Low roughness, low silicon MLCC release agent and MLCC release film

Abstract

The present invention discloses a low-roughness, low-silicon MLCC release agent and MLCC release film. The release agent comprises the following components by weight: 8-12 parts of alkyd resin, 0.8-1.2 parts of modified silicone additive, 2-4 parts of curing agent, 1-2 parts of catalyst, and 80-90 parts of solvent. Alkyd resin is used as the main resin in the release agent. The alkyd resin is formed by condensation of a large amount of weak polar oil. Its surface tension can reach as low as 20mN / m. The lower the surface tension of the resin, the more conducive it is to spreading the resin on the substrate, thereby effectively reducing the surface roughness of the release film. As the oil content of the alkyd resin increases, the polarity and surface tension of the alkyd resin will decrease, so that the prepared release agent solution has better wettability with the substrate, thereby further reducing the surface roughness of the release film.

Description

Technical Field

[0001] The present invention relates to the field of release materials, and in particular to a low-roughness, low-silicon MLCC release agent and an MLCC release film. Background Art

[0002] MLCC, short for multilayer ceramic capacitor, is a basic passive electronic component. With the rapid development of 5G communications and new energy vehicles, the use of MLCCs has increased dramatically. The MLCC manufacturing process involves evenly coating a ceramic slurry onto a release film. After drying, electrodes are printed on the surface of the ceramic layer. After the release film is removed, the ceramic layer undergoes a series of processes, including lamination, capping, lamination, binder removal, sintering, chamfering, termination, burn-in, terminal processing, appearance selection, testing, and packaging. As a high-consumption auxiliary material in the MLCC manufacturing process, MLCC release film fluctuates in tandem with MLCC production volume, and the market is showing a clear expansion trend. The current minimum ceramic layer thickness can be 2μm, which places high demands on the roughness of the MLCC release film itself, but commercially available release film products often fail to meet this requirement.

[0003] Existing low-silicon or non-silicon release agents on the market are generally based on acrylic or epoxy resin systems. Acrylic and epoxy resins have high polarity, resulting in poor wettability on substrates such as PET, resulting in a rough surface finish. This limits the application of these release agents in high-end MLCC release films. Alkyd resins are generally produced through the polycondensation of polyols, polyacids, and fatty acids (vegetable oils). Fatty acids (vegetable oils) are weakly polar substances. Since alkyd resins generally have lower polarity than acrylic, amino, and epoxy resins, alkyd resins exhibit better wettability on substrates (such as PET). Oil content is a key concept in alkyd resins. Oil content (OL) is the ratio of the amount of oil in the alkyd resin formula to the theoretical yield of the resin. Generally, higher oil content indicates lower polarity. Summary of the Invention

[0004] The technical problem to be solved by the present invention is to provide a low-roughness, low-silicon MLCC release agent and MLCC release film in response to the deficiencies in the above-mentioned prior art.

[0005] In order to solve the above technical problems, the technical solution adopted by the present invention is: a low-roughness, low-silicon MLCC release agent, comprising the following components in parts by weight: 8-12 parts of alkyd resin, 0.8-1.2 parts of modified silicone additive, 2-4 parts of curing agent, 1-2 parts of catalyst, and 80-90 parts of solvent.

[0006] Preferably, the alkyd resin is one or more of SA1203 alkyd resin, SA1202 alkyd resin, SA1201 alkyd resin, and SA1101 alkyd resin.

[0007] Preferably, the curing agent is an amino resin.

[0008] Preferably, the curing agent is 303LF amino resin.

[0009] Preferably, the modified silicone additive is BYK-377.

[0010] Preferably, the catalyst is p-toluenesulfonic acid.

[0011] Preferably, the solvent is xylene.

[0012] The present invention also provides a low-roughness, low-silicon MLCC release film, which is prepared by the following method:

[0013] S1. Prepare the release agent as described above: uniformly mix an alkyd resin, a modified silicone additive, a curing agent, a catalyst, and a solvent to obtain a release agent;

[0014] S2. The release agent obtained in step S1 is evenly coated on the substrate, and cured by first gradually increasing the temperature and then gradually decreasing the temperature to obtain the low-roughness, low-silicon MLCC release film.

[0015] Preferably, in step S2, the coating speed is 30-100 m / min, and the curing temperatures are set to 60°C, 80°C, 120°C, 140°C, 140°C, 110°C, 100°C, and 80°C in sequence.

