CN109627471A - A kind of preparation method and applications of high thermal conductivity flexible membrane - Google Patents
A kind of preparation method and applications of high thermal conductivity flexible membrane Download PDFInfo
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- CN109627471A CN109627471A CN201811470343.9A CN201811470343A CN109627471A CN 109627471 A CN109627471 A CN 109627471A CN 201811470343 A CN201811470343 A CN 201811470343A CN 109627471 A CN109627471 A CN 109627471A
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of 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
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
Abstract
It is first to prepare hydroxylating boron nitride nanosheet aqueous dispersions and nano-cellulose aqueous dispersions the invention discloses a kind of preparation method and applications of high thermal conductivity flexible membrane；Then hydroxylating boron nitride nanosheet aqueous dispersions are mixed with nano-cellulose aqueous dispersions, stirring, ultrasound obtain finely dispersed hydroxylating boron nitride nanosheet/nano-cellulose aqueous dispersions；Moisture removal is filtered again, is dried at room temperature, and hydroxylating boron nitride nanosheet/nano cellulose composite film i.e. high thermal conductivity flexible membrane is obtained.The high thermal conductivity flexible membrane has high heat conductance, very good mechanical properties and thermal stability, can be used as the heat sink material of electronic/electrical gas product.
Description
Technical field
The present invention relates to Material Field, in particular to a kind of preparation method and applications of high thermal conductivity flexible membrane.
Background technique
With the high speed development of electrical equipment and electronic product, such as mobile phone and laptop electronic product are to small ruler
Very little, high-power and high speed direction is developed, and the amount of heat generated in operational process will lead to the component damage of equipment, shortens
Service life, or even explode, therefore it is extremely important to design efficient thermal management materials.Thermal management materials are mainly polymer
Compound high thermal conductivity filler, the stability having had, excellent processability and low cost.Since the thermal conductivity of polymer is often low
In 0.3w.m-1k-1, researchers improve the thermal conductivity of compound system often through addition high thermal conductivity filler.But these are multiple
Zoarium system generally requires to add many filler quantity, will lead to the mechanical performance of deterioration compound system in this way.It is filled out as it can be seen that reducing
The quantity of material and the thermal conductivity for improving compound system are still a challenge.
In recent years, improving thermal conductivity by addition high heat conducting nano filler is an important research direction, such as is added
Add graphene or hydroxylating boron nitride nanosheet.Because limit the scattering of phonon or electronics and obtain superelevation phonon or
Person's velocity of electrons, these nanofillers have the thermal conductivity of superelevation.Such as in the face of graphene thermal conductivity reach 2000~
4000w.m-1k-1, thermal conductivity reaches 2000w.m in the face of boron nitride nanosheet-1k-1, and boron nitride nanosheet present it is excellent
Electrical insulating property and low-k, these performances can make material be applied to complicated and high-energy microelectronics and integrated circuit neck
Domain.Therefore, boron nitride nanosheet obtains the concern in academic and industry.
Cellulose is a kind of bioabsorbable polymer material not had a rest with it, and especially nano-cellulose has excellent mechanical performance
(such as high-intensitive and high-stiffness), biological degradability, the transparency, lightweight and it is easy to functionalization, therefore in research field by very
More concerns.Nano-cellulose can disperse boron nitride nanosheet by electrostatic repulsion and steric hindrance and form uniform complex
System.Document one (Zhu, H.；Li,Y.；Fang,Z.；Xu,J.；Cao,F.；Wan,J.；Preston,C.；Yang,B.；Hu,L.,
Highly Thermally Conductive Papers with Percolative Layered Boron Nitride
Nanosheets.Acs Nano 2014,8 (4), 3606-3613.) it reports and is answered based on nano-cellulose and boron nitride nanosheet
Film is closed, and obtains the thermal conductivity of superelevation, but in order to prepare nano-cellulose dispersion liquid, document is made using isopropanol (IPA)
Removing boron nitride powder is removed for dispersing agent, will lead to the environmental issue of solvent in this way.Document two (Wu, K.；Fang,J.；Ma,J.；
Huang,R.；Chai,S.；Chen,F.；Fu,Q.,Achieving a Collapsible,Strong,and Highly
Thermally Conductive Film Based on Oriented Functionalized Boron Nitride
Nanosheets and Cellulose Nanofiber.Acs Applied Materials&Interfaces 2017,9
(35), 30035-30045.) it reports using nitrogen, nitrogen dimethylformamide (DMF) as dispersing agent and removes boron nitride powder, it is formed
Then boron nitride nanosheet dispersion liquid adds urea in boron nitride nanosheet dispersion liquid and carries out ball-milling treatment, obtains and have ammonia
The boron nitride nanosheet dispersion liquid of base group, finally compound with nano-cellulose, being formed has high flexibility and high-intensitive nitridation
Boron nanometer sheet and nano-cellulose heat conduction composite membrane；But this process requirement solvent, and technique is relatively complicated.Therefore, it needs
A kind of simple and environmentally friendly green method is wanted to obtain boron nitride nanosheet dispersion liquid and, preparation compound with nano-cellulose dispersion liquid
High thermal conductivity flexible membrane.
