Ultrathin high-temperature-resistant and high-pressure-resistant nano electronic film and production process thereof

Abstract

The invention relates to the technical field of metallized film production processes, in particular to an ultrathin high-temperature-resistant and high-pressure-resistant nano electronic film and a production process thereof, and the production process comprises the following steps: S1, preliminarily mixing a solvent and a silane coupling agent; s2, hexagonal boron nitride is added, and stirring is continued; s3, centrifugal separation and washing; s4, heat treatment of the raw materials; s5, performing high-speed mixing to prepare a composite raw material; s6, carrying out melt extrusion granulation; s7, performing two-way stretching forming to prepare a base film; s8, performing chemical vapor deposition to form a homopolymer layer; and S9, vacuum evaporation aluminum plating is carried out to achieve metallization. The copolymer layer can effectively permeate and fill microdefects on the surface of the polypropylene base membrane to form a smoother and more compact barrier layer. Therefore, electric field concentration points are eliminated, the breakdown field strength of the composite film is remarkably improved, and the high-voltage resistance is excellent.

Description

Technical Field

[0001] This invention relates to the field of metallized thin film production technology, specifically to an ultrathin high-temperature and high-pressure resistant nanoelectronic thin film and its production process. Background Technology

[0002] Polypropylene film has broad application prospects in capacitors, flexible electronic devices, and packaging materials due to its excellent electrical insulation, low density, low cost, and good chemical stability. However, as modern industry develops towards miniaturization and high performance, the inherent defects of traditional polypropylene film are becoming increasingly prominent, severely limiting its application in high-end fields.

[0003] In the fabrication of metallized thin films, the inherent low surface energy of the polypropylene base film and the microscopic defects that may form during the film-forming process significantly affect the deposition quality of the subsequent metal layer. Poor adhesion between the metal layer and the base film makes it prone to peeling under thermal or mechanical stress, leading to increased contact resistance and even open circuits. Simultaneously, defects on the base film surface become electric field concentration points, significantly reducing the film's breakdown field strength and affecting its high-voltage resistance. Therefore, we propose an ultrathin, high-temperature and high-voltage resistant nanoelectronic thin film and its fabrication process. Summary of the Invention

[0004] The purpose of this invention is to provide an ultrathin high-temperature and high-voltage resistant nanoelectronic thin film and its manufacturing process, which solves the problems mentioned in the background art.

[0005] To achieve the above objectives, the present invention provides the following technical solution: A process for producing ultrathin, high-temperature and high-voltage resistant nanoelectronic thin films includes the following steps: S1. Preliminary mixing of solvent and silane coupling agent: Stir and mix 1000-1500 parts by weight of solvent with 5-30 parts by weight of silane coupling agent for 5-10 minutes; S2. Add hexagonal boron nitride and continue stirring; add 1-5 parts by weight of hexagonal boron nitride to the mixture obtained in step S1 and continue stirring for 10-30 minutes; S3. Centrifugation and washing: The mixture obtained in step S2 is separated by centrifugation, and the powder is washed with anhydrous ethanol after separation. S4. Heat treatment of raw materials: The powder obtained in step S3 is reacted at 105-120℃ for 1-2 hours to obtain pretreated raw material one. S5. High-speed mixing to prepare composite raw materials; add pretreated raw material 1, polypropylene granular raw material and inorganic additives to a high-speed mixer and mix for 10-30 minutes; S6. Melt extrusion granulation: The uniformly mixed raw materials from step S5 are added to a twin-screw extruder, and the resulting melt is cooled, drawn, and granulated to produce uniformly sized modified plastic granules. S7. Preparation of base film by biaxial stretching molding: The modified plastic particles obtained in step S6 are used to prepare a modified polypropylene base film by biaxial stretching molding process. S8. Forming a homopolymer layer by chemical vapor deposition: The base film obtained in step S7 is subjected to vapor-initiated chemical vapor deposition technology to form a homopolymer layer on the surface of the base film by two monomers, 1,3,5-trimethyl-1,3,5-trivinylcyclotrisiloxane and 1-vinylimidazolium. S9. Metallization is achieved by vacuum evaporation aluminum deposition; the film roll obtained in step S8 is deposited with aluminum on the surface of the homopolymer layer by vacuum evaporation aluminum deposition, thereby producing a metallized thin film.

