CN115975464A - Composition for preparing high-temperature-resistant adhesion promoter and preparation method of high-temperature-resistant adhesion promoter - Google Patents

Composition for preparing high-temperature-resistant adhesion promoter and preparation method of high-temperature-resistant adhesion promoter Download PDF

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CN115975464A
CN115975464A CN202211711661.6A CN202211711661A CN115975464A CN 115975464 A CN115975464 A CN 115975464A CN 202211711661 A CN202211711661 A CN 202211711661A CN 115975464 A CN115975464 A CN 115975464A
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silane coupling
coupling agent
nano
temperature
adhesion promoter
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CN115975464B (en
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张岳
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Shanghai Parylene Biotechnology Co ltd
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Shanghai Parylene Biotechnology Co ltd
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Abstract

The application provides a composition for preparing a high-temperature-resistant adhesion promoter and a preparation method of the high-temperature-resistant adhesion promoter, and belongs to the technical field of protective materials. The composition comprises: the acidic hydrolysis catalyst, the first silane coupling agent, the second silane coupling agent, the nano metal oxide, the adhesive and the solvent are separately stored. The first silane coupling agent comprises tetraethyl orthosilicate and the second silane coupling agent comprises at least one of 3-methacryloxypropyltrimethoxysilane and 3-acryloxypropyltrimethoxysilane. The high-temperature-resistant adhesion promoter formed after uniformly mixing the components in the composition for preparing the high-temperature-resistant adhesion promoter has better heat resistance, can be simultaneously and stably connected with a parylene coating and a device to be protected even in a high-temperature environment, and is favorable for ensuring the protection effect of the parylene coating on the device to be protected at high temperature.

Description

Composition for preparing high-temperature-resistant adhesion promoter and preparation method of high-temperature-resistant adhesion promoter
Technical Field
The application relates to the technical field of protective materials, in particular to a composition for preparing a high-temperature-resistant adhesion promoter and a preparation method of the high-temperature-resistant adhesion promoter.
Background
The parylene coating is widely used as a protective coating on the surface of an electronic component at present because of good waterproof effect. Due to the fact that the molecular structure of the parylene is very symmetrical, charge separation in parylene molecules is not remarkable, and the parylene is connected with the surface of an electronic component through weak electrostatic adsorption, so that the adhesion force of the parylene coating on the surface of the electronic component is weak.
In order to improve the adhesion of the parylene coating to the surface of the electronic component, the current method for forming the parylene coating is as follows: selecting a silane coupling agent A174 (namely 3-methacryloxypropyl trimethoxy silane) as an adhesion promoter, and adding the adhesion promoter into dimeric p-xylene; in the process of forming a parylene coating deposited on the surface of an electronic component by polymerization after the gasification and pyrolysis of the dimeric paraxylene, a methacrylate group at one end of an A174 molecular structure can be polymerized into a parylene framework in a free radical form to change the charge distribution on the parylene framework, so that the parylene framework is more polar, and the electrostatic adsorption between the parylene coating and the surface of the electronic component is greatly improved; the trimethoxy silane at the other end of the A174 molecular structure can be hydrolyzed into a silanol structure under the condition of contacting with water vapor, and the silanol structure formed by the A174 molecules can form covalent connection with hydroxyl on the surface of an electronic component, so that the adhesion of the parylene coating to the surface of the electronic component is improved.
However, the hydroxyl group-containing material is generally glass, metal oxide, metal hydroxide, or some pure metal with a passivated surface, and when the surface material of the electronic component is plastic, the silanol structure formed by the a174 molecule cannot form covalent bonds with the plastic.
In addition, with the continuous increase of the power consumption of the electronic component, the heat generation of the electronic component is also large, so that the electronic component can be operated in a high-temperature environment (for example, 100-150 ℃) for a long time, and the trimethoxysilane in the A174 molecular structure can not be hydrolyzed into a silanol structure under the high-temperature environment, so that the parylene coating can not form covalent connection with the hydroxyl on the surface of the electronic component; and the electrostatic adsorption effect of the parylene coating and the surface of the electronic component is very easily damaged in a high-temperature environment, so that the parylene coating can fall off from the surface of the electronic component, and the electronic component cannot be effectively protected.
Disclosure of Invention
The application aims to provide a composition for preparing a high-temperature-resistant adhesion promoter and a preparation method of the high-temperature-resistant adhesion promoter, and aims to improve the adhesion of a parylene coating to the surface of a to-be-protected device (including the condition that the surface material is plastic) in a high-temperature environment (such as 100-150 ℃).
