CN109228549B - Preparation method of high-thermal-conductivity nanocellulose-based electrical insulation film material - Google Patents

Preparation method of high-thermal-conductivity nanocellulose-based electrical insulation film material Download PDF

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CN109228549B
CN109228549B CN201810881867.0A CN201810881867A CN109228549B CN 109228549 B CN109228549 B CN 109228549B CN 201810881867 A CN201810881867 A CN 201810881867A CN 109228549 B CN109228549 B CN 109228549B
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insulating film
nanocellulose
film material
heat
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CN109228549A (en
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杨洁
李翔
王秀
俞智怀
戴红旗
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Nanjing Forestry University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar form; Layered products having particular features of form
    • B32B3/26—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar form; Layered products having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer
    • B32B3/266—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar form; Layered products having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer characterised by an apertured layer, the apertures going through the whole thickness of the layer, e.g. expanded metal, perforated layer, slit layer regular cells B32B3/12
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/10—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of paper or cardboard
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
    • B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
    • B32B27/304—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising vinyl halide (co)polymers, e.g. PVC, PVDC, PVF, PVDF
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/34—Layered products comprising a layer of synthetic resin comprising polyamides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/02—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by a sequence of laminating steps, e.g. by adding new layers at consecutive laminating stations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
    • B32B2307/206—Insulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/302—Conductive

Abstract

The invention discloses a preparation method of a high-thermal-conductivity nano cellulose-based insulating film material, which comprises the steps of carrying out freeze drying on a nano fiber solution and polyamide epichlorohydrin resin to obtain nano fiber aerogel, carrying out high-temperature curing, then filling and filling uniformly dispersed h-BN suspension into pores of the nano fiber aerogel, and carrying out drying, press polishing and other steps to prepare the thermal-conductivity nano cellulose-based insulating film material. Compared with the traditional method for preparing the insulating film by conventional filling and blending, the method overcomes the fiber gap between the heat conduction materials, enables more interpenetrating heat conduction channels to be arranged between the two sides of the heat conduction insulating film, and greatly improves the heat conduction performance of the film.

