CN115612134A - High-thermal-conductivity cast film and preparation method thereof - Google Patents
High-thermal-conductivity cast film and preparation method thereof Download PDFInfo
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J2329/14—Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
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- C—CHEMISTRY; METALLURGY
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- C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
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Abstract
The invention discloses a preparation method of a high-thermal-conductivity cast film, which comprises the steps of adding a high-molecular base material into a dispersing agent to obtain a mixed solution, adding thermal-conductivity filler powder into the mixed solution, stirring to obtain slurry, defoaming, casting and drying the slurry in sequence to obtain a cast film, wherein the thickness of the cast film is 20-70 mu m, and carrying out hot pressing and stripping on the cast film to obtain the high-thermal-conductivity cast film. The preparation method is simple and efficient, and the cast film prepared by the preparation method has high in-plane thermal conductivity, high insulativity and high mechanical property. The invention also discloses a high-thermal-conductivity cast film prepared by the preparation method of the high-thermal-conductivity cast film.
Description
Technical Field
The invention belongs to the field of heat-conducting films, and particularly relates to a high-heat-conducting cast film and a preparation method thereof.
Background
With the rapid development of electronic devices, the electronic devices have trends of miniaturization, integration and high power, and the power density of the devices is greatly improved. High power dense packaging can accumulate a significant amount of heat during operation of the electronic components. Therefore, the problem of heat dissipation of electronic packaging materials is becoming more and more a key factor affecting the performance and reliability of electronic devices.
The polymer has the advantages of light weight, flexibility, low cost, easy processing and forming and the like, and has wide application prospect in the aspect of heat management of modern electronic products. However, the polymers have very low intrinsic thermal conductivity (<0.5W m -1 k -1 ) Limiting its application to thermoelectric materials. In order to overcome the disadvantage of low thermal conductivity of polymers, the addition of high thermal conductivity fillers is an effective method. At present, direct filling of highly thermally conductive fillers such as metals, ceramics, carbon fillers, etc. is considered to be a common method for improving the heat transfer performance of polymer matrices.
Therefore, how to construct a more efficient heat conducting network in a high loading polymer matrix is crucial for the application of polymer composites in high power density electronic devices. Thus, there is a need for a film having excellent mechanical properties while using fillers with higher thermal conductivity at high filler loading to enhance the thermal conductivity of the polymer composite.
The production process of the cast sheet material is that resin is melted and plasticized by an extruder, extruded by a die orifice of a slit machine head, so that a melt material is attached to a cooling roller tightly, and the sheet material is prepared by the working procedures of stretching, trimming, coiling and the like. Sheets produced by the "casting process" for processing plastic thermoformed packaging articles are referred to as "cast" thermoformed sheets. The 'casting method' thermoforming sheet, the 'calendering method' thermoforming sheet and the 'calendering method' thermoforming sheet are essentially different from each other in the aspects of equipment, process, formula, performance, application, characteristics and the like.
The high-thermal-conductivity cast film prepared by the casting method can ensure higher in-plane thermal conductivity and has certain strength and toughness. The method can meet the requirement of the current-generation industrialization and bring a wide prospect for the development of electronic products.
Chinese patent No. CN 103738940A discloses an insulating polyvinyl alcohol composite heat conducting film, its preparation method and application, the prepared insulating polyvinyl alcohol composite heat conducting film includes a polyvinyl alcohol-graphene layer and polyvinyl alcohol layers located at two sides of the polyvinyl alcohol-graphene layer; the composite heat-conducting film prepared by the method has a sandwich structure, the two sides of the composite heat-conducting film are polyvinyl alcohol layers, the middle layer is a polyvinyl alcohol-graphene layer, and the surface of the film does not contain graphene, so that the composite heat-conducting film has good insulating property; the heat-conducting network can be formed in the film, so that the composite heat-conducting film has excellent heat-conducting property. However, the thermal conductivity and mechanical properties of the high thermal conductivity flexible film still cannot meet the requirements.
There is therefore a need to design a cast film that not only needs to have high in-plane heat transfer properties, but also needs to have excellent mechanical properties for use in modern electronic products.
Disclosure of Invention
The invention provides a preparation method of a high-thermal-conductivity cast film, which is simple and efficient, and the cast film prepared by the preparation method has higher in-plane thermal conductivity, higher insulativity and stronger mechanical property.
A preparation method of a high-thermal-conductivity cast film comprises the following steps:
adding a high-molecular base material into a dispersing agent to obtain a mixed solution, adding heat-conducting filler powder into the mixed solution, stirring to obtain slurry, defoaming, casting and drying the slurry in sequence to obtain a casting film, wherein the thickness of the casting film is 20-70 mu m, and carrying out hot pressing and stripping on the casting film to obtain the high-heat-conducting casting film.
