CN104596923B - 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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- CN104596923B CN104596923B CN201410850484.9A CN201410850484A CN104596923B CN 104596923 B CN104596923 B CN 104596923B CN 201410850484 A CN201410850484 A CN 201410850484A CN 104596923 B CN104596923 B CN 104596923B
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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 is and in particular to a kind of flexible base material coating adhesive strength
Measuring method.
Background technology
Lithium ion battery mainly includes pole piece and nonaqueous electrolytic solution, and described pole piece and nonaqueous electrolytic solution are sealed in battery case
In vivo, described pole piece includes battery electrode and barrier film, and described battery electrode includes anode pole piece and cathode pole piece, described positive pole pole
Piece includes plus plate current-collecting body and coating/or is filled in positive electrode on plus plate current-collecting body, and described cathode pole piece includes negative pole collection
Fluid and coating and/or be filled in the negative material on negative current collector.
In lithium battery, the impact to battery performance for the pole piece is very big, lithium battery is being carried out, in charge and discharge process, can lead to
Positive/negative active substance is separated with collector, and then reduces battery capacity and deteriorate cycle life.So to battery pole piece
Control is the key factor directly influencing battery performance.Wherein with the bonding between active substance on pole piece in the control of pole piece
Intensity and active substance are mostly important with the adhesion strength of substrate.
At present, the method for testing of pole piece adhesion strength is mainly Grid Method, peel test force method.The concrete operations of Grid Method
It is: draw knife by pole piece coating with the spacing of 1-3 millimeter and 45 ° of -90 ° of stagger angles with steel, be divided into a number of square
Or little lattice of prismatic scratching.Then special adhesive tape is smooth is bonded on little lattice for the cohesive force test being produced with 3m company of the U.S.,
Do not stay a space, then vertically uncovered with prestissimo, observe and draw dropping off and peeling situation, with the amount of dropping off and peeling at lattice
Situation come to weigh pole piece bond force intensity size.The method is simple, but a disadvantage is that the line depth is not easily-controllable during line
System, is not directly bonding force intensity to be measured, measurement result is subjective, repeated and accurately establishes a capital poor.Patent
Mention in publication number cn101206173a, peel test force method is that the surface one end being coated with coating is not less than with bonding strength
The adhesive tape of coating adhesive strength needed for coated body fits tightly and fixes, then that coated body is never curved with adhesive tape joint place
Bent 180 ° so that the two ends of coated body are parallel to each other and make fit with adhesive tape the two of surface short close to each other, tailing edge this
The direction that the coated body other end extends applies pulling force to this coated body other end, makes coating separate required minimum with substrate and draws
Power.The shortcoming of the method is, when measuring it is impossible to ensure that coating is kept completely separate with substrate, some local coatings and substrate
Can be kept completely separate, some local coatings still remain in substrate, the lowest pull of so test cannot represent makes coating divide
From pulling force, the position that coating and substrate are not properly separated obtain pulling force value be coat inside granule between bonding
Power, is not the cohesive force between coating and substrate.When carrying out disbonded test it is necessary to bend the flexible substrates after coating
180 °, will there is stress in bending position, especially when testing lithium battery anode piece, coating is thicker, and this stress is just
Cause coming off so that test result is inaccurate of coating.
Content of the invention
The purpose of the present invention is to overcome Grid Method and peel test force method to test the shortcoming of pole piece adhesion strength, provides one
Plant the measuring method of flexible base material coating adhesive strength, relatively accurate, objective.
A kind of measuring method of flexible base material coating adhesive strength of the present invention it is characterised in that: include applying
The test of adhesion strength between the test of layer internal bond power and coating and substrate:
The test of coat inside cohesive force is: calculates coat inside cohesive force according to below equation: θ=f/s, f are to peel off
Power, s is bonding bandwidth, and described peeling force is: is measured using peel test force instrument, coated body is coated with coating
Surface fit with adhesive tape, by the adhesive tape other end not with coating bonding part bend 180 °, then with peel test force
Mobile corrosion resistant plate bonding in instrument, apply pulling force in the horizontal direction so that with the adhesive tape of coating bonding and coating segregation,
Peeling force f in record separation process；
The test of adhesion strength between coating and substrate is: coated body is wound on the different stainless steel bar of diameter, root
Whether separate with flexible substrates according to coat during winding, draw cohesive force intensity level between coat and substrate.
Wherein: coated body refers to comprise the flexible base material of coating.
