CN105860143A - Flexible nanocellulose-graphene composite membrane and preparation method thereof - Google Patents
Flexible nanocellulose-graphene composite membrane and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a flexible nanocellulose-graphene composite membrane and a preparation method thereof. The composite membrane comprises the following components in percentage by weight: 0.1-90% of grapheme and 10-99.9% of nanocellulose. The preparation method comprises the following steps: (1) an oxidized grapheme dispersion liquid with concentration of 0.05-5 mg/ml and a nanocellulose dispersion liquid with concentration of 0.05-5 mg/ml are prepared, and after 1-2 h of ultrasonic dispersion and mixing, first dispersion liquid of nanocellulose-oxidized grapheme with concentration of 0.05-5 mg/ml is obtained; (2) a reducing agent is added into the first dispersion liquid, and second dispersion liquid of nanocellulose-graphene is obtained after heating and even stirring; (3) the composite membrane is obtained after centrifugal degassing and vacuum filtering of the second dispersion liquid, the composite membrane is transferred into a drying oven, and the flexible nanocellulose-graphene composite membrane is obtained after vacuum drying. No agglomeration occurs between grapheme slice layers in the composite membrane; the flexible nanocellulose-graphene composite membrane is characterized in that the parallel heat conductivity coefficient is equal to or larger than 2 W.m<-1>.K<-1>, the vertical heat conductivity coefficient is equal to or smaller than 0.3 W.m<-1>.K<-1>, and the anisotropy ratio of heat conductivity coefficient is equal to or larger than 5.
Description
Technical field
The present invention relates to a kind of heat conduction composite membrane, particularly relate to a kind of flexible nano cellulose-graphene composite film and preparation method thereof, belong to heat-conductive composite material field.
Background technology
Graphene, as a kind of novel Two-dimensional Carbon nano material, has high heat conductivity, high specific surface area and Young's modulus.The single-layer graphene heat conductivity when room temperature is up to 5300 W m-1•K-1, it is the material that the heat conductivity being currently known is the highest, is a kind of ideal heat filling.
The two-dimension plane structure of Graphene determines regularly arranged along plane of wherein carbon, this regularly arranged can give composite anisotropic performance., such as polyamide-graphene composite material, silicone rubber-graphene composite material etc., there is difficult forming, filler orientation is not enough, anisotropic heat conductivity is poor, the shortcoming of matrix-filler poor compatibility in anisotropic thermal material prepared by traditional polymeric matrix.Although, pure Graphene heat conducting film or graphite guide hotting mask solution can avoid the problems referred to above, but owing to this material lacks substrate support, not only poor mechanical property, too increase cost.Cellulosic material has the features such as wide material sources, low cost, light weight, renewable and biodegradation.The nano-cellulose of 1-dimention nano size has many unique features, bigger specific surface area, superpower absorbability etc., and nano-cellulose rich surface oxy radical Han polarity, can the noncovalent interaction such as the oxy radical generation hydrogen bond action remaining with graphenic surface and electrostatic force.
Both at home and abroad for the research of anisotropic thermal material, in existing technology, China Patent Publication No. CN103740110A, publication date 2014.04.23, invention entitled " the flexible Heat Conduction Material of a kind of orientation and moulding process thereof and application ", the flexible Heat Conduction Material of a kind of orientation of this disclosure of the invention, its bulk composition is silicone rubber and anisotropic thermal filler, this Heat Conduction Material has good heat conductivility at specific direction, but owing to Graphene is poor with the compatibility of silicone rubber, Graphene easily forms irreversible reunion in silastic product.China Patent Publication No. CN101407322A, publication date 2009.04.15, invention entitled " a kind of preparation method with anisotropic graphite heat conducting and heat radiating fin ", the method is by the graphite of acid treatment, through washing, after high-temperature expansion, producing apparatus processing molding with soft graphite coiled material, the heat conductivility of its product is significantly improved, but, owing to the mechanical properties such as pure graphite film strength, toughness are poor, limit its popularization and application.
Summary of the invention
It is an object of the invention to provide a kind of flexible nano cellulose-graphene composite film and preparation method thereof, the heat conductivility of composite membrane prepared by the method has obvious anisotropy, and composite membrane has good flexibility simultaneously.
In order to achieve the above object, the technical solution of the present invention is:
A kind of flexible nano cellulose-graphene composite film, this composite membrane is made up of Graphene and nano-cellulose, and the mass fraction of described composite membrane consists of: Graphene 0.1%～90%, nano-cellulose 10%～99.9%, and each component sum is 100%.
