Method for detecting adhesive force of coating on surface of base material

Abstract

The invention provides a method for detecting the adhesive force of a coating on the surface of a base material. The detection method comprises the following steps: step S1, obtaining the surface density of a single-side coating of a sample to be measured and the quality of a 3M adhesive tape with a preset length in advance; s2, pasting a 3M adhesive tape on the surface of the to-be-measured sample wafer, rolling the to-be-measured sample wafer, and then uncovering the 3M adhesive tape upwards at a preset speed; s3, cutting the 3M adhesive tape adhered with the coating into a fixed specification, weighing the 3M adhesive tape with the fixed specification, and calculating the mass difference between the 3M adhesive tape before and after adhesion; and S4, calculating the area of the adhered 3M adhesive tape with the fixed specification, obtaining the adhesion mass per unit area according to the area, comparing the adhesion mass with the surface density of the single-side coating of the sample to be measured to obtain a comparison result, and evaluating the adhesive force of the sample to be measured according to the comparison result. The method for detecting the adhesive force of the coating on the surface of the base material does not need precise equipment, and the adhesive force grade can be quantitatively output through on-site rapid detection.

Description

Technical Field

[0001] The present invention relates to the technical field of material surface coating performance detection, and in particular to a method for detecting the adhesion of a substrate surface coating. Background Art

[0002] Coating adhesion, a key indicator for evaluating coating quality, is gaining increasing attention. Coating adhesion directly impacts the coating's ability to protect the substrate, making coating adhesion testing increasingly common. Ultra-thin substrates (thickness ≤ 20 μm) are susceptible to substrate deformation during coating adhesion testing. Traditional cross-hatch testing (ASTM D3359) can penetrate the substrate, damaging it and failing to accurately reflect coating bond strength.

[0003] The existing laser scattering method is not sensitive enough to nano-scale coatings, while the ultrasonic resonance method is limited by the thickness of the substrate and has an error rate of more than 30%. In addition, these methods require complex and precise instruments and are generally expensive.

[0004] Therefore, the industry often uses tape adhesion to measure the adhesion of such materials. However, the existing adhesion method generally rates by comparing with a standard color chart, which is highly subjective. Moreover, due to the different appearance colors of the products, the standard color chart becomes invalid, resulting in poor adhesion detection accuracy. Summary of the Invention

[0005] The embodiment of the present invention provides a method for detecting the adhesion of a substrate surface coating, which is used to solve the problems of subjectivity and limitations of the existing method for determining the adhesion grade of a substrate surface coating using a colorimetric card.

[0006] An embodiment of the present invention provides a method for detecting the adhesion of a coating on a substrate surface, the method comprising the following steps:

[0007] Step S1: obtaining in advance the single-side coating density of the sample to be measured and the mass of a 3M tape of a preset length;

[0008] Step S2, sticking the 3M tape on the surface of the sample to be measured, and peeling the 3M tape upward at a preset speed after rolling;

[0009] Step S3, cutting the 3M tape with the coating adhered thereto into fixed specifications, weighing the 3M tape with fixed specifications, and calculating the difference in mass between the 3M tape before and after adhesion;

[0010] Step S4: Calculate the area of ​​the 3M tape of fixed specifications after adhesion, obtain the adhesion mass per unit area based on the area, compare the adhesion mass with the single-side coating surface density of the sample to be measured to obtain a comparison result, and use the comparison result to evaluate the adhesion of the sample to be measured.

[0011] Preferably, in step S1, the thickness of the sample to be measured is 5um-100um.

[0012] Preferably, in step S1, the surface density of the coating on one side of the sample to be measured is 0.1 to 2.0 g / m 2 .

[0013] Preferably, it is characterized in that, in step S1, the 3M tape itself has a consistent width and uniform quality.

[0014] Preferably, the step S2 specifically includes the following steps:

[0015] Step S21: Before adhering the 3M tape, fold the starting end of the 3M tape by 0.5 cm to form a hand-grip point for subsequently tearing off the 3M tape;

[0016] Step S22: When the 3M tape is adhered, the 3M tape is gradually unfolded and adhered to the surface of the sample to be measured using a synchronous progressive adhesion method;

[0017] Step S23: Select a roller with a fixed mass to roll along the glue-applying direction; wherein, during the rolling process, no pressure is applied to the roller in a direction perpendicular to the surface of the sample to be measured;

[0018] Step S24: Before peeling off the 3M tape, hold the 3M tape at the fulcrum point and tear off the 3M tape at an average speed of 5 mm / s in a fixed direction.

[0019] Preferably, the fixed direction is the direction when the force point is 60°, 90° or 180° to the surface of the sample to be measured.