Description

Preparation method of high-thermal-conductivity nanocellulose-based electrical insulation film material
Technical Field
The invention relates to the technical field of heat-conducting electrical insulation diaphragm materials of electronic equipment, in particular to a preparation method of a high-heat-conducting nanocellulose-based electrical insulation film.
Background
With the rapid progress of electronic information technology, electronic devices and components are developing towards miniaturization and high power, and higher requirements are put forward on the dielectric property and heat dissipation performance of insulating materials in the electronic devices and the components. To ensure proper and efficient operation of electronic equipment, it is necessary to conduct away internally generated heat in a timely manner. Therefore, development of insulating and encapsulating materials having more excellent thermal conductivity is required.
The nanocellulose has excellent mechanical properties, high elastic modulus and high tensile strength, and compared with a common synthetic high polymer, the nanocellulose has relatively low thermal expansion coefficient, so the nanocellulose is an ideal raw material for preparing the insulating diaphragm. However, due to the low intrinsic thermal conductivity of cellulose molecules and the microporous structure of the cellulose nanocellulose membrane, the thermal conductivity of the membrane is low (about 0.41W/(m · K)), which affects the heat dissipation performance of electronic devices and components. Therefore, the development of a novel nano cellulose membrane with good thermal conductivity has great application value.
Polyamide epichlorohydrin resins (PAE) are water-soluble thermosetting polymers having abundant reactive groups, including nitrogen heterocycles and alkyl functional groups, and are often added to paper products to improve their wet strength.
Hexagonal boron nitride (h-BN) is a non-oxide ceramic material with a crystal structure very similar to graphite. h-BN is one of the materials with the best heat conductivity in ceramic materials, the in-plane (001) heat conductivity of the h-BN reaches 180-200W/(m.K), and the heat conductivity of a pressed product reaches 30W/(m.K); the thermal expansion coefficient of the ceramic material is the minimum, and the deformation degree is small in the temperature rise process. In addition, h-BN is the best high temperature insulating material among ceramic materials and has a room temperature resistivity of 1014Omega cm, high-temperature breakdown voltage of 3kV/mm, low dielectric loss of 1082.5 × 10 at Hz-4The relative dielectric constant at room temperature was 4. Therefore, h-BN can be used as a heat-conducting insulating filler to fill the nano cellulose film to prepare the heat-conducting nano cellulose base composite insulating film.
The existing cellulose-based heat-conducting insulating paper or film material is generally prepared by adding heat-conducting mineral powder particles into aqueous-phase pulp fibers or nano-fiber suspension and performing blending, filtering and forming or casting and forming. The biggest defect of the method is that the fibers or the nano fibers are in direct contact with the heat-conducting mineral particles, so that the heat-conducting filler particles cannot be in full contact with each other to form a heat-conducting channel, and the heat-conducting property of the cellulose-based composite material is greatly weakened.
Disclosure of Invention
Aiming at the problem that fibers or nano fibers are in direct contact with heat conducting mineral particles in an isolation mode, and the heat conducting property of a cellulose-based composite material is not enough, the invention aims to provide a preparation method of a nano cellulose-based electrical insulation film with higher heat conducting property, which meets the requirements of strength property and insulation property of insulation films in electronic equipment and components, can conduct heat in the insulation films more quickly, and improves the heat dissipation performance of the equipment.
In order to achieve the purpose of the invention, the invention adopts the technical scheme that:
a preparation method of a high-thermal-conductivity nanocellulose-based insulating film material comprises the following steps:
1) preparing nano-cellulose aerogel by using a nano-cellulose fiber solution and polyamide epichlorohydrin resin (PAE) as raw materials; and allowing the PAE to cure;
2) infusing the nanofiber aerogel with a hexagonal boron nitride (h-BN) suspension; drying to remove most of water to obtain a heat-conducting insulating film blank sample;
3) attaching polyvinylidene fluoride microporous filter membranes (PVDF membranes) and filter paper on two sides of a blank sample of the heat-conducting insulating membrane, pressing tightly, and replacing the filter paper at regular time to obtain the heat-conducting insulating membrane with the water content of 8-12 wt%;
4) performing calendaring treatment on the heat-conducting insulating film with the moisture content of 8-12 wt%, and then performing constant-temperature and constant-humidity treatment to obtain the high-heat-conductivity nanocellulose-based insulating film material.
In the step 1), the raw materials are subjected to quick freezing and freeze drying at the temperature of-18 ℃ to obtain the nano cellulose aerogel.
In step 1), the nanocellulose aerogel was placed in an oven at 105 ℃ for 0.5h to cure the PAE.
In step 2), the nano-fiber aerogel is infused with a hexagonal boron nitride (h-BN) suspension with a solid content of 2 wt%.
In the step 2), drying the nanofiber aerogel poured with the h-BN heat-conducting filler particles in an oven at 30 ℃ for 5 hours to obtain a heat-conducting insulating film blank sample.
And 4) performing calendaring treatment on the heat-conducting insulating film with the moisture content of 10 wt%, and then performing constant temperature and humidity for 72h to obtain the high-heat-conductivity nano cellulose-based insulating film material.
The high-thermal-conductivity nanocellulose-based insulating film material is obtained by the preparation method of the high-thermal-conductivity nanocellulose-based insulating film material.
Has the advantages that: compared with the prior art, the method comprises the steps of mixing a nano-cellulose solution with polyamide epichlorohydrin resin, quickly freezing, freeze-drying to obtain nano-cellulose aerogel, solidifying PAE, filling the nano-cellulose aerogel with hexagonal boron nitride heat-conducting mineral particle water dispersion suspension, drying, and press polishing to obtain the nano-cellulose-based electrical insulation film material with network interpenetrating channels, so that the overall heat-conducting performance of the film material is greatly improved, the fiber gap between heat-conducting materials is overcome, more interpenetrating heat-conducting channels are formed between two sides of the heat-conducting insulation film, the heat-conducting performance of the film is greatly improved, the requirements of strength and insulation performance of the insulation film in electronic equipment and components can be met, the internal heat can be conducted more quickly, the heat dissipation performance of the equipment is improved, and the method has good practicability.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
Example 1
