A sample for determining the bonding performance of a bonding resin to a metal and a method for preparing the same

Abstract

The present application relates to the field of sample preparation for polymer material performance testing, and particularly relates to a sample for testing the bonding performance of bonding resin on metal and a preparation method thereof. The sample has the following structure from bottom to top: a first flat curing mold, a first type PET film I, a second type PET film I, a second mold loaded with bonding resin, a third type PET film, the first mold, a second type PET film II, a first type PET film II, and a second flat curing mold. The second mold has a plurality of cutting positions loaded with bonding resin cut through the second mold in a top-to-bottom manner. A fourth type PET film is arranged between the cutting positions and the bonding resin to prevent overflow of the bonding resin. The third type PET film effectively separates the bonding resin in the non-working area from the first mold as the test metal plate, facilitating the test operation of reversing the bending of the non-working area during the test. The second mold ensures the width and thickness of the bonding resin, and ensures the size consistency of the bonding resin sample and the stability and accuracy of the data.

Description

Technical Field

[0001] This invention relates to the field of sample preparation for polymer material performance testing, specifically to a sample for determining the bonding performance of a bonding resin to a metal and its preparation method. Background Technology

[0002] Steel-plastic composite pipe is a type of composite pipe that combines the advantages of metal and plastic pipes. It typically consists of an inner metal layer (such as steel mesh, steel strip, or seamless steel pipe) and an outer plastic layer (such as high-density polyethylene, HDPE). This structure gives steel-plastic composite pipe excellent pressure resistance, corrosion resistance, chemical resistance, and a long service life.

[0003] Polyethylene plastic is a non-polar material, while the metal layer is a polar material. Due to the significant difference in polarity, their compatibility is poor, and the interfacial adhesion between them is not ideal. Currently, various methods exist to improve the adhesion performance between polyethylene plastic and the metal layer, depending on specific application requirements and environment. These methods include epoxy resin adhesives, instant adhesives, and UV adhesives. Composite pipes currently primarily improve the bonding strength between polyethylene and metals or other polar materials by adding adhesive resins (such as PE-g-MAH), thereby enhancing the strength, pressure resistance, and durability of steel-plastic composite pipes in practical applications.

[0004] The adhesion between the metal layer and the plastic layer was improved by adding PE-g-MAH pipe bonding resin. The adhesion strength was determined by measuring the peel strength after the metal layer and polyethylene were bonded. There is a national standard for measuring peel strength, but there is no unified method or detailed preparation method for preparing the sample for measuring the adhesion between the metal layer and the plastic layer.

[0005] Current structures used for testing the adhesion performance of metal and plastic layers have several problems in use. For example, CN215640434U discloses a sample structure for testing the peel force of adhesive resin, which includes a steel sheet, an aluminum sheet, and an adhesive layer. The adhesive layer is placed between the steel sheet and the aluminum sheet, and the steel sheet and the aluminum sheet are fixed together by the adhesive layer. However, when this structure is used for testing, there are problems such as poor controllability and dimensional consistency of the adhesive resin width and thickness, easy overflow of adhesive resin, and difficulty in clearly distinguishing the working area and non-working area of ​​the adhesive resin and the test metal plate. Moreover, the sample may have problems with uncertain peel surface due to the different adhesion forces of the adhesive resin to the aluminum sheet and the steel sheet. Summary of the Invention

[0006] In view of the lack of a method for preparing samples in which the adhesive resin and the metal layer are bonded together in the current experiment for testing the peel strength of adhesive resin, this invention prepares a sample for measuring the bonding performance of adhesive resin to metal by means of repeated experiments and technical verification, based on the peel strength test standard.

[0007] This invention provides a sample for determining the bonding performance of a bonding resin to a metal and a method for preparing the same. The sample comprises a bonding resin and a first mold serving as a metal plate. From bottom to top, the sample consists of a first flat vulcanization mold, a type I PET film, a type II PET film, a second mold containing the bonding resin, a type III PET film, a first mold, a type II PET film, a type I PET film, and a second flat vulcanization mold. The second mold has multiple cut sections of a certain size for loading the bonding resin cut out in a vertically penetrating manner. The length and width of the cut sections are less than or equal to the length and width of the first mold. A type IV PET film covers the cut sections and the bonding resin. The method of use is as follows: After preset the pressure, temperature and time of the flat vulcanizing machine, place Type I PET film I, Type II PET film I and the second mold in sequence on the first flat vulcanizing mold. Place the adhesive resin in the cutting part of the second mold. Before placing the adhesive resin, wrap the cutting part with Type IV PET film. The Type IV PET film includes polar and non-polar sides, with the polar side facing the inside of the cutting part. Cover the second mold with a layer of third PET film. Lay the third PET film vertically on half of one side of the cutting part of the second mold. Place the corresponding number of first molds, which are metal plates, above the third PET film above the center of the cutting part of the second mold. The third PET film partially covers the first mold below the first mold. Then, cover the second mold with Type II PET film II, Type I PET film II and the second flat vulcanizing mold in sequence on top. Place the first flat vulcanizing mold in the flat vulcanizing machine. After heating and pressurizing the flat vulcanizing machine within the set time, take it out and then perform cold pressing and cooling. Take out the sample for peel force testing.

