Quantitative test method for silicon transfer of silica gel protective film

Abstract

The invention discloses a quantitative test method for silicon transfer of a silica gel protective film, and relates to the technical field of silicon transfer detection. The method comprises the following steps: taking a pasted object sample with a flat and clean surface, measuring a water drop angle on the surface of the pasted object sample by using a water drop angle measuring instrument, and recording the water drop angle as theta 0; attaching the to-be-tested silica gel protective film to the surface of the to-be-attached object sample, and placing the to-be-tested silica gel protective film for a preset time after attaching is completed; after the standing time is over, tearing off the silica gel protective film to be measured, and measuring a water drop angle on the surface of the attached object sample by using a water drop angle measuring instrument, and recording the water drop angle as theta1; s4, calculating the silicon transfer amount of the to-be-detected silica gel protective film according to the water drop angle change value delta theta = theta 1-theta 0 on the surface of the attached object sample. According to the invention, accurate quantitative evaluation of the silicon transfer degree is realized. By comparing the difference between the initial water drop angle before fitting and the water drop angle after tearing, the silicon transfer amount can be directly correlated, the trace silicon transfer which is originally difficult to detect is converted into quantifiable data, and the detection sensitivity and accuracy are remarkably improved.

Description

Technical Field

[0001] The present invention relates to the technical field of silicon transfer quantitative testing, and in particular to a method for quantitative testing silicon transfer of a silicone protective film. Background Art

[0002] In modern industrial production, silicone protective films are widely used in a wide range of fields, including electronics, display panels, hardware, and automotive manufacturing, thanks to their excellent temperature resistance, chemical stability, and good adhesion. In electronic device manufacturing, silicone protective films are often used to protect precision components such as screens and chips, preventing scratches and contamination during processing, transportation, and storage. In the optical field, silicone protective films are used to protect optical lenses, ensuring their surface finish and optical performance are not compromised.

[0003] However, a key issue with silicone protective films in practical applications is silicon transfer, which occurs when they come into contact with the surface being applied. This silicon transfer forms a very thin layer of silicon residue on the surface of the object being applied. During subsequent processing steps such as bonding electronic components, impurities produced by silicon transfer can reduce adhesion, leading to quality issues such as product detachment, significantly impacting product yield. In the manufacture of optical lenses, silicon transfer can also alter the optical properties of the lens surface, causing abnormal refraction and reflection of light, and compromising image quality.

[0004] Currently, the industry primarily relies on X-ray fluorescence (XRF) analyzers to detect silicon transfer. However, because the amount of silicon transfer is extremely small, typically measured in micrograms per square centimeter or even lower, X-ray fluorescence analyzers are limited by their precision and struggle to accurately detect such trace amounts, hindering reliable data support for production and quality control. Therefore, developing a quantitative test method that can accurately and efficiently evaluate silicon transfer in silicone protective films has become a critical technical challenge that needs to be addressed, crucial for ensuring product quality and improving production efficiency. Summary of the Invention

[0005] The technical problem to be solved by the present invention is to provide a quantitative testing method that can accurately and efficiently evaluate the silicon transfer of a silicone protective film.

[0006] In order to solve the above problems, the present invention proposes the following technical solutions:

[0007] The present invention provides a method for quantitatively testing silicon transfer of a silicone protective film, comprising the following steps:

[0008] S1. Take a sample with a flat and clean surface and use a water drop angle measuring instrument to measure the water drop angle on the surface of the sample, which is recorded as θ0;

[0009] S2. Attach the silicone protective film to be tested to the surface of the sample at a preset bonding pressure and bonding speed. After bonding is completed, leave it for a preset time;

[0010] S3. After the placement time is over, the silicone protective film to be tested is evenly peeled off from the surface of the attached sample at a preset peeling speed, and the water drop angle on the surface of the attached sample after the peeling is measured with a water drop angle measuring instrument, which is recorded as θ1;

[0011] S4. Calculate the amount of silicon transferred from the silicone protective film to be tested based on the change in the water drop angle on the surface of the sample being applied. The change in the water drop angle is denoted as Δθ, where Δθ = |θ1 - θ0|. The amount of silicon transferred is positively correlated with the change in the water drop angle Δθ.

