece adhesive force |
| CN111077069A (en) * | 2019-12-09 | 2020-04-28 | 陕西煤业化工技术研究院有限责任公司 | Method for rapidly screening binder for lithium battery |
| CN111426629A (en) * | 2020-05-20 | 2020-07-17 | 天津市捷威动力工业有限公司 | Method and device for testing peeling force between lithium battery binder and foil |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106644935A (en) * | 2017-03-02 | 2017-05-10 | 天津市捷威动力工业有限公司 | Method and apparatus for measuring bonding force between graphite and binder of negative electrode of lithium battery |
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| CN106990036A (en) * | 2017-04-25 | 2017-07-28 | 天能电池集团有限公司 | A kind of device and detection method for Detection electrode active material softening degree |
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| CN111077069A (en) * | 2019-12-09 | 2020-04-28 | 陕西煤业化工技术研究院有限责任公司 | Method for rapidly screening binder for lithium battery |
| CN111426629A (en) * | 2020-05-20 | 2020-07-17 | 天津市捷威动力工业有限公司 | Method and device for testing peeling force between lithium battery binder and foil |
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Application publication date: 20141008 |