[0008] The Type I and Type II PET films of this invention help to prevent overflowing adhesive resin from adhering to the flat vulcanizing machine and causing cleaning difficulties. The Type III PET film effectively isolates the adhesive resin in the non-working area and serves as the first mold for the test metal plate, facilitating the testing operation after the non-working area is bent in the opposite direction. The second mold ensures the width and thickness of the adhesive resin, and its cutting part ensures the dimensional consistency of the adhesive resin sample, ensuring the stability and accuracy of the data.

[0009] The four-type PET film covers the four sidewalls of the cutting part of the second mold, isolating it between the adhesive resin and the second mold, and its polar side faces the adhesive resin side, so that the adhesive resin and the first mold can be removed after the flat vulcanizer treatment is completed.

[0010] In a specific embodiment, the thickness of the type IV PET film is 0.001 mm.

[0011] This invention first provides a sample for determining the bonding performance of a bonding resin to metal, comprising a first and a second flat vulcanizing mold with a planar structure. The first flat vulcanizing mold serves as the lower mold, and the second flat vulcanizing mold serves as the upper mold. A second mold is placed on the first flat vulcanizing mold. At least two parallel cuboids are cut through the interior of the second mold from top to bottom. The inner walls of the cut parts of the cuboids are covered and isolated by a type IV PET film. A first mold with a corresponding number of sheet-like cuboids is placed parallel to the center of the cut parts of the cuboids in the second mold. The cut parts of the cuboids in the second mold are filled with bonding resin particles. The second flat vulcanizing mold is positioned above the first and second molds.

[0012] A type III PET film is placed below the first mold. After the second mold is filled with the adhesive resin sample, the type III PET film longitudinally covers 50% of the surface area of ​​the side below the first mold. The type III PET film is a PET ultra-thin film with one polar side and one non-polar side. Its polar side faces the side of the second mold containing the adhesive resin, thus partially isolating the first mold and the adhesive resin sample.

[0013] The intermediate spacing of the first mold is determined based on the cutting part of the second mold.

[0014] Preferably, between the first flat vulcanizing mold and the second mold, a type I PET film and a type II PET film are arranged sequentially from bottom to top. Between the first mold and the second flat vulcanizing mold, a type II PET film and a type I PET film are arranged sequentially from bottom to top. The type I PET film is a thick PET film that is non-polar on both sides, and the type II PET film is a thin PET film that is polar on one side and non-polar on the other. The non-polar side of the type II PET film faces the first flat vulcanizing mold, and the non-polar side of the type II PET film faces the second flat vulcanizing mold. The polar sides of the type II PET film and the type II PET film face the second mold and the first mold, respectively.

[0015] The Type I and Type II PET films serve to shape and isolate the sample. The Type I thick PET film provides support, isolates the flat vulcanizing mold, provides a flat contact surface, and protects the mold from sample contamination. The Type II PET film has its non-polar side facing the flat vulcanizing mold and its polar side facing the first and second molds. The Type II PET film provides isolation, preventing the sample from overflowing and sticking to the metal flat vulcanizing mold. Its polar side facilitates sample cleaning.

[0016] Preferably, the cuboid cutting part has two parts, and the first mold has two pieces.

[0017] In this scheme, the thickness of Type I PET film is generally greater than 0.2mm to ensure that it has a certain stiffness, the thickness of Type II PET film is 0.03-0.2mm, and the thickness of Type III and Type IV PET film is less than 0.05mm.

[0018] Preferably, the inner wall of the cuboid cutting part of the second mold is covered with a type IV PET film for isolation, which isolates it between the adhesive resin and the second mold, and its polar side faces the adhesive resin side, so that the adhesive resin and the first mold can be removed after the flat vulcanizing machine is finished.