[0012] A further technical solution is that step S4 specifically includes:

[0013] Δθ<30°, it is determined that the silicon transfer amount of the silicone protective film to be tested is low transfer;

[0014] 30°≤Δθ≤50°, the silicon transfer amount of the silicone protective film to be tested is determined to be medium transfer;

[0015] If Δθ>50°, the silicon transfer amount of the tested silicone protective film is determined to be high.

[0016] A further technical solution is that the steps S1 and S3 include randomly selecting three or more measuring points on the surface of the object sample to test the water drop angle, and taking the average of the water drop angles of all the measuring points as the final result.

[0017] A further technical solution is that the test environments of steps S1 and S3 are the same.

[0018] A further technical solution is that the test environment of steps S1 and S3 is: temperature 23±2° C., relative humidity 55±5%.

[0019] A further technical solution is that the water drop angle measuring instrument has an accuracy of ±0.1°.

[0020] A further technical solution is that the temperature during lamination is room temperature and the lamination pressure is 0.01 to 8.0 MPa.

[0021] A further technical solution is that in step S2, the preset placement time is 30 minutes or more.

[0022] A further technical solution is that in step S2, the placement temperature is -20°C to 120°C.

[0023] A further technical solution is that the object to be adhered includes copper foil tape, high molecular polymer film material, and glass plate.

[0024] The high molecular polymer film material includes PE, PET, CPP, PVC, OPP and the like.

[0025] The surface of the object to be attached includes the nickel-plated surface of the copper foil tape, the corona-treated surface of the PET film, the glass surface, etc.

[0026] A further technical solution is that the structure of the silicone protective film consists of a substrate layer, a silicone pressure-sensitive layer and a release film layer from bottom to top; the thickness of the silicone pressure-sensitive layer is 10 to 1000 μm.

[0027] The thickness of the base layer is 10 to 360 μm, and the thickness of the protective layer is 10 to 360 μm.

[0028] The material of the substrate layer is one of BOPP, BOPET, BOPA, PET, PE, PC, TAC, PP, PS, PMMA, TPU, PI, PVB, and PVC.

[0029] The material of the release film layer is one of BOPP, BOPET, BOPA, PET, PE, PC, TAC, PP, PS, PMMA, TPU, PI, PVB, PVC, non-silicone protective film, and fluorine release film.

[0030] The principle of the present invention is: when the silicone protective film comes into contact with the object to be adhered, silicon transfer may occur, resulting in changes in the chemical composition and microstructure of the surface of the object to be adhered. This change will directly affect the surface energy of the object to be adhered, and the difference in surface energy can be intuitively reflected through the indicator of water drop angle. Specifically, the water drop angle reflects the wetting characteristics of the liquid on the solid surface. When silicon transfer occurs, the change in the surface energy of the object to be adhered will significantly affect the value of the water drop angle. Based on this characteristic, the present invention measures the change in the water drop angle on the surface of the object to be adhered before and after the silicone protective film is adhered, thereby achieving a quantitative assessment of the degree of silicon transfer. By comparing the difference between the initial water drop angle before adhesion and the water drop angle after tearing off the protective film, the surface energy change caused by silicon transfer can be accurately captured, thereby providing a reliable basis for the quality control of the silicone protective film. The method of the present invention converts the microscopic silicon transfer phenomenon into quantifiable and analyzable data through simple water drop angle measurement, effectively solving the problem that traditional detection technology is difficult to accurately assess trace silicon transfer.