The preparation method of a kind of flexible nano cellulose-graphene composite film of the present invention, comprises the following steps:
(1). a certain amount of graphene oxide and a certain amount of nano-cellulose are added separately in dispersant, be configured to graphene oxide dispersion that concentration is 0.05～5mg/ml, concentration be 0.05～5mg/ml nano-cellulose dispersion liquid, ultrasonic disperse 1～2h, then above-mentioned graphene oxide dispersion is mixed with volume ratio 1:1 with above-mentioned nano-cellulose dispersion liquid, continue stirring and ultrasonic 0.5h, obtaining the first dispersion liquid of nano-cellulose-graphene oxide that concentration is 0.05～5mg/ml, described dispersant is deionized water；
(2). nano-cellulose-graphene oxide the first dispersion liquid that will obtain in above-mentioned steps (1) adds reducing agent, is warming up to 80～100 DEG C, stir 0.5～8h, stir, be cooled to room temperature, obtain the second dispersion liquid of nano-cellulose-Graphene；
(3). the second dispersion liquid of nano-cellulose-Graphene above-mentioned steps (2) obtained is centrifuged degassing, gas present in removing dispersion liquid, after degassing, vacuum filtration becomes composite membrane again, composite membrane after vacuum filtration is transferred in the baking oven of 25～60 DEG C, it is dried 2～12h under vacuum, i.e. obtains a kind of flexible nano cellulose-graphene composite film.
Reducing agent described in above-mentioned steps (2) is one or more in hydrazine hydrate, sodium borohydride, ascorbic acid, sodium hydroxide, hydrogen iodide.
Owing to have employed above technical scheme, a kind of flexible nano cellulose-graphene composite film of the present invention and preparation method thereof has the advantage that
(1). the preparation method of a kind of flexible nano cellulose-graphene composite film of the present invention, technique is simple, and preparation process environmentally safe can realize large-scale production.
(2). a kind of flexible nano cellulose-graphene composite film of the present invention, the oxy radical that its nano-cellulose rich surface contains, the noncovalent interaction such as hydrogen bond or electrostatic force can be formed with the oxy radical of graphenic surface residual, nano-cellulose adsorbs on graphene sheet layer, make will not reunite between graphene sheet layer, make Graphene dispersed in nano-cellulose matrix；Graphene is height-oriented in in-plane, and heat conductivility has obvious anisotropy, can reach following heat conductivility parameter: parallel direction heat conductivity >=2W m-1•K-1, vertical direction heat conductivity≤0.3W m-1•K-1, heat conductivity anisotropy ratio >=5.
(3). a kind of flexible nano cellulose-graphene composite film of the present invention has good mechanical property, its hot strength >=100MPa；Having excellent flexibility and bending resistance folding endurance, after composite membrane bends 500 times, heat conductivity excursion is 0～10% simultaneously.
Accompanying drawing explanation
Fig. 1 is the Raman spectrogram of the flexible nano cellulose-graphene composite film of embodiment 1 preparation.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
The preparation method of a kind of flexible nano cellulose-graphene composite film of the present embodiment, comprises the following steps:
(1). the graphene oxide of 0.0075g and the nano-cellulose of 0.1425g are added separately in dispersant, respectively compound concentration be the graphene oxide dispersion of 0.075mg/ml, concentration be the nano-cellulose dispersion liquid of 1.425mg/ml, ultrasonic disperse 1h, then above-mentioned graphene oxide dispersion is mixed with volume ratio 1:1 with above-mentioned nano-cellulose dispersion liquid, continue stirring and ultrasonic 0.5h, obtaining nano-cellulose-graphene oxide the first dispersion liquid that concentration is 0.75mg/ml, described dispersant is deionized water；
(2). adding reducing agent in nano-cellulose-graphene oxide the first dispersion liquid that will obtain in above-mentioned steps (1), be warming up to 90 DEG C, stir 5h, stir, obtain the second dispersion liquid of nano-cellulose-Graphene, described reducing agent is sodium borohydride；
(3). the second dispersion liquid of nano-cellulose-Graphene above-mentioned steps (2) obtained is centrifuged degassing, gas present in removing dispersion liquid, after degassing, vacuum filtration becomes composite membrane again, composite membrane after vacuum filtration is transferred in the baking oven of 40 DEG C, 4h it is dried under vacuum, i.e. obtaining a kind of flexible nano cellulose-graphene composite film, wherein, Graphene radius-thickness ratio is 1000～9000；A diameter of the 5 of nano-cellulose～100nm, draw ratio is 100～1000 nm, as it is shown in figure 1, as seen from the figure, the Graphene contained in the composite membrane that the present embodiment 1 obtains is the Graphene being reduced.