According to the invention, the scraper in the casting process is used for scraping and coating the heat-conducting filler in the slurry at a proper height, so that the composite layers of the heat-conducting filler and the polymer matrix are arranged in an oriented manner in the scraping and coating direction of the scraper, and the prepared high-heat-conducting cast film is ensured to have certain uniformity and density, so that the cast film with higher mechanical property and higher heat conductivity is obtained, the scraper with too high thickness of the cast film cannot scrape the heat-conducting filler flat, a heat-conducting network cannot be formed, the heat conductivity is reduced, the polymer matrix material with too low thickness of the cast film cannot be fully filled into the heat-conducting filler, and the mechanical property is reduced.
Drying the heat-conducting filler powder before adding the heat-conducting filler powder into the mixed solution, wherein the drying temperature is as follows: 80-85 ℃, and the drying time is as follows: 24-48h.
The mass ratio of the heat-conducting filler to the polymer matrix is 1.
The polymer matrix material is polyvinyl alcohol, polyvinyl butyral, acrylic emulsion or silicon rubber.
The grain diameter of the heat-conducting filler is 0.5-10 mu m.
The particle size is too small, part of the heat-conducting filler cannot be scraped by a scraper to form directional arrangement, the heat conductivity is reduced, the particle size is too large, the heat-conducting filler is easy to deposit and agglomerate, and the filler cannot be directionally arranged.
The heat-conducting filler is boron nitride, a boron nitride nanosheet, a boron nitride nanotube or an aluminum oxide sheet.
The dispersant is phosphate, polyacrylic acid, an ethoxy compound, triolein, absolute ethyl alcohol or deionized water.
The drying temperature of the casting film is 48-100 ℃, and the drying time is 0.5-4h.
Further, the thickness of the casting film is 35-65 μm, the mass ratio of the heat-conducting filler to the polymer matrix is 4-8.5.
According to the invention, the heat-conducting filler with proper particle size and quality is added under the condition of proper thickness of the cast film, so that the heat-conducting filler can be scraped by a scraper to form directional arrangement in the scraping process, the proper particle size of the heat-conducting filler can form proper film layer number, and the proper polymer matrix content enables the film to have good flexibility.
The high-thermal-conductivity cast film is prepared by the preparation method of the high-thermal-conductivity cast film, and comprises a high-molecular matrix and high-thermal-conductivity fillers, wherein the high-molecular matrix is filled among the high-thermal-conductivity fillers, and the high-thermal-conductivity fillers are arranged in an oriented manner.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention enables the heat-conducting filler in the slurry to be directionally arranged under the combined action of the blade coating process of the casting process and the proper thickness of the casting film, thereby forming a heat-conducting network in the heat-conducting casting film, enabling the composite heat-conducting film to have excellent heat-conducting property, simultaneously filling enough polymer matrix between the heat-conducting fillers, enabling the film to have good flexibility, and finally forming the casting film with the in-plane heat conductivity of 12.05-45W m -1 K -1 Elongation at break of 3-5% and maximum volume resistance of 5.2X 10 13 Omega cm, and the tensile strength is 55-62.3MPa.
(2) The preparation method provided by the invention can be carried out at normal temperature, is simple and efficient, and can be industrialized on a large scale.
Drawings
FIG. 1 is an SEM image of an ultra-thin high thermal conductivity cast film prepared in example 1;
FIG. 2 is SEM image of an ultra-thin high thermal conductivity cast film prepared in example 2;
FIG. 3 is an SEM image of an ultra-thin high thermal conductivity cast film prepared in example 3;
fig. 4 is an SEM image of the ultra-thin high thermal conductive cast film prepared in example 5.
Detailed Description
The thermal conductivity of the tough high-thermal-conductivity film prepared in each embodiment is measured by an ASTM E1461-2013 test method; the elongation at break of the tough and high-thermal-conductivity film prepared in each embodiment is measured by a GB50150-2006 test method; the maximum volume resistance of the tough high-thermal-conductivity film prepared in each embodiment is measured by a GBT228-2002 test method; the tensile strength of the tough high-thermal-conductivity film prepared in each embodiment is measured by a GB/T34520.4-2017 test method.
Example 1
Raw materials: 12g of boron nitride nanosheets, 8g of polyvinyl butyral and 90mL of absolute ethanol.