[0031] Compared with the prior art, the present invention can achieve the following technical effects:

[0032] The present invention provides a quantitative testing method for silicon transfer from silicone protective films. By measuring the change in the water drop angle on the surface of the object before and after the silicone protective film is applied, the degree of silicon transfer can be accurately and quantitatively assessed. When the silicone protective film comes into contact with the object, silicon transfer alters the chemical composition and microstructure of the surface, thereby affecting its surface energy properties. The water drop angle, as a direct indicator of surface energy, can sensitively reflect this change. By comparing the difference between the initial water drop angle before application and the water drop angle after removal, the amount of silicon transfer can be directly correlated. This converts the previously difficult-to-detect trace silicon transfer into quantifiable data, significantly improving detection sensitivity and accuracy.

[0033] The method for quantitatively testing silicon transfer on silicone protective films provided by this invention is simple to operate and requires no complex instrumentation or destructive testing. Testing can be completed with a conventional water drop angle measuring instrument, effectively reducing technical barriers and testing costs. Furthermore, by presetting lamination and peeling parameters and environmental conditions, it can simulate actual production scenarios, ensuring that test results closely align with actual process requirements. This method provides a reliable basis for quality control and process optimization of silicone protective films, and has broad applicability and practical value. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for use in the description of the embodiments. Obviously, the drawings described below are 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.

[0035] Figure 1 Flowchart of the quantitative testing method for silicon transfer of a silicone protective film provided in an embodiment of the present invention. DETAILED DESCRIPTION

[0036] The following will be combined with the accompanying drawings of the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments. Similar component numbers in the drawings represent similar components. Obviously, the embodiments described below are only some of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0037] It will be understood that when used in this specification and the appended claims, the terms “comprises” and “comprising” indicate the presence of described features, integers, steps, operations, elements and / or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components and / or groups thereof.

[0038] It should also be understood that the terms used in this description of the embodiments of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the embodiments of the present invention. As used in the description of the embodiments of the present invention and the appended claims, the singular forms "a", "an", and "the" are intended to include the plural forms unless the context clearly indicates otherwise.

[0039] See also Figure 1 , which is a flow chart of the quantitative testing method for silicon transfer of a silicone protective film provided by an embodiment of the present invention. As can be seen from the figure, the quantitative testing method for silicon transfer of a silicone protective film provided by this embodiment includes the following steps:

[0040] S1. Take a sample with a flat and clean surface and use a water drop angle measuring instrument to measure the water drop angle on the surface of the sample, which is recorded as θ0;

[0041] S2. Attach the silicone protective film to be tested to the surface of the sample at a preset bonding pressure and bonding speed. After bonding is completed, leave it for a preset time;

[0042] S3. After the placement time is over, the silicone protective film to be tested is evenly peeled off from the surface of the attached sample at a preset peeling speed, and the water drop angle on the surface of the attached sample after the peeling is measured with a water drop angle measuring instrument, which is recorded as θ1;

[0043] S4. Calculate the amount of silicon transferred from the silicone protective film to be tested based on the change in the water drop angle on the surface of the sample being applied. The change in the water drop angle is denoted as Δθ, where Δθ = |θ1 - θ0|. The amount of silicon transferred is positively correlated with the change in the water drop angle Δθ.

[0044] In a specific embodiment, step S4 specifically includes:

[0045] Δθ<30°, it is determined that the silicon transfer amount of the silicone protective film to be tested is low transfer;

[0046] 30°≤Δθ≤50°, the silicon transfer amount of the silicone protective film to be tested is determined to be medium transfer;

[0047] If Δθ>50°, the silicon transfer amount of the tested silicone protective film is determined to be high.

[0048] This embodiment uses clear grading standards to transform the abstract concept of silicon transfer into an intuitive, quantifiable rating. Users can quickly determine the suitability of silicone protective films based on specific application scenarios. For example, a high transfer rating indicates that the film may affect subsequent processing quality, providing a direct basis for material screening and process adjustments, improving the efficiency and pertinence of quality control.