In a first aspect, embodiments of the present application provide a composition for preparing a high temperature adhesion promoter, comprising: the acid hydrolysis catalyst, the silane coupling compound, the nano metal oxide, the adhesive and the solvent are separately stored.
The silane coupling material comprises a first silane coupling agent and a second silane coupling agent; the first silane coupling agent comprises at least one of tetraethyl orthosilicate, tetrapropyl orthosilicate, tetrabutyl orthosilicate and tetraisopropyl orthosilicate, and the second silane coupling agent comprises at least one of 3-methacryloxypropyltrimethoxysilane, 3-acryloxypropyltrimethoxysilane, methacryloxypropyltriisopropoxysilane, methacryloxypropylmethyldiethoxysilane, 3-methacryloxypropylmethyldimethoxysilane and methacryloxypropyltriethoxysilane.
The components in the composition provided by the application are uniformly mixed to prepare the high-temperature-resistant adhesion promoter, and the high-temperature-resistant adhesion promoter is used for coating the surface of a device to be protected and drying the surface to form a film layer before the deposition of the parylene coating. Wherein the acidic hydrolysis catalyst can hydrolyze the first silane coupling agent and the second silane coupling agent. The nano metal oxide has higher heat resistance, can improve the heat resistance of the adhesion promoter, has hydroxyl groups on the surface, and can provide connecting sites for the hydrolyzed first silane coupling agent and the hydrolyzed second silane coupling agent. The hydrolyzed first silane coupling agent has a silicon-oxygen-silicon bond, so that the heat resistance of the adhesion promoter can be improved, and the hydrolyzed first silane coupling agent can also provide a bridge function to firmly connect the nano metal oxide and the hydrolyzed second silane coupling agent together. The hydrolyzed second silane coupling agent also provides a bridge function, so that the adhesion force between the nano metal oxide (or the hydrolyzed first silane coupling agent) and the parylene coating can be improved, and the adhesion promoter can be stably connected with the parylene coating. The adhesive can bond the nano metal oxides together and can firmly bond with the surface of the device to be protected. The presence of the solvent facilitates the full dispersion of the components and also facilitates the coating of the adhesion promoter on the surface of the device to be protected.
The high-temperature-resistant adhesion promoter formed by uniformly mixing the components in the composition for preparing the high-temperature-resistant adhesion promoter can be used for simultaneously and stably connecting the parylene coating with a device to be protected (including the condition that the surface of the device to be protected is made of plastic), has better heat resistance, is beneficial to avoiding the condition that the adhesion of the parylene coating to the device to be protected is weaker in a high-temperature environment (such as 100-150 ℃), and the parylene coating is easy to separate from the surface of the device to be protected, and is beneficial to ensuring the protection effect of the parylene coating to the device to be protected in a high-temperature environment (such as 100-150 ℃).
In an alternative embodiment of the present application in combination with the first aspect, the mass ratio of the acidic hydrolysis catalyst, the silane coupling agent, the nano metal oxide, the binder, and the solvent is (0.1-1): 7-30): 10-40): 15-45): 20-70, and the mass ratio of the first silane coupling agent to the second silane coupling agent is (1-4): 1.
Under the condition of the mixture ratio, the mixture ratio of each component in the composition is proper, so that each component can exert respective effect fully, the stability of the high-temperature-resistant adhesion promoter in connection with a parylene coating and a device to be protected can be improved synergistically, and the heat resistance of the high-temperature-resistant adhesion promoter can be improved.
Optionally, the mass ratio of the acidic hydrolysis catalyst, the silane coupling compound, the nano metal oxide, the adhesive and the solvent is (0.3-0.5): (12-22): (15-25): (25-35): (20-40).
Optionally, the mass ratio of the first silane coupling agent to the second silane coupling agent is (2-3): 1.
In an alternative embodiment of the present application in combination with the first aspect, the first silane coupling agent is tetraethyl orthosilicate and the second silane coupling agent is 3-methacryloxypropyl trimethoxysilane.
In the technical scheme, the first silane coupling agent is tetraethyl orthosilicate, the second silane coupling agent is 3-methacryloxypropyl trimethoxysilane, the two substances can be matched with each other, the hydrolyzed tetraethyl orthosilicate is favorable for more stably connecting the nano metal oxide and the hydrolyzed second silane coupling agent together, and the hydrolyzed 3-methacryloxypropyl trimethoxysilane is also favorable for more stably connecting the nano metal oxide (or the hydrolyzed tetraethyl orthosilicate) and the parylene coating together.
In an alternative embodiment of the present application in combination with the first aspect, the nano metal oxide is at least one selected from nano alumina, nano silica and nano zirconia.
