CN104596923A - Measuring method for adhesive strength of flexible substrate material coating - Google Patents
Measuring method for adhesive strength of flexible substrate material coating Download PDFInfo
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- CN104596923A CN104596923A CN201410850484.9A CN201410850484A CN104596923A CN 104596923 A CN104596923 A CN 104596923A CN 201410850484 A CN201410850484 A CN 201410850484A CN 104596923 A CN104596923 A CN 104596923A
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Abstract
The invention relates to a measuring method of adhesive strength, and in particular relates to a measuring method for adhesive strength of flexible substrate material coating. The measuring method for adhesive strength of flexible substrate material coating comprises the following steps: measuring the interior binding power of the coating and measuring the bonding strength between the coating and a substrate; the measurement of the interior binding power of the coating comprises the following steps: calculating the interior binding power of the coating according to the formula: theta=F/S, wherein F is stripping force, S is the width of the binding strip; the measurement of the bonding strength between the coating and the substrate comprises the following steps: winding a coating body on stainless steel bars with different diameters, and calculating the strength value of the binding power between the coating layer and the flexible substrate according to the separation state between the coating layer and the flexible substrate during winding. According to the measuring method, the repeatability is good, the operation is simple, the defects that the measurement result subjectivity is strong and the repeatability and the veracity are poor in the grid method in the prior art can be overcome. The defect that the coating is impacted by 180-degree bending during the testing process of the stripping method is also overcome, and the interior adhesive force of the coating and the adhesive force between the coating and the flexible substrate are separately measured.
Description
Technical field
The present invention relates to a kind of measuring method of adhesive strength, be specifically related to a kind of measuring method of flexible base material coating adhesive strength.
Background technology
Lithium ion battery mainly comprises pole piece and nonaqueous electrolytic solution, described pole piece and nonaqueous electrolytic solution are sealed in battery container, described pole piece comprises battery electrode and barrier film, described battery electrode comprises anode pole piece and cathode pole piece, the positive electrode that described anode pole piece comprises plus plate current-collecting body and coating/or is filled on plus plate current-collecting body, the negative material that described cathode pole piece comprises negative current collector and coating and/or is filled on negative current collector.
In lithium battery, pole piece is very large on the impact of battery performance, is carrying out in charge and discharge process, positive/negative active substance can be caused to be separated with collector to lithium battery, and then reduces battery capacity and worsen cycle life.So be the key factor directly having influence on battery performance to the control of battery pole piece.The most important with the cohesive strength of the cohesive strength on pole piece between active substance and active substance and substrate in the control of wherein pole piece.
At present, the method for testing of pole piece cohesive strength mainly Grid Method, peel test force method.The concrete operations of Grid Method are: draw cutter by pole piece coating with the spacing of 1-3 millimeter and 45 ° of-90 ° of stagger angles with steel, are divided into the square of some or the little lattice of prismatic and scratch.Then test that special adhesive strip is smooth to be bonded on little lattice by the cohesive force that Minnesota Mining and Manufacturing Company produces, do not stay a space, then vertically uncover with prestissimo, observe draw lattice place fall material and peeling situation, to fall doses and peeling situation to weigh the size of pole piece cohesive force intensity.The method is simple, but when shortcoming is line, the line depth is wayward, is not directly measure cohesive force intensity, and measurement result is subjective, repeated and accurately establish a capital poor.Mention in patent publication No. CN101206173A, peel test force method the cated surperficial one end of coating and bond strength is not less than the adhesive strip of coating adhesive strength needed for coated body fit tightly and fix, then coated body is never bent 180 ° with adhesive strip joint place to make the two ends of coated body be parallel to each other and to make two of the surface of not fitting with adhesive strip short close to each other, along the direction that this coated body other end extends, pulling force is applied to this coated body other end afterwards, make coating be separated required lowest pull with substrate.The shortcoming of the method is, when measuring, can not ensure that coating is separated completely with substrate, some local coating can be separated completely with substrate, the coating in some place is still stayed in substrate, the lowest pull of such test just can not represent the pulling force making coating segregation, and the value obtaining pulling force in the position that coating and substrate are not separated completely is the cohesive force between coat inside particle, is not the cohesive force between coating and substrate.When carrying out disbonded test, must by bending 180 ° of the flexible substrates after coating, will there is stress at bending position, especially when testing lithium battery anode piece, coating is thicker, and this stress just causes coming off of coating, makes test result inaccurate.
