CN118619700A - Composite film and preparation method thereof - Google Patents
Composite film and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 49
- 239000004917 carbon fiber Substances 0.000 claims abstract description 49
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 49
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 38
- 238000000151 deposition Methods 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 239000000428 dust Substances 0.000 claims abstract description 14
- 238000003490 calendering Methods 0.000 claims abstract description 12
- 238000003763 carbonization Methods 0.000 claims abstract description 12
- 238000005087 graphitization Methods 0.000 claims abstract description 11
- 239000002002 slurry Substances 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 238000005507 spraying Methods 0.000 claims abstract description 5
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 4
- 238000005520 cutting process Methods 0.000 claims abstract description 4
- 238000000280 densification Methods 0.000 claims abstract description 4
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 4
- 239000010439 graphite Substances 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 238000007873 sieving Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 13
- 230000008021 deposition Effects 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 6
- 239000003595 mist Substances 0.000 claims description 5
- 239000000758 substrate Substances 0.000 claims description 2
- 238000005096 rolling process Methods 0.000 claims 2
- 239000004743 Polypropylene Substances 0.000 claims 1
- 238000010000 carbonizing Methods 0.000 claims 1
- 239000000835 fiber Substances 0.000 claims 1
- -1 polypropylene Polymers 0.000 claims 1
- 229920001155 polypropylene Polymers 0.000 claims 1
- 239000012462 polypropylene substrate Substances 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract 1
- 230000017525 heat dissipation Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 1
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B19/00—Machines or methods for applying the material to surfaces to form a permanent layer thereon
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/522—Graphite
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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Abstract
本申请涉及一种复合膜及制备方法，包括如下步骤，将碳毡/石墨毡切割、研磨、过筛，震动分散于密闭空间，获得连续均匀掉落的碳纤维粉尘；将氧化石墨烯浆料均匀喷洒于密闭空间与碳纤维粉尘物理以一定比例混合，获得固液均匀混合的混合液；混合液沉积于丙纶基材上，获得氧化石墨烯/碳纤维复合膜；将复合膜经过烘干机，获得氧化石墨烯/碳纤维复合干膜；将氧化石墨烯/碳纤维复合干膜在无氧环境下进行碳化热处理，获得碳化膜；将碳化膜在无氧环境下进行石墨化热处理，获得石墨化膜；将石墨化膜进行压延增密处理，获得高导热超薄石墨烯/碳纤维复合膜。本申请具有碳纤维粉在氧化石墨烯浆料中均匀的较好的优点。The present application relates to a composite film and a preparation method, comprising the following steps: cutting, grinding, sieving, and vibrating carbon felt/graphite felt in a confined space to obtain continuous and uniformly falling carbon fiber dust; spraying graphene oxide slurry in a confined space to physically mix with carbon fiber dust in a certain proportion to obtain a solid-liquid mixed solution; depositing the mixed solution on a polypropylene substrate to obtain a graphene oxide/carbon fiber composite film; passing the composite film through a dryer to obtain a graphene oxide/carbon fiber composite dry film; subjecting the graphene oxide/carbon fiber composite dry film to carbonization heat treatment in an oxygen-free environment to obtain a carbonized film; subjecting the carbonized film to graphitization heat treatment in an oxygen-free environment to obtain a graphitized film; subjecting the graphitized film to a calendering and densification treatment to obtain a high thermal conductivity ultra-thin graphene/carbon fiber composite film. The present application has the advantage that carbon fiber powder is uniformly distributed in the graphene oxide slurry.
Description
技术领域Technical Field
本申请涉及复合膜制备的技术领域，尤其是涉及一种复合膜及制备方法。The present application relates to the technical field of composite membrane preparation, and in particular to a composite membrane and a preparation method thereof.