First, polyvinyl butyral was uniformly mixed with 50mL of absolute ethanol to obtain a mixed solution a. And drying the boron nitride nanosheets at the temperature of 80 ℃ for 24 hours, wherein the particle size of the boron nitride nanosheets is about 3 mu m, and uniformly mixing the dried boron nitride nanosheets with 40mL of absolute ethyl alcohol to obtain a mixed solution B. And adding the mixed solution A into the mixed solution B, and uniformly mixing to obtain a mixed solution C. And then placing the mixed solution C in a mixer for defoaming and accelerating mixing, and finally stirring the mixed solution for 2 hours by using a stirrer so as to prepare the uniformly dispersed slurry suitable for tape casting. And finally pouring the slurry at the feed inlet of the casting machine, setting the temperature of an oven to be 58 ℃, and coating the cast film by using a roll-to-roll type casting coating machine. Standing at the constant temperature of 58 ℃ for 1h to obtain an ultrathin high-thermal-conductivity casting film with the boron nitride content of 60wt% as shown in figure 1, wherein the thickness of the casting film is 60 mu m. The in-plane thermal conductivity of the formed casting film can reach 12.05W m -1 K -1 Elongation at break up to 4.7%, maximum volume resistance 4.5X 10 13 Omega cm, tensile strength 59MPa.
Example 2
Raw materials: 16g of boron nitride nanosheets, 4g of polyvinyl butyral esters and 90mL of absolute ethyl alcohol.
First, 4g of polyvinyl butyral was uniformly mixed with 50mL of absolute ethanol to obtain a mixed solution a. And drying the boron nitride nanosheets at 82 ℃ for 30 hours, wherein the particle size of the boron nitride nanosheets is 5-6 microns, and uniformly mixing 16g of the boron nitride nanosheets with 40mL of absolute ethyl alcohol to obtain a mixed solution B. And adding the mixed solution A into the mixed solution B, and uniformly mixing to obtain a mixed solution C. And then placing the mixed solution C in a mixer for defoaming and accelerating mixing, and finally stirring the mixed solution for 2 hours by using a stirrer so as to prepare the uniformly dispersed slurry suitable for tape casting. And finally pouring the slurry at the feed inlet of the casting machine, setting the temperature of an oven to be 58 ℃, and coating the cast film by using a roll-to-roll type casting coating machine. Standing at the constant temperature of 58 ℃ for 1h to obtain an ultrathin high-heat-conductivity cast film with the boron nitride content of 80wt% as shown in figure 2, wherein the thickness of the cast film is 50 mu m. The in-plane thermal conductivity of the formed casting film can reach 45W m -1 K -1 Elongation at break of 3.2% and maximum volume resistance of 5.2 × 10 13 Omega cm, tensile strength 60.2MPa.
Example 3
Raw materials: 16g of aluminum oxide sheet, 4g of polyvinyl butyral ester and 90mL of absolute ethanol.
First, 4g of polyvinyl butyral was uniformly mixed with 40mL of absolute ethanol to obtain a mixed solution a. Then, 16g of aluminum oxide sheet was uniformly mixed with 50mL of absolute ethanol to obtain a mixed solution B. And adding the mixed solution A into the mixed solution B, and uniformly mixing to obtain a mixed solution C. And then placing the mixed solution C in a mixer for defoaming and accelerating mixing, and finally stirring the mixed solution for 2 hours by using a stirrer so as to prepare the uniformly dispersed slurry suitable for tape casting. And finally pouring the slurry at the feed inlet of the casting machine, setting the temperature of an oven at 60 ℃, and coating the casting film by using a roll-to-roll casting coating machine. Standing at 60 deg.C for 1 hr to obtain alumina powder with alumina content of 80wt%Thin high thermal conductivity cast film, the thickness of the cast film is 50 μm. The in-plane thermal conductivity of the formed casting film can reach 15.75W m -1 K -1 Elongation at break of 3.5% and maximum volume resistance of 2.1 × 10 13 Omega cm, tensile strength 60.3MPa.
Example 4
Raw materials: 18g of aluminum oxide sheet, 2g of polyvinyl butyral and 90mL of absolute ethanol.
First, 2g of polyvinyl butyral was uniformly mixed with 30mL of absolute ethanol to obtain a mixed solution A. The particle size of the alumina sheet is 8-9 μm, and then 18g of the alumina sheet is uniformly mixed with 60mL of absolute ethyl alcohol to obtain a mixed solution B. And adding the mixed solution A into the mixed solution B, and uniformly mixing to obtain a mixed solution C. And then placing the mixed solution C in a mixer for defoaming and accelerating mixing, and finally stirring the mixed solution for 2 hours by using a stirrer, thereby preparing the uniformly dispersed slurry suitable for tape casting. And finally pouring the slurry at the feed inlet of the casting machine, setting the temperature of an oven at 60 ℃, and coating the casting film by using a roll-to-roll casting coating machine. Standing for 1h at a constant temperature of 60 ℃ to obtain the ultrathin high-thermal-conductivity cast film with the aluminum oxide content of 90wt%, wherein the thickness of the cast film is 50 mu m. The in-plane thermal conductivity of the formed casting film can reach 19.20W m -1 K -1 Elongation at break of 5% and maximum volume resistance of 1.2X 10 13 Omega cm, tensile strength 48.5MPa.