The test of coat inside cohesive force, comprises the following steps:
(1) coated body is fixed on horizontal corrosion resistant plate；
(2) pass through to apply pressure, coated body is had a cated surface and fits tightly with adhesive tape；
(3) adhesive tape is not bent 180 ° with the part of coated body bonding, make the two ends of adhesive tape parallel to each other；
(4) adhesive tape is not fixed on the corrosion resistant plate of peel test force machine transfer arm with one end of coating bonding；
(5) start peel test force machine, so that peel test force machine transfer arm is moved, so that adhesive tape is kept completely separate with coating,
The pressure that applied by rate-determining steps (2) is so that adhesive tape is only separated with coating, and coating and flexible substrates do not occur point
From, and the test software being carried by peel test force machine obtains the curve of peeling force and strip length；
(6) obtain the size of peeling force f according to curve obtained, and calculated between coat inside according to formula θ=f/s
Adhesive strength size.
In step (1), coated body is horizontally fixed on horizontal corrosion resistant plate.
S is the contact area of adhesive tape and coating, and the area of adhesive tape is preferably the 30-60% coating bulk area, accurately
Du Genggao.
The thickness of the corrosion resistant plate of peel test force machine transfer arm is 1-1.5mm, and length is the 1.2-1.5 of coating body length
Times, width is 1.1-1.2 times of coated body width.
Make in step (3) adhesive tape two ends parallel to each other for making not adhesive tape and the coated body coating with coated body bonding
Surface bonding band is parallel to each other.
The translational speed controlling peel test force machine transfer arm in step (5) is 40-80mm/min.
The bonding strength of adhesive tape is more than the coating adhesive strength needed for coated body, and it is public that adhesive tape is preferably U.S. 3m
Department's adhesive tape.
Described adhesive tape can be cated by adhesive tape sticks to the tool of coated body with fitting of coated body coating
On surface, then pressurization is so that adhesive tape is combined closely with coating.The size of pressure and action time are so that adhesive tape and coating
Coating and flexible substrates are not caused to be separated into standard when farthest fitting together and carry out adhesive tape with coating stripping.Viscous
The total length of crossed belt is that adhesive tape bonds more than the length twice of adhesive tape of contact portion with coating.Adhesive tape is surveyed with peeling force
The adhesion strength of test instrument transfer arm corrosion resistant plate is more than the adhesion strength between adhesive tape and coating.
Described peeling force can be the mean force in transient force or a period of time or distance range.For further
Improve accuracy of measurement, the preferably described peeling force of the present invention is the mean force in a period of time or distance range.In order to more enter one
Step improves the accuracy of measurement, the preferably meansigma methodss of the lowest pull needed for 1/4-3/4 section.
Step (6) obtains the size of peeling force f according to curve obtained 1/4-3/4 section.
Preferably each sample retest three times, it is final result that result takes minima.
The test of adhesion strength between coating and substrate, comprises the following steps:
(1) paste double faced adhesive tape or adhesive tape in stainless steel bar one end, then coated body is wound up on stainless steel bar, coating
Outside, another side is contacted the cated one side of body with stainless steel bar；
(2) coated body is wound on stainless steel bar a circle, observe the situation of change of coat face coat；
(3) change the stainless steel bar of different numberings, until the coating of the coated body after winding occurs skin effect phenomenon, record is not
Rust rod iron numbering.
Wherein: step is wound as compact winding in (2).
Preferably each sample test three times, result is by minimum being defined of rank.
Substrate is generally Copper Foil or aluminium foil.
In step (1), double faced adhesive tape or adhesive tape are pasted in one end, and the amount for double faced adhesive tape or adhesive tape does not require, as long as energy
Coated body is wound up on stainless steel bar, without departing from just permissible.
Stainless steel bar length is identical to be 150mm, diameter respectively 1 grade: 30mm, 2 grades: 20mm, 3 grades: 15mm, 4 grades:
10mm, 5 grades: 8mm, 6 grades: 7mm, 7 grades: 6mm, 8 grades: 5mm, 9 grades: 4mm, 10 grades: 3mm.Test result series is higher, represents soft
Property base material coating adhesive strength is higher.Because the stainless steel bar of different-diameter produces certain when being wound in curved surface
Tension force, due to coating tension force different from flexible substrates tension force so that coating is separated with flexible substrates under tension.Adopt
Use identical flexible substrates, the coating of same thickness, the tension force producing in winding is identical, therefore can compare different paintings
Cover the magnitude relationship of adhesive strength between body coating and flexible substrates.