[0020] Preferably, the roller is a handheld tape rolling roller; wherein the pressure of the roller is 1.5-2.5 kgf, and the speed of the roller is 5-15 mm / s.

[0021] Preferably, the 3M tape is a transparent tape with a width of 12 mm to 35 mm.

[0022] Preferably, in step S3, an analytical balance is used to weigh the 3M tape of fixed specifications; wherein, the analytical balance is an analytical balance with a sensitivity of 0.0001 g.

[0023] Preferably, in step S4, the comparison result is used to evaluate the adhesion of the surface coating of the sample to be measured by the ratio η, which satisfies the following conditions:

[0024]

[0025] Wherein, S represents the area of ​​the 3M tape, ρ represents the surface density of the coating on one side of the sample to be measured, and ΔM represents the difference in mass before and after the 3M tape is adhered.

[0026] Compared with the prior art, the method for detecting the adhesion of the coating on the surface of the substrate in the present invention, through the above-mentioned steps S1 to S4, uses a specific tape to adhere the coating without damaging the substrate, measures the coating adhesion amount by weighing and converts it into the coating adhesion amount per unit area using the tape area, and then compares it with the single-side coating surface density of the sample itself to obtain the coating shedding situation after adhesion, and finally conducts a targeted assessment of the adhesion of different samples; at the same time, the detection tool required by the present invention is simple, easy to operate, easy to implement, and applicable to different types of carbon-coated aluminum foil coatings. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0028] Figure 1 This is a flow chart of a method for detecting adhesion of a coating on a substrate surface provided by an embodiment of the present invention;

[0029] Figure 2 This is a specific flow chart of step S2 of the method for detecting adhesion of a substrate surface coating provided by an embodiment of the present invention;

[0030] Figure 3 Schematic diagram of the "synchronous progressive" adhesive application method provided by an embodiment of the present invention;

[0031] Figure 4 yes Figure 3 Local map of the handheld site for the adhesive application method;

[0032] Figure 5 is a schematic diagram of a manual rolling roller provided in an embodiment of the present invention;

[0033] Figure 6 Schematic diagram of different tape tearing angles provided by an embodiment of the present invention;

[0034] Figure 73 is a schematic diagram of a comparison curve of the η value provided in an embodiment of the present invention and the color chart grade of a certain product.

[0035] In the figure, 1. Sample to be measured, 2. Coated surface, 3. 3M tape, 4. Roller. DETAILED DESCRIPTION

[0036] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, any other embodiments obtained by ordinary technicians in this field without making any creative efforts shall fall within the scope of protection of the present invention.

[0037] Combined with attachment Figure 1-Figure 7 As shown, an embodiment of the present invention provides a method for detecting the adhesion of a coating on a substrate surface, the method comprising the following steps:

[0038] Step S1: Pre-obtain the density of the single-side coating surface 2 of the sample 1 to be measured and the mass of a preset length of 3M tape 3. Through surface density correlation design, the single-side coating surface 2 density ρ is introduced as a reference value to eliminate the influence of coating density on the adhesion test results.

[0039] The single-side coating surface 2 density ρ will be sampled and measured during the actual production process, and the measured value can be directly used as the single-side coating surface 2 density value of the sample.

[0040] Among them, the width of 3M tape 3 is fixed, and the tape length should be consistent with the tape length when measuring the coating adhesion.

[0041] Step S2: stick the 3M tape 3 on the surface of the sample 1 to be measured, and then peel the 3M tape 3 upward at a preset speed after rolling. By standardizing the sticking method, the influence of too many bubbles on the test results during the bonding method test can be reduced.

[0042] In this embodiment, Figure 2-6 As shown, step S2 specifically includes the following steps:

[0043] Step S21: Before adhering the 3M tape 3, fold the starting end of the 3M tape 3 by 0.5 cm to form a hand-grip point for subsequently tearing off the 3M tape 3;

[0044] Step S22: When adhering the 3M tape 3, a "synchronous and progressive" adhering method is adopted to gradually unfold the 3M tape 3 and adhere it to the surface of the sample 1 to be measured;

[0045] Step S23 , selecting a roller 4 with a fixed mass to perform rolling along the glue-applying direction; wherein, during the rolling process, no pressure is applied to the roller 4 in a direction perpendicular to the surface of the sample 1 to be measured.

[0046] Step S24: Before peeling off the 3M tape 3, hold the 3M tape 3 at the support point and tear off the 3M tape 3 at an average speed of 5 mm / s in a fixed direction.

[0047] In this embodiment, Figure 6 As shown, the fixed direction is the direction when the force point is 60°, 90° or 180° to the surface of the sample 1 to be measured.