The above substances all have strong heat resistance, are further favorable for improving the heat resistance of the high-temperature-resistant adhesion promoter, and can also be stably connected with the hydrolyzed first silane coupling agent and the hydrolyzed second silane coupling agent.
In an alternative embodiment of the present application in combination with the first aspect, the nano metal oxide is selected from nano alumina and nano silica.
In the technical scheme, the nano-alumina and the nano-silica have higher reaction activity and more hydroxyl groups on the surfaces thereof, so that the connection stability of the nano-alumina and the nano-silica with the hydrolyzed first silane coupling agent and the hydrolyzed second silane coupling agent is improved; and the nano aluminum oxide and the nano silicon dioxide can be matched with each other, so that the heat resistance of the high-temperature-resistant adhesion promoter can be further improved, the connection stability of the high-temperature-resistant adhesion promoter, the hydrolyzed first silane coupling agent and the hydrolyzed second silane coupling agent can be further improved, the structural strength of the whole high-temperature-resistant adhesion promoter can be improved, and the stability of the high-temperature-resistant adhesion promoter in connection with a parylene coating and a device to be protected can be further improved.
Optionally, the mass ratio of nano-alumina to nano-silica is (1-100): 1.
Optionally, the mass ratio of nano-alumina to nano-silica is (2-3): 1.
Optionally, the nano-alumina is in the alpha crystal form.
In an alternative embodiment of the present application in combination with the first aspect, the acidic hydrolysis catalyst comprises at least one of acetic acid, methacrylic acid, phosphoric acid, and trifluoroacetic acid.
The above-mentioned substance can rapidly hydrolyze the first silane coupling agent and the second silane coupling agent.
Optionally, the acidic hydrolysis catalyst is selected from at least one of acetic acid and trifluoroacetic acid.
In an alternative embodiment of the present application in combination with the first aspect, the adhesive includes at least one of a methacrylate copolymer and an acrylate copolymer.
The substances can ensure that the high-temperature-resistant adhesion promoter is stably connected with the surface of the device to be protected.
Optionally, the adhesive is selected from methacrylate copolymers.
Optionally, the adhesive is selected from a copolymer of n.n dimethylacrylamide and lauryl methacrylate.
Alternatively, the molecular weight of the copolymer of n.n dimethylacrylamide and lauryl methacrylate is 3 to 15 ten thousand, and the mass fraction of n.n dimethylacrylamide and lauryl methacrylate in the copolymer of n.n dimethylacrylamide and lauryl methacrylate is 50 to 70% and 30 to 50%, respectively.
In an alternative embodiment of the present application in combination with the first aspect, the solvent includes at least one of ethyl 3-ethoxypropionate, ethyl acetate, and butyl acetate.
The substances have good dissolving and dispersing effects on each component in the composition; the high-temperature resistant adhesion promoter is easy to volatilize after being coated.
Alternatively, the solvent is selected from butyl acetate.
In a second aspect, an embodiment of the present application provides a method for preparing a high temperature adhesion promoter, including: mixing the composition for preparing the high-temperature-resistant adhesion promoter provided by the first aspect.
Mixing the composition for preparing the high-temperature-resistant adhesion promoter provided by the first aspect to prepare the high-temperature-resistant adhesion promoter; when the high-temperature-resistant adhesive force promoter is used, the prepared high-temperature-resistant adhesive force promoter is coated on the surface of a device to be protected and dried, and then the parylene coating is deposited on the surface of the film layer formed by the high-temperature-resistant adhesive force promoter, the high-temperature-resistant adhesive force promoter can be simultaneously and stably connected with the parylene coating and the device to be protected, and the high-temperature-resistant adhesive force promoter has high heat resistance, is favorable for avoiding the condition that the parylene coating is weak in adhesive force to the device to be protected under a high-temperature environment (such as 100-150 ℃), so that the parylene coating is easy to separate from the surface of the device to be protected, and is favorable for ensuring the protection effect of the parylene coating to the device to be protected under the high-temperature environment (such as 100-150 ℃).
In an alternative embodiment of the present application in combination with the second aspect, the mixing is stirring mixing, the stirring and mixing time is 2-10min, and the stirring and mixing speed is 1500-2500rpm.
In the technical scheme, the components in the composition can be sufficiently dispersed so as to realize uniform mixing.
Detailed Description
The application provides a composition for preparing a high-temperature-resistant adhesion promoter, which comprises the following components: the catalyst comprises an acidic hydrolysis catalyst, a silane coupling compound, a nano metal oxide, an adhesive and a solvent, wherein the acidic hydrolysis catalyst and the silane coupling compound are stored separately.
