Method for Measuring the Bonding Strength of Ceramic Films

Abstract

The present invention discloses a method for measuring the bonding strength of a ceramic thin film. First, multiple layers are stacked to obtain a Ba block. The last layer of the Ba block is stacked according to the second stacking pressure, and the other layers are stacked according to the first stacking pressure. Then, a ceramic thin film is stacked on one side of the Ba block according to the third stacking pressure, and the second, first, and third stacking pressures decrease in sequence. Then, an adhesive tape is pasted on the ceramic thin film. Both ends of the adhesive tape in the first direction protrude outside the Ba block, and one end in the second direction protrudes outside the Ba block to form a connection end. A tensiometer is connected to the connection end and the tensiometer forms an angle with the surface of the Ba block. Then, the tensiometer is pulled uniformly until the ceramic thin film completely falls off the Ba block, and the tensile force value displayed by the tensiometer is recorded to obtain the bonding strength of the ceramic thin film. This method can quantify the bonding strength data of the ceramic thin film, facilitate the comparison of the bonding strengths of ceramic thin films produced by different formulations, and improve the development efficiency of the slurry for new specification products.

Description

Technical Field

[0001] The present invention relates to the technical field of peel strength testing, and particularly to a method for measuring the bonding strength of ceramic films. Background Art

[0002] Ceramic films are a type of ceramic material made by special process technology with a thickness of less than a few micrometers while still maintaining the excellent properties of ceramics. They can be used to manufacture large-capacity thin-film devices. For example, High Temperature Co-fired Ceramic (HTCC), Low Temperature Co-fired Ceramic (LTCC), Multi-layer Ceramic Capacitors (MLCC), etc. all use ceramic films in the production process.

[0003] Among them, the processes of HTCC and LTCC are basically the same. Their typical process flows include green tape casting, cutting, punching, hole filling printing, lamination, firing, etc. The only difference is that due to the different materials selected, the sintering temperatures are different. HTCC is generally sintered at a high temperature above 1500°C, and LTCC is generally sintered at a temperature below 1000°C. The manufacturing process of MLCC is to stack ceramic film sheets printed with internal electrodes in a cross-misaligned manner to form a block, then cut and separate them into ceramic green bodies in alignment, and form a monolithic-like structure through a one-time high-temperature sintering to form a ceramic blank, and then prepare three or more layers of metal outer electrodes (end electrodes) at both ends of the ceramic blank.

[0004] The performances and requirements of the ceramic films required in the above-mentioned HTCC, LTCC, MLCC, and other components are different. Correspondingly, ceramic films produced from different materials also have different performance and bonding strength parameters. Among them, the evaluation of the bonding strength of ceramic films is of great significance for their production. At present, the methods for evaluating the bonding strength of ceramic films in the industry often rely on the product results of the subsequent processes and cannot obtain the specific numerical value of the bonding strength, which has a greater impact on the development test efficiency of the slurry formula for new specification ceramic films.

[0005] Therefore, it is necessary to provide a method that can quantify the bonding strength data of ceramic films to provide guidance for the development of new specification ceramic film formulas. Summary of the Invention

[0006] The purpose of the present invention is to provide a method that can quantify the bonding strength data of ceramic films to provide guidance for the development of new specification ceramic film formulas.

[0007] To achieve the above object, the technical solution of the present invention is: to provide a method for measuring the bonding strength of a ceramic film, which includes the following steps:

[0008] (1) Use a laminator to laminate the film sheets multiple times according to the first lamination pressure, and then laminate the last film sheet according to the second lamination pressure to obtain a Ba block with a certain thickness, wherein the first lamination pressure is less than the second lamination pressure;

[0009] (2) Use a laminator to stack a layer of ceramic film on the last film sheet of the Ba block according to the third lamination pressure, wherein the third lamination pressure is less than the first lamination pressure;

[0010] (3) Paste an adhesive tape on the ceramic film. Both ends of the adhesive tape protrude outside the Ba block in the first direction, and one end of the adhesive tape protrudes outside the Ba block in the second direction to form a connection end, wherein the first direction intersects with the second direction;

[0011] (4) Connect the hook of the tensiometer to the connection end, then make the tensiometer form an angle with the surface of the Ba block, and zero the tensiometer;

[0012] (5) Pull the tensiometer at a constant speed and keep the angle between the tensiometer and the surface of the Ba block unchanged until the entire ceramic film falls off the Ba block, and record the minimum and maximum tensile force values displayed by the tensiometer.