背景技术Background Art
为了起到较好的散热效果，部分需要散热的设备采用石墨烯/碳纤维复合膜的方式进行散热，但是现有的石墨烯/碳纤维复合膜的制备过程中，存在碳纤维粉在氧化石墨烯浆料中均匀度较差的问题。In order to achieve better heat dissipation effect, some equipment that needs heat dissipation adopts graphene/carbon fiber composite film for heat dissipation. However, in the preparation process of existing graphene/carbon fiber composite film, there is a problem of poor uniformity of carbon fiber powder in graphene oxide slurry.
发明内容Summary of the invention
针对现有技术存在的不足，本申请的目的之一是提供一种复合膜及制备方法，其具有碳纤维粉在氧化石墨烯浆料中均匀的较好的优点。In view of the shortcomings of the prior art, one of the purposes of the present application is to provide a composite membrane and a preparation method thereof, which has the advantage of better uniformity of carbon fiber powder in graphene oxide slurry.
本申请的上述目的是通过以下技术方案得以实现的：The above-mentioned purpose of the present application is achieved through the following technical solutions:
一种复合膜制备方法，包括如下步骤，碳纤维制备：将碳毡/石墨毡切割、研磨、过筛，震动分散于密闭空间，获得连续均匀掉落的碳纤维粉尘；混合：将氧化石墨烯浆料均匀喷洒于密闭空间与碳纤维粉尘物理以一定比例混合，获得固液均匀混合的混合液；沉积：混合液沉积于丙纶基材上，获得氧化石墨烯/碳纤维复合膜；烘干：将复合膜经过烘干机，获得氧化石墨烯/碳纤维复合干膜；碳化：将氧化石墨烯/碳纤维复合干膜在无氧环境下进行碳化热处理，获得碳化膜；石墨化：将碳化膜在无氧环境下进行石墨化热处理，获得石墨化膜；压延：将石墨化膜进行压延增密处理，获得高导热超薄石墨烯/碳纤维复合膜。A composite film preparation method comprises the following steps: carbon fiber preparation: cutting, grinding, sieving, and vibrating and dispersing carbon felt/graphite felt in a closed space to obtain continuously and evenly falling carbon fiber dust; mixing: spraying graphene oxide slurry evenly in a closed space and physically mixing it with carbon fiber dust in a certain proportion to obtain a mixed solution in which solid and liquid are evenly mixed; depositing: depositing the mixed solution on a polypropylene substrate to obtain a graphene oxide/carbon fiber composite film; drying: passing the composite film through a drying machine to obtain a graphene oxide/carbon fiber composite dry film; carbonization: subjecting the graphene oxide/carbon fiber composite dry film to carbonization heat treatment in an oxygen-free environment to obtain a carbonized film; graphitization: subjecting the carbonized film to graphitization heat treatment in an oxygen-free environment to obtain a graphitized film; and calendering: subjecting the graphitized film to a calendering and densification treatment to obtain a high thermal conductivity ultrathin graphene/carbon fiber composite film.
通过采用上述技术方案，将氧化石墨烯连续均匀喷洒于密闭空间中，同时将碳纤维粉通过多孔筛连续震动均匀分散于密闭空间，掉落过程中碳纤维粉尘与呈雾状的氧化石墨烯混合均匀后沉积在基材上，烘干-碳化-石墨化-压延后最终获得碳纤维粉和石墨烯均匀混合的高导热超薄石墨烯/碳纤维复合膜。通过喷洒氧化石墨烯并通过使碳纤维粉均匀分散于密闭空间，掉落过程中碳纤维粉尘与呈雾状的氧化石墨烯混合，从而使得碳纤维粉在氧化石墨烯浆料均匀度较好。By adopting the above technical scheme, graphene oxide is continuously and evenly sprayed in a confined space, and carbon fiber powder is continuously vibrated and evenly dispersed in a confined space through a porous sieve, and carbon fiber dust is evenly mixed with graphene oxide in a mist form during the falling process and then deposited on a substrate, and finally a high thermal conductivity ultra-thin graphene/carbon fiber composite film in which carbon fiber powder and graphene are evenly mixed is obtained after drying-carbonization-graphitization-calendering. By spraying graphene oxide and evenly dispersing carbon fiber powder in a confined space, carbon fiber dust is mixed with graphene oxide in a mist form during the falling process, so that the carbon fiber powder has a better uniformity in the graphene oxide slurry.