Summary of the invention
It is an object of the invention to overcome disadvantage existing in the prior art, provide a kind of environmental-friendly, simple process
The preparation method of high thermal conductivity flexible membrane.
Another object of the present invention is to provide a kind of applications of above-mentioned high thermal conductivity flexible membrane.
The purpose of the invention is achieved by the following technical solution:
A kind of preparation method of high thermal conductivity flexible membrane, includes the following steps:
(1) boron nitride powder and deionized water are mixed, so that the concentration of boron nitride is 1~10mg/ml, then ultrasound 8
~48 hours, obtain uniform dispersion；Dispersion liquid is put into a centrifuge again, under the conditions of 1000~10000rpm, centrifugation 10
~30min, then supernatant is poured out rapidly, obtain the hydroxylating boron nitride nanosheet water dispersion that concentration is 0.05~0.1mg/ml
Liquid；
(2) nano-cellulose is diluted to 0.1~0.5wt% with deionized water, forms nano-cellulose aqueous dispersions；So
Hydroxylating boron nitride nanosheet aqueous dispersions are mixed with nano-cellulose aqueous dispersions afterwards, 30~60min of stirring, ultrasound 30~
60min obtains finely dispersed hydroxylating boron nitride nanosheet/nano-cellulose aqueous dispersions；Moisture removal is filtered again, in room
It is dried under temperature, obtains hydroxylating boron nitride nanosheet/nano cellulose composite film i.e. high thermal conductivity flexible membrane.
In hydroxylating boron nitride nanosheet/nano cellulose composite film, the mass ratio of hydroxylating boron nitride nanosheet is
12.5~75wt%, the mass ratio of nano-cellulose are 25~87.5wt%.
In step 1, the size of hydroxylating boron nitride nanosheet is 100nm, with a thickness of 2nm.
The application of the high thermal conductivity flexible membrane is the heat sink material as electronic/electrical gas product.
The principle of the present invention is: removing boron nitride powder using water, obtains hydroxylating boron nitride nanosheet aqueous dispersions.Hydroxyl
Base boron nitride nanosheet is prepared for a kind of high heat conductance, excellent mechanical as high thermal conductivity fillers and nano-cellulose are compound
It can be with the flexible membrane of thermal stability.In hydroxylating boron nitride nanosheet/nano cellulose composite film, hydroxylating boron nitride nanometer
Piece and nano-cellulose layer and layer are packed together composition and are similar to natural clam shell feature, and nano-cellulose is filled out similar to clay
It fills between hydroxylating boron nitride nanosheet.Direction thermal conductivity in hydroxylating boron nitride nanosheet/nano cellulose composite film face
Rate reaches 22.67w.m-1k-1, tensile strength reaches 45.8MPa and most degradation temperature reaches 296 DEG C.
The present invention has the following advantages that compared with prior art and effect:
(1) present invention does not use any solvent, and boron nitride powder is directly removed by water by ultrasonic device, obtains hydroxylating
Boron nitride nanosheet aqueous dispersions.This method is not only simple, but also environmental-friendly, while making hydroxylating boron nitride nanometer on piece
With hydroxyl group.
(2) high thermal conductivity flexible membrane prepared by the present invention has high heat conductance, very good mechanical properties and thermal stability, such as
When concentration is 25wt%, direction thermal conductivity reaches 22.67w.m in the face of the film-1k-1, vertical direction thermal conductivity reaches
1.08w.m-1k-1, tensile strength reaches 45.8MPa, and elongation at break reaches 15.7%, and most degradation temperature reaches 298 DEG C.
Detailed description of the invention
Fig. 1 is that the SEM of high thermal conductivity flexible membrane schemes.