[0049] In a specific embodiment, steps S1 and S3 include randomly selecting three or more measuring points on the surface of the object sample to test the water drop angle, and taking the average of the water drop angles of all the measuring points as the final result.

[0050] This embodiment uses multi-point measurement to eliminate interference from local surface variations or accidental errors. For example, the surface of nickel-plated copper foil may have slight undulations, which can easily lead to deviations from a single measurement point. The multi-point averaging method can more accurately reflect the overall silicon transfer situation, significantly improving the representativeness and reliability of the data and ensuring the objectivity of the measurement results.

[0051] In this specific embodiment, the test environment in steps S1 and S3 is identical. Temperature and humidity fluctuations can cause slight fluctuations in the surface energy of the object being bonded. Environmental consistency ensures comparability of pre- and post-bonding data, avoiding additional errors introduced by varying conditions and thus improving the stability and repeatability of test results. This embodiment rigorously controls experimental variables to minimize the impact of environmental fluctuations on water droplet angle measurement, ensuring the accuracy of measurement results.

[0052] In a specific embodiment, the test environment in steps S1 and S3 is standardized to establish a unified testing benchmark: temperature of 23±2°C and relative humidity of 55±5%. This test environment simulates the environmental parameters of conventional production or storage, ensuring that the test results are highly consistent with actual application scenarios, providing more valuable data support for process optimization.

[0053] In a specific embodiment, the water drop angle measuring instrument has an accuracy of ±0.1°. This embodiment uses a high-precision instrument to capture subtle changes in the water drop angle. When the amount of silicon transfer is extremely low, Δθ may differ by only a few degrees. High-precision measurement can effectively distinguish such small differences, avoiding misjudgments due to instrument error, thereby significantly improving detection sensitivity and accuracy.

[0054] In a specific embodiment, in step S2, the laminating temperature is room temperature and the laminating pressure is 0.01 to 8.0 MPa. The test method of the present invention has wide versatility and can cover a variety of industrial needs. For example, high-temperature laminating scenarios (such as electronic component packaging) need to simulate actual process conditions, and the laminating pressure can be set according to the coating machine or laminating machine to ensure that the laminating process does not curl or wrinkle, and to avoid bubbles and other appearance defects.

[0055] When using a coating machine or laminating machine for lamination, set an appropriate machine speed, generally 1-50 m / min, to ensure that the lamination appearance is normal and the lamination is completed as quickly as possible to improve test efficiency.

[0056] In a specific embodiment, in step S2, the preset placement time is 30 minutes or more, and the placement temperature is -20°C to 120°C.

[0057] Generally speaking, the object being bonded with the silicone protective film is kept at room temperature (0-35°C). After bonding, the object may be exposed to extreme temperatures (-20°C to 60°C or 120°C) during storage and transportation. Therefore, during testing, the placement environment can be set according to the processing, storage, and usage conditions of the object being bonded.

[0058] For example, placement time can be 1 hour, 2 hours, 8 hours, 24 hours, 10 days, 20 days, 1 month, 3 months, 6 months, 24 months, etc. The placement temperature can be -20°C, -10°C, 0°C, 20°C, 40°C, 50°C, 80°C, 120°C, etc. Understandably, silicon transfer may gradually accumulate over time and temperature, and a placement time that is too short cannot reflect the actual amount of transfer. Extending the placement time can fully assess the stability of the protective film under different usage cycles, avoiding underestimated results due to insufficient testing, thereby improving the comprehensiveness and credibility of the test. During testing, after lamination is completed, placing the film for more than 1 hour helps ensure that the silicon transfer process is fully completed.

[0059] In a specific embodiment, the object to be attached includes copper foil tape, polymer film, and glass plate. The testing method of the present invention is compatible with a variety of materials and can serve the quality inspection needs of cross-industry.

[0060] In a specific embodiment, the silicone protective film structure comprises a substrate layer, a silicone pressure-sensitive layer (10-1000 μm), and a release film layer. Generally speaking, the thickness of the silicone pressure-sensitive layer directly affects adhesion and the risk of silicone transfer. This method is suitable for various types of silicone protective films and is highly versatile.