[0019] Preferably, the surface of the first mold is coated with a coupling agent, which is one or more of vinyltrimethoxysilane (A-171), vinyltris(2-methoxyethoxy)silane (A-172), vinyltriethoxysilane (A-151), γ-glycidyl etheroxypropyltrimethoxysilane (KH560), γ-methacryloyloxypropyltrimethoxysilane (KH570), and γ-aminopropyltriethoxysilane (KH550), and the coating amount is preferably 0.01-0.04 g / cm³. 3 .

[0020] Preferably, the length, width, and height of the first mold are 200mm, 40mm, and 2mm, respectively; the length, width, and height of the second mold are 200mm, 140mm, and 3mm, respectively, and the length, width, and height of the internal cuboid cut are 150mm, 25mm, and 3mm, respectively; the length, width, and height of Type I PET film I and Type I PET film II are 297mm, 210mm, and 0.3mm, respectively; the length, width, and height of Type II PET film I and Type II PET film II are 210mm, 148mm, and 0.03mm, respectively; the length, width, and height of Type III PET film are 148mm, 105mm, and 0.001mm, respectively; and the thickness of Type IV PET film is 0.001mm, with its length and width determined according to the cutting surfaces.

[0021] Preferably, the bonding resin is a resin with metal bonding properties, including one or more of polyethylene grafted maleic anhydride particles (PE-g-MAH), polyethylene grafted acrylic acid particles (PE-g-AA), polypropylene grafted maleic anhydride particles (PP-g-MAH), polypropylene grafted acrylic acid particles (PP-g-AA), epoxy resin, polyurethane resin, and acrylic resin; the aforementioned bonding resin types are some of the test materials that can be used to test the bonding performance of the mold samples of this scheme, and other resin materials with metal bonding properties can also be used as test samples.

[0022] The present invention further provides a method for preparing the sample. After setting the parameters of the flat vulcanizing apparatus, the inner wall of the cutting part of the second mold is covered with a type IV PET film. Then, the lower surface of the first mold is cleaned and coated with a coupling agent. After drying, the first flat vulcanizing mold, type I PET film, type II PET film, and second mold are assembled in sequence, and adhesive resin particles are inserted into the cutting part. Then, type III PET film, first mold, type II PET film, type I PET film, and second flat vulcanizing mold are installed. The obtained sample is placed in the flat vulcanizing apparatus for high-temperature pressing. After pressing, the first mold bonded with the adhesive resin is removed for testing.

[0023] More specifically, it includes the following steps: 1) Pretreatment: Prepare a clean first mold and a second mold; clean the flat platen of the flat vulcanizing machine and the inner surfaces of the first and second flat vulcanizing molds; prepare the corresponding quality of bonding resin; prepare sufficient Type I, Type II, Type III and Type IV PET films; preset the temperature of the flat vulcanizing machine to 180℃, the pressure to 15MPa, the pre-pressing time to 5min, and the pressing time to 15min. 2) Pre-treatment of the second mold: Use type 4 PET film to cover and fix the part of the second mold that is in direct contact with the adhesive resin, so that the adhesive resin and the second mold do not come into direct contact during high-temperature pressing; The type IV PET film can be fixed to the second mold by conventional methods in the art, such as by tape. Conventional tapes available in the art can be used, and will not be described in detail here. 3) Surface treatment of the first mold: First, apply a layer of acetic acid solution to the cleaned surface of the first mold to be bonded to the adhesive resin to remove residual grease and plastic. After the acetic acid solution dries naturally, clean the surface a second time with anhydrous ethanol to ensure it is clean and free of contaminants. After the ethanol dries naturally, finally apply a 0.01-0.04 g / cm³ coating to the surface. 3 The coupling agent KH550 is applied and allowed to dry completely before the surface treatment of the first mold is completed. Insufficient application of coupling agent will result in inadequate surface treatment, while excessive application will create a barrier effect, both of which will adversely affect the bonding effect. 4) Lower mold arrangement: Place the first flat vulcanizing mold and the corresponding PET film into the flat vulcanizing apparatus, and place them from bottom to top in the following order: first flat vulcanizing mold, type I PET film I, type II PET film I, and second mold; wherein, the polar surface of type II PET film I is placed upward and the non-polar surface is placed downward. 5) Place the sample: Place the adhesive resin particles into the two cuboid cutting parts of the second mold in step 4), ensuring that the particles can completely fill the hollow space of the second mold. It is expected that about 12 grams will be placed in each space. 6) Upper mold arrangement: Cover the upper surface of the second mold in step 5) with a type III PET film, covering 50% of the surface area of ​​the longitudinal side of the cutting part of the second mold; place the two first molds parallel to each other at the center of the two cuboid cutting parts of the second mold to ensure that the adhesive resin adheres to the corresponding position of the first mold. Place the second molds above the first molds from bottom to top in the order of type II PET film II, type I PET film II, and the second flat vulcanizing mold, and then place them between the two plates of the flat vulcanizing machine; wherein the non-polar surface of the type II PET film II is facing upwards and the polar surface is facing downwards; 7) High-temperature pressing: The flat vulcanizing apparatus with the temperature stabilized and other parameters set performs preheating, degassing, high-temperature and high-pressure pressing, and sampling and cooling of the sample after the above preparation work is completed according to the set program. 8) Sample post-processing: Remove the sample prepared in step 7) from the flat vulcanizer, remove the Type I PET film, Type II PET film, and Type III PET film, trim any burrs or flash that have overflowed from the sample, remove the bonding resin and the first mold from the second mold, and bend the free end of the bonding resin that is not bonded to the first mold (i.e., the part covered by the Type III PET film) backward by 180° so that the sample can meet the test method specified in the national standard GB / T 2790-1995, thus completing the sample preparation work for determining the bonding performance of the bonding resin to the metal.