[0013] Preferably, the first lamination pressure is 12000 kgf ≤ F1 ≤ 20000 kgf, and the second lamination pressure is 20000 kgf < F2 ≤ 40000 kgf. By using a larger second lamination pressure to laminate the last film sheet, the purpose is to press the Ba block more tightly to avoid lifting the underlying film sheets of the Ba block during peeling, thereby affecting the measurement results.

[0014] Preferably, the third lamination pressure is 6000 kgf ≤ F3 ≤ 9000 kgf. By using a third lamination pressure smaller than the first lamination pressure to stack the ceramic film, the purpose is to avoid the combination between the ceramic film and the Ba block being too tight, thereby causing damage to the ceramic film during peeling and resulting in measurement failure.

[0015] Preferably, the thickness of the Ba block obtained in step (1) is 200 μm.

[0016] Preferably, in step (3), at least half of the adhesive tape protrudes outside the Ba block in the second direction.

[0017] Preferably, in step (4), the hook of the tensiometer is connected to the middle of the connection end corresponding to the bar block in the first direction, so that the force on the ceramic film is as balanced as possible during the subsequent pulling process.

[0018] Preferably, in step (4), the angle between the tensiometer and the surface of the bar block is 30°-60°, and during the pulling process, a substantially constant angle is maintained.

[0019] Preferably, in step (4), "making the tensiometer form an angle with the surface of the bar block" specifically means: folding the adhesive tape along the first direction, turning the connection end above the ceramic film and forming an angle with the ceramic film.

[0020] Preferably, in step (5), the tensiometer is connected to a driving motor, and the tensiometer is pulled uniformly by the driving motor.

[0021] Compared with the prior art, due to the ceramic film bonding force measurement method of the present invention, first, the diaphragm is laminated multiple times according to the conventional lamination pressure (the first lamination pressure), and then the last diaphragm is laminated according to the second lamination pressure, so as to obtain a bar block with a certain thickness. Then, a layer of ceramic film is stacked on the last diaphragm of the bar block according to the third lamination pressure, wherein the third lamination pressure is less than the first lamination pressure, and the first lamination pressure is less than the second lamination pressure; then, an adhesive tape is pasted on the ceramic film, and both ends of the adhesive tape in the first direction (X-axis direction) protrude outside the bar block, and one end of the adhesive tape in the second direction (Y-axis direction) protrudes outside the bar block to form a connection end; then, the hook of the tensiometer is connected to the connection end, and then the tensiometer forms an angle with the surface of the bar block; next, the tensiometer is pulled uniformly and always maintains the same angle with the surface of the bar block until the ceramic film completely falls off the bar block, and then the minimum and maximum tensile force values displayed by the tensiometer are recorded, so as to obtain the specific numerical range of the bonding force. The ceramic film bonding force measurement method of the present invention can quantify the bonding force data between ceramic films, facilitate the comparison of the bonding forces of ceramic films produced by different formulations, thereby improving the slurry development efficiency of new specification ceramic films, and has positive guiding significance for the development of ceramic film formulations. Description of the Drawings

[0022] Figure 1 is a flowchart of the ceramic film bonding force measurement method of the present invention.

[0023] Figure 2 is a schematic diagram of the state where the bar block and the adhesive tape are bonded in the present invention.