[0048] Step S3: cutting the 3M tape 3 with the coating adhered thereto into fixed specifications, weighing the 3M tape 3 with fixed specifications, and calculating the difference in mass between the 3M tape 3 before and after adhesion.

[0049] When the adhesion amount measurement fluctuates greatly, the steps S1 to S3 may be repeated to measure the adhesion amounts of multiple tapes using a cumulative method for calculation.

[0050] Among them, by adopting the double mass difference method, the traditional qualitative judgment can be converted into a quantitative η value through precise weighing before and after tape adhesion, with a resolution of up to 0.1%.

[0051] Step S4: Calculate the area of ​​the 3M tape 3 of fixed specifications after adhesion, obtain the adhesion mass per unit area based on the area, compare the adhesion mass with the density of the single-sided coating surface 2 of the sample 1 to be measured, obtain a comparison result, and use the comparison result to evaluate the adhesion of the sample 1 to be measured.

[0052] Specifically, through the above steps S1 to S4, without damaging the substrate, a specific tape is used to adhere the coating, the coating adhesion amount is measured by weighing and converted into the coating adhesion amount per unit area with the help of the tape area, and then the ratio is made with the density of the single-sided coating surface 2 of the sample itself to obtain the coating shedding situation after adhesion, and finally the adhesion of different samples is evaluated in a targeted manner. At the same time, the whole process only requires a balance, a roller 4 and a calculator, and the detection time is ≤5 minutes. The equipment investment is less than 1 / 10 of the traditional method. In the coating thickness range of 0.5-50μm, the η value is linearly correlated with the standard tensile method coefficient R 2 ≥0.9.

[0053] In this embodiment, in step S1 , the thickness of the sample 1 to be measured is 5 μm-100 μm.

[0054] In this embodiment, in step S1, the density of the single-side coating surface 2 of the sample 1 to be measured is 0.1-2.0 g / m2 .

[0055] In this embodiment, it is characterized in that, in the step S1, the 3M tape 3 itself has a consistent width and uniform quality.

[0056] In this embodiment, the roller 4 is a handheld tape rolling roller 4. The pressure of the roller 4 is 1.5-2.5 kgf, and the speed of the roller 4 is 5-15 mm / s.

[0057] In this embodiment, the 3M tape 3 is a transparent tape with a width of 12 mm to 35 mm, an adhesive force of 4.5 to 5.5 N / cm, and a width of ≥10 mm.

[0058] In this embodiment, in step S3, an analytical balance is used to weigh the 3M tape 3 of fixed specifications; wherein, the analytical balance is an analytical balance with a sensitivity of 0.0001 g.

[0059] Specifically, analytical balances are the most important instruments for accurate weighing in experiments. They can be divided into mechanical and electronic types. While all balances utilize the lever principle, they differ in structure and usage. Mechanical balances can meet the accuracy requirements of general quantitative analysis, with a sensitivity of 0.1 mg.

[0060] In this embodiment, in step S4, the comparison result is used to evaluate the adhesion of the surface coating of the sample 1 to be measured by the ratio η, which satisfies the following conditions:

[0061]

[0062] Wherein, S represents the area of ​​the 3M tape 3, ρ represents the density of the single-sided coating surface 2 of the sample 1 to be measured, and ΔM represents the difference in mass between the 3M tape 3 before and after adhesion.

[0063] In this embodiment, corresponding tests may be performed on the measurement sample, as follows.

[0064] Sample requirements:

[0065] The sample surface should be flat and clean, and the sample size should not be less than 200mm×300mm.

[0066] Test conditions:

[0067] The test should be carried out in a stable environment at room temperature.

[0068] Test steps

[0069] (1) Place the test sample on the sample clamp and fix the sample position with the sample clamp to ensure that the sample surface is flat and not easy to slide.

[0070] (2) Tear off the three ends of the 3M tape and fold the starting end about 0.5 cm to serve as the handhold for subsequently tearing off the tape.

[0071] (3) Stick the starting end on the sample to be tested, touch the starting end of the tape with your finger and gently push the tape roll to one side to cause the tape roll to roll and adhere flatly to the sample.

[0072] (4) When the pasting length of the 3M tape 3 reaches a certain value, the tape is adhered and cut with a utility knife.

[0073] (5) Place the handheld roller 4 at one end of the holding position of the tape, and roll the tape back and forth three times along the direction of the tape at a speed of about 300 mm / min. (Note that when rolling, only the force generated by the mass of the roller can be applied to the tape.) Make sure that the tape is fully adhered to the sample coating.