[0024] In step 8), the Type IV PET film is generally undamaged and does not need to be removed if it is undamaged. If it is damaged, a new Type IV PET film needs to be replaced for the next use.

[0025] Preferably, in step 7), the preheating temperature is 180±2℃, the preheating time is 5 min, the pressure is 15MPa, the gas is vented 6 times to remove the gas, and then the pressure is increased to 15MPa for 15 min. After the mold is taken out, it is placed in a vulcanizing instrument at room temperature and cooled by water for 20 min to 1 h to reduce the temperature to below 50℃.

[0026] The sample for determining the bonding performance of adhesive resin to metal and the preparation method thereof provided by this invention have the following beneficial technical effects: Existing methods for preparing samples to determine the bonding performance of adhesive resins to metals are mostly temporary methods and means developed by front-line testing personnel based on accumulated experience and skills. These methods lack uniformity and stability, and have not gained widespread market acceptance and application. This invention, based on summarizing experience and hundreds of sample preparation trials, develops a simple, easy-to-operate, and stable standardized method for preparing samples to determine the bonding performance of adhesive resins to metals, facilitating rapid testing of the bonding performance of adhesive resins (such as pipe bonding resins). The use of Type I and Type II PET films makes it easier to clean up excess adhesive generated during sample preparation, saving mold cleaning time. The second mold is covered with Type IV PET film to isolate the adhesive resin from the mold, making it easier to remove the sample from the second mold. The mold design in this invention produces two samples per mold, saving time during the sample pressing process.

[0027] The type IV PET film covers the cutting part of the second mold, isolating it between the adhesive resin and the second mold, and its polar side faces the adhesive resin side, so that the adhesive resin and the first mold can be removed after the flat vulcanizing machine is finished.

[0028] This solution improves the dimensional controllability and consistency of the adhesive resin sample by setting a cutting part in the second mold. The use of Type I and Type II PET films improves the overflow problem of adhesive resin to a certain extent. Furthermore, the use of Type III PET film to block the adhesive resin from the corresponding metal parts improves the problem of unclear boundaries between the working and non-working areas of the adhesive resin and the test metal plate (first mold) after sample preparation. Attached Figure Description

[0029] Figure 1 A schematic diagram of a sample used to determine the bonding performance of the adhesive resin to metal; Figure 2 This is a schematic diagram of the second mold; Figure 3 This is a schematic diagram of a sample prepared for peel performance testing.

[0030] Wherein: 1 is the first flat vulcanizing mold, 2 is type I PET film, 3 is type II PET film, 4 is the second mold, 4-1 is the cutting part; 5 is type III PET film, 6 is the first mold, 7 is type II PET film, 8 is type I PET film, and 9 is the second flat vulcanizing mold. Detailed Implementation

[0031] The technical solution of the present invention will be further described below with reference to specific embodiments. These embodiments are only used to illustrate the technical solution of the present invention in more detail and should not be construed as limiting the scope of protection of the present invention.

[0032] The flat vulcanizer used was a Labtech LP-S-30 single-stage vulcanizing device with a maximum pressure of 30 tons and a maximum stage temperature of 300℃.