In sum, the invention has the advantages that
The number value of minimum stainless steel bar that peeling does not occur according to coated body winding and is as measurement coating and flexible base
Adhere to force intensity between bottom, can more intuitively know that on coated body, the adhesive force between coat inside and coating and substrate is big
Little, and reproducible, simple to operate, thus overcome prior art Grid Method measurement result subjective, repeated and
The all poor shortcoming of accuracy.The shortcoming overcoming 180 ° of knee impact to coating when peeling off force method test, overcomes stripping
From method, coat inside adhesive force and coating and flexible substrates adhesive force are lumped together the shortcoming measuring.Using the present invention's
Method can accurately know the adhesive strength of battery pole piece upper electrode material, thus not only can really be used for quality of battery pole piece
On-line monitoring and monitoring, and the optimization for dispensing and slurry technique parameter has great directive significance.The present invention provides
Method can be also used for measuring on the coated body that other substrates are flexible material the adhesive force between coat inside and coating with
Attachment force intensity between flexible substrates, can be used for measuring and adheres to force intensity size in rigid basement between coat inside.
Brief description
Fig. 1 is the schematic diagram of the embodiment of the present invention 1 coat inside cohesive force test.
In figure: 1, the mobile corrosion resistant plate in peel test force instrument；2nd, adhesive tape；3rd, coated body substrate；4th, coated body
Coating；5th, horizontal corrosion resistant plate.
Specific embodiment
With reference to embodiment, the present invention will be further described.
Embodiment
Prepare anode pole piece to be tested: by 100 weight portion licoo2, 2.5 parts by weight of binder pvdf, 3 weight portions lead
Electric agent acetylene black is added in 65 weight portion nmp solvents, and then in de-airing mixer, stirring forms uniform anode sizing agent.Will
The uniform single spreading of this slurry on wide 400mm, latter 20 μm of aluminium foil, then 120 DEG C dry, after roll-in cutting obtain size
Anode pole piece for 140mm × 50mm.
Prepare cathode pole piece to be tested: 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 white carbon blacks are added in the nmp solvent of 120 weight portions, then stir shape in de-airing mixer
Become stable, homogeneous cathode size.By uniform for this slurry single spreading on wide 400mm, thick 10 μm of Copper Foil, through 120 DEG C
The cathode pole piece of 140mm × 45mm is cut into after drying, roll-in.
The test of coat inside cohesive force, comprises the following steps:
(1) positive plate preparing embodiment or negative plate are fixed on horizontal corrosion resistant plate；
(2) pass through to apply certain pressure, the positive plate that prepare embodiment or negative plate have a cated table
Face is fitted tightly with adhesive tape；
(3) adhesive tape is not bent 180 ° with the part of positive plate or negative plate bonding, make the two ends of adhesive tape mutually equal
OK, though not with pole piece bonding adhesive tape with parallel to each other with the adhesive tape that pole piece bonds；
(4) adhesive tape is not fixed on the corrosion resistant plate of peel test force machine transfer arm with one end of coating bonding；
(5) start peel test force machine, so that the tache motorice of peel test force machine is slowly moved, make adhesive tape complete with coating
Separate, by the loading pressure in rate-determining steps (2) so that adhesive tape is only separated with coating, and coating and flexible substrates
Do not occur to separate, and the test software being carried by peel test force machine obtains the curve of peeling force and strip length；Control stripping
It is 60mm/min from the translational speed of power test machine transfer arm；
(6) obtain the size of peeling force f according to curve obtained, and calculated between coat inside according to formula θ=f/s
Adhesive strength size.
Wherein: the thickness of the corrosion resistant plate of peel test force machine transfer arm is 1.5mm, length is the 1.3 of coating body length
Times, width is 1.2 times of coated body width.
Test result is: positive pole: f is 50gf, and s is 20mm, and θ is 2.5gf/mm, and negative pole: f is 38gf, and s is 20mm, and θ is
1.9gf/mm.
The test of adhesion strength between coating and substrate:
(1) paste adhesive tape in stainless steel bar one end, then coated body is wound up on stainless steel bar, coated body has coating
One side outside, another side is contacted with stainless steel bar；
(2) coated body is wound on stainless steel bar a circle, observe the situation of change of coat face coat；
(3) if peeling changes the stainless steel bar of another numbering, until the coating of the coated body after winding occurs just
Skin phenomenon, the numbering of the stainless steel bar that record uses.
Test result is: positive pole: 9 grades (4mm)；Negative pole: 7 grades (6mm).
