Interface Pull-out Force Test Sample of Adhesive, and Its Preparation Device and Test Method

Abstract

The present invention provides a preparation device for an interface pull-out force test sample of an adhesive, which includes a lower clamp, a substrate, a template, and an upper clamp arranged in sequence from bottom to top. A mold cavity for accommodating the adhesive to form a test sample is provided in the template. One end of the mold cavity communicates with the substrate so that the formed test sample is bonded to the substrate. The preparation device is further configured with a metal connecting member, one end of the metal connecting member is formed as a tip, the metal connecting member is inserted into the mold cavity and the tip is in contact connection with the substrate. Based on the above preparation device, the present invention also provides an interface pull-out force test sample, which includes a substrate, an adhesive pudding mold connected to the substrate, and a metal connecting member inserted into the adhesive pudding mold. The preparation device and the interface pull-out force test sample provided by the present invention can improve the stability and accuracy of the interface pull-out force test of the adhesive.

Description

Technical Field

[0001] The present invention belongs to the technical field of adhesive testing, and particularly relates to an interface pull-out force test sample for an adhesive, a preparation device therefor, and a test method therefor. Background Art

[0002] Adhesives generally consist of resin, curing agent, coupling agent, toughening agent, diluent and other minor additives. Some adhesives also contain inorganic fillers and other components, such as more than 50% silica microspheres in the underfill adhesive for chips. The main function of adhesives is to firmly bond two interfaces together, and they are usually widely used in industries such as electronic packaging, building materials, aerospace, automotive manufacturing, and medical and health.

[0003] The most important parameter of adhesives is the bonding performance, that is, the bonding strength or firmness of the adhesive at the bonding interface. The measurement methods of bonding performance mainly include shear force test and pull-out force test. The one parallel to the bonding material is called shear force, and the one perpendicular to the bonding material direction is called pull-out force.

[0004] Regarding the method for determining the interface pull-out force of adhesives, Chinese Patent Application (Publication No.: CN111257223A) discloses a test device for the pull-out force of soft adhesives. The device first prepares two sample plates with a length of 50 mm, a width of 15 - 20 mm, and a thickness of 2 - 5 mm. The material of the sample plates is plastic or metal. The two sample plates are stacked crosswise, and the cross-contact part is coated with the adhesive to be tested, and then the adhesive is cured under certain curing conditions. During the test, the lower sample plate is fixed with a designed fixture, and then the upper sample plate is clamped with a designed fixture and pulled upward at a rate of 0.5 - 1 mm / min. When the upper sample plate is separated from the adhesive, the pull-out force at this time is the pull-out force between the sample plate and the adhesive. The above test scheme mainly has the following deficiencies: (1) This scheme is only applicable to soft adhesives with low fluidity, and is not applicable to adhesives that require high-temperature curing and have high fluidity before curing; (2) The test sample in this scheme is essentially a test sample with a sandwich structure, with many bonding interfaces. When the sample is tested, the crack path is tortuous and complex, and it cannot accurately reflect the pull-out force between the adhesive and the connection interface; (3) During the test of this scheme, since the adhesive is coated on the sample plate, the amount of adhesive used is not easy to control. Too much or too little amount will affect the test results, and the test stability needs to be improved. Summary of the Invention

[0005] In view of the deficiencies in the prior art, the present invention provides an interface pull-out force test sample for an adhesive, a preparation device therefor, and a test method therefor, so as to improve the stability and accuracy of the interface pull-out force test of adhesives.

[0006] To achieve the above-mentioned invention object, one aspect of the present invention provides a preparation device for a test sample of the interfacial pull-out force of an adhesive, which includes a lower fixture, a substrate, a template, and an upper fixture arranged in sequence from bottom to top. A locking mechanism is connected between the lower fixture and the upper fixture; a cavity for accommodating the adhesive to form a test sample is provided in the template. One end of the cavity communicates with the substrate so that the formed test sample is bonded to the substrate. The other end of the cavity communicates with the upper fixture, and a first through hole is provided at the corresponding position of the upper fixture for injecting the adhesive; the preparation device is further configured with a metal connector, one end of the metal connector is formed into a tip, and the metal connector is inserted into the cavity through the first through hole and the tip is in contact connection with the substrate.