[0033] The first flat vulcanizing mold 1 and the second flat vulcanizing mold 9 are both flat on both sides, with smooth and flat surfaces without scratches; the second mold 4 has two cuboid cutting parts 4-1.

[0034] Anhydrous ethanol is industrial-grade anhydrous ethanol with a purity of 99.9%, and it is manufactured by Zibo Danyang Chemical Co., Ltd.

[0035] Acetic acid was of analytical grade, with a mass concentration of 36%, and was produced by Xi'an Tianmao Chemical Co., Ltd.

[0036] Coupling agent KH550 is an industrial-grade coupling agent with a content greater than 98.9%, manufactured by Fenghua Chemical Co., Ltd.

[0037] First, a sample for determining the bonding performance of an adhesive resin to a metal is provided, the sample being prepared by the following method: 1) Pretreatment: Prepare a clean first mold 6 and a second mold 4; clean the inner surfaces of the flat vulcanizing machine and the first flat vulcanizing mold 1 and the second flat vulcanizing mold 9; prepare 25g of bonding resin; prepare sufficient type I, type II, type III and type IV PET films; preset the temperature of the flat vulcanizing machine to 180℃, the pressure to 15MPa, the pre-pressing time to 5min, and the pressing time to 15min. The length, width, and height of the first mold 6 are 200mm, 40mm, and 2mm, respectively; the length, width, and height of the second mold 4 are 200mm, 140mm, and 3mm, respectively, and the length, width, and height of the internal cuboid cutting part are 150mm, 25mm, and 3mm, respectively; the length, width, and height of Type I PET film I 2 and Type I PET film II 8 are 297mm, 210mm, and 0.3mm, respectively; the length, width, and height of Type II PET film I 3 and Type II PET film II 7 are 210mm, 148mm, and 0.03mm, respectively; the length, width, and height of Type III PET film 5 are 148mm, 105mm, and 0.001mm, respectively; and the thickness of Type IV PET film is 0.001mm, with its length and width determined according to the various faces of the cutting part 4-1. 2) Pre-treatment of the second mold: Use type 4 PET film to cover and fix the part of the second mold 4 that is in direct contact with the adhesive resin, so that the adhesive resin and the second mold 4 do not come into direct contact during high-temperature pressing; The type IV PET film can be fixed to the second mold by conventional methods in the art, such as by tape. Conventional tapes available in the art can be used, and will not be described in detail here. 3) Surface treatment of the first mold: The cleaned surface of the first mold 6, where it is bonded to the adhesive resin, is first coated with an acetic acid solution to remove residual grease and plastic. After the acetic acid solution dries naturally, the surface is cleaned a second time with anhydrous ethanol to ensure it is clean and free of contaminants. Finally, after the ethanol dries naturally, a 0.01-0.04 g / cm³ coating is applied to the surface. 3 The coupling agent KH550 was used, and after the surface was completely dry, the surface treatment of the first mold 6 was completed. The acetic acid was analytical grade acetic acid with a mass fraction of 36%, purchased from Xi'an Tianmao Chemical Co., Ltd. 4) Lower mold arrangement: Place the first flat vulcanizing mold 1 and the corresponding PET film into the flat vulcanizing apparatus, and place them from bottom to top in the following order: first flat vulcanizing mold 1, type I PET film I 2, type II PET film I 3, and second mold 4; wherein, the polar surface of type II PET film I 3 is placed upward and the non-polar surface is placed downward. 5) Place the sample: Place the adhesive resin particles into the two cuboid cutting parts 4-1 of the second mold 4 in step 4), ensuring that the particles can completely fill the hollow space of the second mold 4. It is expected that about 12 grams will be placed in each space. 6) Upper mold arrangement: Cover the upper surface of the second mold 4 in step 5) with a type III PET film 5, covering 50% of the surface area of ​​the longitudinal side of the cutting part 4-1 of the second mold 4; place two first molds 6 in parallel at the center of the two cuboid cutting parts 4-1 of the second mold 4 to ensure that the adhesive resin adheres to the corresponding position of the first mold 6. Place the type II PET film II 7, type I PET film II 8 and the second flat vulcanizing mold 9 on top of the first mold 6 from bottom to top, and then place them between the two plates of the flat vulcanizing machine; wherein the non-polar surface of the type II PET film II 7 faces upward and the polar surface faces downward. 7) High-temperature pressing: The flat vulcanizing apparatus with the temperature stabilized and other parameters set performs preheating, degassing, high-temperature and high-pressure pressing, and sampling and cooling of the sample after the above preparation work is completed according to the set program. 8) Sample post-processing: Remove the sample prepared in step 7) from the flat vulcanizer, remove the type I PET film, type II PET film, and type III PET film 5, trim the burrs that overflow the sample, remove the bonding resin and the first mold 6 from the second mold 4, bend the free end of the bonding resin that is not bonded to the first mold 6 (i.e. the part covered by type III PET film 5) backward by 180°, so that the sample can meet the test method specified in the national standard GB / T 2790-1995, and complete the sample preparation work for determining the bonding performance of the bonding resin to metal.