Summary of the invention
The object of the invention is to overcome the shortcoming that Grid Method and peel test force method test pole piece cohesive strength, a kind of measuring method of flexible base material coating adhesive strength is provided, relatively accurate, objective.
The measuring method of a kind of flexible base material coating adhesive strength of the present invention, is characterized in that: the test and the test of cohesive strength between coating and substrate that comprise coat inside cohesive force:
The test of coat inside cohesive force is: according to following formulae discovery coat inside cohesive force: θ=F/S, F is peeling force, S is adhesive strip width, described peeling force is: use peel test force instrument to measure, coated body is applied cated surface and adhesive strip is fitted, by the adhesive strip other end not with the bend portions 180 ° of coating adhesion, then bond with the mobile corrosion resistant plate in peel test force instrument, apply pulling force in the horizontal direction, make and the adhesive strip of coating adhesion and coating segregation, peeling force F in record detachment process;
Whether between coating from substrate, the test of cohesive strength is: reeled on the stainless steel bar that diameter is different by coated body, be separated, draw cohesive force intensity level between coat and substrate according to coat during winding with flexible substrates.
Wherein: coated body refers to the flexible base material comprising coating.
The test of coat inside cohesive force, comprises the following steps:
(1) coated body is fixed on horizontal corrosion resistant plate;
(2) by applying pressure, cated for a coated body tool surface and adhesive strip are fitted tightly;
(3) bend portions 180 ° do not bonded with coated body by adhesive strip, makes the two ends of adhesive strip parallel to each other;
(4) adhesive strip is not fixed on the corrosion resistant plate of peel test force machine transfer arm with one end of coating adhesion;
(5) peel test force machine is started, peel test force machine transfer arm is moved, adhesive strip is separated completely with coating, by rate-determining steps (2) applied pressure, adhesive strip is only separated with coating, and coating and flexible substrates are not separated, and obtained the curve of peeling force and strip length by the testing software that peel test force machine carries;
(6) obtain the size of peeling force F according to curve obtained, and calculate adhesive strength size between coat inside according to formula θ=F/S.
In step (1), coated body is horizontally fixed on horizontal corrosion resistant plate.
S is the contact area of adhesive strip and coating, and the area of adhesive strip is preferably the 30-60% of coated body area, and accuracy is higher.
The thickness of the corrosion resistant plate of peel test force machine transfer arm is 1-1.5mm, and length is 1.2-1.5 times of coated body length, and width is 1.1-1.2 times of coated body width.
Make the two ends of adhesive strip parallel to each other in step (3) for make the adhesive strip that do not bond with coated body and coated body coating surface adhesive strip parallel to each other.
The translational speed controlling peel test force machine transfer arm in step (5) is 40-80mm/min.
The bond strength of adhesive strip is greater than the coating adhesive strength needed for coated body, and adhesive strip is preferably Minnesota Mining and Manufacturing Company's adhesive strip.
The laminating of described adhesive strip and coated body coating can, by being sticked to by adhesive strip on the cated surface of tool of coated body, then be pressurizeed adhesive strip and coating are combined closely.Coating and flexible substrates is not caused to be separated into standard when the size of pressure and action time are to make adhesive strip and coating farthest fit together and to carry out adhesive strip and coating stripping.The total length of adhesive strip is more than the length twice of the adhesive strip of adhesive strip and coating adhesion contact portion.The cohesive strength of adhesive strip and peel test force instrument transfer arm corrosion resistant plate is greater than the cohesive strength between adhesive strip and coating.
Described peeling force can be transient force, also can be the mean force in a period of time or distance range.For improving accuracy of measurement further, the preferred described peeling force of the present invention is the mean force in a period of time or distance range.In order to further improve the accuracy of measurement, the mean value of the lowest pull needed for preferred 1/4-3/4 section.
Step (6) obtains the size of peeling force F according to curve obtained 1/4-3/4 section.
Preferred each sample repeated test three times, it is net result that result gets minimum value.
The test of cohesive strength between coating and substrate, comprises the following steps:
(1) paste double faced adhesive tape or adhesive strip in stainless steel bar one end, be then wound up on stainless steel bar by coated body, outside, another side contacts with stainless steel bar the cated one side of coated body;
(2) reel coated body on stainless steel bar a circle, observes the situation of change of coat surface coating;
(3) stainless steel bar of different numbering is changed, until the coating generation skin effect phenomenon of coated body after winding, record stainless steel bar numbering.
Wherein: step is wound as tight winding in (2).
Preferred each sample test three times, result is with minimum being as the criterion of rank.
Substrate is generally Copper Foil or aluminium foil.