[0007] Preferably, a fixing plate member is assembled in the first through hole. The size of the fixing plate member is adapted to the first through hole. A second through hole is provided in the fixing plate member. The size of the second through hole is adapted to the metal connector. The metal connector is inserted into the cavity through the second through hole.

[0008] Preferably, the top width of the cavity is 3 mm to 6 mm, the bottom width of the cavity is 4 mm to 8 mm, and the height of the cavity is 4 mm to 6 mm; wherein, the top width of the cavity refers to the width between the two points farthest apart in the top of the cavity, and the bottom width of the cavity refers to the width between the two points farthest apart in the bottom of the cavity.

[0009] Preferably, the length of the tip of the metal connector is 2 mm to 5 mm, and the included angle of the tip is 20° to 40°.

[0010] Preferably, the metal connector is a metal sheet structure with a thickness of 0.3 mm to 1 mm and a width of 3 mm to 5 mm.

[0011] Another aspect of the present invention provides a test sample of the interfacial pull-out force of an adhesive, which includes a substrate, an adhesive pudding mold connected to the substrate, and a metal connector inserted into the adhesive pudding mold; wherein, the adhesive pudding mold is formed by curing the adhesive to be tested to form a pudding mold, the metal connector is inserted into the adhesive pudding mold during the curing process, and the bonding interface between the adhesive pudding mold and the substrate is the interface to be subjected to the pull-out force test; one end of the metal connector is formed into a tip, and the tip of the metal connector is in contact connection with the substrate.

[0012] Specifically, the top width of the adhesive pudding mold is 3 mm to 6 mm, the bottom width of the adhesive pudding mold is 4 mm to 8 mm, and the height of the adhesive pudding mold is 4 mm to 6 mm; wherein, the top width of the adhesive pudding mold refers to the width between the two points with the farthest distance in the top of the adhesive pudding mold, and the bottom width of the adhesive pudding mold refers to the width between the two points with the farthest distance in the bottom of the adhesive pudding mold.

[0013] Specifically, the length of the tip of the metal connector is 2 mm to 5 mm, and the included angle of the tip is 20° to 40°.

[0014] Specifically, the metal connector is a metal sheet structure, its thickness is 0.3 mm to 1 mm, and its width is 3 mm to 5 mm.

[0015] The present invention also provides a method for testing the interfacial pull-out force of an adhesive, which includes:

[0016] Preparing the interfacial pull-out force test sample by using the preparation device as described above;

[0017] Providing a pull-out force test device, the pull-out force test device includes a sample bonding plate, a first clamp and a second clamp; fixing and connecting the substrate of the interfacial pull-out force test sample to the sample bonding plate, clamping the metal connector of the interfacial pull-out force test sample with the first clamp, and clamping the sample bonding plate with the second clamp;

[0018] Starting the pull-out force test device, controlling the first clamp and the second clamp to pull in the opposite direction, and when the adhesive pudding mold is peeled off from the substrate, recording the pull-out force value on the pull-out force test device to obtain the pull-out force parameter.