26.6g of nano-cellulose suspension with the concentration of 0.5 wt% is put into a beaker, 1.14g of PAE with the concentration of 0.1 wt% is added while stirring, after uniform dispersion, the nano-cellulose suspension is transferred into a plastic culture dish with the diameter of 6.5cm, the plastic culture dish is put into a refrigerator to be fully frozen at the temperature of 18 ℃ below zero, the frozen sample is frozen and dried for 72 hours in a freeze dryer with the temperature of 80 ℃ below zero and 15Pa, and the frozen sample is taken out and put into a drying oven with the temperature of 105 ℃ for 0.5 hour to obtain the nano-cellulose aerogel solidified by the PAE (the wet strength can be improved by about 8% under the condition that the PAE is not added under the dosage of 0.5 wt%). Placing the nano cellulose aerogel in a hexagonal boron nitride (h-BN) solution with the concentration of 2 wt% for ultrasonic vibration for 15min under the power of 120w for perfusion, taking out and then drying in a 30 ℃ drying oven for 5h, removing most of water, attaching a polyvinylidene fluoride microporous filter membrane (PVDF membrane) with the pore diameter of 0.22 mu m and filter paper on two sides, compacting under the pressure of 0.5MPa, and replacing the filter paper once every 6-8 h to obtain a heat-conducting insulating film with the water content of about 10 wt%; and performing calendaring treatment on the heat-conducting insulating film with the moisture content of 10 wt%, and then performing constant temperature and humidity for 72h to obtain the heat-conducting nano cellulose-based composite film with the filler content of 6 wt%, wherein the heat conductivity coefficient is 0.651W/(m.K).
Example 2
26.6g of nano-cellulose suspension with the concentration of 0.5 wt% is put into a beaker, 1.14g of PAE with the concentration of 0.1 wt% is added while stirring, after uniform dispersion, the nano-cellulose suspension is transferred into a plastic culture dish with the diameter of 6.5cm, the plastic culture dish is put into a refrigerator to be fully frozen at the temperature of 18 ℃ below zero, the frozen sample is frozen and dried for 72 hours in a freeze dryer with the temperature of 80 ℃ below zero and 15Pa, and the frozen sample is taken out and put into a drying oven with the temperature of 105 ℃ for 0.5 hour to obtain the nano-cellulose aerogel solidified by the PAE (the wet strength can be improved by about 8% under the condition that the PAE is not added under the dosage of 0.5 wt%). Then placing the nano-cellulose aerogel in a hexagonal boron nitride (h-BN) solution with the concentration of 2 wt% for ultrasonic vibration for 30min under the power of 120w for perfusion, taking out and then drying in a drying oven at the temperature of 30 ℃ for 5h, removing most of water, attaching a polyvinylidene fluoride microporous filter membrane (PVDF membrane) with the pore diameter of 0.22 mu m and filter paper on two sides, compacting under the pressure of 0.5MPa, and replacing the filter paper once every 6-8 h to obtain a heat-conducting insulating film with the water content of about 10 wt%; and performing calendaring treatment on the heat-conducting insulating film with the moisture content of 10 wt%, and then performing constant temperature and humidity for 72h to obtain the heat-conducting nano cellulose-based composite film with the filler content of 10 wt%, wherein the heat conductivity coefficient is 0.882W/(m.K).
Example 3
26.6g of nano-cellulose suspension with the concentration of 0.5 wt% is put into a beaker, 1.14g of PAE with the concentration of 0.1 wt% is added while stirring, after uniform dispersion, the nano-cellulose suspension is transferred into a plastic culture dish with the diameter of 6.5cm, the plastic culture dish is put into a refrigerator to be fully frozen at the temperature of 18 ℃ below zero, the frozen sample is frozen and dried for 72 hours in a freeze dryer with the temperature of 80 ℃ below zero and 15Pa, and the frozen sample is taken out and put into a drying oven with the temperature of 105 ℃ for 0.5 hour to obtain the nano-cellulose aerogel solidified by the PAE (the wet strength can be improved by about 8% under the condition that the PAE is not added under the dosage of 0.5 wt%). Then placing the nano-cellulose aerogel in a hexagonal boron nitride (h-BN) solution with the concentration of 2 wt% for ultrasonic vibration for 45min under the power of 120w for perfusion, taking out and then drying in a 30 ℃ drying oven for 5h, removing most of water, attaching a polyvinylidene fluoride microporous filter membrane (PVDF membrane) with the pore diameter of 0.22 mu m and filter paper on two sides, compacting under the pressure of 0.5MPa, and replacing the filter paper once every 6-8 h to obtain a heat-conducting insulating film with the water content of about 10 wt%; performing calendaring treatment on the heat-conducting insulating film with the moisture content of 10 wt%, and then performing constant temperature and humidity for 72h to obtain the heat-conducting nano cellulose-based composite film with the filler content of 14 wt%, wherein the heat conductivity coefficient is 1.005W/(m.K).
The properties of the thermal conductive nanocellulose-based composite insulation films prepared by the preparation methods of the above examples 1, 2 and 3 were compared with those of the nanocellulose films not filled with the thermal conductive insulating filler and the composite insulation films prepared by the blending method, and the results are shown in table 1 below.
TABLE 1 comparative results
Figure BDA0001753232480000041
Wherein the thermal conductivity is improved relative to a nano-cellulose film not filled with a thermally conductive insulating filler.
The blending method comprises the following steps: 26.6g of nano-cellulose suspension with the concentration of 0.5 wt% is taken to be put in a beaker, 1.14g of PAE with the concentration of 0.1 wt% is added while stirring, after uniform mixing, h-BN is added and placed on a magnetic stirrer to be stirred for 30min, and then the mixture is transferred to an ultrasonic disperser to be subjected to ultrasonic treatment for 10min under the power of 120w, so that the mixture is uniformly mixed. Pouring the fully mixed h-BN/PAE/CNF dispersion into a culture dish with the diameter of 6.5cm, drying the culture dish in a drying oven at the temperature of 30 ℃ for 5 hours, removing most of water, attaching a polyvinylidene fluoride microporous filter membrane (PVDF membrane) with the pore diameter of 0.22 mu m and filter paper on two sides, compacting the filter paper under the pressure of 0.5MPa, and replacing the filter paper every 6 to 8 hours to obtain a heat-conducting insulating film with the water content of about 10 weight percent; and performing calendaring treatment on the heat-conducting insulating film with the moisture content of 10 wt%, and then performing constant temperature and humidity for 72h to obtain the h-BN/PAE/CNF heat-conducting nanocellulose-based composite film.
From the above examples, it can be seen that when h-BN particles are added as a filler to the nano cellulose film, the thermal conductivity of the composite insulating film increases with the increase of the content of h-BN, but the thermal conductivity is improved more remarkably by the perfusion method under the condition that the content of the filler is approximately the same, and when the content of h-BN is 6%, 10% and 14%, the thermal conductivity of the composite film is respectively 0.651, 0.882 and 1.005W/m.K, which are respectively increased by 57.63%, 113.56% and 143.34% compared with the pure nano cellulose film.