[0061] In the following examples, the silicon transfer amounts of different silicone protective films were tested under different test conditions according to the above method.

[0062] Example 1

[0063] The parameters involved in the quantitative testing method for silicon transfer of the silicone protective film provided in this embodiment are as follows:

[0064] (1) Surface of the object to be adhered: nickel-plated surface of copper foil tape, size 10cm*10cm; silicone protective film to be tested: commercially available protective film A, B, or C; the size of the object to be adhered is the same as that of the silicone protective film to be tested.

[0065] (2) The test environment temperature was kept constant at 23±2°C and the relative humidity was maintained at 55±5%.

[0066] (3) The temperature during bonding is 23±2°C, the bonding pressure is 0.5 MPa, and the bonding speed is 20 m / min. After bonding is completed, the bonding state is maintained at 23±2°C for 2 hours.

[0067] (4) The silicone protective film is evenly peeled off from the nickel-plated surface of the copper foil tape at a constant peeling speed of 300 mm / min.

[0068] The silicon transfer test results of different silicone protective films in this embodiment are shown in Table 1.

[0069] Table 1 Test results of Example 1

[0070]

[0071] After two hours of application, Type C showed the highest silicon transfer, with a Δθ greater than 50° considered high transfer. Type B showed the second highest, with 30° ≤ Δθ ≤ 50° considered medium transfer. Type A showed the lowest, with a Δθ less than 30° considered low transfer. X-ray fluorescence spectrometry testing of the nickel-plated surfaces of the three copper foil tapes revealed zero silicon content in all three.

[0072] Example 2

[0073] The difference between this embodiment and embodiment 1 is that:

[0074] In parameter (3), the bonding state is maintained at 23±2°C for 7 days and 28 days respectively.

[0075] The silicon transfer test results of different silicone protective films in this embodiment are shown in Table 2.

[0076] Table 2 Test results of Example 2

[0077]

[0078]

[0079] The results in Table 2 show that the amount of silicon transfer gradually accumulates with the extension of the bonding time. The nickel-plated surfaces of the copper foil tapes were tested using an X-ray fluorescence spectrometer, and the silicon content was shown to be 0.

[0080] Example 3

[0081] The difference between this embodiment and embodiment 1 is that:

[0082] In parameter (3), the laminated state was maintained at 80°C and 120°C for 2 hours respectively.

[0083] The silicon transfer test results of different silicone protective films in this embodiment are shown in Table 3.

[0084] Table 3 Test results of Example 3

[0085]

[0086] The results in Table 3 show that the amount of silicon transfer gradually accumulates with the extension of the storage temperature. The nickel-plated surfaces of the copper foil tapes were tested using an X-ray fluorescence spectrometer, and the silicon content was shown to be 0.

[0087] Example 4

[0088] The difference between this embodiment and embodiment 1 is that:

[0089] In parameter (3), the bonding temperature is 23±2°C, the bonding pressure is 6.86 MPa, and the bonding speed is 20 m / min. After bonding is completed, the bonding state is maintained at 23±2°C for 2 hours.

[0090] The silicon transfer test results of different silicone protective films in this example are shown in Table 4.

[0091] Table 4 Test results of Example 4

[0092]

[0093] The results in Table 4 show that as the pressure during bonding increases, the amount of silicon transferred also increases. X-ray fluorescence spectrometer was used to test the nickel-plated surfaces of the copper foil tapes, and both showed that the silicon content was 0.

[0094] Example 5

[0095] The difference between this embodiment and embodiment 1 is that:

[0096] Parameters (1) Surface of the sample to be attached: corona surface of PET film and glass surface.

[0097] The silicone protective film used for the test is type B protective film.

[0098] The silicon transfer test results of different silicone protective films in this example are shown in Table 5.