[0019] The preparation device of the interfacial pull-out force test sample and the corresponding interfacial pull-out force test sample provided by the embodiment of the present invention: on the one hand, there is only one connection interface between the adhesive pudding mold and the substrate, which can more accurately reflect the bonding strength between the adhesive and the substrate, and the test result is more accurate; on the other hand, the adhesive pudding mold is cured and formed in the mold cavity of the preparation device, which is not only applicable to soft adhesives with less fluidity, but also applicable to adhesives that require high-temperature curing and have a large fluidity before curing, and the amount of the adhesive is easy to control, which is beneficial to improving the stability of the test result. Description of the Drawings

[0020] Figure 1 is an exploded structure diagram of the preparation device of the interfacial pull-out force test sample of the embodiment of the present invention;

[0021] Figure 2 is a bottom view of the template of the preparation device of the test sample in the preferred embodiment of the present invention;

[0022] Figure 3 is the sectional view of the template as shown in Figure 2 ;

[0023] Figure 4 is the bottom view of the template of the preparation device for the test sample in another preferred embodiment of the present invention;

[0024] Figure 5 is the sectional view of the template as shown in Figure 4 ;

[0025] Figure 6 is the schematic structural view of the metal connector in the embodiment of the present invention;

[0026] Figure 7 is the front view of the interfacial pull-out force test sample provided in the embodiment of the present invention;

[0027] Figure 8 is the side view of the interfacial pull-out force test sample provided in the embodiment of the present invention;

[0028] Figure 9 is the exemplary illustration of the interfacial pull-out force test method provided in the embodiment of the present invention;

[0029] Figures 10a to 10c is the photographic illustration of the peeling interface for testing the sample to be tested in the present invention. Detailed Embodiments

[0030] To make the objectives, technical solutions and advantages of the present invention clearer, the following will describe the detailed embodiments of the present invention with reference to the accompanying drawings. Examples of these preferred embodiments are illustrated in the accompanying drawings. The embodiments of the present invention shown in the drawings and described according to the drawings are merely exemplary, and the present invention is not limited to these embodiments.

[0031] Here, it should also be noted that in order to avoid obscuring the present invention with unnecessary details, only the structures and / or processing steps closely related to the solution of the present invention are shown in the drawings, while other details less related to the present invention are omitted.

[0032] The embodiment of the present invention first provides a preparation device for an interfacial pull-out force test sample of an adhesive, as shown in Figure 1 . The preparation device includes a lower clamp 10, a substrate 20, a template 30, and an upper clamp 40 which are sequentially arranged from bottom to top, and a locking mechanism is connected between the lower clamp 10 and the upper clamp 40.

[0033] Among them, a cavity 31 for accommodating an adhesive to form a test sample is provided in the template 30. One end of the cavity 31 is connected to the substrate 20 so that the formed test sample is bonded to the substrate 20. The other end of the cavity 31 is connected to the upper fixture 40, and a first through hole 41 is provided in the upper fixture 40 at a position corresponding to the cavity 31. The first through hole 41 is used for injecting the adhesive.

[0034] Among them, the preparation device is further configured with a metal connecting piece 50. One end of the metal connecting piece 50 is formed into a tip 51. The metal connecting piece 50 is inserted into the cavity 31 through the first through hole 41, and the tip 51 is in contact connection with the substrate 20.

[0035] Among them, the materials of the lower fixture 10 and the upper fixture 40 are hard and high-temperature resistant materials, such as plates made of stainless steel, aluminum, iron, etc. that can be selected; the material of the template 30 can be selected as a Teflon plate; the material of the substrate 20 can be selected as hard materials such as copper, PCB board, aluminum, stainless steel, etc., or brittle materials such as silicon, silicon nitride, gallium arsenide, etc.

[0036] In a preferred solution, as Figure 1 shown, a fixing plate member 60 is assembled in the first through hole 41. The size of the fixing plate member 60 is adapted to the first through hole 41. A second through hole 61 is provided in the fixing plate member 60. The size of the second through hole 61 is adapted to the metal connecting piece 50. The metal connecting piece 50 is inserted into the cavity 31 through the second through hole 61. By providing the fixing plate member 60, the position where the metal connecting piece 50 is inserted into the cavity 31 can be limited, and it can better ensure that the metal connecting piece 50 is inserted into the central position in the cavity 31. Specifically, the material of the fixing plate member 60 can be selected as plastic or metal.