[0038] In step 8), the Type IV PET film is generally undamaged and does not need to be removed if it is undamaged. If it is damaged, a new Type IV PET film needs to be replaced for the next use.

[0039] Step 7) includes preheating, venting, high-temperature and high-pressure pressing, and sampling and cooling. The preheating temperature is 180±2℃, preheating for 5 min, pressure is 15MPa, venting is performed 6 times to remove all gas, and then pressurizing at 15MPa for 15 min. After the mold is removed, it is placed in a vulcanizing apparatus at room temperature and cooled by water for 20 min to 1 h to reduce the temperature to below 50℃.

[0040] like Figure 1 As shown, a sample for determining the bonding performance of the bonding resin to metal is prepared by the above method. The sample includes a first flat vulcanizing mold 1 and a second flat vulcanizing mold 9 with a planar structure. A second mold 4 is set on the first flat vulcanizing mold 1. Two parallel cuboids are cut through the interior of the second mold 4. The inner walls of the cuboid cutting parts 4-1 are covered and isolated by a type IV PET film with their polar faces facing the bonding resin side. The first mold 6, consisting of two sheet-like cuboids, is placed parallel to each other at the center of the two cuboid cutting parts 4-1 of the second mold 4. The cuboid cutting parts 4-1 of the second mold 4 are filled with bonding resin particles. The second flat vulcanizing mold 9 is set above the first and second molds 4.

[0041] like Figure 2 As shown, two parallel cuboids are cut through the interior of the second mold 4 from top to bottom.

[0042] The surface of the first mold 6 is coated with a coupling agent, namely KH550, and the coating amount is (0.01-0.04) g / cm³. 3 .

[0043] Between the first flat vulcanizing mold 1 and the second mold 4, a type I PET film I 2 and a type II PET film I 3 are arranged sequentially from bottom to top. Between the first mold 6 and the second flat vulcanizing mold 9, a type II PET film II 7 and a type I PET film II 8 are arranged sequentially from bottom to top. The type I PET film I 2 and the type I PET film II 8 are double-sided non-polar PET thick films. The type II PET film I 3 and the type II PET film II 7 are PET thin films with one side polar and the other side non-polar. The non-polar side of the type II PET film I 3 faces the first flat vulcanizing mold 1, and the non-polar side of the type II PET film II 7 faces the second flat vulcanizing mold 9. The polar sides of the type II PET film I 3 and the type II PET film II 7 both face the first mold 6 and the second mold 4. The type III PET film 5 is a PET ultra-thin film with one side polar and the other side non-polar. Its polar side faces the side of the second mold 4 containing the adhesive resin, thus partially isolating the first mold 6 and the adhesive resin sample.

[0044] Two first molds 6 are fitted with a type 3 PET film 5. After the second mold 4 is filled with a bonding resin sample, the type 3 PET film 5 longitudinally covers 50% of the surface area of ​​one side below the first mold 6.

[0045] like Figure 3 As shown, after high-temperature pressing and sample preparation in a flat vulcanizing apparatus, the adhesive resin and the first mold 6 are taken out as samples. The samples are then tested according to GB / T 2790-1995. Specifically, the free end A of the adhesive resin sample not bonded to the first mold 6 (i.e., the part covered by the type 3 PET film 5) is bent backward by 180°. The B end of the first mold 6 is fixed to a clamp below a tensile testing machine (such as a ZWICK BTE-TC02.00 tensile testing machine), and the A end of the adhesive resin is fixed to a clamp above the tensile testing machine. The adhesive resin is at a 180° angle to the first mold 6. Tension is applied at the speed specified in GB / T 2790-1995 to peel the adhesive resin off the first mold 6. The peel strength is calculated according to Clause 8 of GB / T 2790-1995.

[0046] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Any equivalent substitutions or modifications made by those skilled in the art within the spirit and principle of the present invention without any creative effort should be included within the protection scope of the present invention.

