CN109971020A - A kind of functional nano-fiber element-boron nitride laminated film and preparation method thereof - Google Patents
A kind of functional nano-fiber element-boron nitride laminated film and preparation method thereof Download PDFInfo
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- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/04—Oxycellulose; Hydrocellulose
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Abstract
It is to form sedimentary after filtering on mixed cellulose ester microporous membrane, the manufactured laminated film internal layer to the sedimentary hot-pressing drying by nano-cellulose-boron nitride dispersion the invention discloses a kind of functional nano-fiber element-boron nitride laminated film；And the laminated film internal layer is nano-cellulose-nitridation boron composite type single layer structure, wherein the content of boron nitride is 1%-7wt%.The invention also discloses preparation methods comprising: (1) nano-cellulose dispersion liquid and boron nitride dispersion are mixed, stirring, Ultrasonic Pulverization, obtains nano-cellulose-boron nitride dispersion；(2) dispersion liquid is placed on mixed ester membranes be filtered by vacuum and forms sedimentary, removed mixed ester membranes, laminated film internal layer will be obtained after sedimentary hot-pressing drying.Laminated film thermal coefficient provided by the invention is high, and hydrophobic insulation performance is high, can be widely applied to electronic device and technical field of biological material.
Description
Technical field
The present invention relates to a kind of functional nano-fiber element-boron nitride laminated films and preparation method thereof, more particularly to one kind
Heat conducting insulating film with hydrophobic function belongs to heat-conductive composite material field.
Background technique
With the fast development of electronics technology, the equipment such as communicating circuit, semiconductor tend to miniaturization, densification.These are high
Also a large amount of heat can be generated while power apparatus is rapidly run, prolonged use not only will affect the essence of electronic device
Degree can also cause equipment to damage and then influence its service life.So being highly desirable the high property that research has good heat radiating characteristic
It can management device.Most of substrates of heat-conducting plastic do not allow after petrochemicals, discarding it is degradable, to economical and
Environment brings serious problems.
Nano-cellulose rich content in nature, diameter is generally in 100nm hereinafter, length is from 100nm to several microns
It differs, there is excellent intensity, Young's modulus, toughness and the transparency.In addition, also having biodegradability concurrently, it is widely used in
Electronic device, biomaterial and aerospace field etc..At the same time, nano-cellulose limits it there is also some defects and makes
With cannot radiate in time when as electronic device material, shorten the service life of device if heating conduction is poor.Therefore, exist
Guarantee how to effectively improve the pole that its heating conduction causes researcher except the excellent comprehensive performance of nano-cellulose itself
Big interest.
Hexagonal boron nitride belongs to hexagonal crystal system, has the layer structure similar to graphite, therefore has the title of white graphite.Every layer by
Nitrogen-atoms and boron atom six side cyclic structures of spaced formation, atom is tightly combined by being covalently keyed in layer；Interlayer is logical
Molecular link connection is crossed, interaction force is weak, therefore is easily peeled off.Boron nitride superior performance, direction thermal coefficient is up to 400W/ in face
(mK), in current ceramic material, boron nitride is the best material of heating conduction.In addition, boron nitride forbidden bandwidth is big
(5.9eV), therefore there is good electrical insulating property (high resistivity, low-k, low dielectric absorption), resistivity at room temperature is
1016-1018Ω cm, resistivity at 2000 DEG C can also reach 104Ω cm is splendid high temperature insulating material.Boron nitride
These excellent characteristics make it have potential application in fields such as thermal management materials, aerospace and supercapacitors.
In the prior art, a kind of MULTILAYER COMPOSITE thermally conductive film of Chinese invention application 201711313427.7 disclosure of the invention and
Preparation method.The middle layer of the thermally conductive film is nano-cellulose film, and the upper and lower surface of the nano-cellulose film is distinguished
Successively coated with nano cellulose/graphene film layer or (and) nano-cellulose/boron nitride thin film layer, pass through fibre between layers
Tie up the hydrogen bond action connection between plain matrix and the ABA three-decker of formation and the composite heat-conducting film of ACBCA five-layer structure, every layer
The mass range of film is 15-30mg；The content of graphene is 6~10wt% in the nano-cellulose/graphene film layer；
The content of boron nitride is 6~10wt% in the nano-cellulose/boron nitride thin film layer.Boron nitride has higher with graphene
Thermal conductivity, therefore film thermal conductivity with higher；The core toughening and multilayer biomimetic features of median fiber element layer, make it
Possess excellent mechanical property；Outer layer is the mixed layer of boron nitride and cellulose, and the film is made to have good electrical insulating property.This
Invention can solve the heat dissipation problem of modern electronic devices, be applied in heat conduction and heat radiation component.