[0037] In a preferred solution, the thickness of the lower fixture 10 and the upper fixture 40 can be set within the range of 4 mm to 8 mm, the thickness of the template 30 can be set within the range of 4 mm to 6 mm, the thickness of the substrate 20 can be set within the range of 0.4 mm to 2 mm, and the thickness of the fixing plate member 60 is set to be the same as the thickness of the upper fixture 40.

[0038] In a preferred solution, the first through hole 41 in the upper fixture 40 is a circular through hole, and its diameter can be set within the range of 8 mm to 12 mm.

[0039] In a preferred embodiment, the top width of the mold cavity 31 is set within the range of 3 mm to 6 mm, the bottom width of the mold cavity 31 is set within the range of 4 mm to 8 mm, and the height of the mold cavity 31 is set within the range of 4 mm to 6 mm. Herein, the top width of the mold cavity 31 refers to the width between the two points farthest apart in the top of the mold cavity 31, and the bottom width of the mold cavity 31 refers to the width between the two points farthest apart in the bottom of the mold cavity 31.

[0040] In a specific embodiment, referring to Figure 2 and Figure 3 , the internal space of the mold cavity 31a of the template 30 has the shape of a frustum of a cone, with its top being a circle with a diameter of 3 mm to 6 mm and its bottom being a circle with a diameter of 4 mm to 8 mm. In another specific embodiment, referring to Figure 4 and Figure 5 , the internal space of the mold cavity 31b of the template 30 has the shape of a frustum of a pyramid, with its top being a square with a side length of 3 mm to 6 mm and its bottom being a square with a side length of 4 mm to 8 mm.

[0041] In a preferred embodiment, the locking mechanism is a detachable threaded fastener. Specifically, referring to Figure 1 , through holes are respectively provided at the four corners of the lower clamp 10 and the upper clamp 40. The threaded fastener includes a screw rod 71 and a nut 72. The screw rod 71 is passed through the through holes at the corners of the lower clamp 10 and the upper clamp 40 and tightened in cooperation with the nut 72, thereby achieving the purpose of locking the various layers of the device.

[0042] In a preferred embodiment, referring to Figure 6 , the length L of the tip 51 of the metal connector 50 is 2 mm to 5 mm, and the included angle α of the tip 51 is 20° to 40°. It should be noted that the length L of the tip 51 of the metal connector 50 is set to be less than the height of the mold cavity 31. The material of the metal connector 50 can be stainless steel, copper, aluminum, etc.

[0043] In a more preferred embodiment, the metal connector 50 is a metal sheet structure, with a thickness of 0.3 mm to 1 mm, a width of 3 mm to 5 mm, and its length can be set according to actual needs.

[0044] For the apparatus for preparing the adhesive interface pull-out force test sample as described above, the process for preparing the test sample can be carried out according to the following steps:

[0045] S1. Use an ethanol solution to ultrasonically clean the lower clamp 10, the substrate 20, the template **********, the upper clamp 40, the metal connector 50, and the fixed plate 60 for 2 to 3 times, and dry them for later use.

[0046] S2. Place the substrate 20 at the center position of the lower fixture 10, completely cover the substrate 20 with the template 30, cover the upper fixture 40 on the template 30, and lock the upper fixture 40 and the lower fixture 10 through the locking mechanism, so that the substrate 20 and the template 30 are firmly clamped between the upper and lower fixtures. Then place the assembled preparation device on the heating table for preheating.

[0047] S3. Inject an appropriate amount of adhesive into the cavity 31 of the template 30 through the first through-hole 41 of the upper fixture 40. It should be noted that try to avoid the overflow of the adhesive.

[0048] S4. Assemble the fixing plate member 60 in the first through-hole 41, and then insert the metal connecting member 50 into the adhesive in the cavity 31 through the second through-hole 61 in the fixing plate member 60, and make the tip 51 of the metal connecting member 50 contact and connect with the substrate 20.