Flexible nano cellulose-the graphene composite film using laser flash method to prepare embodiment 1 makees multinomial detection, and result is as follows: the in-plane heat conductivity of composite membrane is 3.53W m-1•K-1；The vertical direction heat conductivity of composite membrane is 0.06W m-1•K-1；The anisotropic heat conductivity ratio of composite membrane is 59；The hot strength of composite membrane is 107MPa, and has good flexibility；After the bending of composite membrane 500 times, heat conductivity is 3.32W m-1•K-1。
Embodiment 2
The preparation method of the present embodiment a kind of flexible nano cellulose-graphene composite film comprises the following steps:
(1). the graphene oxide of 0.03g and the nano-cellulose of 0.12g are added separately in dispersant, respectively compound concentration be the graphene oxide dispersion of 0.3mg/ml, concentration be the nano-cellulose dispersion liquid for 1.2mg/ml, ultrasonic disperse 1h, then above-mentioned graphene oxide dispersion is mixed with volume ratio 1:1 with above-mentioned nano-cellulose dispersion liquid, continue stirring and ultrasonic 0.5h, obtaining nano-cellulose-graphene oxide the first dispersion liquid that concentration is 0.75mg/ml, described dispersant is deionized water；
(2). nano-cellulose-graphene oxide the first dispersion liquid that will obtain in above-mentioned steps (1) adds reducing agent, it is warming up to 95 DEG C, stirs 2h, stir, obtaining the second dispersion liquid of nano-cellulose-Graphene, described reducing agent is hydrazine hydrate and ascorbic acid；
(3). nano-cellulose-Graphene the second dispersion liquid above-mentioned steps (2) obtained is centrifuged degassing, gas present in removing dispersion liquid, after degassing, vacuum filtration becomes composite membrane again, composite membrane is transferred in baking oven, it is dried 8h under 30 DEG C of condition vacuum, i.e. obtains a kind of flexible nano cellulose-graphene composite film.As shown in the Raman spectrum of accompanying drawing 1, embodiment 2 containing having plenty of the Graphene being reduced in the composite membrane obtained.
Flexible nano cellulose-the graphene composite film using laser flash method to prepare embodiment 2 makees multinomial detection, and result is as follows: the in-plane heat conductivity of composite membrane is 6.54W m-1•K-1；The vertical direction heat conductivity of composite membrane is 0.06W m-1•K-1；The anisotropic heat conductivity ratio of composite membrane is 109, and the hot strength of composite membrane is 117MPa, and has good flexibility；It is 5.94W m that composite membrane bends the heat conductivity after 500 times-1•K-1。
Embodiment 3
The preparation method of a kind of flexible nano cellulose-graphene composite film of the present embodiment, comprises the following steps:
(1). the graphene oxide of 0.06g and the nano-cellulose of 0.14g are added separately in dispersant, respectively compound concentration be the graphene oxide dispersion of 0.6mg/ml, concentration be the nano-cellulose dispersion liquid for 1.4mg/ml, ultrasonic disperse 1h, then above-mentioned graphene oxide dispersion is mixed with volume ratio 1:1 with above-mentioned nano-cellulose dispersion liquid, continue stirring and ultrasonic 0.5h, obtaining nano-cellulose-graphene oxide the first dispersion liquid that concentration is 1mg/ml, described dispersant is deionized water；
(2). nano-cellulose-graphene oxide the first dispersion liquid that will obtain in above-mentioned steps (1) adds reducing agent, it is warming up to 90 DEG C, stirs 6h, stir, obtaining the second dispersion liquid of nano-cellulose-Graphene, described reducing agent is sodium hydroxide；
(3). nano-cellulose-Graphene the second dispersion liquid above-mentioned steps (2) obtained is centrifuged degassing, gas present in removing dispersion liquid, after degassing, vacuum filtration becomes composite membrane again, composite membrane is transferred in baking oven, it is dried 4h under 60 DEG C of condition vacuum, i.e. obtains a kind of flexible nano cellulose-graphene composite film.