But the laminated film number of plies in foregoing invention is more, preparation process is complicated and is difficult to stably produce；Meanwhile by
Very big in nano-cellulose specific surface area, and surface hydroxyl rich in, hydrophily is strong, once water droplet be adhered to it is compound
Material surface can be such that material is seriously destroyed；On the other hand, strong hydrogen bonding effect easy to form between hydroxyl, leads to Nanowire
Dimension element is reunited, the poor biocompatibility with hydrophobic matrix, thus the laminated film is made not have hydrophobicity, in very great Cheng
Application of the laminated film in real life is limited on degree, it is difficult to meet a variety of need of electronic device and technical field of biological material
It asks and (is provided simultaneously with thermally conductive, insulation, hydrophobic performance).
Therefore, for a variety of demands of electronic device and technical field of biological material, research provide one kind be provided simultaneously with it is good
Thermally conductive, insulation, hydrophobic function performance, and the number of plies is few, the convenient new laminated film of preparation, becomes more urgent.
Summary of the invention
It is an object of the invention to be directed to the above-mentioned deficiency of the prior art, provide that a kind of number of plies is few, there have to be good thermally conductive, exhausted
Functional nano-fiber element-boron nitride laminated film of edge, hydrophobic function；There is provided preparation method simultaneously, this method is easy to operate,
It is easy to volume production and stable product quality.
In order to achieve the above object, technical solution of the invention are as follows:
A kind of functional nano-fiber element-boron nitride laminated film, which is characterized in that it is by nano-cellulose-boron nitride
Dispersion liquid is to form deposition after filtering on mixed cellulose ester microporous membrane by nano-cellulose-boron nitride dispersion
Layer, the manufactured laminated film internal layer to the sedimentary hot-pressing drying；And the laminated film internal layer is nano-cellulose-boron nitride
Compound single layer structure, wherein the content of boron nitride is 1%-7wt%.
Wherein, the diameter of the mixed ester membranes be 44mm, aperture 0.45um.
Functional nano-fiber element-boron nitride the laminated film, which is characterized in that the upper following table of the laminated film internal layer
On face, it is respectively provided with the hydrophobic outer layer that modified organosilicon material is formed, which coats the laminated film internal layer completely,
Form functional nano-fiber element-boron nitride laminated film.
A method of preparing the functional nano-fiber element-boron nitride laminated film, which is characterized in that it includes following
Step:
(1) set amount nano-cellulose and boron nitride are added separately in dispersing agent ionized water, are configured to Nanowire
Plain dispersion liquid, boron nitride dispersion are tieed up, then mixes above-mentioned nano-cellulose dispersion liquid and boron nitride dispersion, is stirred, is surpassed
Sound crushes, and obtains nano-cellulose-boron nitride dispersion；
(2) by nano-cellulose-boron nitride dispersion obtained in above-mentioned steps (1), mixed ester membranes are placed in
On carry out vacuum filtration and form sedimentary, then remove mixed ester membranes, sedimentary hot-pressing drying is dry, answered
Close film internal layer；
(3) in the upper and lower surface of the laminated film internal layer, one layer of modified organic silicon material is respectively sprayed, is formed after dry hydrophobic
Functional nano-fiber element-boron nitride laminated film is made in outer layer.
Mixed ester membranes diameter in the step (2) is 44mm, aperture 0.45um.
The utility model has the advantages that
A kind of nano-cellulose-boron nitride laminated film of the invention and preparation method thereof has the advantage that
(1) nano-cellulose provided by the invention-boron nitride laminated film, the number of plies is few (for single layer or three-decker),
Its thermal coefficient is high, and hydrophobic insulation performance is high, can be widely applied to electronic device and technical field of biological material.