[0006] Preferably, in step S1, the solvent is one or more of N-methylpyrrolidone, N,N-dimethylformamide, and dimethyl sulfoxide, and the silane coupling agent is γ-aminopropyltriethoxysilane or γ-(2,3-epoxypropoxy)propyltrimethoxysilane.

[0007] Preferably, in step S2, the particle size of hexagonal boron nitride is 50-200 nanometers.

[0008] Preferably, in step S5, the weight ratio of the raw material components is: 100 parts by weight of polypropylene granular raw material, 3-8 parts by weight of pretreatment raw material, and 1 part by weight of inorganic additives, including antioxidants and lubricants.

[0009] Preferably, in step S6, the processing temperature range of the twin-screw extruder is 180-210℃, and the screw speed is 150-250rpm.

[0010] Preferably, in step S7, the specific parameters of the biaxial stretching process are: longitudinal stretching ratio of 2.5:1 to 4:1, transverse stretching ratio of 2.5:1 to 4:1, and stretching temperature controlled at 120-135℃.

[0011] Preferably, in step S8, the molar ratio of 1,3,5-trimethyl-1,3,5-trivinylcyclotrisiloxane to 1-vinylimidazole is 1:0.8 to 1:1.2; the reaction temperature for gas-phase initiated chemical vapor deposition is 50-60°C, and the reaction pressure is 30-100 Pa.

[0012] Preferably, in step S9, the thickness of the aluminum layer formed by vacuum evaporation aluminum deposition is 50-200 nanometers.

[0013] Preferably, before step S9, a step of plasma treatment is further included on the base film with the deposited homopolymer layer, wherein the working gas of the plasma treatment is argon, the treatment power is 200-500W, and the treatment time is 30-120 seconds.

[0014] An ultrathin, high-temperature and high-voltage resistant nanoelectronic thin film is prepared by an ultrathin, high-temperature and high-voltage resistant nanoelectronic thin film production process.

[0015] By employing the above technical solution, the present invention provides an ultrathin high-temperature and high-pressure resistant nanoelectronic thin film and its manufacturing process, which have at least the following beneficial effects: This invention achieves a stable nanocomposite material by uniformly dispersing hexagonal boron nitride nanosheets within a polypropylene matrix. The hexagonal boron nitride nanosheets, acting as a two-dimensional reinforcement, effectively transfer and disperse stress, hindering the slippage of polypropylene molecular chains, thereby significantly improving the tensile strength and modulus of the composite film. This allows the film to achieve ultra-thinness while possessing excellent mechanical integrity, enabling it to withstand various stresses during subsequent processing and use.

[0016] The introduction of highly thermally stable hexagonal boron nitride greatly improves the thermal properties of the polypropylene matrix. Its robust skeletal structure can suppress the thermal motion of polypropylene molecular chains at high temperatures, thereby significantly increasing the heat distortion temperature and the upper limit of long-term service temperature of the film, enabling it to adapt to more demanding working environments.

[0017] The copolymer layer effectively fills the microscopic defects on the surface of the polypropylene base film, forming a smoother and denser barrier layer. This eliminates electric field concentration points, significantly improving the breakdown field strength of the composite film and resulting in excellent high-voltage resistance. Simultaneously, as an intermediate layer, the copolymer layer forms a strong bond with the polypropylene base film through molecular chain diffusion or chemical reaction. Furthermore, its activated surface provides numerous nucleation sites for subsequent metal deposition and forms strong chemical bonds with metal atoms. This greatly enhances the adhesion between the metal layer and the composite film, effectively preventing the metal layer from peeling off under thermal cycling or mechanical stress, ensuring the long-term reliability of the metallized thin-film device. Detailed Implementation

[0018] The technical solutions of the present invention will be clearly and completely described below with reference to the data in the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0019] A process for producing ultrathin, high-temperature and high-voltage resistant nanoelectronic thin films includes the following steps: S1. Initial mixing of solvent and silane coupling agent: Take 1000-1500 parts by weight of DMF solvent and 5-30 parts by weight of silane coupling agent KH-550, and add them to a glass reactor equipped with mechanical stirrer. Stir at 300 rpm for 10 minutes at room temperature to fully disperse the silane coupling agent in the solvent and form a homogeneous solution to promote silane hydrolysis and prepolymerization.

