CN108995316B - Graphene paper composite material - Google Patents
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- CN108995316B CN108995316B CN201810757762.4A CN201810757762A CN108995316B CN 108995316 B CN108995316 B CN 108995316B CN 201810757762 A CN201810757762 A CN 201810757762A CN 108995316 B CN108995316 B CN 108995316B
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- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
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- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B9/045—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance 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
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- B32B2262/0253—Polyolefin fibres
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- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
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- B32B2307/00—Properties of the layers or laminate
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Abstract
The invention provides a graphene paper composite material, and belongs to the technical field of graphene paper application. The graphene paper composite material provided by the invention comprises a graphene paper layer and a resin layer which are arranged in a stacked mode. The graphene paper composite material provided by the invention has excellent deicing and flame retardant properties, and can be applied to flame retardance, deicing, monitoring of a resin forming process and monitoring of the health condition of resin.
Description
Technical Field
The invention relates to the technical field of graphene paper application, in particular to a graphene paper composite material.
Background
The graphene paper is a two-dimensional material based on graphene, has small density, high strength and hardness, excellent flexibility and foldability, and is also an environment-friendly material. And graphene is sp2Due to the special structure of graphene, the thinnest two-dimensional atomic crystal material formed by the hybridization of carbon atoms in a net shape has various excellent mechanical, thermal and electrical properties and extremely high Young modulus and breaking stress. Has great application prospect in the fields of sensors, composite materials and wearable intelligent equipment.
Resin-based composite materials are fiber-reinforced materials using a high-molecular organic polymer as a matrix, and usually glass fibers, carbon fibers, and aramid fibers are used as reinforcements. The resin-based composite material has wide application in aviation, automobile and marine industries.
In the research of graphene modified composite materials, the application of graphene modified composite materials is generally expanded by directly doping graphene with the composite materials. The method for preparing the graphene composite material has high requirement on the dispersion uniformity of the graphene, and the process is complicated, so that the method cannot be effectively popularized and applied.
Disclosure of Invention
In view of the above, the present invention provides a graphene paper composite material, which has excellent comprehensive properties and can be applied to flame retardation, deicing, monitoring of a resin molding process and monitoring of resin structure health.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a graphene paper composite material which comprises a graphene paper layer and a resin layer which are arranged in a stacked mode.
Preferably, the graphene paper composite material has multiple resin layers, and the graphene paper is located between the multiple resin layers.
Preferably, the material of the resin layer comprises thermosetting resin, thermosetting resin prepreg, thermoplastic resin or thermoplastic resin prepreg.
Preferably, the material of the resin layer comprises fiber epoxy resin or fiber epoxy resin prepreg.
Preferably, the fiber in the fiber epoxy resin or the fiber epoxy resin prepreg comprises glass fiber, carbon fiber, boron fiber, aramid fiber, silicon carbide fiber and high-density polyethylene fiber.
The invention also provides a preparation method of the graphene paper composite material, which comprises the following steps: obtaining the graphene paper composite material through bonding or curing; the curing includes oven curing or joule heating self-curing.
The invention also provides application of the graphene paper composite material in the technical scheme in the flame retardant field.
The invention also provides application of the graphene paper composite material in the technical scheme in the deicing field.
The invention also provides application of the graphene paper composite material in the technical scheme in monitoring resin molding.
The invention also provides application of the graphene paper composite material in the technical scheme in resin structure health monitoring.
The invention provides a graphene paper composite material which comprises a graphene paper layer and a resin layer which are arranged in a stacked mode. The graphene paper composite material disclosed by the invention has excellent comprehensive properties such as flame retardance, deicing performance and sensing performance, and is widely applied to the fields of flame retardance, deicing, resin molding monitoring and resin structure health monitoring. The data of the examples show that the graphene paper composite provided by the invention ignites after 30 seconds; melting ice blocks on the graphene paper composite material within 300 s; the graphene paper composite material can also effectively monitor the resin forming process; at the same time, structural health monitoring was performed on the resin.
Drawings
Fig. 1 is a graph of the flame retardant test effect of the graphene paper composite and the glass fiber epoxy resin of example 1;
FIG. 2 is a graph of deicing test effects of the graphene paper composite and the glass fiber epoxy resin of example 2;
FIG. 3 is a graph of the relationship between the heating temperature and power of the graphene paper composite material of example 3 before and after the joule heating curing;
FIG. 4 is a graph comparing mechanical properties of a graphene paper composite material obtained by self-curing by Joule heating and a graphene paper composite material obtained by curing in an oven;
fig. 5 is a data graph of monitoring a resin curing molding process for the graphene paper composite of example 4;
fig. 6 is a data plot of the graphene paper composite of example 5 monitoring resin structure health.