Fig. 2 is that the size TEM of hydroxylating boron nitride nanosheet schemes.
Fig. 3 is that the thickness TEM of hydroxylating boron nitride nanosheet schemes.
Specific embodiment
Further detailed description is done to the present invention below with reference to embodiment, embodiments of the present invention are not limited thereto.
Embodiment 1
(1) preparation of hydroxylating boron nitride nanosheet aqueous dispersions
1.6g boron nitride powder and 800ml deionized water are added in 1000ml beaker, in magnetic stirring apparatus uniformly
30min is stirred, ultrasound 8 hours in ultrasonic instrument is then placed over, obtains uniform dispersion.Dispersion liquid is put into a centrifuge,
Under the conditions of 5000rpm, be centrifuged 10min, after pour out supernatant rapidly, obtain the hydroxylating boron nitride nanometer of 0.1mg/ml
Piece aqueous dispersions.
(2) preparation of high thermal conductivity flexible membrane
1g nano-cellulose is diluted to 0.1wt%, forms nano-cellulose aqueous dispersions.By 50ml hydroxylating boron nitride
Nanometer sheet aqueous dispersions and 35g nano-cellulose aqueous dispersions are placed in beaker, and by stirring 30min, ultrasonic 30min is total
It is mixed, uniform hydroxylating boron nitride nanosheet/nano-cellulose aqueous dispersions are obtained, moisture removal are gone by the method for suction filtration, so
It dries at room temperature afterwards, finally obtains 12.5wt% (mass ratio of hydroxylating boron nitride nanosheet) hydroxylating boron nitride nanometer
Piece/nano cellulose composite film.Hydroxylating boron nitride nanosheet/nano cellulose composite film performance characterization is as follows: in face side
It is 14.95w.m to thermal conductivity-1k-1, vertical direction thermal conductivity is 0.34w.m-1k-1, tensile strength 47.7MPa, extension at break
Rate is 28.3%, and most degradation temperature is 297 DEG C.
Embodiment 2:
(1) preparation of hydroxylating boron nitride nanosheet aqueous dispersions
1g boron nitride powder and 500ml deionized water are added in 1000ml beaker, uniformly stirred in magnetic stirring apparatus
30min is mixed, ultrasound 8 hours in ultrasonic instrument is then placed over, obtains uniform dispersion.Dispersion liquid is put into a centrifuge,
Under the conditions of 5000rpm, be centrifuged 10min, after pour out supernatant rapidly, obtain the hydroxylating boron nitride nanosheet of 0.1mg/ml
Aqueous dispersions.
(2) preparation of high thermal conductivity flexible membrane
1g nano-cellulose is diluted to 0.1wt%, forms nano-cellulose aqueous dispersions.100ml hydroxylating is nitrogenized
Boron nanometer sheet aqueous dispersions are blended with 30g nano-cellulose aqueous dispersions, stir 30min, and ultrasonic 30min obtains uniform hydroxyl
Base boron nitride nanosheet/nano-cellulose aqueous dispersions removes moisture removal by the method for suction filtration, then dries at room temperature,
Finally obtain 25wt% hydroxylating boron nitride nanosheet/nano cellulose composite film.Hydroxylating boron nitride nanosheet and Nanowire
The performance characterization for tieing up plain composite membrane is as follows: direction thermal conductivity is 22.67w.m in face-1k-1, vertical direction thermal conductivity is 1.08w.m-1k-1, tensile strength 45.8MPa, elongation at break 15.7%, most degradation temperature is 298 DEG C.
Embodiment 3:
(1) preparation of hydroxylating boron nitride nanosheet aqueous dispersions
1.2g boron nitride powder and 600ml deionized water are added in 1000ml beaker, in magnetic stirring apparatus uniformly
30min is stirred, ultrasound 8 hours in ultrasonic instrument is then placed over, obtains uniform dispersion.Dispersion liquid is put into a centrifuge,
Under the conditions of 5000rpm, be centrifuged 10min, after pour out supernatant rapidly, obtain the hydroxylating boron nitride nanometer of 0.1mg/ml
Piece aqueous dispersions.