Wherein the silane coupling compound comprises a first silane coupling agent and a second silane coupling agent; the first silane coupling agent includes at least one of tetraethyl orthosilicate (CAS number: 562-90-3), tetrapropyl orthosilicate (CAS number: 682-01-9), tetrabutyl orthosilicate (CAS number: 4766-57-8), and tetraisopropyl orthosilicate (CAS number: 1992-48-9), and the second silane coupling agent includes at least one of 3-methacryloxypropyltrimethoxysilane (CAS number: 2530-85-0), 3-acryloxypropyltrimethoxysilane (CAS number: 4369-14-6), methacryloxypropyltriisopropoxysilane (CAS number: 80750-05-6), methacryloxypropylmethyldiethoxysilane (CAS number: 65100-04-1), 3-methacryloxypropylmethyldimethoxysilane (CAS number: 14513-34-9), and methacryloxypropyltriethoxysilane (CAS number: 21142-29-0).
It should be noted that, in the present application, the acidic hydrolysis catalyst and the silane conjugate in the composition need to be stored separately; the acidic hydrolysis catalyst may be stored separately, while the remaining components of the composition are stored together; alternatively, the silane conjugate may be stored separately, while the remaining components of the composition are stored together; other storage methods are also possible as long as the acidic hydrolysis catalyst and the silane conjugate in the composition are stored separately.
The high-temperature-resistant adhesion promoter is used for coating the surface of a device to be protected and drying the surface to form a film layer before the deposition of a parylene coating, is used for stably connecting the surface of the device to be protected (including the condition that the surface of the device to be protected is made of plastic) and the parylene coating, so that the condition that the parylene coating is separated from the surface of the device to be protected under a high-temperature environment (such as 100-150 ℃) is avoided, and the protection effect of the parylene coating on the device to be protected under the high-temperature environment (such as 100-150 ℃) is favorably ensured.
Wherein the acidic hydrolysis catalyst can hydrolyze the first silane coupling agent and the second silane coupling agent.
The nano metal oxide has higher heat resistance, can improve the heat resistance of the adhesion promoter, has hydroxyl groups on the surface, and can provide connecting sites for the hydrolyzed first silane coupling agent and the hydrolyzed second silane coupling agent.
The hydrolyzed first silane coupling agent has a silicon-oxygen-silicon bond, so that the heat resistance of the adhesion promoter can be improved, and the hydrolyzed first silane coupling agent can also provide a bridge function to firmly connect the nano metal oxide and the hydrolyzed second silane coupling agent together.
The hydrolyzed second silane coupling agent also provides a bridge function, so that the adhesion force between the nano metal oxide (or the hydrolyzed first silane coupling agent) and the parylene coating can be improved, and the adhesion promoter can be stably connected with the parylene coating.
The adhesive can bond the nano metal oxides together and can firmly bond with the surface of the device to be protected.
The presence of the solvent facilitates the complete dispersion of the components and also facilitates the application of the adhesion promoter to the surface of the device to be protected.
The high-temperature-resistant adhesion promoter formed by uniformly mixing the components in the composition for preparing the high-temperature-resistant adhesion promoter can be used for simultaneously and stably connecting the parylene coating with a device to be protected (including the condition that the surface of the device to be protected is made of plastic), has better heat resistance, is beneficial to avoiding the condition that the adhesion of the parylene coating to the device to be protected is weaker in a high-temperature environment (such as above 100-150 ℃), and the resulting parylene coating is easy to separate from the surface of the device to be protected, and is beneficial to ensuring the protection effect of the parylene coating to the device to be protected in a high-temperature environment (such as above 100-150 ℃).
In the composition, the mass ratio of the acidic hydrolysis catalyst, the silane coupling agent, the nano metal oxide, the adhesive and the solvent is (0.1-1): 7-30): 10-40): 15-45): 20-70, and the mass ratio of the first silane coupling agent to the second silane coupling agent is (1-4): 1.
The proportion of each component in the composition is proper under the above proportion conditions, so that each component in the composition can exert respective effect fully, the stability of the high-temperature-resistant adhesion promoter in connection with a parylene coating and a device to be protected can be improved synergistically, and the heat resistance of the high-temperature-resistant adhesion promoter can be improved.
As an example, the mass ratio of the first silane coupling agent to the second silane coupling agent may be 1.
Furthermore, the mass ratio of the acidic hydrolysis catalyst, the silane coupling compound, the nano metal oxide, the adhesive and the solvent is (0.3-0.5): (12-22): (15-25): (25-35): (20-40).
The proportion of the components in the composition is favorable for further improving the stability of the high-temperature-resistant adhesion promoter in connection with a parylene coating and a device to be protected under the condition of the proportion, and is also favorable for further improving the heat resistance of the high-temperature-resistant adhesion promoter.