Claims

1. A sample for determining the bonding performance of a bonding resin to a metal, comprising a first flat vulcanizing mold (1) and a second flat vulcanizing mold (9) with planar structures, wherein the first flat vulcanizing mold (1) serves as the lower mold and the second flat vulcanizing mold (9) serves as the upper mold, characterized in that: A second mold (4) is set on a first flat vulcanizing mold (1). At least two parallel cuboids are cut through the inside of the second mold (4) from top to bottom. The inner walls of the cuboid cutting parts (4-1) are covered and isolated by a type 4 PET film. A number of sheet-shaped cuboid first molds (6) are placed parallel to the center of the cuboid cutting parts (4-1) of the second mold (4). The cuboid cutting parts (4-1) of the second mold (4) are filled with adhesive resin particles. The second flat vulcanizing mold (9) is set above the first mold (6) and the second mold (4). A type 3 PET film (5) is set below the first mold (6). After the second mold (4) is filled with the adhesive resin sample, the type 3 PET film (5) longitudinally covers 50% of the surface area of ​​the side below the first mold (6). The type 3 PET film (5) is a PET ultra-thin film with one polar side and one non-polar side. Its polar side faces the side of the second mold (4) containing the adhesive resin, partially isolating the first mold (6) and the adhesive resin sample. Between the first flat vulcanizing mold (1) and the second mold (4), a type I PET film I (2) and a type II PET film I (3) are arranged sequentially from bottom to top. Between the first mold (6) and the second flat vulcanizing mold (9), a type II PET film II (7) and a type I PET film II (8) are arranged sequentially from bottom to top. The type I PET film is a thick PET film with non-polarity on both sides, and the type II PET film is a PET film with one polarity and one non-polarity. The non-polar side of the type II PET film I (3) faces the first flat vulcanizing mold (1), and the non-polar side of the type II PET film II (7) faces the second flat vulcanizing mold (9). The polar sides of the type II PET film I (3) and the type II PET film II (7) face the second mold (4) and the first mold (6), respectively. There are two cuboid cutting parts (4-1), and the first mold consists of two pieces (6); the inner wall of the cuboid cutting part (4-1) of the second mold (4) is covered and isolated by a type 4 PET film, which is isolated between the adhesive resin and the second mold (4). The type 4 PET film includes a polar surface and a non-polar surface, and its polar surface faces the adhesive resin.

2. The sample for determining the bonding performance of the bonding resin to metal according to claim 1, characterized in that: Type I PET film has a thickness greater than 0.2 mm, Type II PET film has a thickness of 0.03-0.2 mm, and Type III PET film (5) and Type IV PET film have a thickness of <0.05 mm.

3. The sample for determining the bonding performance of the bonding resin to metal according to claim 2, characterized in that: The length, width, and height of the first mold (6) are 200mm, 40mm, and 2mm, respectively; the length, width, and height of the second mold (4) are 200mm, 140mm, and 3mm, respectively, and the length, width, and height of the internal cuboid cut are 150mm, 25mm, and 3mm, respectively; the length, width, and height of Type I PET film I (2) and Type I PET film II (8) are 297mm, 210mm, and 0.3mm, respectively; the length, width, and height of Type II PET film I (3) and Type II PET film II (7) are 210mm, 148mm, and 0.03mm, respectively; the length, width, and height of Type III PET film (5) are 148mm, 105mm, and 0.001mm, respectively; and the thickness of Type IV PET film is 0.001mm, with the length and width determined according to the cutting part (4-1) on each side.

4. The sample for determining the bonding performance of the bonding resin to metal according to claim 2 or 3, characterized in that: The surface of the first mold (6) is coated with a coupling agent, which is one or more of vinyltrimethoxysilane, vinyltri(2-methoxyethoxy)silane, vinyltriethoxysilane, γ-glycidyl ether propyltrimethoxysilane, γ-methacryloyl oxypropyltrimethoxysilane, and γ-aminopropyltriethoxysilane, with a coating amount of 0.01-0.04 g / cm³. 3 .

5. The sample for determining the bonding performance of the bonding resin to metal according to claim 1, characterized in that: The bonding resin is a resin with metal bonding properties, including one or more of polyethylene grafted maleic anhydride particles, polyethylene grafted acrylic acid particles, polypropylene grafted maleic anhydride particles, polypropylene grafted acrylic acid particles, epoxy resin, polyurethane resin, and acrylic resin.