[0049] S5. Wait for the adhesive to cure (cure at room temperature or by heating).

[0050] S6. After the adhesive cures, disassemble the locking mechanism and remove the lower fixture 10, the upper fixture 40, and perform demolding on the template 30, thereby obtaining an interface pull-out force test sample.

[0051] Based on the above preparation device and preparation process for the interface pull-out force test sample of the adhesive, an interface pull-out force test sample of an adhesive is obtained in an embodiment of the present invention. Refer to Figure 7 and Figure 8 , the interface pull-out force test sample 100 includes a substrate 20, an adhesive pudding mold 80 connected to the substrate 20, and a metal connecting member 50 inserted into the adhesive pudding mold 80. Among them, referring to the above process steps S3 - S5, the adhesive pudding mold 80 is formed by curing the adhesive to be tested to form a pudding mold, and the metal connecting member 50 is inserted into the adhesive pudding mold during the curing process.

[0052] Among them, the adhesive pudding mold 80 has the same shape structure as the internal space of the cavity 31, and the bonding interface between the adhesive pudding mold 80 and the substrate 20 is the interface to be subjected to the pull-out force test; one end of the metal connecting member 50 is formed into a tip, and the tip of the metal connecting member 50 is in contact and connection with the substrate 20.

[0053] An embodiment of the present invention also provides a method for testing the interface pull-out force of an adhesive, including the following steps:

[0054] S10. Use the preparation device described in the above embodiment of the present invention (refer to Figure 1 the preparation device) to prepare the above-mentioned interface pull-out force test sample (refer to Figure 7 andFigure 8 of the test sample).

[0055] S20. Provide a pull-out force test device. Refer to Figure 9 , the pull-out force test device includes a sample cementing plate 1, a first fixture 2 and a second fixture 3. Fix the substrate 20 of the interfacial pull-out force test sample 100 to the sample cementing plate 1 in a fixed connection manner, clamp the metal connecting member 50 of the interfacial pull-out force test sample 100 with the first fixture 2, and clamp the sample cementing plate 1 with the second fixture 3.

[0056] Among them, the sample cementing plate 1 has a T-shaped structure. The substrate 20 of the interfacial pull-out force test sample 100 is cemented to the plane of the T-shaped sample cementing plate 1 through another adhesive. The second fixture 3 clamps the connecting arm in the vertical direction of the sample cementing plate 1. It should be noted that when selecting the other adhesive, it is necessary to ensure that the bonding force between the substrate 20 and the sample cementing plate 1 is greater than the bonding force between the substrate 20 and the adhesive pudding mold 80.

[0057] In a preferred solution, the pull-out force test device is further equipped with an oven, and the test conditions for the pull-out force test can be set to be tested under high-temperature conditions.

[0058] S30. Start the pull-out force test device, control the first fixture 2 and the second fixture 3 to pull in the opposite direction. When the adhesive pudding mold 80 is peeled off from the substrate 20, record the pull-out force value on the pull-out force test device to obtain the pull-out force parameter.

[0059] Specifically, control the first fixture 2 to pull the metal connecting member 50 at a certain tensile rate. The pull-out force F gradually increases. When the adhesive pudding mold 80 is peeled off from the substrate 20, the first fixture 2 automatically stops stretching.

[0060] The preparation device for the interfacial pull-out force test sample provided by the embodiment of the present invention, the corresponding interfacial pull-out force test sample and the test method have the following advantages: on the one hand, there is only one connection interface between the adhesive pudding mold and the substrate, which can more accurately reflect the bonding strength between the adhesive and the substrate, and the test result is more accurate; on the other hand, the adhesive pudding mold is cured and formed in the mold cavity of the preparation device, which is not only applicable to soft adhesives with relatively small fluidity, but also applicable to adhesives that require high-temperature curing and have relatively large fluidity before curing, and the amount of the adhesive is easy to control, which is beneficial to improving the stability of the test result; in addition, when performing the test, the substrate of the test sample is cemented to the sample cementing plate with a larger area through an adhesive with a greater bonding force. Therefore, the substrate of the test sample can be selected as hard materials such as copper, PCB board, aluminum, stainless steel, etc., or brittle materials such as silicon, silicon nitride, gallium arsenide, etc., which improves the flexibility of the test.