Detailed Description
The invention provides a graphene paper composite material which comprises a graphene paper layer and a resin layer which are arranged in a stacked mode. In the present invention, the material of the resin layer preferably includes a thermosetting resin, a thermosetting resin prepreg, a thermoplastic resin, or a thermoplastic resin prepreg. In the present invention, the material of the resin layer preferably includes a fiber epoxy resin or a fiber epoxy resin prepreg. In the present invention, the fiber epoxy resin or the fiber in the fiber epoxy resin prepreg preferably includes a fiber epoxy resin or a fiber in a fiber epoxy resin prepreg includes a glass fiber, a carbon fiber, a boron fiber, an aramid fiber, a silicon carbide fiber or a high-density polyethylene fiber.
The preparation method of the graphene paper is not particularly limited, and a graphene paper preparation method known to those skilled in the art can be adopted, specifically, for example, a redox method or a laser induction method is adopted. In the present invention, the method for preparing graphene paper by using the laser induction method preferably includes the following steps: reducing the polyimide paper by adopting laser induction to obtain graphene paper; the laser induced laser is preferably a continuous laser or a pulsed laser; the laser induced laser preferably comprises a gas laser, a solid laser and a semiconductor laser; the laser focusing distance induced by the laser is preferably 33.1-43.1 mm; the laser-induced power is preferably 0.25-25W; the laser-induced scanning speed is preferably 2.54-254 mm/s; the laser-induced printing resolution is preferably 10-1000; carrying out laser-induced reduction on one side or two sides of the polyimide paper; the laser-induced atmosphere preferably comprises air, oxygen, hydrogen or an inert gas.
In the present invention, the resin layers in the graphene paper composite are preferably multi-layered, and the graphene paper is positioned between the multi-layered resin layers.
The thicknesses of the graphene paper layer and the resin layer are not particularly limited, and can be selected by a person skilled in the art according to actual needs.
The invention also provides a preparation method of the graphene paper composite material, which comprises the following steps: obtaining the graphene paper composite material through bonding or curing; the curing includes oven curing or joule heating self-curing. In the present invention, when the material of the resin layer is a thermosetting resin or a thermoplastic resin, the graphene paper composite material is preferably obtained by bonding; the bonding agent preferably comprises a room temperature curing adhesive or a room temperature pressure sensitive adhesive.
In the invention, when the material of the resin layer is a thermosetting resin prepreg or a thermoplastic resin prepreg, the graphene paper composite material is obtained by curing. In the present invention, the curing is preferably performed during the molding process of the graphene paper composite material, that is, the composite material including one of the thermosetting resin prepreg or the thermoplastic resin prepreg and the graphene paper is cured, so that the thermosetting resin prepreg or the thermoplastic resin prepreg is cured, thereby forming the final graphene paper composite material. In the present invention, the curing preferably comprises oven curing or joule heating self-curing. In the present invention, the temperature of the oven curing is preferably 140 ℃. In the present invention, the step of joule heating self-curing includes: and connecting electrodes on two sides of the graphene paper, introducing current, and curing the thermoplastic resin prepreg or the thermosetting resin prepreg through self-heating of the graphene paper. In the present invention, the current is preferably 0.45A.
When the graphene paper composite material is prepared by adopting a curing method, the substrate and the anti-sticking cloth used for transferring the graphene composite material are not particularly limited, and the substrate and the anti-sticking cloth which are well known by the technical personnel in the field can be adopted, specifically, the substrate adopts an aluminum substrate, and the anti-sticking cloth adopts high-temperature cloth.
The invention also provides application of the graphene paper composite material in the technical scheme in the flame retardant field.
The invention also provides application of the graphene paper composite material in the technical scheme in the deicing field.
The invention also provides application of the graphene paper composite material in the technical scheme in monitoring resin molding. In an embodiment of the invention, said applying preferably comprises the steps of: the graphene paper composite material is formed by positioning graphene paper in the middle of a glass fiber epoxy resin prepreg; and connecting electrodes on two sides of the graphene paper, and introducing current to cure the glass fiber epoxy resin prepreg. The total curing time of the glass fiber epoxy resin prepreg is different due to different flowing time of the glass fiber epoxy resin prepreg before molding at different temperatures, so that the time distribution of resistance change of the graphene paper is different due to the curing time of the glass fiber epoxy resin prepreg, and the resin molding process is monitored.