Claims (6)
1. a kind of measuring method of flexible base material coating adhesive strength it is characterised in that: include coat inside cohesive force
The test of adhesion strength between test and coating and substrate:
The test of coat inside cohesive force is: calculates coat inside cohesive force according to below equation: θ=f/s, f are peeling force, s
For bonding bandwidth, described peeling force is: is measured using peel test force instrument, coated body is coated cated table
Being fitted with adhesive tape in face, the adhesive tape other end is not bent 180 ° with the part of coating bonding, then with peel test force instrument
In the bonding of mobile corrosion resistant plate, apply pulling force in the horizontal direction so that with the adhesive tape of coating bonding and coating segregation, record
Peeling force f in separation process；
The test of coat inside cohesive force, comprises the following steps:
(1) coated body is fixed on horizontal corrosion resistant plate；
(2) pass through to apply pressure, coated body is had a cated surface and fits tightly with adhesive tape；
(3) adhesive tape is not bent 180 ° with the part of coated body bonding, make the two ends of adhesive tape parallel to each other；
(4) adhesive tape is not fixed on the corrosion resistant plate of peel test force machine transfer arm with one end of coating bonding；
(5) start peel test force machine, so that peel test force machine transfer arm is moved, so that adhesive tape is kept completely separate with coating, pass through
The pressure that rate-determining steps (2) apply is so that adhesive tape is only separated with coating, and coating is not separated with flexible substrates,
And the test software being carried by peel test force machine obtains the curve of peeling force and strip length；
(6) obtain the size of peeling force f according to curve obtained, and attachment between coat inside is calculated according to formula θ=f/s
Intensity size；
The test of adhesion strength between coating and substrate is: coated body is wound on the different stainless steel bar of diameter, according to volume
Around when coat whether separate with flexible substrates, draw cohesive force intensity level between coat and substrate.
2. flexible base material coating adhesive strength according to claim 1 measuring method it is characterised in that: peeling force
The thickness of the corrosion resistant plate of test machine transfer arm is 1-1.5mm, and length is 1.2-1.5 times of coating body length, and width is coating
1.1-1.2 times of body width.
3. flexible base material coating adhesive strength according to claim 1 measuring method it is characterised in that: step
(5) translational speed controlling peel test force machine transfer arm in is 40-80mm/min.
4. flexible base material coating adhesive strength according to claim 1 measuring method it is characterised in that: step
(6) size of peeling force f is obtained according to curve obtained 1/4-3/4 section.
5. flexible base material coating adhesive strength according to claim 1 measuring method it is characterised in that: coating with
The test of adhesion strength between substrate, comprises the following steps:
(1) paste double faced adhesive tape or adhesive tape in stainless steel bar one end, then coated body is wound up on stainless steel bar, coated body has
Outside, another side is contacted the one side of coating with stainless steel bar；
(2) coated body is wound on stainless steel bar a circle, observe the situation of change of coat face coat；
(3) change the stainless steel bar of different numberings, until the coating of the coated body after winding occurs skin effect phenomenon, record rustless steel
Rod numbering.
6. flexible base material coating adhesive strength according to claim 5 measuring method it is characterised in that: rustless steel
Excellent length is identical to be 150mm, and diameter is respectively 1 grade: 30mm, 2 grades: 20mm, 3 grades: 15mm, 4 grades: 10mm, 5 grades: 8mm, 6
Level: 7mm, 7 grades: 6mm, 8 grades: 5mm, 9 grades: 4mm, 10 grades: 3mm.
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| CN105181584A (en) * | 2015-09-23 | 2015-12-23 | 合肥国轩高科动力能源有限公司 | Device for qualitatively testing adhesion performance of battery pole piece |
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| SU953535A1 (en) * | 1981-01-14 | 1982-08-23 | Татарский Научно-Исследовательский Институт Нефтяного Машиностроения | Polymeric compound adhesion strength determination method |
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| JP2002005817A (en) * | 2000-06-16 | 2002-01-09 | Mitsubishi Heavy Ind Ltd | Coating film adhesion evaluating method and device therefor and electrode plate manufacturing method |
| JP4619893B2 (en) * | 2005-08-09 | 2011-01-26 | 藤倉化成株式会社 | Adhesion test method for exterior wall finishing coating |
| CN101206173B (en) * | 2006-12-22 | 2010-10-13 | 上海比亚迪有限公司 | Method for measuring coating adhesive strength on a coating body using flexible material as substrate |
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