[0024] Figure 3 is Figure 2Schematic diagram of the state where the bonding tape and the bar block form an angle. Detailed implementation manners

[0025] Now, embodiments of the present invention will be described with reference to the accompanying drawings, in which like reference numerals represent like elements. It should be noted that the orientation descriptions involved in the present invention, such as up, down, left, right, front, back, etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings. This is only for the convenience of describing the technical solutions of the present application or / and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation. Therefore, it should not be construed as a limitation to the present application. The first, second, etc. described are only used to distinguish technical features and cannot be understood as indicating or implying relative importance or implicitly indicating the quantity of the indicated technical features or implicitly indicating the sequence of the indicated technical features.

[0026] First, refer to Figure 1 As shown, the method for measuring the bonding strength of ceramic films provided by the present invention is mainly used to quantify the bonding strength data of ceramic films to provide guidance for the development of slurry formulations for new specification products. However, this method is not limited to the measurement of the bonding strength of ceramic films. It can of course also be used for other similar products to test the bonding strength / peeling strength.

[0027] Next, in combination with Figures 1 - 3 As shown, the method for measuring the bonding strength of ceramic films of the present invention will be described in detail. In a preferred implementation manner of this method, the following steps are included:

[0028] S01. Use a laminator to laminate the film sheets multiple times according to the first lamination pressure, and then laminate the last film sheet according to the second lamination pressure to obtain a bar block with a certain thickness. Among them, the last film sheet is the uppermost film sheet of the bar block, and the first lamination pressure is less than the second lamination pressure;

[0029] In a specific implementation manner, the first lamination pressure is the normal pressure for laminating the bar block. The range of this first lamination pressure is preferably 12000 kgf ≤ F1 ≤ 20000 kgf; while the range of the second lamination pressure is preferably 20000 kgf < F2 ≤ 40000 kgf; the purpose of laminating the last film sheet with a larger second lamination pressure is to press the bar block 100 more tightly to avoid lifting the underlying several film sheets of the bar block 100 during peeling, thereby affecting the measurement results. It can be understood that the range values of the first lamination pressure F1 and the second lamination pressure F2 are not limited to this and can be flexibly set according to needs.

[0030] In combination with Figures 2 - 3As shown, the obtained bar block 100 can be rectangular, square or other shapes, which are not specifically limited herein. In this specific embodiment, the obtained bar block 100 is generally rectangular, and the thickness h of the bar block 100 is approximately 200 μm. Of course, it is not limited to this thickness, and the thickness of the bar block 100 can be flexibly selected and stacked according to specific products and test requirements.

[0031] S02. Use a laminator to stack a layer of ceramic film onto the uppermost film of the bar block according to the third lamination pressure, where the third lamination pressure is less than the first lamination pressure;

[0032] In the present invention, the material of the ceramic film can be the same as or different from the film in the above step S01, which is not specifically limited herein. In a specific embodiment, the ceramic film and the above film are preferably of the same material.

[0033] In a specific embodiment, the range of the third lamination pressure is preferably 6000 kgf ≤ F3 ≤ 9000 kgf. Using a third lamination pressure less than the first lamination pressure to stack the ceramic film aims to prevent the combination between the ceramic film and the bar block 100 from being too tight, thereby causing the ceramic film to be damaged during peeling and resulting in measurement failure. Of course, the range of the third lamination pressure F3 is not limited to that in this embodiment and can be flexibly set according to needs.

[0034] S03. Paste an adhesive tape on the ceramic film. Both ends of the adhesive tape protrude outside the bar block in the first direction, and one end of the adhesive tape protrudes outside the bar block in the second direction to form a connection end, where the first direction intersects with the second direction;

[0035] See Figure 2 As shown, in a specific embodiment, the first direction (X-axis direction) and the second direction (Y-axis direction) are two perpendicular directions, and the bar block 100 is generally rectangular in structure. The width of the bar block 100 is along the first direction (X-axis direction), and the length of the bar block 100 is along the second direction (Y-axis direction).