[0016] Preferably, the substrate is a PET substrate.

[0017] The beneficial effects of the present invention are:

[0018] The present invention provides a low-roughness, low-silicon MLCC release agent and MLCC release film. The release agent uses an alkyd resin as the main resin. The alkyd resin is formed by condensation of a large amount of weakly polar oils and fats, and its surface tension can reach as low as 20mN / m. The lower the surface tension of the resin, the more conducive it is to spreading the resin on the substrate, thereby effectively reducing the surface roughness of the release film. Moreover, as the oil content of the alkyd resin increases, the polarity and surface tension of the alkyd resin decrease, so that the prepared release agent solution has better wettability with the substrate, thereby further reducing the surface roughness of the release film.

[0019] The release agent of the present invention, by adding modified silicone oil BYK-377, can improve the compatibility of silicone oil and main resin, reduce surface roughness and significantly reduce release force, thereby achieving better use effect;

[0020] The release film product of the present invention can meet the stringent requirements of MLCC release films on surface roughness and has broad market application prospects. DETAILED DESCRIPTION

[0021] The present invention is further described in detail below with reference to the embodiments so that those skilled in the art can implement the invention with reference to the description.

[0022] It should be understood that terms such as “having”, “including” and “comprising” used herein do not preclude the existence or addition of one or more other elements or combinations thereof.

[0023] Unless otherwise specified, the experimental methods used in the following examples are conventional methods. Materials and reagents used in the following examples are commercially available unless otherwise specified. In the following examples, where specific conditions are not specified, the experiments were conducted under conventional conditions or those recommended by the manufacturer. Reagents and instruments used, where the manufacturer is not specified, are commercially available conventional products.

[0024] The present invention provides a low-roughness, low-silicon MLCC release agent, comprising the following components in parts by weight: 8-12 parts of alkyd resin, 0.8-1.2 parts of modified silicone additive, 2-4 parts of curing agent, 1-2 parts of catalyst, and 80-90 parts of solvent.

[0025] In a preferred embodiment, the alkyd resin is one or more of SA1203 alkyd resin, SA1202 alkyd resin, SA1201 alkyd resin, and SA1101 alkyd resin.

[0026] In a preferred embodiment, the curing agent is an amino resin, and more preferably, the curing agent is 303LF amino resin.

[0027] In a preferred embodiment, the modified organic silicon auxiliary agent is BYK-377 (polyether-modified polydimethylsiloxane solution containing hydroxyl functional groups).

[0028] In a preferred embodiment, the catalyst is p-toluenesulfonic acid.

[0029] In a preferred embodiment, the solvent is xylene.

[0030] The present invention also provides a low-roughness, low-silicon MLCC release film, which is prepared by the following method:

[0031] S1. Prepare the release agent as above: mix alkyd resin, modified silicone additive, curing agent, catalyst, and solvent to obtain a release agent;

[0032] S2. The release agent obtained in step S1 is evenly coated on the substrate, and cured by gradually increasing the temperature and then gradually decreasing the temperature to obtain a low-roughness, low-silicon MLCC release film.

[0033] In a preferred embodiment, in step S2, the coating speed is 30-100 m / min, and the curing temperatures are set to 60°C, 80°C, 120°C, 140°C, 140°C, 110°C, 100°C, and 80°C in sequence.

[0034] In a preferred embodiment, the substrate is a PET substrate.

[0035] The above is the overall concept of the present invention. Detailed embodiments and comparative examples are provided below to further illustrate the present invention.

[0036] The sources of the main raw materials in the following examples and comparative examples are as follows:

[0037] Alkyd resin: SA1203 oil content 60%, SA1202 oil content 65%, SA1201 oil content 70%, SA1101 oil content 75%), Smet Chemical Industries Co., Ltd.

[0038] Amino resin: Model 303LF, Zhanxin Resin (China) Co., Ltd.

[0039] Polyether-modified polydimethylsiloxane solution containing hydroxyl groups BYK-377, BYK Chemicals;

[0040] Hydroxyl-containing acrylic resin: CFU2460B, Weifang Fule New Materials Co., Ltd.

[0041] p-Toluenesulfonic acid, xylene, and PET substrate are all conventional commercially available products.