In step (1), double faced adhesive tape or adhesive strip are pasted in one end, and the amount for double faced adhesive tape or adhesive strip does not require, as long as can be wound up on stainless steel bar by coated body, do not depart from just passable.
Stainless steel bar length is identical is 150mm, and diameter is respectively 1 grade: 30mm, and 2 grades: 20mm, 3 grades: 15mm, 4 grades: 10mm, 5 grades: 8mm, 6 grades: 7mm, 7 grades: 6,8 grades: 5mm, 9 grades: 4mm, 10 grades: 3mm.Test result progression is higher, represents that flexible base material coating adhesive strength is higher.Because the stainless steel bar of different-diameter produces certain tension force when reeling at curved surface, because coating tension force is different from flexible substrates tension force, coating is separated under tension with flexible substrates.Adopt identical flexible substrates, the coating of same thickness, the tension force produced when reeling is identical, therefore can the magnitude relationship of adhesive strength between more different coated body coating and flexible substrates.
In sum, the present invention has the following advantages:
According to coated body winding and the number value that the minimum stainless steel bar of peeling do not occur as adhesion intensity between measurement coating and flexible substrates, coat inside and the adhesion size between coating and substrate on coated body can be known more intuitively, and reproducible, simple to operate, thus overcome the shortcoming that prior art Grid Method measurement result is subjective, repeated and accuracy is all poor.To overcome when peeling off force method test 180 ° of knees to the shortcoming of the impact of coating, overcome stripping method and coat inside adhesion and coating and flexible substrates adhesion to be lumped together the shortcoming carrying out measuring.Adopt method of the present invention accurately can know the adhesive strength of battery pole piece upper electrode material, thus not only really for on-line monitoring and the monitoring of quality of battery pole piece, and great directive significance can be had for the optimization of batching and slurry technological parameter.Method provided by the invention can also for measuring the adhesion on the coated body that other substrates are flexible material between coat inside and the adhesion intensity between coating and flexible substrates, to may be used for measuring in stiff base adhesion intensity size between coat inside.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the embodiment of the present invention 1 coat inside cohesive force test.
In figure: the mobile corrosion resistant plate 1, in peel test force instrument; 2, adhesive strip; 3, coated body substrate; 4, coated body coating; 5, horizontal corrosion resistant plate.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment
Prepare anode pole piece to be tested: by 100 weight portion LiCoO
2, 2.5 parts by weight of binder PVDF, 3 weight portion conductive agent acetylene blacks join in 65 weight portion nmp solvents, then stir in de-airing mixer and form uniform anode sizing agent.Uniform for this slurry one side is coated on wide 400mm, the aluminium foil of latter 20 μm, after then 120 DEG C of oven dry, roll-in, cuts the anode pole piece obtaining being of a size of 140mm × 50mm.
Prepare cathode pole piece to be tested: join in the nmp solvent of 120 weight portions by 100 weight portion negative electrode active material native graphites, 1.0 parts by weight of binder PVDF and 1.0 weight portion conductive agent carbon blacks, then stir in de-airing mixer and form stable, homogeneous cathode size.Uniform for this slurry one side is coated on wide 400mm, the Copper Foil of thick 10 μm, after 120 DEG C of oven dry, roll-in, cuts into the cathode pole piece of 140mm × 45mm.
The test of coat inside cohesive force, comprises the following steps:
(1) positive plate embodiment prepared or negative plate are fixed on horizontal corrosion resistant plate;
(2) by applying certain pressure, positive plate embodiment prepared or the cated surface of negative plate tool and adhesive strip fit tightly;
(3) by the bend portions 180 ° that adhesive strip does not bond with positive plate or negative plate, make the two ends of adhesive strip parallel to each other, even if the adhesive strip do not bonded with pole piece is parallel to each other with the adhesive strip bonded with pole piece;
(4) adhesive strip is not fixed on the corrosion resistant plate of peel test force machine transfer arm with one end of coating adhesion;
(5) peel test force machine is started, make the tache motorice slowly movement of peel test force machine, adhesive strip is separated completely with coating, by the loading pressure in rate-determining steps (2), adhesive strip is only separated with coating, and coating and flexible substrates are not separated, and obtained the curve of peeling force and strip length by the testing software that peel test force machine carries; The translational speed controlling peel test force machine transfer arm is 60mm/min;
(6) obtain the size of peeling force F according to curve obtained, and calculate adhesive strength size between coat inside according to formula θ=F/S.