(2) material provided by the invention and preparation method promote nano-cellulose strand by the method for hot-pressing drying
With boron nitride along face direction orientations.Since hydrolysis occurs, the boron nitride after ultrasound is peeled off contains hydroxyl at edge
Hydrogen bond is formed between amino, and the hydroxyl on nano-cellulose surface, so that will not reunite between boron nitride, is equably divided
It is dispersed in nano-cellulose matrix.And the hydrogen bond action between nano-cellulose and boron nitride makes boron nitride shape in the base
At good thermal conducting path, when boron nitride content is 7%, thermal coefficient can achieve 11.8Wm in the face of laminated film-1·K-1。
(3) film outside of the invention, using treated the modified organic silicon material such as silane, such as silica, by
Contain a large amount of methyl in its surface, be tightly combined with the internal layer of laminated film, while middle can significantly improve its outer surface
Hydrophobicity is significantly expanded the application range of laminated film.
(4) preparation method of the invention, production technology is compact, easy to implement, is suitable for industrial mass production, and product
Quality is stablized.
Detailed description of the invention
Fig. 1 is the hydrophobic figure of functional nano-fiber element-boron nitride laminated film prepared by embodiment 1.
Fig. 2 is the hydrophobic figure of functional nano-fiber element-boron nitride laminated film prepared by embodiment 2.
Fig. 3 is the hydrophobic figure of functional nano-fiber element-boron nitride laminated film prepared by embodiment 3.
Fig. 4 is the hydrophobic figure of functional nano-fiber element-boron nitride laminated film prepared by embodiment 4.
With reference to the accompanying drawing and specific embodiment the invention will be described in further detail.
Specific embodiment
Embodiment 1:
Functional nano-fiber element-boron nitride laminated film provided in this embodiment is by nano-cellulose-boron nitride point
Dispersion liquid forms sedimentary after filtering on mixed cellulose ester microporous membrane, manufactured compound to the sedimentary hot-pressing drying
Film internal layer；And the laminated film internal layer is nano-cellulose-nitridation boron composite type single layer structure, wherein the content of boron nitride is
1%-7wt% (content for accounting for film dry matter).
Wherein, the diameter of the mixed ester membranes be 44mm, aperture 0.45um.
Functional nano-fiber element-boron nitride the laminated film in the upper and lower surface of the laminated film internal layer, is respectively provided with
The hydrophobic outer layer that modified organosilicon material is formed, the outer layer coat the laminated film internal layer completely, form function and receive
Rice cellulose-boron nitride laminated film.
A method of preparing aforementioned functional nano-fiber element-boron nitride laminated film comprising following steps:
(1) set amount nano-cellulose and boron nitride are added separately in dispersing agent ionized water, are configured to Nanowire
Plain dispersion liquid, boron nitride dispersion are tieed up, then mixes above-mentioned nano-cellulose dispersion liquid and boron nitride dispersion, is stirred, is surpassed
Sound crushes, and obtains nano-cellulose-boron nitride dispersion；
(2) by nano-cellulose-boron nitride dispersion obtained in above-mentioned steps (1), mixed ester membranes are placed in
On carry out vacuum filtration formed sedimentary (also referred to as filter cake), remove mixed ester membranes, after sedimentary hot-pressing drying, i.e.,
Obtain laminated film internal layer；
(3) on the outer surface of the two sides up and down of the laminated film internal layer, one layer of modified organic silicon material is respectively sprayed, after dry
Hydrophobic outer layer is formed, functional nano-fiber element-boron nitride laminated film is made.
Specifically, preparation method, comprising the following steps:
(1) nano-cellulose of the boron nitride of 0.0007g and 0.0693g is added separately in dispersing agent, is prepared respectively
The nano-cellulose dispersion liquid that boron nitride dispersion that concentration is 2.2mg/mL, concentration are 1.5mg/mL, then by above-mentioned nanometer
Cellulose dispersion liquid and boron nitride dispersion mixing, stir 30min, continue ultrasound 15min at cell disruptor (80W), make it
It is uniformly dispersed, obtains nano-cellulose-boron nitride dispersion, the dispersing agent is deionized water；
(2) nano-cellulose-boron nitride dispersion obtained in above-mentioned steps (1) is placed in film (mixed cellulose ester
Miillpore filter, diameter 44mm, aperture 0.45um) on filtered, form sedimentary；The sedimentary is thoroughly clear with deionized water
It washes away except impurity；Sedimentary carefully is removed, is clamped between the steel plate with certain pressure, 50 DEG C is heated to and continues drying out 12h,
Obtain nano-cellulose-boron nitride laminated film internal layer.
(3) spraying concentration is the silane-modified silica of 1.5mg/mL in both side surface above and below laminated film internal layer
Alcohol dispersion liquid obtains the heat conductive insulating functional nano-fiber element-boron nitride THIN COMPOSITE with hydrophobic function after natural drying
Film.