6. The method for preparing a sample for determining the bonding performance of an adhesive resin to a metal according to any one of claims 1-5, characterized in that, After setting the parameters of the flat vulcanizer, the inner wall of the cutting part (4-1) of the second mold (4) is covered with the four-type PET film. Then, the lower surface of the first mold (6) is cleaned and coated with coupling agent. After drying, the first flat vulcanizing mold (1), the first type PET film I (2), the second type PET film I (3), and the second mold (4) are assembled in sequence and the adhesive resin particles are inserted into the cutting part (4-1). Then, the third type PET film (5), the first mold (6), the second type PET film II (7), the first type PET film II (8), and the second flat vulcanizing mold (9) are installed. The obtained sample is placed in the flat vulcanizer and pressed at high temperature. After pressing, the first mold (6) bonded with the adhesive resin is taken out for testing.

7. The method for preparing a sample for determining the bonding performance of an adhesive resin to a metal according to claim 6, characterized in that, Specifically, the following steps are included: 1) Pretreatment: Prepare a clean first mold (6) and a second mold (4); clean the inner surfaces of the flat plate vulcanizer and the first flat plate vulcanizing mold (1) and the second flat plate vulcanizing mold (9); prepare bonding resin of corresponding quality; prepare sufficient type I, type II, type III and type IV PET films; preset the temperature of the flat plate vulcanizer to 180℃, the pressure to 15MPa, the pre-pressing time to 5min, and the pressing time to 15min. 2) Pre-treatment of the second mold: Use type 4 PET film to cover and fix the part of the second mold (4) that is in direct contact with the adhesive resin; 3) Surface treatment of the first mold: The surface of the first mold (6) to be bonded with the adhesive resin is first coated with an acetic acid solution to clean the residual grease and plastic on the surface of the first mold (6). After the acetic acid solution dries naturally, the surface is cleaned a second time with anhydrous ethanol to ensure that the surface is clean and free of dirt. After the ethanol dries naturally, a 0.01-0.04 g / cm³ coating is finally applied to the surface. 3 The coupling agent KH550 was used. After the surface was completely dry, the surface treatment of the first mold (6) was completed. 4) Lower mold arrangement: Place the first flat vulcanizing mold (1) and the corresponding PET film into the flat vulcanizing instrument, and place them from bottom to top in the order of first flat vulcanizing mold (1), type I PET film I (2), type II PET film I (3), and second mold (4); wherein, the polar surface of type II PET film I (3) is placed upward and the non-polar surface is placed downward. 5) Place the sample: Place the adhesive resin particles into the two cuboid cutting parts (4-1) of the second mold (4) in step 4), ensuring that the particles can completely fill the hollow space of the second mold (4); 6) Upper mold arrangement: Cover the upper surface of the second mold (4) in step 5) with a type III PET film (5), covering 50% of the surface area of ​​the cutting part (4-1) of the second mold (4) on one longitudinal side; place two first molds (6) in parallel at the center of the two cuboid cutting parts (4-1) of the second mold (4), ensuring that the adhesive resin adheres to the corresponding position of the first mold (6), and place the second mold (6) above the first mold (6) from bottom to top in the order of type II PET film II (7), type I PET film II (8), and second flat vulcanizing mold (9), and then place it between the two plates of the flat vulcanizing apparatus; wherein the non-polar surface of type II PET film II (7) is facing upward and the polar surface is facing downward; 7) High-temperature pressing: The flat vulcanizing apparatus, with the temperature stabilized and other parameters set, performs preheating, degassing, high-temperature and high-pressure pressing, and sampling and cooling of the prepared sample according to the set program. 8) Sample post-processing: Remove the sample prepared in step 7) from the flat vulcanizer, remove the type I PET film, type II PET film and type III PET film (5), trim the burrs that overflow the sample, remove the bonding resin and the first mold (6) from the second mold (4), bend the free end of the bonding resin that is not bonded to the first mold (6) backward by 180°, and complete the preparation of the sample for determining the bonding performance of the bonding resin to the metal.

8. The method for preparing a sample for determining the bonding performance of an adhesive resin to a metal according to claim 7, characterized in that: Step 7) includes preheating, venting, high-temperature and high-pressure pressing, and sampling and cooling. The preheating temperature is 180±2℃, preheating time is 5 minutes, pressure is 15MPa, venting is performed 6 times to remove all gas, and then pressurizing at 15 MPa for 15 minutes. After removing the mold, it is placed in a vulcanizing apparatus at room temperature and cooled by water for 20 minutes to 1 hour until the temperature drops to below 50℃.

Images