[0099] Table 5 Test results of Example 5

[0100]

[0101] The nickel-plated surfaces of the copper foil tapes were tested using an X-ray fluorescence spectrometer, and both showed that the silicon content was 0.

[0102] The results of the above examples show that the quantitative testing method for silicon transfer of silicone protective film provided by the present invention is not only applicable to the detection of silicon transfer between the nickel-plated surface of copper foil tape and silicone protective film, but can also be extended to the combination of various other objects and silicone protective films, meeting the testing needs of different industries and products. It has strong versatility and high sensitivity, and can keenly capture tiny silicon transfer, providing a reliable basis for quality monitoring in the production process.

[0103] In the above embodiments, the description of each embodiment has its own focus. For parts that are not described in detail in a certain embodiment, reference can be made to the relevant descriptions of other embodiments.

[0104] The above description is a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any person skilled in the art can easily conceive of various equivalent modifications or substitutions within the technical scope disclosed in the present invention, and such modifications or substitutions are intended to be within the scope of protection of the present invention. Therefore, the scope of protection of the present invention shall be subject to the scope of protection of the claims.

Claims

1. A quantitative test method for silicon transfer of a silicone protective film, characterized in that: The following steps are involved: S1. Take a sample with a flat and clean surface and use a water drop angle measuring instrument to measure the water drop angle on the surface of the sample, which is recorded as θ0; S2. Attach the silicone protective film to be tested to the surface of the sample at a preset bonding pressure and bonding speed. After bonding is completed, leave it for a preset time; S3. After the placement time is over, the silicone protective film to be tested is evenly peeled off from the surface of the attached sample at a preset peeling speed, and the water drop angle on the surface of the attached sample after the peeling is measured with a water drop angle measuring instrument, which is recorded as θ1; S4. Calculate the amount of silicon transferred from the silicone protective film to be tested based on the change in the water drop angle on the surface of the sample being applied. The change in the water drop angle is denoted as Δθ, where Δθ = |θ1 - θ0|. The amount of silicon transferred is positively correlated with the change in the water drop angle Δθ.

2. The method for quantitatively testing silicon transfer of a silicone protective film according to claim 1, wherein: The step S4 specifically includes: Δθ<30°, it is determined that the silicon transfer amount of the silicone protective film to be tested is low transfer; 30°≤Δθ≤50°, the silicon transfer amount of the silicone protective film to be tested is determined to be medium transfer; If Δθ>50°, the silicon transfer amount of the tested silicone protective film is determined to be high.

3. The method for quantitatively testing silicon transfer of a silicone protective film according to claim 1, wherein: The steps S1 and S3 include randomly selecting three or more measuring points on the surface of the object sample to test the water drop angle, and taking the average of the water drop angles of all the measuring points as the final result.

4. The method for quantitatively testing silicon transfer of a silicone protective film according to claim 1, wherein: The test environments of steps S1 and S3 are the same.

5. The method for quantitatively testing silicon transfer of a silicone protective film according to claim 4, wherein: The test environment of steps S1 and S3 is: temperature 23±2° C., relative humidity 55±5%.

6. The method for quantitatively testing silicon transfer of a silicone protective film according to claim 1, wherein: The water drop angle measuring instrument has an accuracy of ±0.1°.

7. The method for quantitatively testing silicon transfer of a silicone protective film according to claim 1, wherein: In the step S2, the lamination temperature is room temperature, and the lamination pressure is 0.01 to 8.0 MPa.

8. The method for quantitatively testing silicon transfer of a silicone protective film according to claim 1, wherein: In step S2, the preset placement time is 30 minutes or more.

9. The method for quantitatively testing silicon transfer of a silicone protective film according to claim 1, wherein: In the step S2, the temperature of the storage is -20°C to 120°C.

10. The method for quantitatively testing silicon transfer of a silicone protective film according to claim 1, wherein: The objects to be attached include copper foil tape, high molecular polymer film material and glass plate.

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