(2) preparation of high thermal conductivity flexible membrane
1g nano-cellulose is diluted to 0.1wt%, forms nano-cellulose aqueous dispersions.200ml hydroxylating is nitrogenized
Boron nanometer sheet aqueous dispersions are blended with 20g nano-cellulose aqueous dispersions, stir 30min, and ultrasonic 30min obtains uniform hydroxyl
Base boron nitride nanosheet/nano-cellulose aqueous dispersions removes moisture removal by the method for suction filtration, then dries at room temperature,
Finally obtain 50wt% hydroxylating boron nitride nanosheet/nano cellulose composite film.Hydroxylating boron nitride nanosheet/nanofiber
The performance characterization of plain composite membrane is as follows: direction thermal conductivity is 17.89w.m in face-1k-1, vertical direction thermal conductivity is 0.98w.m- 1k-1, tensile strength 25.9MPa, elongation at break 5.5%, most degradation temperature is 301 DEG C.
Embodiment 4:
(1) preparation of hydroxylating boron nitride nanosheet aqueous dispersions
1.6g boron nitride powder and 800ml deionized water are added in 1000ml beaker, in magnetic stirring apparatus uniformly
30min is stirred, ultrasound 8 hours in ultrasonic instrument is then placed over, obtains uniform dispersion.Dispersion liquid is put into a centrifuge,
Under the conditions of 5000rpm, be centrifuged 10min, after pour out supernatant rapidly, obtain the hydroxylating boron nitride nanometer of 0.1mg/ml
Piece aqueous dispersions.
(2) preparation of high thermal conductivity flexible membrane
1g nano-cellulose is diluted to 0.1wt%, forms nano-cellulose aqueous dispersions.300ml hydroxylating is nitrogenized
Boron nanometer sheet aqueous dispersions are blended with 10g nano-cellulose aqueous dispersions, stir 30min, and ultrasonic 30min obtains uniform hydroxyl
Base boron nitride nanosheet/nano-cellulose aqueous dispersions removes moisture removal by the method for suction filtration, then dries at room temperature,
Finally obtain 75wt% hydroxylating boron nitride nanosheet/nano cellulose composite film.Hydroxylating boron nitride nanosheet/nanofiber
The performance characterization of plain composite membrane is as follows: direction thermal conductivity is 15.46w.m in face-1k-1, vertical direction thermal conductivity is 0.45w.m- 1k-1, tensile strength 14.1MPa, elongation at break 2.5%, most degradation temperature is 316 DEG C.
Test case
Using 25wt% hydroxylating boron nitride nanosheet/nano cellulose composite film that embodiment 2 is prepared as sample
It is tested.As shown in Figure 1, seeing hydroxyl from SEM picture in hydroxylating boron nitride nanosheet/nano cellulose composite film
Base boron nitride nanosheet is closely packed together between layers with nano-cellulose, is similar to nature clam shell feature,
Middle nano-cellulose is filled between hydroxylating boron nitride nanosheet as clay.This tight structure is conducive to improve film
Heat-conducting effect.
Tem observation is carried out to hydroxylating boron nitride nanosheet, as shown in Figure 2 and Figure 3, is clear that hydroxylating nitrogenizes
The size of boron nanometer sheet is 100nm, with a thickness of 2nm.
Thermogravimetric analysis is carried out to hydroxylating boron nitride nanosheet/nano cellulose composite film, studies its thermostable effect.It grinds
Study carefully discovery, with the continuous improvement of hydroxylating boron nitride nanosheet content, maximum thermal degradation temperature is also being continuously improved, it is seen that hydroxyl
Base boron nitride nanosheet can be improved the thermal stability of compound system.
In order to more intuitively observe, respectively to pure nano-cellulose film and hydroxylating boron nitride nanosheet/nano-cellulose
Composite membrane carries out combustion test comparison.Pure nano-cellulose film, hydroxylating boron nitride nanosheet/nano cellulose composite film are existed
After burning 10 seconds in flame, pure nano-cellulose film, which is all burnt, not to be had, but hydroxylating boron nitride nanosheet/nano-cellulose
Composite membrane can also retain most shape, it is seen that hydroxylating boron nitride nanosheet/nano cellulose composite film thermal stability
Preferably.