[0036] Continue to see Figure 2As shown, the length of the bonding tape 200 extends along the first direction (X-axis direction), and the width of the bonding tape 200 extends along the second direction (Y-axis direction). And the bonding tape 200 is flatly attached to one side edge of the bar block 100. Specifically, the bonding tape 200 is attached to the ceramic film of the bar block 100. At the same time, both ends of the bonding tape 200 in the length direction (X-axis direction) are longer than the width of the bar block 100. In other words, both ends of the bonding tape 200 in the length direction protrude outside the bar block 100; while in the width direction (Y-axis direction) of the bonding tape 200, less than or equal to half of its width is bonded to the ceramic film, and greater than or equal to half of its width protrudes outside the bar block 100. Preferably, half of the width of the bonding tape 200 in the width direction is bonded to the ceramic film, and the other half protrudes outside the bar block 100, as Figures 2 - 3 shown. Therefore, with the straight line L where the edge of the bar block 100 is located as the boundary, half of the bonding tape 200 bonded to the ceramic film forms a fixed end 220, and the half of the bonding tape 200 that protrudes outside the bar block 100 forms a connection end 210, as Figure 2 shown.

[0037] In the present invention, the bonding tape 200 is preferably a tape, but it is not limited thereto. Of course, other adhesive layer-like or film-like products can be selected according to needs to facilitate pasting the ceramic film and tearing off the ceramic film.

[0038] S04. Connect the hook of the tensiometer to the connection end, then make the tensiometer form an angle with the surface of the bar block, and zero the tensiometer;

[0039] Continue to refer to Figure 2 shown. In a preferred embodiment, the position corresponding to the middle of the bar block 100 in the width direction of the connection end 210 is set as the connection point P. Specifically, the connection point P corresponds to the middle of the bar block 100 in the width direction, rather than the middle of the bonding tape 200 in the length direction, because the parts of the two ends of the bonding tape 200 in the length direction protruding outside the bar block 200 are not specifically limited and are not necessarily equal. Connect the hook of the tensiometer 300 to the connection point P. The purpose of such connection is to make the force on the ceramic film as balanced as possible. Among them, the connection method between the hook of the tensiometer 300 and the connection end 210 is a conventional method.

[0040] Combined with Figures 2 - 3 shown, fold the bonding tape 200 along the first direction (X-axis direction). Specifically, fold the connection end 210 of the bonding tape 200 along the straight line L where the edge of the bar block 100 is located, as Figure 2 shown, so that the connection end 210 is folded above the ceramic film and forms a certain angle a, as Figure 3As shown, the included angle a is preferably 30°-60°. Of course, the included angle a can be other angles according to needs.

[0041] In a specific embodiment, the included angle a between the connecting end 210 and the ceramic film is 45°, that is, the angle between the tensiometer 300 and the surface of the bar 100 is 45°, as Figure 3 shown.

[0042] S05. Pull the tensiometer at a constant speed and keep the included angle between the tensiometer and the surface of the bar unchanged until all the ceramic film falls off the bar, and record the minimum and maximum tensile force values shown on the tensiometer.

[0043] In a preferred embodiment, the tensiometer 300 is connected to a driving motor 400, and the driving motor 400 is used to pull the tensiometer 300 at a constant speed to ensure the balanced force on the tensiometer 300. At the same time, during the process of pulling the tensiometer 300, the included angle a between the tensiometer 300 and the surface of the bar 100 is always kept substantially unchanged. For example, it is always kept at an included angle of 45°. Of course, it is not limited to keeping an included angle of 45°, and this angle can be adjusted flexibly according to needs.

[0044] It can be understood that it is not limited to pulling the tensiometer 300 by the driving motor 400. For example, in other embodiments, the speed of the tensiometer 300 can also be controlled by the stopwatch countdown method.

[0045] When all the ceramic film completely falls off the bar 100, record the minimum and maximum tensile force values shown on the tensiometer 300. The range of the minimum and maximum tensile force values is the range value of the bonding force of the ceramic film.