[0074] (6) Hold the tape at the starting point so that the starting end of the tape is at 90° to the sample, keep the angle unchanged, and slowly tear off the tape upward at a speed of no more than 20 mm / s until the tape is completely detached from the sample.

[0075] (7) Using a steel ruler and a utility knife, cut 10 cm from the tested tape, place it on an electronic balance, and weigh the tape mass M. d1 , the unit is mg, and the result is expressed to 1 decimal place.

[0076] (8) The ratio of the adhesion amount of 3M tape 3 coating to the density of the single-sided coating surface 2 is used as the adhesion coefficient. The adhesion coefficient η meets the following conditions and is expressed in %.

[0077] Where η=(M d1 -M d0 ) / (0.0019ρ);

[0078] Where:

[0079] M d0 Indicates the mass of 10 cm long 3M tape 3 in milligrams (mg);

[0080] M d1 Indicates the mass of 3M tape 3 of the adhesive coating in milligrams (mg);

[0081] ρ represents the density of the single-side coating of the sample, which is pre-measured by differential weight method and is expressed in mg (g / m 2 ).

[0082] (9) Repeat (1)-(8) to measure multiple tapes and take the average value of η.

[0083] The results are assessed as follows:

[0084] η≤15%→Adhesion Grade A (Excellent);

[0085] 15% <η≤35% → Adhesion Grade B (qualified);

[0086] η>35% → Adhesion grade C (unqualified).

[0087] Example 1

[0088] The present invention provides a method for detecting the adhesion of a coating on a substrate surface, wherein the thickness of the substrate is 12 μm aluminum foil and the density of the carbon coating layer is ρ 1.0 g / m 2 The 3M tape 3 used is Scotch 600 series transparent tearable tape with a width of 19mm. The roller 4 used has a load of 2500±30g. The roller 4 surface is made of rubber with a thickness of 8mm and a hardness of HS80±5. The width of the roller 4 is 45mm, which can fully ensure that the tape is rolled during rolling.

[0089] The "synchronous progressive" adhesive application method is used to ensure that the tape is in full contact with the material surface and there is basically no bubble residue at the adhesion point. If the tape length is 10 cm, the adhesion area S is 0.0019 m 2 .

[0090] During rolling, the rolling speed is 10mm / s, the rolling method is reciprocating rolling, the force applied in the vertical direction during rolling is 0N, and the reciprocating rolling is repeated 3 times.

[0091] Judgment level: η≤15%→adhesion grade A (excellent); 15%<η≤35%→adhesion grade B (qualified); η>35%→adhesion grade C (unqualified).

[0092] Test results: ΔM = 0.0003g, S = 0.0019m 2 ,ρ=1.0g / m 2 , adhesion η=15.79%, the adhesion grade is judged to be B, which is qualified.

[0093] Comparison verification: after comparing the adhesive tape with the standard color card of the product, the adhesion grade is determined to be B. The results of the two are consistent.

[0094] Example 2

[0095] Flexible copper foil test data can be used to establish a dynamic compensation mechanism for the water absorption characteristics of water-based coating slurries. In high temperature and high humidity environments (e.g., temperature > 40°C, humidity > 80%), the adhesive strength of the tape can be compensated for temperature and humidity. The correction factor k = 1-0.02×(T-25)+0.01×(RH-60). T is defined as temperature and RH is humidity.

[0096] Special conditions: ambient temperature 30°C, ambient humidity 85%, compensation coefficient k = 1.15;

[0097] After correction, η=12.3%×1.15=14.1%, and the A-level judgment is still maintained.

[0098] Comparative Example 1

[0099] Detection was performed using the colorimetric card method after adhesion.

[0100] The standard colorimetric card is fixed, but when the coating composition is a graphite system, the measurement judgment result grade is often better than the measurement result of the coating composition is a carbon black system. The colorimetric card is not universally applicable to products with different coating compositions.

[0101] Comparative Example 2

[0102] Detection was performed using the colorimetric card method after adhesion.

[0103] The standard colorimetric card is fixed, but because customers have different requirements for coating surface density, when the single-sided coating surface density is high, the coating color is darker, and the measurement judgment result grade is often inferior to the measurement result when the single-sided coating surface density is low. The colorimetric card is not accurate for products with different coating surface density levels.

[0104] Comparative Example 3

[0105] Comparison of this test method with the 100-grid method for shedding testing.

[0106] When using the 100-grid method, the 100-grid knife scratches the coating and the substrate together, causing the material itself to be torn and broken when the tape is used to adhere it. The measurement process is terminated and the measurement fails.

[0107] Comparative Example 4

[0108] The peel strength was tested using a tensile testing machine.