Hydroxylating boron nitride nanosheet/nano cellulose composite film heat dissipation effect is tested, by hydroxylating boron nitride nanometer
Piece/nano cellulose composite film, pure nano-cellulose film and printing paper (80g/cm2) are placed on together on hot table, by heat at
As instrument carries out heat dissipation effect displaying.Experiment discovery, when heating 10 seconds, 20% pure nano-cellulose surface has been transformed into pale yellow
Color, printing paper is almost without surface conversion at light yellow, but hydroxylating boron nitride nanosheet/nano cellulose composite film is
There is 60% surface conversion at light yellow.It is excellent that this absolutely proves that hydroxylating boron nitride nanosheet/nano cellulose composite film has
Heat dissipation performance.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (4)
1. a kind of preparation method of high thermal conductivity flexible membrane, it is characterised in that include the following steps:
(1) boron nitride powder and deionized water are mixed, so that the concentration of boron nitride is 1~10mg/ml, then ultrasound 8~48
Hour, obtain uniform dispersion；Dispersion liquid is put into a centrifuge again, under the conditions of 1000~10000rpm, centrifugation 10~
30min, then supernatant is poured out rapidly, obtain the hydroxylating boron nitride nanosheet aqueous dispersions that concentration is 0.05~0.1mg/ml；
(2) nano-cellulose is diluted to 0.1~0.5wt% with deionized water, forms nano-cellulose aqueous dispersions；Then will
Hydroxylating boron nitride nanosheet aqueous dispersions are mixed with nano-cellulose aqueous dispersions, 30~60min of stirring, and ultrasound 30~
60min obtains finely dispersed hydroxylating boron nitride nanosheet/nano-cellulose aqueous dispersions；Moisture removal is filtered again, in room
It is dried under temperature, obtains hydroxylating boron nitride nanosheet/nano cellulose composite film i.e. high thermal conductivity flexible membrane.
2. the preparation method of high thermal conductivity flexible membrane according to claim 1, it is characterised in that: hydroxylating boron nitride nanometer
In piece/nano cellulose composite film, the mass ratio of hydroxylating boron nitride nanosheet is 12.5~75wt%, nano-cellulose
Mass ratio is 25~87.5wt%.
3. the preparation method of high thermal conductivity flexible membrane according to claim 1, it is characterised in that: in step 1, hydroxylating nitridation
The size of boron nanometer sheet is 100nm, with a thickness of 2nm.
4. a kind of application of high thermal conductivity flexible membrane, it is characterised in that: the heat sink material as electronic/electrical gas product.
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| CN112048088A (en) * | 2020-08-28 | 2020-12-08 | 华南理工大学 | Heat-conducting, insulating and flame-retardant flexible composite film and preparation method and application thereof |
| CN112874043A (en) * | 2021-01-19 | 2021-06-01 | 上海大学 | High-thermal-conductivity high-polymer material composite membrane with thermal response performance and preparation method thereof |
| CN113002082A (en) * | 2021-02-07 | 2021-06-22 | 中国科学院合肥物质科学研究院 | Biomass-based high-thermal-conductivity flexible composite membrane and preparation method thereof |
| WO2021139038A1 (en) * | 2020-01-06 | 2021-07-15 | 武汉华星光电半导体显示技术有限公司 | Organic light-emitting diode device structure and fabrication method therefor |
| CN114763627A (en) * | 2021-01-14 | 2022-07-19 | 上海大学 | Electrostatic spinning cellulose nanofiber and preparation method thereof |
| CN115233493A (en) * | 2022-07-25 | 2022-10-25 | 北京林业大学 | Water vapor barrier coating and preparation method thereof, water vapor barrier coated paper and preparation method thereof |
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Cited By (9)
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| WO2021139038A1 (en) * | 2020-01-06 | 2021-07-15 | 武汉华星光电半导体显示技术有限公司 | Organic light-emitting diode device structure and fabrication method therefor |
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| CN114763627A (en) * | 2021-01-14 | 2022-07-19 | 上海大学 | Electrostatic spinning cellulose nanofiber and preparation method thereof |
| CN112874043A (en) * | 2021-01-19 | 2021-06-01 | 上海大学 | High-thermal-conductivity high-polymer material composite membrane with thermal response performance and preparation method thereof |
| CN113002082A (en) * | 2021-02-07 | 2021-06-22 | 中国科学院合肥物质科学研究院 | Biomass-based high-thermal-conductivity flexible composite membrane and preparation method thereof |
| CN115233493A (en) * | 2022-07-25 | 2022-10-25 | 北京林业大学 | Water vapor barrier coating and preparation method thereof, water vapor barrier coated paper and preparation method thereof |
| CN115233493B (en) * | 2022-07-25 | 2023-09-15 | 北京林业大学 | Water vapor barrier coating and preparation method thereof, water vapor barrier coated paper and preparation method thereof |
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Application publication date: 20190416 |
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| RJ01 | Rejection of invention patent application after publication |