Still further, the mass ratio of the first silane coupling agent to the second silane coupling agent is (2-3): 1. Under the condition of the mixture ratio, the first silane coupling agent and the second silane coupling agent can be matched with each other, so that the stability of the high-temperature-resistant adhesion promoter in connection with the parylene coating and the device to be protected can be further improved.
In some alternative embodiments, the first silane coupling agent is tetraethyl orthosilicate and the second silane coupling agent is 3-methacryloxypropyl trimethoxysilane.
The two substances can be matched with each other, the hydrolyzed tetraethyl orthosilicate is favorable for more firmly connecting the nano metal oxide and the hydrolyzed second silane coupling agent, and the hydrolyzed 3-methacryloxypropyl trimethoxy silane is also favorable for more firmly connecting the nano metal oxide (or the hydrolyzed tetraethyl orthosilicate) and the parylene coating.
In the present application, the nano metal oxide is at least one selected from nano alumina, nano silica, and nano zirconia. The above substances all have strong heat resistance, are further favorable for improving the heat resistance of the high-temperature-resistant adhesion promoter, and can also be stably connected with the hydrolyzed first silane coupling agent and the hydrolyzed second silane coupling agent.
In some alternative embodiments, the nano metal oxide is selected from nano alumina and nano silica. The nano-alumina and the nano-silica have higher reaction activity and more hydroxyl groups on the surfaces thereof, so that the connection stability of the nano-alumina and the nano-silica with the hydrolyzed first silane coupling agent and the hydrolyzed second silane coupling agent is improved; and the nano aluminum oxide and the nano silicon dioxide can be mutually matched, so that the heat resistance of the high-temperature-resistant adhesion promoter can be further improved, the connection stability of the high-temperature-resistant adhesion promoter, the hydrolyzed first silane coupling agent and the hydrolyzed second silane coupling agent can be further improved, the structural strength of the whole high-temperature-resistant adhesion promoter can be improved, and the stability of the high-temperature-resistant adhesion promoter in connection with a parylene coating and a device to be protected can be further improved.
Further, the nano metal oxide is selected from nano aluminum oxide and nano silicon dioxide, and the mass ratio of the nano aluminum oxide to the nano silicon dioxide is (1-100): 1. Under the condition of the mixture ratio, the heat resistance of the whole high-temperature-resistant adhesion promoter is favorably improved, the connection sites of the nano metal oxide and the hydrolyzed first silane coupling agent and the hydrolyzed second silane coupling agent are favorably increased, and the structural strength of the whole high-temperature-resistant adhesion promoter is favorably improved.
As an example, the mass ratio of nano alumina to nano silica may be 1, 5.
And furthermore, the nano metal oxide is selected from nano aluminum oxide and nano silicon dioxide, and the mass ratio of the nano aluminum oxide to the nano silicon dioxide is (2-3): 1, so that the stability of the high-temperature-resistant adhesion promoter in connection with the parylene coating and the device to be protected is further improved.
Furthermore, the nano aluminum oxide is in an alpha crystal form, and has better heat resistance.
In the present application, the adhesive includes at least one of a methacrylate-based copolymer and an acrylate-based copolymer. The high-temperature-resistant adhesion promoter can be stably connected with the surface of a device to be protected.
In some alternative embodiments, the adhesive is selected from methacrylate copolymers, which is beneficial for further improving the stability of the high temperature adhesion promoter in connecting the parylene coating and the device to be protected.
Illustratively, the methacrylate-based copolymer includes at least one of a copolymer of n.n Dimethylacrylamide (DMAA) and Lauryl Methacrylate (LMA) and a copolymer of isooctyl methacrylate (EHMA) and Methyl Methacrylate (MMA).
In some alternative embodiments, the adhesive is selected from a copolymer of n.n dimethylacrylamide and lauryl methacrylate, which can further improve the stability of the high temperature adhesion promoter in connecting the parylene coating and the device to be protected.
Illustratively, the molecular weight of the copolymer of n.n dimethylacrylamide and lauryl methacrylate is 3 to 15 ten thousand, and the mass fraction of n.n dimethylacrylamide and lauryl methacrylate in the copolymer of n.n dimethylacrylamide and lauryl methacrylate is 50 to 70% and 30 to 50%, respectively.
Further, the molecular weight of the copolymer of N.N dimethylacrylamide and lauryl methacrylate is 6-8 ten thousand, and the mass parts of N.N dimethylacrylamide and lauryl methacrylate in the copolymer of N.N dimethylacrylamide and lauryl methacrylate are 70-85% and 15-30%, respectively; the stability of the high-temperature-resistant adhesion promoter in connection with the parylene coating and the device to be protected is further improved.