[0020] S2. Add hexagonal boron nitride and continue stirring; add 1-5 parts by weight of hexagonal boron nitride nanopowder to the mixture in S1, increase the stirring speed to 500 rpm, and continue stirring for 20 minutes. Ensure that there is no agglomeration during stirring, so that the hexagonal boron nitride powder is evenly dispersed and the surface is modified by the functional groups of the silane coupling agent, thereby enhancing the compatibility with the polymer.

[0021] S3. Centrifugation and washing: Transfer the mixture from S2 to a high-speed centrifuge and centrifuge at 8000 rpm for 15 minutes to separate the solid precipitate. Discard the supernatant and wash the precipitate three times with 200 parts by weight of anhydrous ethanol. After each wash, centrifuge at 5000 rpm for 5 minutes to remove residual solvent and impurities. Finally, wet hexagonal boron nitride composite powder is obtained.

[0022] S4. Heat treatment of raw materials: Place the powder washed in S3 into a vacuum drying oven and heat treat it for 1.5 hours at 110℃ and a vacuum degree ≤0.095MPa to allow the silane coupling agent to fully react with the surface of hexagonal boron nitride to form pretreated raw material one.

[0023] S5. High-speed mixing to prepare composite raw materials: Take 100 parts by weight of polypropylene granules, 3-8 parts by weight of pretreated raw material one, and 1 part by weight of inorganic additives, including 0.7 parts of antioxidant and 0.3 parts of lubricant, and add them to a high-speed mixer. Mix at 1000 rpm for 20 minutes at 50°C to ensure uniform dispersion of all components and form a composite powder.

[0024] S6. Melt extrusion granulation: The composite raw material obtained in step S5 is added to a twin-screw extruder. The screw temperature is set to 180℃ in zone 1, 190℃ in zone 2, 200℃ in zone 3, and 205℃ at the die head. The screw speed is 200 rpm. After the melt is extruded through the die, it is cooled in a water bath, drawn into strips by a traction machine, and finally cut into modified plastic granules with a diameter of about 2 mm and a length of 3 mm by a pelletizer.

[0025] S7. Preparation of the base film by biaxial stretching: The modified plastic granules obtained in step S6 are added to a biaxial stretching machine, first melt-extruded into a thick film, then longitudinally stretched at a stretch ratio of 3:1 at 125°C, and then transversely stretched at a stretch ratio of 3:1 at 130°C, finally obtaining a modified polypropylene base film with a thickness of approximately 20 μm. During both longitudinal and transverse stretching processes, the stretching speed is controlled at 10 m / min.

[0026] S8. A homopolymer layer is formed by chemical vapor deposition. The substrate film from S7 is placed in the reaction chamber of the CVD system. The chamber is first evacuated to 0.1 Pa, then a mixed vapor of 1,3,5-trimethyl-1,3,5-trivinylcyclotrisiloxane and 1-vinylimidazole is introduced, along with argon gas at a flow rate of 50 sccm as the carrier gas. At 60 °C and 50 Pa pressure, a gas-phase polymerization reaction is initiated for 30 minutes using ultraviolet light with a wavelength of 254 nm and a power of 100 W, forming a homopolymer layer on the substrate film surface.

[0027] S9. Metallization is achieved by vacuum evaporation aluminum deposition; the film roll obtained in step S8 is subjected to plasma treatment, wherein the working gas for plasma treatment is argon, the treatment power is 200W, and the treatment time is 30 seconds. It is then loaded into a vacuum evaporation aluminum deposition machine and evacuated to a vacuum level of 5*10. -3 After Pa, high-purity aluminum wire is evaporated by resistance heating, and the aluminum vapor condenses on the surface of the homopolymer layer to form an aluminum metal layer. During the aluminum plating process, the plating speed is controlled at 2 nm / s, and the base film tension is maintained at 10 N / m to obtain the final ultrathin metallized film.

[0028] Example 1 An ultrathin high-temperature and high-voltage resistant nanoelectronic film is prepared by the above-mentioned production process of an ultrathin high-temperature and high-voltage resistant nanoelectronic film. In step S1, the amount of DMF solvent added is 1500 parts by weight, the amount of silane coupling agent KH-550 added is 30 parts by weight, the amount of hexagonal boron nitride nanopowder added is 5 parts by weight in step S2, and the amount of pretreatment raw material one added is 5 parts by weight in step S5. The ultrathin high-temperature and high-voltage resistant nanoelectronic film Example 1 is finally obtained.