[0061] Furthermore, in an embodiment of the present invention, one end of the metal connector is formed into a pointed end, and is inserted into the adhesive pudding mold and is in contact with the substrate, thereby having the following beneficial effects during testing: when the sample is stretched, the metal connector is tightly combined with the pudding mold colloid, and the metal connector pulls the pudding mold colloid to separate the pudding mold colloid from the substrate. When the metal connector is prepared as a pointed end, since the contact area between the tip and the colloid is small, the tensile force borne by the metal connector is mainly at the back of the contact between the metal connector and the colloid (non-tip part), which will make it more stable during stretching; if the metal connector is not set as a pointed end, the head of the metal connector (corresponding to the tip part) will be subjected to a large force from the beginning, which can easily cause the head to break off from the colloid during the stretching process, resulting in pulling failure.

[0062] Example 1

[0063] Provide a test sample preparation device as described above in the embodiment of the present invention, refer to Figure 1 、 Figure 2 and Figure 3 , among which: the lower fixture 10 is a 4mm thick stainless steel plate; the upper fixture 40 is a 4mm thick stainless steel plate with a circular through hole with a diameter of 10mm in the center; the template 30 is a 6mm thick, 20mm side length Teflon plate, and the mold cavity 31 in the template 30 is a frustum mold (size: top diameter 3mm, bottom diameter 4mm, height 6mm); the substrate 20 is a 0.5mm thick silicon nitride substrate with a side length of 15mm×15mm.

[0064] The metal connector 50 is a 304 stainless steel plate with a length of 60 mm, a width of 3 mm, and a thickness of 0.3 mm. The tip height is 3 mm and the tip angle is 30°.

[0065] The fixing plate 60 is a circular stainless steel plate with a diameter of 9 mm and a thickness of 4 mm, and a rectangular opening with a length of 4 mm and a width of 0.4 mm in the center.

[0066] Prepare the test samples as follows:

[0067] (1) Use ethanol solution to ultrasonically clean the lower fixture 10, substrate 20, template 30, upper fixture 40, metal connector 50 and fixing plate 60, and dry them for use.

[0068] (2) Place the silicon nitride substrate 20 at the center of the lower fixture 10, completely cover the template 30 on the substrate 20, cover the upper fixture 40 on the template 30, and lock the upper fixture 40 and the lower fixture 10 through the locking mechanism so that the substrate 20 and the template 30 are firmly clamped between the upper and lower fixtures. Then place the assembled preparation device on a heating table for preheating, specifically, place it on a heating table at 120°C and heat it for 30 minutes.

[0069] (3) The adhesive to be tested is injected into the mold cavity 31 through the first through hole 41 of the upper fixture 40 .

[0070] (4) Assemble the fixing plate 60 in the first through hole 41, and then insert the metal connector 50 into the adhesive in the mold cavity 31 through the second through hole 61 in the fixing plate 60, and make the tip 51 of the metal connector 50 contact and connect with the substrate 20.

[0071] (5) Wait for the adhesive to solidify. In this embodiment, the adhesive is placed in an oven for heating and solidification, with the set temperature being 160° C. and the time being 120 minutes.

[0072] (6) After the adhesive is cured, the locking mechanism is disassembled and the lower clamp 10 and the upper clamp 40 are removed, and the template 30 is demolded, thereby preparing an interface pull-out force test sample.