It should be noted that in other possible embodiments, the adhesive may also be selected from an acrylate copolymer, which illustratively includes a copolymer of Butyl Acrylate (BA) and Methyl Acrylate (MA).
In the present application, the acidic hydrolysis catalyst includes at least one of acetic acid, methacrylic acid, phosphoric acid, and trifluoroacetic acid. The above-mentioned substance can rapidly hydrolyze the first silane coupling agent and the second silane coupling agent.
Further, the acidic hydrolysis catalyst is selected from at least one of acetic acid and trifluoroacetic acid.
In the present application, the solvent includes at least one of ethyl 3-ethoxypropionate, ethyl acetate, and butyl acetate. The substances have good dissolving and dispersing effects on each component in the composition; the high-temperature resistant adhesion promoter is easy to volatilize after being coated.
Further, the solvent is selected from butyl acetate.
The application also provides a preparation method of the high-temperature-resistant adhesion promoter, which comprises the following steps: and mixing the composition for preparing the high-temperature-resistant adhesion promoter.
The composition for preparing the high-temperature-resistant adhesion promoter is mixed to prepare the high-temperature-resistant adhesion promoter; when the high-temperature-resistant adhesive force promoter is used, the prepared high-temperature-resistant adhesive force promoter is coated on the surface of a device to be protected and dried, and then the parylene coating is deposited on the surface of the film layer formed by the high-temperature-resistant adhesive force promoter, so that the high-temperature-resistant adhesive force promoter can be simultaneously and stably connected with the parylene coating and the device to be protected, has better heat resistance, is favorable for avoiding the condition that the parylene coating is easy to separate from the surface of the device to be protected due to weaker adhesive force of the parylene coating to the device to be protected under a high-temperature environment (such as 100-150 ℃), and is favorable for ensuring the protection effect of the parylene coating to the device to be protected under the high-temperature environment (such as 100-150 ℃).
Further, the components in the composition are mixed by stirring for 2-10min at 1500-2500rpm, so that the components in the composition can be fully dispersed to realize uniform mixing.
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
The embodiment provides a high-temperature-resistant adhesion promoter, which is prepared by the following steps:
31.4g of a copolymer of DMAA and LMA are dissolved in 31.4g of butyl acetate. After the dissolution, 15.7g of nano alumina and 5.3g of nano silica are respectively added. Dispersing in a high-speed mixer at 2000rpm for 2min to obtain suspension. Then 10.5g of tetraethyl orthosilicate, 5.2g of 3-methacryloxypropyltrimethoxysilane and finally 0.5g of a 90% aqueous acetic acid solution in parts by mass were added. Dispersing for 2min in a high-speed mixer at the rotating speed of 2000rpm to obtain the high-temperature-resistant adhesion promoter.
Wherein the molecular weight of the copolymer of DMAA and LMA is 7 ten thousand, and the mass parts of DMAA and LMA in the copolymer of DMAA and LMA are 85% and 15% respectively.
Example 2
The present embodiment provides a high temperature adhesion promoter, and the present embodiment is different from embodiment 1 in that: the mass of the copolymer of DMAA and LMA was 24.3g, the mass of butyl acetate was 24.3g, the mass of nano-alumina was 30g and the mass of nano-silica was 5.2g.
Example 3
This example provides a high temperature adhesion promoter, and the difference between this example and example 1 is: the masses of tetraethyl orthosilicate and 3-methacryloxypropyl trimethoxysilane were both 7.85g.
Example 4
The present embodiment provides a high temperature adhesion promoter, and the present embodiment is different from embodiment 1 in that: 3-methacryloxypropyltrimethoxysilane was replaced with 3-acryloxypropyltrimethoxysilane.
Example 5
This example provides a high temperature adhesion promoter, and the difference between this example and example 1 is: "15.7g of nano alumina and 5.3g of nano silica" was replaced with 21g of nano alumina.
Example 6
The present embodiment provides a high temperature adhesion promoter, and the present embodiment is different from embodiment 1 in that: the mass of the nano alumina and the nano silica is 10.5g.
Example 7
The present embodiment provides a high temperature adhesion promoter, and the present embodiment is different from embodiment 1 in that: the molecular weight of the copolymer of DMAA and LMA was 10 ten thousand.
Comparative example 1
This comparative example differs from example 1 in that: tetraethyl orthosilicate was not used and the mass of 3-methacryloxypropyltrimethoxysilane was 15.7g.
Comparative example 2
This comparative example differs from example 1 in that: 3-methacryloxypropyltrimethoxysilane was not used, and the mass of tetraethylorthosilicate was 15.7g.