[0029] Example 2 An ultrathin high-temperature and high-voltage resistant nanoelectronic film was prepared by the above-mentioned production process. In step S1, the amount of DMF solvent added was 1200 parts by weight, the amount of silane coupling agent KH-550 added was 15 parts by weight, the amount of hexagonal boron nitride nanopowder added was 1 part by weight in step S2, and the amount of pretreatment raw material one added was 5 parts by weight in step S5. The ultrathin high-temperature and high-voltage resistant nanoelectronic film Example 2 was finally obtained.

[0030] Example 3 An ultrathin high-temperature and high-voltage resistant nanoelectronic film was prepared by the above-mentioned production process. In step S1, the amount of DMF solvent added was 1200 parts by weight, the amount of silane coupling agent KH-550 added was 15 parts by weight, the amount of hexagonal boron nitride nanopowder added was 5 parts by weight in step S2, and the amount of pretreatment raw material one added was 3 parts by weight in step S5. The ultrathin high-temperature and high-voltage resistant nanoelectronic film Example 3 was finally obtained.

[0031] Example 4 An ultrathin high-temperature and high-voltage resistant nanoelectronic film was prepared by the above-mentioned production process. In step S1, the amount of DMF solvent added was 1000 parts by weight, the amount of silane coupling agent KH-550 added was 5 parts by weight, the amount of hexagonal boron nitride nanopowder added was 1 part by weight in step S2, and the amount of pretreatment raw material one added was 3 parts by weight in step S5. The ultrathin high-temperature and high-voltage resistant nanoelectronic film was finally obtained in Example 4.

[0032] Comparative Example A metallized thin film is prepared by the same method as steps S7 and S9 in the preparation method of Example 1, wherein the modified plastic particles used in step S7 are replaced with polypropylene plastic particles, and step S9 directly uses the base film prepared in step S7.

[0033] According to the GB / T 24123-2009 standard, the adhesion strength between the metallized thin film coating and the film in the examples and comparative examples was tested, wherein the adhesive tape was used with an adhesion strength of 5 N / cm. 2 Using 3M double-sided tape, the sample (120 mm long and 50 mm wide) was evenly adhered to a stainless steel plate. The test sample was then evenly adhered onto the double-sided tape. A 500g roller was used to secure the sample. Next, a 2 cm long and 12.7 mm wide 3M single-sided tape was applied to the test sample and secured with another roller. A high-speed rail tensile testing machine was then used to peel the conductive and insulating layers of the test sample. Based on the tensile force and displacement data, the maximum tensile force was recorded. This value was divided by 0.02 N to calculate the metal layer adhesion, which is the bonding force F (N / m) between the insulating and conductive layers. Subsequently, in accordance with GB / T13542.2 The 2021 standard specifies that the thickness, tensile fracture resistance, corona resistance duration, and thermal conductivity of the metallized thin films in the examples and comparative examples be tested. The test conditions for corona resistance duration are: experimental voltage 2kV, experimental frequency 20kHz, pulse rise time 50ns, bipolar pulse square wave, and 6mm cylindrical electrode.

[0034] The test results are shown in the table below.

[0035] Table 1 Performance test results of the metallized thin films in the examples and comparative examples The data results show that the modified polypropylene film with added hexagonal boron nitride nanopowder in this invention has significantly improved tensile strength and thermal conductivity, thereby improving the high-temperature resistance of the film surface. At the same time, the homopolymer layer formed by 1,3,5-trimethyl-1,3,5-trivinylcyclotrisiloxane and 1-vinylimidazole has significantly improved corona resistance and bonding strength. The homopolymer layer fills the defects on the surface of the base film, thereby improving the puncture resistance and the bonding strength between the metal layer and the base film.

[0036] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.