[0046] Next, with reference to Figures 1 - 3 shown, the specific embodiments of using the ceramic film bonding force measurement method of the present invention to measure the bonding force of ceramic films produced by different formulations will be described.

[0047] Taking the ceramic films produced by two formulations A and B as an example, the bars 100 are obtained by laminating in the same manner and pressure. In a specific embodiment, a laminator is used to laminate at a first lamination pressure of 12000 kgf respectively, and the last layer is laminated with a second lamination pressure of 35000 kgf for the film sheets. Finally, two bars 100 with a thickness of about 200 μm are obtained respectively, which are respectively referred to as the first bar and the second bar here. Then, a layer of ceramic film is laminated on the uppermost film sheet of the first bar and the second bar respectively with a third lamination pressure of 9000 kgf. Here, the ceramic film is preferably of the same material as the film sheet, and the ceramic film produced by formulation A is laminated on the first bar, and the ceramic film produced by formulation B is laminated on the second bar.

[0048] Next, paste the bonding tape 200 on the ceramic film of the first bar block. The length direction of the bonding tape 200 is perpendicular to the length direction of the first bar block. That is, the length direction of the bonding tape 200 extends along the width direction of the first bar block, and both ends in the length direction of the bonding tape 200 are longer than the width of the first bar block. In the width direction of the bonding tape 200, half is pasted on the ceramic film and the other half protrudes outside the first bar block. Therefore, the bonding tape 200 is divided into two in the width direction. One half forms a fixed end 220 pasted on the first bar block, and the other half forms a connecting end 210 protruding outside the first bar block. Specifically, refer to Figure 2 as shown.

[0049] Then, paste the bonding tape 200 on the second bar block in the same manner as above.

[0050] Next, first connect the hook of the tensiometer 300 to the bonding tape 200 of the first bar block. Specifically, the hook is connected to the connection point P on the connecting end 210, and this connection point P corresponds to the middle part in the width direction of the first bar block. Then fold the connecting end 210 of the bonding tape 200 along the X-axis direction. Specifically, fold the connecting end 210 of the bonding tape 200 along the straight line L where the edge of the bar block 100 is located. As Figure 2 shown, so that the connecting end 210 is folded above the ceramic film and forms a 45° angle, so that the tensiometer 300 forms a 45° angle with the surface of the first bar block. As Figure 3 shown, and then zero the tensiometer 300.

[0051] Next, connect the tensiometer 300 to a driving motor 400. The driving motor 400 pulls the tensiometer 300 at a constant speed. During the pulling process, always keep the tensiometer 300 forming a 45° angle with the surface of the first bar block 100. The tensiometer 300 pulls the ceramic film through the bonding tape 200. When all the ceramic film falls off the first bar block, the measurement ends. Record the maximum and minimum values displayed by the tensiometer 300 during the measurement process. In this embodiment, for the ceramic film on the first bar block (that is, the ceramic film produced by A formula), the measured corresponding bonding force is 0.33 - 0.37 mN.

[0052] For the ceramic film produced by B formula on the second bar block, measure it in the same way as the first bar block, and the obtained bonding force is 0.06 - 0.08 mN.

[0053] Through the above process, it can be seen that through the method of the present invention, the bonding force data between ceramic films produced by different matching parties can be quantified, which has positive significance for the development of ceramic film formulas.