Comparative example 3
This comparative example differs from example 1 in that: tetraethyl orthosilicate and 3-methacryloxypropyltrimethoxysilane were not used, and the mass of butyl acetate was 47.1g.
Comparative example 4
This comparative example differs from example 1 in that: nano-alumina and nano-silica were not used, and the mass of the copolymer of DMAA and LMA was 41.9, and the mass of butyl acetate was 41.9g.
Comparative example 5
The comparative example differs from example 1 in that: no aqueous acetic acid solution was used, and the mass of butyl acetate was 31.9g.
Examples of the experiments
The adhesion promoting ability of the products obtained in examples 1 to 7 and comparative examples 1 to 5 was tested, and the test results are shown in table 1.
Wherein, the testing step comprises: the FR4 test board, the metallic aluminum test board and the glass test board were subjected to plasma treatment for oxygen filling for 3min. After the plasma treatment, the products obtained in examples 1 to 10 and comparative examples 1 to 5 were sprayed on an FR4 test board, an aluminum metal test board and a glass test board, respectively, and baked at 100 ℃ for 10min to form a film layer. Then depositing a parylene coating on the film layer. The test pieces were baked in an oven at 130 ℃ for 72 hours and then subjected to a hundred grid test.
TABLE 1
FR4 test board Metal aluminium test board Glass testing board
Example 1 Without peeling off Without peeling off Without peeling off
Example 2 10% exfoliation Without peeling off Without peeling off
Example 3 10% exfoliation 10% exfoliation Without peeling off
Example 4 20% exfoliation 15% no peeling off Without peeling off
Example 5 25% peeling and falling off 10% exfoliation 15% peeling and peeling
Example 6 30% peeling and falling off 15% peeling and peeling 15% peeling and peeling
Example 7 5% peeling off 10% exfoliation Without peeling off
Comparative example 1 50% exfoliation 30% peeling and falling off 25% peeling and falling off
Comparative example 2 65% peeling and peeling 60% peeling and falling off 75% peeling off
Comparative example 3 Almost total exfoliation Almost total exfoliation Almost total exfoliation
Comparative example 4 40% peeling and peeling 20% peeling off 10% exfoliation
Comparative example 5 40% peeling and peeling 50% peeling off 40% exfoliation
As can be seen from Table 1, the adhesion of the high temperature adhesion promoters provided in examples 1-7 to the parylene coating at high temperature (oven baking at 130 ℃ for 72 hours) is significantly better than the adhesion of the products prepared in comparative examples 1-5 to the parylene coating at high temperature (oven baking at 130 ℃ for 72 hours); the adhesion of the parylene coating to the device to be protected under a high-temperature environment (such as 100-150 ℃) can be effectively improved by simultaneously adopting a first silane coupling agent comprising tetraethyl orthosilicate, a second silane coupling agent comprising 3-methacryloxypropyltrimethoxysilane, a nano metal oxide, an adhesive and an acidic hydrolysis catalyst, so that the protection effect of the parylene coating to the device to be protected under the high-temperature environment (such as 100-150 ℃) is further ensured.
As can be seen from the comparison between example 1 and example 2, the ratio of the raw material components for preparing the high-temperature-resistant adhesion promoter can affect the adhesion of the high-temperature-resistant adhesion promoter to the parylene coating.
As can be seen from the comparison between example 1 and example 3, the adhesion of the high temperature resistant adhesion promoter to the parylene coating can be improved when the mass ratio of tetraethyl orthosilicate (TEOS) to 3-methacryloxypropyltrimethoxysilane (a 174) in example 3 is 1; it is shown that the mass ratio of TEOS and a174 can affect the adhesion of the high temperature adhesion promoter to the parylene coating.
As can be seen from the comparison of example 1 with example 4, the adhesion of the high temperature adhesion promoter to the parylene coating is further improved by the 3-methacryloxypropyltrimethoxysilane (A174) selected in example 1 compared to the 3-acryloxypropyltrimethoxysilane selected in example 4.
From the comparison between example 1 and example 5, it can be seen that the adhesion of the high temperature resistant adhesion promoter to the parylene coating can be further improved by using nano alumina and nano silica simultaneously in example 1, compared with using only nano alumina in example 5; the use of the nano aluminum oxide is very important for improving the high temperature resistance, and the peeling strength of the parylene coating relative to the surface of the device to be protected at high temperature can be effectively improved.
As can be seen from the comparison between example 1 and example 6, compared with the mass ratio of nano alumina to nano silica in example 6 being 1, and the mass ratio of nano alumina to nano silica in example 1 being 2.96; the mass ratio of the nano aluminum oxide to the nano silicon oxide is shown to influence the adhesion of the high-temperature-resistant adhesion promoter to the parylene coating.