[0073] Based on the above process flow, this example prepared interface pull-out test sample A, which includes a silicon nitride substrate 20, an adhesive pudding mold 80 connected to the silicon nitride substrate 20, and a metal connector 50 inserted into the adhesive pudding mold 80. The adhesive pudding mold 80 is truncated cone-shaped, with a top diameter of 3 mm, a bottom diameter of 4 mm, and a height of 6 mm.

[0074] Example 2

[0075] The difference between this embodiment and embodiment 1 is that in the test sample preparation device, the mold cavity 31 in the template 30 is a quadrangular pyramid inverted mold (size: top side length 3mm, bottom side length 4mm, height 6mm).

[0076] The remaining structural features of the test sample preparation device in this embodiment are the same as those in Example 1, and the test sample preparation process is also the same as that in Example 1, so they are not described in detail.

[0077] In this example, a sample B for interfacial pull-out strength testing was prepared. The sample B comprises a silicon nitride substrate 20, an adhesive pudding mold 80 connected to the silicon nitride substrate 20, and a metal connector 50 inserted into the adhesive pudding mold 80. The adhesive pudding mold 80 is in the shape of a quadrangular pyramid, with a top side length of 3 mm, a bottom side length of 4 mm, and a height of 6 mm.

[0078] Example 3

[0079] This example performs a pull-out force test on the interface pull-out force test samples obtained in Examples 1 and 2.

[0080] Based on the interface pull-out force test method for an adhesive provided by an embodiment of the present invention, referring to the aforementioned steps S10 to S30, the following three groups of sample tests are respectively carried out:

[0081] (1) Conduct a pull-out force test on a group of test samples A prepared in Example 1;

[0082] (2) Conduct a pull-out force test on a group of test samples B prepared in Example 2;

[0083] (3) Based on a group of test samples A obtained in Example 1, when testing, first use the oven of the pull-out force test device to heat the sample to 80 °C and keep it warm for 5 minutes, and then conduct a pull-out force test. This group of samples is denoted as test samples C.

[0084] Among them, when conducting the pull-out force test, control the first fixture to pull the metal connector of the test sample at a speed of 0.5 mm / min, the pull-out force gradually increases, and when the adhesive pudding mold of the test sample is peeled off from the substrate, record the corresponding pulling force value.

[0085] Figures 10a to 10c is a photographic illustration of the peeling interface for testing the sample to be tested in this embodiment, where Figure 10a is a photographic illustration of the peeling interface of test sample A, Figure 10b is a photographic illustration of the peeling interface of test sample B, Figure 10c is a photographic illustration of the peeling interface of test sample C.

[0086] The pull-out force test results of the above test samples are as shown in Table 1 below (5 samples are tested for each type of sample).

[0087] Table 1:

[0088] Sample Mean (N) Standard Deviation (N) Test Sample A 62.6 1.5 Test Sample B 48.5 1.2 Test Sample C 21.3 0.7

[0089] Based on Figures 10a to 10c and the test data in Table 1, it can be seen that: for the preparation device of the test sample provided by the embodiment of the present invention and the test sample obtained by the preparation, the peeling interface between the adhesive layer and the substrate is relatively clean and flat, indicating that the fracture path is at the bonding interface, the mean square deviation of the test results is small, the data stability is good, and the accuracy is relatively high.

[0090] In summary, the preparation device for the interface pull-out force test sample and the corresponding interface pull-out force test sample provided by the embodiments of the present invention: on the one hand, there is only one connection interface between the adhesive pudding mold and the substrate, which can more accurately reflect the bonding strength between the adhesive and the substrate, and the test results are more accurate; on the other hand, the adhesive pudding mold is cured and formed in the mold cavity of the preparation device, which is not only applicable to soft adhesives with low fluidity, but also applicable to adhesives that require high-temperature curing and have high fluidity before curing, and the amount of the adhesive is easy to control, which is beneficial to improving the stability of the test results.

[0091] The above are only specific embodiments of the present application. It should be noted that for those of ordinary skill in the art, without departing from the principle of the present application, several improvements and refinements can be made, and these improvements and refinements should also be regarded as the protection scope of the present application.