[0042] Example 1

[0043] A low-roughness, low-silicon MLCC release film is prepared by the following method:

[0044] S1. Weigh 9 parts of SA1203 alkyd resin, 1 part of BYK-377 additive, 2 parts of 303LF resin, and 1 part of p-toluenesulfonic acid, then add 87 parts of xylene and stir thoroughly until completely dissolved to obtain a release agent;

[0045] S2. The release agent obtained in step S1 is evenly coated on the PET substrate and cured by gradient heating and then gradient cooling. The coating speed is 40m / min. The temperature settings during multi-step gradient heating curing are: 60℃, 80℃, 120℃, 140℃, 140℃, 110℃, 100℃, and 80℃, respectively. After curing, a low-roughness, low-silicon MLCC release film is obtained.

[0046] Example 2

[0047] A low-roughness, low-silicon MLCC release film is prepared by the following method:

[0048] S1. Weigh 9 parts of SA1202 alkyd resin, 1 part of BYK-377 additive, 2 parts of 303LF resin, and 1 part of p-toluenesulfonic acid, then add 87 parts of xylene and stir thoroughly until completely dissolved to obtain a release agent;

[0049] S2. The release agent obtained in step S1 is evenly coated on the PET substrate and cured by gradient heating and then gradient cooling. The coating speed is 40m / min. The temperature settings during multi-step gradient heating curing are: 60℃, 80℃, 120℃, 140℃, 140℃, 110℃, 100℃, and 80℃, respectively. After curing, a low-roughness, low-silicon MLCC release film is obtained.

[0050] Example 3

[0051] A low-roughness, low-silicon MLCC release film is prepared by the following method:

[0052] S1. Weigh 9 parts of SA1201 alkyd resin, 1 part of BYK-377 additive, 2 parts of 303LF resin, and 1 part of p-toluenesulfonic acid, then add 87 parts of xylene and stir thoroughly until completely dissolved to obtain a release agent;

[0053] S2. The release agent obtained in step S1 is evenly coated on the PET substrate and cured by gradient heating and then gradient cooling. The coating speed is 40m / min. The temperature settings during multi-step gradient heating curing are: 60℃, 80℃, 120℃, 140℃, 140℃, 110℃, 100℃, and 80℃, respectively. After curing, a low-roughness, low-silicon MLCC release film is obtained.

[0054] Example 4

[0055] A low-roughness, low-silicon MLCC release film is prepared by the following method:

[0056] S1. Weigh 9 parts of SA1101 alkyd resin, 1 part of BYK-377 additive, 2 parts of 303LF resin, and 1 part of p-toluenesulfonic acid, then add 87 parts of xylene and stir thoroughly until completely dissolved to obtain a release agent;

[0057] S2. The release agent obtained in step S1 is evenly coated on the PET substrate and cured by gradient heating and then gradient cooling. The coating speed is 40m / min. The temperature settings during multi-step gradient heating curing are: 60℃, 80℃, 120℃, 140℃, 140℃, 110℃, 100℃, and 80℃, respectively. After curing, a low-roughness, low-silicon MLCC release film is obtained.

[0058] Comparative Example 1

[0059] An MLCC release film is prepared by the following method:

[0060] S1. Weigh 9 parts of CFU2460B acrylic resin, 1 part of BYK-377 additive, 2 parts of 303LF resin, and 1 part of p-toluenesulfonic acid, then add 87 parts of xylene and stir thoroughly until completely dissolved to obtain a release agent.

[0061] S2. The release agent obtained in step S1 is evenly coated on the PET substrate and cured by gradient heating and then gradient cooling. The coating speed is 40m / min. The temperature settings during multi-step gradient heating curing are: 60℃, 80℃, 120℃, 140℃, 140℃, 110℃, 100℃, and 80℃, respectively. After curing, a low-roughness, low-silicon MLCC release film is obtained.

[0062] Comparative Example 2

[0063] A low-roughness, low-silicon MLCC release film is prepared by the following method:

[0064] S1. Weigh 10 parts of SA1203 alkyd resin, 2 parts of 303LF resin, and 1 part of p-toluenesulfonic acid, then add 87 parts of xylene and stir thoroughly until completely dissolved to obtain a release agent;

[0065] S2. The release agent obtained in step S1 is evenly coated on the PET substrate and cured by gradient heating and then gradient cooling. The coating speed is 40m / min. The temperature settings during multi-step gradient heating curing are: 60℃, 80℃, 120℃, 140℃, 140℃, 110℃, 100℃, and 80℃, respectively. After curing, a low-roughness, low-silicon MLCC release film is obtained.