Wherein: the thickness of the corrosion resistant plate of peel test force machine transfer arm is 1.5mm, length is 1.3 times of coated body length, and width is 1.2 times of coated body width.
Test result is: positive pole: F is 50gf, S be 20mm, θ is 2.5gf/mm, and negative pole: F is 38gf, S be 20mm, θ is 1.9gf/mm.
The test of cohesive strength between coating and substrate:
(1) paste adhesive strip in stainless steel bar one end, be then wound up on stainless steel bar by coated body, outside, another side contacts with stainless steel bar the cated one side of coated body;
(2) reel coated body on stainless steel bar a circle, observes the situation of change of coat surface coating;
(3) if peeling changes the stainless steel bar of another numbering, until just there is skin effect phenomenon in the coating of coated body after winding, the numbering of the stainless steel bar that record uses.
Test result is: positive pole: 9 grades (4mm); Negative pole: 7 grades (6mm).
Claims (7)
1. a measuring method for flexible base material coating adhesive strength, is characterized in that: the test and the test of cohesive strength between coating and substrate that comprise coat inside cohesive force:
The test of coat inside cohesive force is: according to following formulae discovery coat inside cohesive force: θ=F/S, F is peeling force, S is adhesive strip width, described peeling force is: use peel test force instrument to measure, coated body is applied cated surface and adhesive strip is fitted, by the adhesive strip other end not with the bend portions 180 ° of coating adhesion, then bond with the mobile corrosion resistant plate in peel test force instrument, apply pulling force in the horizontal direction, make and the adhesive strip of coating adhesion and coating segregation, peeling force F in record detachment process;
Whether between coating from substrate, the test of cohesive strength is: reeled on the stainless steel bar that diameter is different by coated body, be separated, draw cohesive force intensity level between coat and substrate according to coat during winding with flexible substrates.
2. the measuring method of flexible base material coating adhesive strength according to claim 1, is characterized in that: the test of coat inside cohesive force, comprises the following steps:
(1) coated body is fixed on horizontal corrosion resistant plate;
(2) by applying pressure, cated for a coated body tool surface and adhesive strip are fitted tightly;
(3) bend portions 180 ° do not bonded with coated body by adhesive strip, makes the two ends of adhesive strip parallel to each other;
(4) adhesive strip is not fixed on the corrosion resistant plate of peel test force machine transfer arm with one end of coating adhesion;
(5) peel test force machine is started, peel test force machine transfer arm is moved, adhesive strip is separated completely with coating, by rate-determining steps (2) applied pressure, adhesive strip is only separated with coating, and coating and flexible substrates are not separated, and obtained the curve of peeling force and strip length by the testing software that peel test force machine carries;
(6) obtain the size of peeling force F according to curve obtained, and calculate adhesive strength size between coat inside according to formula θ=F/S.
3. the measuring method of flexible base material coating adhesive strength according to claim 2, it is characterized in that: the thickness of the corrosion resistant plate of peel test force machine transfer arm is 1-1.5mm, length is 1.2-1.5 times of coated body length, and width is 1.1-1.2 times of coated body width.
4. the measuring method of flexible base material coating adhesive strength according to claim 2, is characterized in that: the translational speed controlling peel test force machine transfer arm in step (5) is 40-80mm/min.
5. the measuring method of flexible base material coating adhesive strength according to claim 2, is characterized in that: step (6) obtains the size of peeling force F according to curve obtained 1/4-3/4 section.
6. the measuring method of flexible base material coating adhesive strength according to claim 1, is characterized in that: the test of cohesive strength between coating and substrate, comprises the following steps:
(1) paste double faced adhesive tape or adhesive strip in stainless steel bar one end, be then wound up on stainless steel bar by coated body, outside, another side contacts with stainless steel bar the cated one side of coated body;
(2) reel coated body on stainless steel bar a circle, observes the situation of change of coat surface coating;
(3) stainless steel bar of different numbering is changed, until the coating generation skin effect phenomenon of coated body after winding, record stainless steel bar numbering.
7. the measuring method of flexible base material coating adhesive strength according to claim 6, it is characterized in that: stainless steel bar length is identical is 150mm, and diameter is respectively 1 grade: 30mm, 2 grades: 20mm, 3 grades: 15mm, 4 grades: 10mm, 5 grades: 8mm, 6 grades: 7mm, 7 grades: 6,8 grades: 5mm, 9 grades: 4mm, 10 grades: 3mm.
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| CN105203451A (en) * | 2015-09-18 | 2015-12-30 | 福建蓝海黑石科技有限公司 | Representation method for cohesion of coating |
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