Claims

1. A device for preparing adhesive interfacial pull-out test samples, characterized in that: The preparation device comprises a lower fixture, a base plate, a template, and an upper fixture, which are sequentially arranged from bottom to top, wherein a locking mechanism is connected between the lower fixture and the upper fixture; a mold cavity for accommodating an adhesive to form a test sample is provided in the template, one end of the mold cavity is connected to the base plate so that the formed test sample is bonded to the base plate, and the other end of the mold cavity is connected to the upper fixture, and a first through hole is provided at a corresponding position of the upper fixture, wherein the first through hole is used for injecting the adhesive; the preparation device is further equipped with a metal connector, one end of the metal connector is formed into a pointed end, the metal connector is inserted into the mold cavity through the first through hole, and the pointed end is in contact with the base plate; The length of the tip of the metal connector is 2mm~5mm, the angle of the tip is 20°~40°, the metal connector is a metal sheet structure, its thickness is 0.3mm~1mm, and its width is 3mm~5mm. The length of the tip of the metal connector is less than the height of the mold cavity.

2. The preparation device according to claim 1, characterized in that A fixing plate is assembled in the first through hole, and the size of the fixing plate is adapted to the first through hole. A second through hole is provided in the fixing plate, and the size of the second through hole is adapted to the metal connector. The metal connector is inserted into the mold cavity through the second through hole.

3. The preparation device according to claim 1, characterized in that The top width of the mold cavity is 3mm~6mm, the bottom width of the mold cavity is 4mm~8mm, and the height of the mold cavity is 4mm~6mm; wherein, the top width of the mold cavity refers to the width between the two farthest points in the top of the mold cavity, and the bottom width of the mold cavity refers to the width between the two farthest points in the bottom of the mold cavity.

4. An adhesive interfacial pull-out test sample, characterized in that: The adhesive pudding mold comprises a substrate, an adhesive pudding mold connected to the substrate, and a metal connector inserted in the adhesive pudding mold; wherein the adhesive pudding mold is formed by a curing process of the adhesive to be tested, the metal connector is inserted in the adhesive pudding mold during the curing process, and the bonding interface between the adhesive pudding mold and the substrate is the interface to be tested for pull-out force; one end of the metal connector is formed into a pointed end, and the pointed end of the metal connector is in contact with the substrate. The length of the tip of the metal connector is 2mm~5mm, the angle of the tip is 20°~40°, the metal connector is a metal sheet structure, the thickness is 0.3mm~1mm, and the width is 3mm~5mm. The length of the tip of the metal connector is less than the height of the adhesive pudding mold.

5. The interface pull-out force test sample according to claim 4, characterized in that: The top width of the adhesive pudding mold is 3 mm to 6 mm, the bottom width of the adhesive pudding mold is 4 mm to 8 mm, and the height of the adhesive pudding mold is 4 mm to 6 mm; wherein, the top width of the adhesive pudding mold refers to the width between the two farthest points on the top of the adhesive pudding mold, and the bottom width of the adhesive pudding mold refers to the width between the two farthest points on the bottom of the adhesive pudding mold.

6. A method for testing the interfacial pull-out force of an adhesive, characterized in that: include: The interface pull-out force test sample according to claim 4 or 5 is prepared by using the preparation device according to any one of claims 1 to 3; A pull-out force testing device is provided, comprising a sample fixing plate, a first clamp, and a second clamp; a substrate of the interface pull-out force testing sample is fixedly connected to the sample fixing plate, the first clamp is clamped to the metal connector of the interface pull-out force testing sample, and the second clamp is clamped to the sample fixing plate; The pull-out force testing device is started to control the first clamp and the second clamp to pull in opposite directions. When the adhesive pudding mold is peeled off from the substrate, the pull-out force value on the pull-out force testing device is recorded to obtain the pull-out force parameter.

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