[0109] The test process is load-intensive and time-consuming.

[0110] It should be noted that, in this document, the terms "comprises," "includes," or any other variations thereof are intended to encompass non-exclusive inclusion, such that a process, method, article, or apparatus comprising a series of elements includes not only those elements but also other elements not explicitly listed, or elements inherent to such process, method, article, or apparatus. In the absence of further limitations, an element defined by the phrase "comprising a ..." does not exclude the presence of other identical elements in the process, method, article, or apparatus comprising the element.

[0111] Through the description of the above embodiments, those skilled in the art can clearly understand that the above-mentioned embodiment methods can be implemented by means of software plus the necessary general hardware platform, and of course can also be implemented by hardware, but in many cases the former is a better embodiment. Based on this understanding, the technical solution of the present invention, or the part that contributes to the prior art, can be embodied in the form of a software product, which is stored in a storage medium (such as ROM / RAM, magnetic disk, optical disk), and includes a number of instructions for enabling a terminal (which can be a mobile phone, computer, server, air conditioner, or network device, etc.) to execute the methods described in each embodiment of the present invention.

[0112] The above disclosure is merely a preferred embodiment of the present invention and certainly cannot be used to limit the scope of the present invention. Therefore, equivalent changes made according to the claims of the present invention are still within the scope of the present invention.

Claims

1. A method for detecting the adhesion of a coating on a substrate surface, characterized in that: The detection method comprises the following steps: Step S1: obtaining in advance the single-side coating density of the sample to be measured and the mass of a 3M tape of a preset length; Step S2, sticking the 3M tape on the surface of the sample to be measured, and peeling the 3M tape upward at a preset speed after rolling; Step S3, cutting the 3M tape with the coating adhered thereto into fixed specifications, weighing the 3M tape with fixed specifications, and calculating the difference in mass between the 3M tape before and after adhesion; Step S4: Calculate the area of ​​the 3M tape of fixed specifications after adhesion, obtain the adhesion mass per unit area based on the area, compare the adhesion mass with the single-side coating surface density of the sample to be measured to obtain a comparison result, and use the comparison result to evaluate the adhesion of the sample to be measured.

2. The method for detecting adhesion of a substrate surface coating according to claim 1, wherein: In the step S1, the thickness of the sample to be measured is 5um-100um.

3. The method for detecting adhesion of a substrate surface coating as claimed in claim 1, wherein: In step S1, the surface density of the coating on one side of the sample to be measured is 0.1 to 2.0 g / m 2 .

4. The method for detecting adhesion of a substrate surface coating as claimed in claim 1, wherein: In step S1, the 3M tape itself has a consistent width and uniform quality.

5. The method for detecting adhesion of a substrate surface coating as claimed in claim 1, wherein: The step S2 specifically includes the following steps: Step S21: Before adhering the 3M tape, fold the starting end of the 3M tape by 0.5 cm to form a hand-grip point for subsequently tearing off the 3M tape; Step S22: When the 3M tape is adhered, the 3M tape is gradually unfolded and adhered to the surface of the sample to be measured using a synchronous progressive adhesion method; Step S23: Select a roller with a fixed mass to roll along the glue-applying direction; wherein, during the rolling process, no pressure is applied to the roller in a direction perpendicular to the surface of the sample to be measured; Step S24: Before peeling off the 3M tape, hold the 3M tape at the fulcrum point and tear off the 3M tape at an average speed of 5 mm / s in a fixed direction.

6. The method for detecting adhesion of a substrate surface coating as claimed in claim 5, wherein: The fixed direction is the direction when the force point is 60°, 90° or 180° to the surface of the sample to be measured.

7. The method for detecting adhesion of a substrate surface coating according to claim 6, wherein: The roller is a handheld tape rolling roller; wherein, the pressure of the roller is 1.5-2.5 kgf, and the speed of the roller is 5-15 mm / s.

8. The method for detecting adhesion of a substrate surface coating as claimed in claim 1, wherein: The 3M tape is a transparent tape with a width of 12mm-35mm.

9. The method for detecting adhesion of a substrate surface coating as claimed in claim 1, wherein: In step S3, the 3M tape of fixed specifications is weighed using an analytical balance; wherein the analytical balance has a sensitivity of 0.0001 g.

10. The method for detecting adhesion of a substrate surface coating according to claim 1, wherein: In step S4, the comparison result is used to evaluate the adhesion of the surface coating of the sample to be measured by the ratio η, which satisfies the following conditions: Wherein, S represents the area of ​​the 3M tape, ρ represents the surface density of the coating on one side of the sample to be measured, and ΔM represents the difference in mass before and after the 3M tape is adhered.

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