Claims (7)

1. A preparation method of a high-thermal-conductivity nanocellulose-based insulating film material is characterized by comprising the following steps:
1) preparing nano-cellulose aerogel by using a nano-cellulose fiber solution and polyamide epichlorohydrin resin as raw materials; and curing the polyamide epichlorohydrin resin;
2) using hexagonal boron nitride suspension to perfuse the nano-cellulose aerogel; drying to remove most of water to obtain a heat-conducting insulating film blank sample;
3) attaching polyvinylidene fluoride microporous filter membranes and filter paper on two sides of a blank sample of the heat-conducting insulating film, compacting, and replacing the filter paper at regular time to obtain the heat-conducting insulating film with the water content of 8-12 wt%;
4) performing calendaring treatment on the heat-conducting insulating film with the moisture content of 8-12 wt%, and then performing constant-temperature and constant-humidity treatment to obtain the high-heat-conductivity nanocellulose-based insulating film material.
2. The method for preparing a nanocellulose-based insulating film material with high thermal conductivity according to claim 1, wherein in step 1), the raw material is subjected to quick freezing and freeze drying at-18 ℃ to obtain nanocellulose aerogel.
3. The method for preparing a high thermal conductivity nanocellulose-based insulating film material as claimed in claim 1, wherein in step 1), the nanocellulose aerogel is placed in an oven at 105 ℃ for 0.5h to cure the polyamide epichlorohydrin resin.
4. The method for preparing a nanocellulose-based insulating film material with high thermal conductivity according to claim 1, wherein in step 2), the nanocellulose aerogel is infused with a hexagonal boron nitride suspension with a solid content of 2 wt%.
5. The preparation method of the high thermal conductivity nanocellulose-based insulating film material as claimed in claim 1, wherein in step 2), the nanocellulose aerogel infused with hexagonal boron nitride thermal conductive filler particles is oven-dried at 30 ℃ for 5h to obtain a thermal conductivity insulating film blank.
6. The method for preparing the high thermal conductivity nanocellulose-based insulating film material as claimed in claim 1, wherein in step 4), the thermal conductive insulating film with the moisture content of 10 wt% is subjected to a calendering treatment, and then the constant temperature and humidity is maintained for 72h to obtain the high thermal conductivity nanocellulose-based insulating film material.
7. The high thermal conductive nanocellulose-based insulating film material obtained by the method for preparing the high thermal conductive nanocellulose-based insulating film material according to any one of claims 1 to 6.
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