本申请在一较佳示例中可以进一步配置为：在碳纤维制备步骤中，碳纤维粉直径为1-100μm，长度为1-1000μm；震动筛目数为10-1000目。In a preferred example, the present application can be further configured as follows: in the carbon fiber preparation step, the diameter of the carbon fiber powder is 1-100 μm, and the length is 1-1000 μm; the mesh number of the vibration sieve is 10-1000 mesh.
本申请在一较佳示例中可以进一步配置为：在混合步骤中，氧化石墨烯固含为0.5％-5％；氧化石墨烯雾状液滴和碳纤维粉尘的流量比为2-8:1-5。In a preferred example, the present application can be further configured as follows: in the mixing step, the solid content of graphene oxide is 0.5%-5%; the flow ratio of graphene oxide mist droplets and carbon fiber dust is 2-8:1-5.
本申请在一较佳示例中可以进一步配置为：在沉积步骤中，沉积温度为常温，沉积速度为1-1000μm/min。In a preferred example, the present application can be further configured as follows: in the deposition step, the deposition temperature is room temperature, and the deposition speed is 1-1000 μm/min.
本申请在一较佳示例中可以进一步配置为：在烘干步骤中，热处理的处理温度50-100摄氏度、处理时间10-1000min。In a preferred example, the present application can be further configured as follows: in the drying step, the heat treatment temperature is 50-100 degrees Celsius and the treatment time is 10-1000 minutes.
本申请在一较佳示例中可以进一步配置为：在碳化步骤中，无氧环境下的碳化热处理的处理温度为1000-1600摄氏度、处理时间为10-200min。In a preferred example, the present application can be further configured as follows: in the carbonization step, the treatment temperature of the carbonization heat treatment in an oxygen-free environment is 1000-1600 degrees Celsius and the treatment time is 10-200 minutes.
本申请在一较佳示例中可以进一步配置为：在石墨化步骤中，石墨化热处理的处理温度为2600-3100摄氏度、处理时间10-600min。In a preferred example, the present application can be further configured as follows: in the graphitization step, the treatment temperature of the graphitization heat treatment is 2600-3100 degrees Celsius and the treatment time is 10-600 minutes.
本申请在一较佳示例中可以进一步配置为：在压延步骤中，压延压力为5-35MPa。In a preferred example, the present application can be further configured as follows: in the calendering step, the calendering pressure is 5-35 MPa.
本申请还公开了一种复合膜，通过上述的复合膜制备方法制备而成。The present application also discloses a composite membrane, which is prepared by the composite membrane preparation method mentioned above.
具体实施方式DETAILED DESCRIPTION
本申请公开了一种复合膜制备方法，包括如下步骤，碳纤维制备：将碳毡/石墨毡切割、研磨、过筛，震动分散于密闭空间，获得连续均匀掉落的碳纤维粉尘；混合：将氧化石墨烯浆料均匀喷洒于密闭空间与碳纤维粉尘物理以一定比例混合，获得固液均匀混合的混合液；沉积：混合液沉积于丙纶基材上，获得氧化石墨烯/碳纤维复合膜；烘干：将复合膜经过烘干机，获得氧化石墨烯/碳纤维复合干膜；碳化：将氧化石墨烯/碳纤维复合干膜在无氧环境下进行碳化热处理，获得碳化膜；石墨化：将碳化膜在无氧环境下进行石墨化热处理，获得石墨化膜；压延：将石墨化膜进行压延增密处理，获得高导热超薄石墨烯/碳纤维复合膜。The present application discloses a composite film preparation method, comprising the following steps: carbon fiber preparation: cutting, grinding, sieving, and vibrating and dispersing carbon felt/graphite felt in a closed space to obtain continuously and evenly falling carbon fiber dust; mixing: spraying graphene oxide slurry evenly in a closed space and physically mixing it with carbon fiber dust in a certain proportion to obtain a mixed solution in which solid and liquid are evenly mixed; depositing: depositing the mixed solution on a polypropylene substrate to obtain a graphene oxide/carbon fiber composite film; drying: passing the composite film through a drying machine to obtain a graphene oxide/carbon fiber composite dry film; carbonization: subjecting the graphene oxide/carbon fiber composite dry film to a carbonization heat treatment in an oxygen-free environment to obtain a carbonized film; graphitization: subjecting the carbonized film to a graphitization heat treatment in an oxygen-free environment to obtain a graphitized film; and calendering: subjecting the graphitized film to a calendering and densification treatment to obtain a high thermal conductivity ultra-thin graphene/carbon fiber composite film.