[0066] The release film products prepared in Examples 1-4 and Comparative Examples 1-2 were tested for release force (31B standard tape) and surface roughness:

[0067] The test method or standard for release force is as follows: stick the standard tape 31B on the release surface of the release material, roll it back and forth twice with a 2 kg roller (speed: 300 mm / min), and then let it stand. 20min The release force value after the test is the 20min quick release force

[0068] The surface roughness test method or standard is as follows: Take the release film to be tested and clean it to remove any impurities or stains that may affect the test results. After aligning the white-light interferometer with the sample area, adjust the laser to form a parallel beam between it and the reflector above the sample. Move the reflector below the sample to an appropriate position to form interference fringes. Gradually adjust the length of the reference arm until the optimal interference pattern is achieved. Move the sample to the center of the interference fringes and record the reading at this point. Then move the sample slightly and record the reading again.

[0069] The test results are shown in Table 1 below:

[0070] Table 1

[0071]

[0072]

[0073] Among them, Ra is the arithmetic mean deviation of the contour, Rp is the maximum contour peak height, and Rz is the height of the ten points of the unevenness observed.

[0074] According to the test results in Table 1, when modified silicone oil 377 is not added (Comparative Example 2), the release force of the release film is as high as 738.5 gf / 25 mm. After adding modified silicone oil 377, the release force drops significantly to about 10 gf / 25 mm (Examples 1-4).

[0075] When the main resin is acrylic resin (Comparative Example 1), the surface roughness Ra of the release film is as high as 35nm, while when an alkyd resin with an oil content of 60% is used (Example 1), the surface roughness of the film is reduced to 25nm, and as the oil content of the alkyd resin increases from 60% to 75%, the surface roughness of the film decreases from 25nm to 13nm (Examples 2-4); the surface roughness of the release film prepared by the alkyd resin with a higher oil content is lower. This is because the higher the oil content, the lower the polarity and surface tension of the alkyd resin, which makes the prepared release agent solution have better wettability with the substrate, thereby greatly reducing the surface roughness of the release film.

[0076] Although the embodiments of the present invention have been disclosed above, they are not limited to the applications listed in the description and implementation methods. They can be fully applied to various fields suitable for the present invention. For those familiar with the art, additional modifications can be easily implemented. Therefore, without departing from the general concept defined by the claims and the scope of equivalents, the present invention is not limited to specific details.

Claims

1. A low-roughness, low-silicon MLCC release agent, characterized in that: The invention comprises the following components in parts by weight: 8-12 parts of alkyd resin, 0.8-1.2 parts of modified silicone additive, 2-4 parts of curing agent, 1-2 parts of catalyst, and 80-90 parts of solvent; The alkyd resin is one or more of SA1203 alkyd resin, SA1202 alkyd resin, SA1201 alkyd resin, and SA1101 alkyd resin; The curing agent is 303LF amino resin; The modified silicone additive is BYK-377.

2. The low-roughness, low-silicon MLCC release agent according to claim 1, characterized in that The catalyst is p-toluenesulfonic acid.

3. The low-roughness, low-silicon MLCC release agent according to claim 1, characterized in that The solvent is xylene.

4. A low-roughness, low-silicon MLCC release film, characterized in that: It is prepared by the following method: S1. Prepare the release agent according to any one of claims 1 to 3: uniformly mix an alkyd resin, a modified silicone additive, a curing agent, a catalyst, and a solvent to obtain a release agent; S2. The release agent obtained in step S1 is evenly coated on the substrate, and cured by first gradually increasing the temperature and then gradually decreasing the temperature to obtain the low-roughness, low-silicon MLCC release film.

5. The low-roughness, low-silicon MLCC release film according to claim 4, characterized in that: In step S2, the coating speed is 30-100 m / min, and the curing temperature is set to 60°C, 80°C, 120°C, 140°C, 140°C, 110°C, 100°C, and 80°C in sequence.

6. The low-roughness, low-silicon MLCC release film according to claim 4, characterized in that: The substrate is a PET substrate.

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