As can be seen from a comparison of example 1 and example 7, the adhesion of the high temperature adhesion promoter to the parylene coating can be further improved compared to the molecular weight of 10 ten thousand for the copolymer of DMAA and LMA in example 7 and 7 ten thousand for the copolymer of DMAA and LMA in example 1; the molecular weight of the copolymer of DMAA and LMA is shown to influence the adhesion of the high-temperature adhesion promoter to the parylene coating.
In conclusion, the high-temperature-resistant adhesion promoter formed by uniformly mixing the components in the composition for preparing the high-temperature-resistant adhesion promoter provided by the application has better heat resistance, can simultaneously and stably connect the parylene coating and the device to be protected (including the condition that the surface material of the device to be protected is plastic) even under a high-temperature environment (such as 100-150 ℃), and is beneficial to ensuring the protection effect of the parylene coating on the device to be protected under the high-temperature environment (such as 100-150 ℃).
The embodiments described above are some, but not all embodiments of the present application. The detailed description of the embodiments of the present application is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.

Claims (10)

1. A composition for use in preparing a high temperature adhesion promoter, comprising: the preparation method comprises the following steps of (1) storing an acidic hydrolysis catalyst, a silane coupling compound, a nano metal oxide, an adhesive and a solvent separately;
the silane coupling compound comprises a first silane coupling agent and a second silane coupling agent; the first silane coupling agent comprises at least one of tetraethyl orthosilicate, tetrapropyl orthosilicate, tetrabutyl orthosilicate and tetraisopropyl orthosilicate, and the second silane coupling agent comprises at least one of 3-methacryloxypropyl trimethoxysilane, 3-acryloxypropyl trimethoxysilane, methacryloxypropyl triisopropoxy silane, methacryloxypropyl methyldiethoxysilane, 3-methacryloxypropyl methyldimethoxysilane and methacryloxypropyl triethoxysilane.
2. The composition of claim 1, wherein the mass ratio of the acidic hydrolysis catalyst, the silane coupling agent, the nano metal oxide, the adhesive, and the solvent is (0.1-1): 7-30): 10-40: 15-45: 20-70, and the mass ratio of the first silane coupling agent to the second silane coupling agent is (1-4): 1;
optionally, the mass ratio of the acidic hydrolysis catalyst, the silane coupling compound, the nano metal oxide, the adhesive and the solvent is (0.3-0.5): 12-22): 15-25): 25-35): 20-40;
optionally, the mass ratio of the first silane coupling agent to the second silane coupling agent is (2-3): 1.
3. The composition of claim 1 or 2, wherein the first silane coupling agent is tetraethyl orthosilicate and the second silane coupling agent is 3-methacryloxypropyl trimethoxysilane.
4. The composition of claim 1 or 2, wherein the nano metal oxide is selected from at least one of nano alumina, nano silica, and nano zirconia.
5. The composition of claim 4, wherein the nano metal oxide is selected from nano alumina and nano silica;
optionally, the mass ratio of the nano-alumina to the nano-silica is (1-100): 1;
optionally, the mass ratio of the nano alumina to the nano silica is (2-3): 1;
optionally, the nano-alumina is in an alpha crystal form.
6. The composition of claim 1 or 2, wherein the acidic hydrolysis catalyst comprises at least one of acetic acid, methacrylic acid, phosphoric acid, and trifluoroacetic acid;
optionally, the acidic hydrolysis catalyst is selected from at least one of acetic acid and trifluoroacetic acid.
7. The composition of claim 1 or 2, wherein the adhesive comprises at least one of a methacrylate copolymer and an acrylate copolymer;
optionally, the adhesive is selected from methacrylate copolymers;
optionally, the adhesive is selected from a copolymer of n.n dimethylacrylamide and lauryl methacrylate;
alternatively, the molecular weight of the copolymer of n.n dimethylacrylamide and lauryl methacrylate is 3 to 15 ten thousand, and the mass fraction of the n.n dimethylacrylamide and the lauryl methacrylate in the copolymer of n.n dimethylacrylamide and lauryl methacrylate is 50 to 70% and 30 to 50%, respectively.
8. The composition of claim 1 or 2, wherein the solvent comprises at least one of ethyl 3-ethoxypropionate, ethyl acetate, and butyl acetate;
alternatively, the solvent is selected from butyl acetate.
9. A preparation method of a high-temperature-resistant adhesion promoter is characterized by comprising the following steps: mixing the composition of any one of claims 1-8.
10. The method according to claim 9, wherein the mixing is stirring mixing, the stirring mixing time is 2 to 10min, and the rotation speed of the stirring mixing is 1500 to 2500rpm.
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