[0054] In summary, in the method for measuring the bonding strength of the ceramic film of the present invention, first, the diaphragm is laminated multiple times according to the conventional lamination pressure (the first lamination pressure), and then the last diaphragm is laminated according to the second lamination pressure, so as to obtain a Ba block 100 with a certain thickness. Then, a layer of ceramic film is stacked on the last diaphragm of the Ba block 100 according to the third lamination pressure, wherein the third lamination pressure is less than the first lamination pressure, and the first lamination pressure is less than the second lamination pressure. Then, an adhesive tape 200 is pasted on the ceramic film. Both ends of the adhesive tape 200 protrude out of the Ba block 100 in the first direction (X-axis direction), and one end of the adhesive tape 200 protrudes out of the Ba block 100 in the second direction (Y-axis direction) to form a connection end 210. Then, the hook of the tensiometer 300 is connected to the connection end 210, and then the tensiometer 300 forms an angle with the surface of the Ba block 100. Next, the tensiometer 300 is pulled uniformly and always kept at the same angle with the surface of the Ba block 100 until the ceramic film completely falls off the Ba block 100, and then the minimum tensile value and the maximum tensile value displayed by the tensiometer 300 are recorded, so as to obtain the specific numerical range of the bonding strength. The method for measuring the bonding strength of the ceramic film of the present invention can quantify the bonding strength data between the ceramic films, facilitate the comparison of the bonding strengths of the ceramic films produced by different formulations, thereby improving the slurry development efficiency of the ceramic films of new specifications, and has positive guiding significance for the development of the ceramic film formulations.

[0055] The foregoing disclosure is only the preferred embodiment of the present invention, and of course cannot be used to limit the scope of rights of the present invention. Therefore, equivalent changes made according to the scope of the patent application of the present invention still fall within the scope covered by the present invention.

Claims

1. A method for measuring the bonding strength of a ceramic thin film, characterized in that, it comprises the following steps: (1) Use a laminator to laminate the diaphragm multiple times according to the first lamination pressure, and then laminate the last diaphragm according to the second lamination pressure to obtain a Ba block with a certain thickness, wherein the first lamination pressure is less than the second lamination pressure; (2) Use a laminator to stack a layer of ceramic thin film onto the last diaphragm of the Ba block according to the third lamination pressure, wherein the third lamination pressure is less than the first lamination pressure; (3) Paste an adhesive tape on the ceramic thin film, both ends of the adhesive tape in the first direction protrude outside the Ba block, and one end of the adhesive tape in the second direction protrudes outside the Ba block to form a connection end, wherein the first direction intersects with the second direction; (4) Connect the hook of a tensiometer to the connection end, then make the tensiometer form an angle with the surface of the Ba block, and zero the tensiometer; (5) Pull the tensiometer at a constant speed and keep the angle between the tensiometer and the surface of the Ba block unchanged until the ceramic thin film completely falls off the Ba block, and record the minimum and maximum tensile force values displayed by the tensiometer.

2. The method for measuring the bonding strength of a ceramic thin film according to claim 1, characterized in that, the first lamination pressure is 12000 kgf ≤ F1 ≤ 20000 kgf, and the second lamination pressure is 20000 kgf < F2 ≤ 40000 kgf.

3. The method for measuring the bonding strength of a ceramic thin film according to claim 1, characterized in that, the third lamination pressure is 6000 kgf ≤ F3 ≤ 9000 kgf.

4. The method for measuring the bonding strength of a ceramic thin film according to claim 1, characterized in that, the thickness of the Ba block obtained in step (1) is 200 μm.

5. The method for measuring the bonding strength of a ceramic thin film according to claim 1, characterized in that, in step (3), at least half of the adhesive tape in the second direction protrudes outside the Ba block.

6. The method for measuring the bonding strength of a ceramic thin film according to claim 1, characterized in that, in step (4), the hook of the tensiometer is connected to the middle part of the connection end corresponding to the Ba block in the first direction.

7. The method for measuring the bonding strength of a ceramic thin film according to claim 1, characterized in that, the angle between the tensiometer and the surface of the Ba block in step (4) is 30° - 60°.

8. The method for measuring the bonding strength of a ceramic thin film according to claim 1 or 7, characterized in that, "making the tensiometer form an angle with the surface of the Ba block" in step (4) specifically means: folding the adhesive tape along the first direction, turning the connection end over above the ceramic thin film and forming an angle with the ceramic thin film.

9. The method for measuring the bonding strength of a ceramic thin film according to claim 1, characterized in that, in step (5), the tensiometer is connected to a driving motor, and the driving motor is used to pull the tensiometer at a constant speed.

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