Multinomial detection is done to the element of functional nano-fiber made from embodiment 1-boron nitride laminated film using laser flash method,
As a result as follows: thermal coefficient is 7.3Wm in the face of laminated film-1·K-1, the hydrophobic performance such as attached drawing after contact angle test
Shown in 1, contact angle 134.1o.
Embodiment 2: functional nano-fiber element-boron nitride laminated film provided in this embodiment and preparation method thereof, with reality
It is essentially identical to apply example 1, the difference is that:
(1) nano-cellulose of the boron nitride of 0.0021g and 0.0679g is added separately in dispersing agent, is prepared respectively
The nano-cellulose dispersion liquid that boron nitride dispersion that concentration is 2.2mg/mL, concentration are 1.5mg/mL, then by above-mentioned nanometer
Cellulose dispersion liquid and boron nitride dispersion mixing, stir 30min, continue ultrasound 15min at cell disruptor (80W), make it
It is uniformly dispersed, obtains nano-cellulose-boron nitride dispersion, the dispersing agent is deionized water.
(2) nano-cellulose-boron nitride dispersion obtained in above-mentioned steps (1) is placed in film (mixed cellulose ester
Miillpore filter, diameter 44nm, aperture 0.45um) on filtered, form sedimentary, obtained sedimentary deionized water is thorough
Bottom cleaning removal impurity.Sedimentary carefully is removed, is clamped between the steel plate with certain pressure, 50 DEG C is heated to and continues drying out
12h to get arrive nano-cellulose-boron nitride laminated film internal layer；
(3) ethyl alcohol for the silane-modified silica that spraying concentration is 1.5mg/mL in laminated film internal layer both side surface
Dispersion liquid obtains the functional nano-fiber element-boron nitride laminated film with hydrophobic function after natural drying.
Multinomial detection is done to nano-cellulose made from embodiment 2-boron nitride laminated film using laser flash method, as a result
As follows: thermal coefficient is 7.8Wm in the face of laminated film-1·K-1, hydrophobic performance is as shown in Fig. 2, and contact angle is
145.0o。
Embodiment 3:
Functional nano-fiber element-boron nitride laminated film provided in this embodiment and preparation method thereof, with embodiment 1,2 bases
This is identical, the difference is that:
(1) nano-cellulose of the boron nitride of 0.0035g and 0.0665g is added separately in dispersing agent, is prepared respectively
The nano-cellulose dispersion liquid that boron nitride dispersion that concentration is 2.2mg/mL, concentration are 1.5mg/mL, then by above-mentioned nanometer
Cellulose dispersion liquid and boron nitride dispersion mixing, stir 30min, continue ultrasound 15min at cell disruptor (80W), make it
It is uniformly dispersed, obtains nano-cellulose-boron nitride dispersion, the dispersing agent is deionized water；
(2) nano-cellulose-boron nitride dispersion obtained in above-mentioned steps (1) is placed in film (mixed cellulose ester
Miillpore filter, diameter 44mm, aperture 0.45um) on filtered to obtain sedimentary, the sedimentary is thoroughly clear with deionized water
It washes away except impurity.Sedimentary carefully is removed, is clamped between the steel plate with certain pressure, 50 DEG C is heated to and continues drying out 12h,
Obtain nano-cellulose-boron nitride laminated film internal layer；
(3) ethyl alcohol for the silane-modified silica that spraying concentration is 1.5mg/mL in laminated film internal layer both side surface
Dispersion liquid obtains the heat conductive insulating functional nano-fiber element-boron nitride laminated film with hydrophobic function after natural drying.