在碳纤维制备步骤中，碳纤维粉直径为1-100μm，长度为1-1000μm；震动筛目数为10-1000目。In the carbon fiber preparation step, the diameter of the carbon fiber powder is 1-100 μm, the length is 1-1000 μm, and the mesh number of the vibration sieve is 10-1000 meshes.
在混合步骤中，氧化石墨烯固含为0.5％-5％；氧化石墨烯雾状液滴和碳纤维粉尘的流量比为2-8:1-5。In the mixing step, the solid content of graphene oxide is 0.5%-5%; the flow ratio of graphene oxide mist droplets and carbon fiber dust is 2-8:1-5.
在沉积步骤中，沉积温度为常温，沉积速度为1-1000μm/min。In the deposition step, the deposition temperature is room temperature, and the deposition speed is 1-1000 μm/min.
在烘干步骤中，热处理的处理温度50-100摄氏度、处理时间10-1000min。In the drying step, the heat treatment temperature is 50-100 degrees Celsius and the treatment time is 10-1000 minutes.
在碳化步骤中，无氧环境下的碳化热处理的处理温度为1000-1600摄氏度、处理时间为10-200min。In the carbonization step, the carbonization heat treatment in an oxygen-free environment has a treatment temperature of 1000-1600 degrees Celsius and a treatment time of 10-200 minutes.
在石墨化步骤中，石墨化热处理的处理温度为2600-3100摄氏度、处理时间10-600min。In the graphitization step, the graphitization heat treatment has a treatment temperature of 2600-3100 degrees Celsius and a treatment time of 10-600 minutes.
在压延步骤中，压延压力为5-35MPa。下表为各实施例的配比和对应的传热系数In the calendering step, the calendering pressure is 5-35 MPa. The following table shows the ratios and corresponding heat transfer coefficients of various embodiments.
由上述表内数据可知，本方法制备的复合膜的均匀度更好，因此具备更加优异的导热效果。It can be seen from the data in the above table that the composite film prepared by this method has better uniformity and therefore has a more excellent thermal conductivity effect.
本实施例的实施原理为：将氧化石墨烯浆料均匀喷洒于密闭空间与碳纤维粉尘物理以一定比例混合，使得碳纤维和氧化石墨烯浆料混合的更为均匀。The implementation principle of this embodiment is: the graphene oxide slurry is evenly sprayed in a closed space and physically mixed with the carbon fiber dust in a certain proportion, so that the carbon fiber and the graphene oxide slurry are mixed more evenly.
本具体实施方式的实施例均为本申请的较佳实施例，并非依此限制本申请的保护范围，故：凡依本申请的结构、形状、原理所做的等效变化，均应涵盖于本申请的保护范围之内。The embodiments of this specific implementation method are all preferred embodiments of the present application, and are not intended to limit the protection scope of the present application. Therefore, all equivalent changes made based on the structure, shape, and principle of the present application should be included in the protection scope of the present application.
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