Example 5
Raw materials: 16g of boron nitride nanosheet, 4g of polymethyl methacrylate and 80mL of N, N-dimethylformamide.
Firstly, dissolving 4g of polymethyl methacrylate in N, N-dimethylformamide, then stirring and ultrasonically treating for 0.5h, then adding a certain amount of boron nitride nanosheets into the solution of the polymethyl methacrylate, magnetically stirring for 2h, ultrasonically treating for more than 30min, and then placing the mixed solution into a mixer for defoaming and accelerating mixing. And finally pouring the slurry at the feed inlet of the casting machine, setting the temperature of an oven to be 75 ℃, and coating the cast film by using a roll-to-roll type cast coating machine. Standing at 75 deg.C for 1 hr to obtain boron nitride content as shown in FIG. 4Is 80wt% of ultrathin high heat conduction casting film, and the thickness of the casting film is 50 mu m. The in-plane thermal conductivity of the formed casting film can reach 20.98W m -1 K -1 Elongation at break of 5% and maximum volume resistance of 4.9 × 10 13 Omega cm, tensile strength of 62.3MPa.
Comparative example 1
Different from the embodiment 1, the polymer matrix is polyvinyl alcohol, the solvent is deionized water, and the mass ratio of boron nitride to the polymer matrix is 4:1, obtaining an ultrathin high-heat-conductivity casting film with the boron nitride content of 80wt%, wherein the thickness of the casting film is 78 mu m, and the in-plane heat conductivity of the formed casting film can reach 5.7W m -1 K -1 The elongation at break can reach 1.5%, and the maximum volume resistance is 2.2 multiplied by 10 11 Omega cm, tensile strength 30MPa.
Although the present invention has been described with reference to a few preferred embodiments, it should be understood that various changes and modifications can be made without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of a high-thermal-conductivity cast film is characterized by comprising the following steps:
adding a high-molecular base material into a dispersing agent to obtain a mixed solution, adding heat-conducting filler powder into the mixed solution, stirring to obtain slurry, defoaming, casting and drying the slurry in sequence to obtain a casting film, wherein the thickness of the casting film is 20-70 mu m, and carrying out hot pressing and stripping on the casting film to obtain the high-heat-conducting casting film.
2. The method for preparing a cast film with high thermal conductivity according to claim 1, wherein the heat-conducting filler powder is dried before being added into the mixed solution, and the drying temperature is as follows: 80-85 ℃, and the drying time is as follows: 24-48h.
3. The method for preparing a high thermal conductive cast film according to claim 1, wherein the mass ratio of the thermal conductive filler to the polymer matrix is 1.
4. The method of claim 1, wherein the polymer matrix material is polyvinyl alcohol, polyvinyl butyral, acrylic emulsion, or silicone rubber.
5. The production method of a high thermal conductive cast film according to claim 1, wherein the particle diameter of the thermal conductive filler is 0.5 to 10 μm.
6. The method of preparing a high thermal conductive cast film according to claim 1, wherein the thermally conductive filler is boron nitride, boron nitride nanosheets, boron nitride nanotubes, or aluminum oxide flakes.
7. The method of preparing a high thermal conductivity cast film according to claim 1, wherein the dispersant is phosphate, polyacrylic acid, ethoxy compound, triolein, absolute ethanol or deionized water.
8. The method of claim 1, wherein the drying temperature of the cast film is 48-100 ℃ and the drying time is 0.5-4h.
9. The method of claim 1, wherein the thickness of the cast film is 35 to 65 μm, the mass ratio of the heat conductive filler to the polymer matrix is 4 to 8.5, and the particle size of the heat conductive filler is 3 to 10 μm.
10. The preparation method of the high thermal conductivity casting film according to any one of claims 1 to 9, wherein the high thermal conductivity casting film comprises a polymer matrix and high thermal conductivity fillers, the polymer matrix is filled in the high thermal conductivity fillers, and the high thermal conductivity fillers are arranged in an oriented manner.
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| JP2011132474A (en) * | 2009-12-25 | 2011-07-07 | Hitachi Maxell Ltd | Method of manufacturing thermally conductive sheet and thermally conductive sheet manufactured by the manufacturing method |
| US20180326451A1 (en) * | 2015-12-09 | 2018-11-15 | University Of Delaware | Device and method for making shear-aligned, solvent-cast films |
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