Flexible nano cellulose-the graphene composite film using laser flash method to prepare embodiment 3 makees multinomial detection, and result is as follows: the in-plane heat conductivity of composite membrane is 5.10W m-1•K-1；The vertical direction heat conductivity of composite membrane is 0.05W m-1•K-1；The anisotropic heat conductivity ratio of composite membrane is 102；The hot strength of composite membrane is 115MPa, and has good flexibility；It is 4.90W m that composite membrane bends the heat conductivity after 500 times-1•K-1。
Embodiment 4
The preparation method of a kind of flexible nano cellulose-graphene composite film of the present embodiment, comprises the following steps:
(1). the graphene oxide of 0.1g and the nano-cellulose of 0.1g are added separately in dispersant, respectively compound concentration be the graphene oxide dispersion of 2mg/ml, concentration be the nano-cellulose dispersion liquid for 2mg/ml, ultrasonic disperse 2h, then above-mentioned graphene oxide dispersion is mixed with volume ratio 1:1 with above-mentioned nano-cellulose dispersion liquid, continue stirring and ultrasonic 0.5h, obtaining nano-cellulose-graphene oxide the first dispersion liquid that concentration is 2mg/ml, described dispersant is deionized water；
(2). adding reducing agent in nano-cellulose-graphene oxide the first dispersion liquid that will obtain in above-mentioned steps (1), be warming up to 90 DEG C, stir 4h, stir, obtain the second dispersion liquid of nano-cellulose-Graphene, described reducing agent is hydrogen iodide；
(3). nano-cellulose-Graphene the second dispersion liquid above-mentioned steps (2) obtained is centrifuged degassing, gas present in removing dispersion liquid, after degassing, vacuum action was descended sucking filtration to obtain nano-cellulose-Graphene and was become composite membrane again, composite membrane after vacuum filtration is transferred in the baking oven of 60 DEG C, it is dried 4h under vacuum, i.e. obtains a kind of flexible nano cellulose-graphene composite film.
Flexible nano cellulose-the graphene composite film using laser flash method to prepare embodiment 4 makees multinomial detection, and result is as follows: the in-plane heat conductivity of composite membrane is 9.62W m-1•K-1；The vertical direction heat conductivity of composite membrane is 0.08W m-1•K-1；The anisotropic heat conductivity ratio of composite membrane is 120；The hot strength of composite membrane is 126MPa, and has good flexibility；It is 9.36W m that composite membrane bends the heat conductivity after 500 times-1•K-1。
Claims (3)
1. flexible nano cellulose-graphene composite film, it is characterised in that this composite membrane is made up of Graphene and nano-cellulose, and the mass fraction of described composite membrane consists of: Graphene 0.1%～90%, nano-cellulose 10%～99.9%, each component sum is 100%.
2. the preparation method of a kind of flexible nano cellulose-graphene composite film, it is characterised in that the method comprises the following steps:
A certain amount of graphene oxide and a certain amount of nano-cellulose are added separately in dispersant, be configured to graphene oxide dispersion that concentration is 0.05～5mg/ml, concentration is the nano-cellulose dispersion liquid of 0.05-5mg/ml, ultrasonic disperse 1～2h, then above-mentioned graphene oxide dispersion is mixed with volume ratio 1:1 with above-mentioned nano-cellulose dispersion liquid, continue stirring and ultrasonic 0.5h, obtaining the first dispersion liquid of nano-cellulose-graphene oxide that concentration is 0.05～5mg/ml, described dispersant is deionized water；
Nano-cellulose-graphene oxide the first dispersion liquid that will obtain in above-mentioned steps (1) adds reducing agent, is warming up to 80～100 DEG C, stir 0.5～8h, stir, be cooled to room temperature, obtain the second dispersion liquid of nano-cellulose-Graphene；
Second dispersion liquid of nano-cellulose-Graphene above-mentioned steps (2) obtained is centrifuged degassing, gas present in removing dispersion liquid, after degassing, vacuum filtration becomes composite membrane again, composite membrane after vacuum filtration is transferred in the baking oven of 25～60 DEG C, it is dried 2～12h under vacuum, i.e. obtains a kind of flexible nano cellulose-graphene composite film.
The preparation method of a kind of flexible nano cellulose-graphene composite film the most according to claim 2, it is characterized in that, the reducing agent described in above-mentioned steps (2) is one or more in hydrazine hydrate, sodium borohydride, ascorbic acid, sodium hydroxide, hydrogen iodide.
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