[0037] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A process for producing ultrathin, high-temperature and high-voltage resistant nanoelectronic thin films, characterized in that, Includes the following steps: S1. Preliminary mixing of solvent and silane coupling agent: Stir and mix 1000-1500 parts by weight of solvent with 5-30 parts by weight of silane coupling agent for 5-10 minutes; S2. Add hexagonal boron nitride and continue stirring; add 1-5 parts by weight of hexagonal boron nitride to the mixture obtained in step S1 and continue stirring for 10-30 minutes; S3. Centrifugation and washing: The mixture obtained in step S2 is separated by centrifugation, and the powder is washed with anhydrous ethanol after separation. S4. Heat treatment of raw materials: The powder obtained in step S3 is reacted at 105-120℃ for 1-2 hours to obtain pretreated raw material one. S5. High-speed mixing to prepare composite raw materials; add pretreated raw material 1, polypropylene granular raw material and inorganic additives to a high-speed mixer and mix for 10-30 minutes; S6. Melt extrusion granulation: The uniformly mixed raw materials from step S5 are added to a twin-screw extruder, and the resulting melt is cooled, drawn, and granulated to produce uniformly sized modified plastic granules. S7. Preparation of base film by biaxial stretching molding: The modified plastic particles obtained in step S6 are used to prepare a modified polypropylene base film by biaxial stretching molding process. S8. Forming a homopolymer layer by chemical vapor deposition: The base film obtained in step S7 is subjected to vapor-initiated chemical vapor deposition technology to form a homopolymer layer on the surface of the base film by two monomers, 1,3,5-trimethyl-1,3,5-trivinylcyclotrisiloxane and 1-vinylimidazolium. S9. Metallization is achieved by vacuum evaporation aluminum deposition; the film roll obtained in step S8 is deposited with aluminum on the surface of the homopolymer layer by vacuum evaporation aluminum deposition, thereby producing a metallized thin film.

2. The manufacturing process for an ultrathin, high-temperature and high-voltage resistant nanoelectronic thin film according to claim 1, characterized in that: In step S1, the solvent is one or more of N-methylpyrrolidone, N,N-dimethylformamide, and dimethyl sulfoxide, and the silane coupling agent is γ-aminopropyltriethoxysilane or γ-(2,3-epoxypropoxy)propyltrimethoxysilane.

3. The manufacturing process for an ultrathin, high-temperature and high-voltage resistant nanoelectronic thin film according to claim 1, characterized in that: In step S2, the particle size of hexagonal boron nitride is 50-200 nanometers.

4. The manufacturing process for an ultrathin, high-temperature and high-voltage resistant nanoelectronic thin film according to claim 1, characterized in that: In step S5, the weight ratio of the raw material components is: 100 parts by weight of polypropylene granules, 3-8 parts by weight of pretreatment raw material, and 1 part by weight of inorganic additives, which include antioxidants and lubricants.

5. The manufacturing process for an ultrathin, high-temperature and high-voltage resistant nanoelectronic thin film according to claim 1, characterized in that: In step S6, the processing temperature range of the twin-screw extruder is 180-210℃, and the screw speed is 150-250rpm.

6. The manufacturing process for an ultrathin, high-temperature and high-voltage resistant nanoelectronic thin film according to claim 1, characterized in that: In step S7, the specific parameters of the biaxial stretching process are: longitudinal stretching ratio of 2.5:1 to 4:1, transverse stretching ratio of 2.5:1 to 4:1, and stretching temperature controlled at 120-135℃.

7. The manufacturing process for an ultrathin, high-temperature and high-voltage resistant nanoelectronic thin film according to claim 1, characterized in that: In step S8, the molar ratio of 1,3,5-trimethyl-1,3,5-trivinylcyclotrisiloxane to 1-vinylimidazole is 1:0.8 to 1:1.2; the reaction temperature for gas-phase initiated chemical vapor deposition is 50-60°C, and the reaction pressure is 30-100 Pa.

8. The manufacturing process for an ultrathin, high-temperature and high-voltage resistant nanoelectronic thin film according to claim 1, characterized in that: In step S9, the thickness of the aluminum layer formed by vacuum evaporation aluminum deposition is 50-200 nanometers.

9. The manufacturing process for an ultrathin, high-temperature and high-voltage resistant nanoelectronic thin film according to claim 1, characterized in that: Before step S9, a plasma treatment step is also included on the base film with the deposited homopolymer layer. The working gas for the plasma treatment is argon, the treatment power is 200-500W, and the treatment time is 30-120 seconds.

10. An ultrathin, high-temperature and high-voltage resistant nanoelectronic thin film, characterized in that: It is prepared by the production process of an ultrathin high temperature and high pressure resistant nanoelectronic thin film according to any one of claims 1-9.

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