Multinomial detection is done to nano-cellulose made from embodiment 3-boron nitride laminated film using laser flash method, as a result
As follows: thermal coefficient is 9.7Wm in the face of laminated film-1·K-1, hydrophobic performance is as shown in Fig. 3, and contact angle is
135.9o。
Embodiment 4: functional nano-fiber element-boron nitride laminated film provided in this embodiment and preparation method thereof, with reality
It is essentially identical to apply example 1~3, the difference is that:
(1) nano-cellulose of the boron nitride of 0.0049g and 0.0651g is added separately in dispersing agent, is prepared respectively
The nano-cellulose dispersion liquid that boron nitride dispersion that concentration is 2.2mg/mL, concentration are 1.5mg/mL, then by above-mentioned nanometer
Cellulose dispersion liquid and boron nitride dispersion mixing, stir 30min, continue ultrasound 15min at cell disruptor (80W), make it
It is uniformly dispersed, obtains nano-cellulose-boron nitride dispersion, the dispersing agent is deionized water；
(2) nano-cellulose-boron nitride dispersion obtained in above-mentioned steps (1) is placed in film (mixed cellulose ester
Filter membrane, diameter 44mm, aperture 0.45um) on filtered, obtain sedimentary, which is thoroughly cleaned and is gone
Except impurity.Carefully remove sedimentary, be clamped between the steel plate with certain pressure, be heated to 50 DEG C continue drying out 12h to get
To nano-cellulose-boron nitride laminated film internal layer；
(3) ethyl alcohol for the silane-modified silica that spraying concentration is 1.5mg/mL in laminated film internal layer both side surface
Dispersion liquid obtains the heat conductive insulating laminated film with hydrophobic function after natural drying.
Multinomial detection is done to nano-cellulose made from embodiment 4-boron nitride laminated film using laser flash method, as a result
As follows: thermal coefficient is 11.8Wm in the face of laminated film-1·K-1, hydrophobic performance is as shown in Fig. 4, and contact angle is
144.9o。
Present invention is not limited to the embodiments described above, using the obtained other nanofibers of same or similar method
Element-boron nitride laminated film and preparation method thereof, such as using approximate component, proportion and step, model is protected in the present invention
In enclosing.
Claims (6)
1. a kind of functional nano-fiber element-boron nitride laminated film, which is characterized in that it is by nano-cellulose-boron nitride point
Dispersion liquid forms sedimentary after filtering on mixed cellulose ester microporous membrane, manufactured compound to the sedimentary hot-pressing drying
Film internal layer；And the laminated film internal layer is nano-cellulose-nitridation boron composite type single layer structure, wherein the content of boron nitride is
1%-7wt%.
2. functional nano-fiber element-boron nitride laminated film according to claim 1, which is characterized in that the mixing
The diameter of cellulose ester membrane filter is 44mm, aperture 0.45um.
3. functional nano-fiber element-boron nitride laminated film according to claim 1 or 2, which is characterized in that the THIN COMPOSITE
In the upper and lower surface of film inner layer, it is respectively provided with the hydrophobic outer layer that modified organosilicon material is formed, the outer layer is by the THIN COMPOSITE
Film inner layer coats completely, forms functional nano-fiber element-boron nitride laminated film.
4. a kind of prepare the element of functional nano-fiber described in claim 1-boron nitride laminated film method, which is characterized in that
Itself the following steps are included:
(1) set amount nano-cellulose and boron nitride are added separately in dispersing agent ionized water, are configured to nano-cellulose
Then dispersion liquid, boron nitride dispersion mix above-mentioned nano-cellulose dispersion liquid and boron nitride dispersion, stirring, ultrasonic powder
It is broken, obtain nano-cellulose-boron nitride dispersion；
(2) by nano-cellulose-boron nitride dispersion obtained in above-mentioned steps (1), it is enterprising that mixed ester membranes are placed in
Row vacuum filtration forms sedimentary, removes mixed ester membranes, by after the sedimentary hot-pressing drying to get arriving laminated film
Internal layer.
5. the preparation method according to claim 4, which is characterized in that method includes the following steps:
(3) in the upper and lower surface of the laminated film internal layer, one layer of modified organic silicon material is respectively sprayed, is formed after dry hydrophobic outer
Functional nano-fiber element-boron nitride laminated film is made in layer.
6. the preparation method according to claim 4, which is characterized in that method includes the following steps:
Mixed ester membranes diameter in the step (2) is 44mm, aperture 0.45um.
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| CN113179611A (en) * | 2021-03-15 | 2021-07-27 | 佛山市晟鹏科技有限公司 | Boron nitride heat dissipation film and preparation method and application thereof |
| CN113416334A (en) * | 2021-07-09 | 2021-09-21 | 陕西科技大学 | Hydroxyethyl cellulose/boron nitride nano composite film and preparation method thereof |
| CN113861947A (en) * | 2021-08-13 | 2021-12-31 | 中国地质大学（武汉） | Boron nitride dispersion method using macromolecules as templates |
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| CN114573932A (en) * | 2022-03-16 | 2022-06-03 | 北京大学 | High-thermal-conductivity boron nitride paper based on large-sheet intrinsic hexagonal boron nitride and preparation method thereof |
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