The invention also provides application of the graphene paper composite material in the technical scheme in monitoring the structural health of the resin. In an embodiment of the invention, said applying preferably comprises the steps of: the graphene paper composite material is formed by positioning graphene paper between two layers of glass fiber epoxy resin prepreg; curing the graphene paper composite material in an oven to obtain a formed graphene paper composite material; the method comprises the steps of cutting the graphene paper composite material into a dumbbell shape, applying tension to two sides of the dumbbell-shaped graphene paper composite material, and monitoring the health condition of a resin structure by observing the resistance change of the graphene paper composite material. In the present invention, the temperature of the curing is preferably 140 ℃. In the invention, as the deformation applied to the graphene paper composite material is increased, the resistance of the graphene paper is increased, after the maximum deformation is reached, the graphene paper composite material is broken, the resistance of the graphene paper composite material is infinite, the change of the internal structure of the resin can be effectively predicted according to the change of the deformation and the resistance, and the method can be effectively used for monitoring the health of the resin structure.
The graphene paper composite material provided by the present invention is described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
Example 1
A graphene paper composite material comprises glass fiber epoxy resin and graphene paper which are arranged in a laminated mode; the graphene paper and the glass fiber epoxy resin are connected through an adhesive before.
The graphene paper composite material and the glass fiber epoxy resin are respectively fired by alcohol outer flame (400-500 ℃), and the effect graph is shown in figure 1. As can be seen from fig. 1, the glass fiber epoxy resin started to ignite in 15 seconds, and the graphene paper composite ignited after 30 seconds; the graphene paper composite material of the embodiment has excellent flame retardance and can be applied to the flame retardant field.
Example 2
A graphene paper composite material comprises glass fiber epoxy resin prepreg and graphene paper which are arranged in a stacked mode; the area of the graphene paper is 9cm2(ii) a The glass fiber epoxy resin prepreg is divided into two layers; the graphene paper is positioned between two layers of epoxy resin glass fiber prepreg. Connecting copper sheets at two ends of the upper side of the graphene paper to serve as electrodes for follow-up deicing; and heating and curing at 140 ℃ by using an oven to obtain the graphene paper composite material.
Respectively placing iceberg-shaped ice blocks with the same volume on the surfaces of the graphene paper composite material and the glass fiber epoxy resin; applying 0.5A of current to the graphene paper composite material through the copper sheet connected with the graphene paper at-24 ℃; the glass fiber epoxy resin was not treated and the change of ice was observed, the effect is shown in fig. 2: in fig. 2, a is a graph showing a change of ice cubes on the glass fiber epoxy resin without any treatment, and b is a graph showing a change of ice cubes on the graphene paper composite material obtained in the present embodiment. Experiments found that the ice blocks on the graphene paper composite completely melted within 300s, while the ice blocks on the glass fiber epoxy did not change. Therefore, the graphene paper composite material has excellent deicing performance and can be well applied to the field of deicing.
Example 3
A graphene paper composite material comprises glass fiber epoxy resin prepreg and graphene paper which are arranged in a stacked mode; the graphene paper is located on the upper surface of the glass fiber epoxy resin prepreg. Electrodes are led out from two sides of the graphene paper, a current of 0.45A is applied to the graphene paper composite material through the electrodes, the temperature of the graphene paper can reach 140 ℃ through the Joule heat of the graphene paper, the glass fiber epoxy resin prepreg is cured, and the performance of the obtained graphene paper composite material is similar to the mechanical performance of the graphene paper composite material obtained by curing in an oven, namely 301MPa and 326 MPa; but the energy consumed by joule heat curing is 32.4kJ, and the energy consumed by oven curing is 10.08 MJ; the Joule thermosetting graphene paper composite material saves 2-3 orders of magnitude of energy. The pictures before and after joule heating curing of the graphene paper composite material and the relationship between the heating temperature and the power of joule heating self-curing are shown in fig. 3. Fig. 4 is a graph comparing mechanical properties of a joule heat self-cured graphene paper composite material and a graphene paper composite material obtained by oven curing. As can be seen from fig. 4, the graphene paper composite material of the present embodiment has similar mechanical properties to those of the oven cured composite material, and saves a large amount of energy.
Example 4
A graphene paper composite material comprises graphene paper and a glass fiber epoxy resin prepreg which are arranged in a stacked mode; the glass fiber epoxy resin prepreg is divided into two layers; the graphene paper is positioned between the two layers of glass fiber epoxy resin prepreg.
Electrodes are led out from two sides of graphene paper of the graphene paper composite material, and current is introduced to cure the glass fiber epoxy resin prepreg. The curing and molding process of the glass fiber epoxy resin prepreg was monitored by the resistance change of the graphene paper, and the result is shown in fig. 5. As can be seen from fig. 5, the lower the curing temperature, the longer the resistance change time of the graphene paper, because the low temperature, the long flow time of the glass fiber epoxy prepreg, and thus the longer the resistance change time of the graphene paper. Therefore, the graphene paper composite material can effectively monitor the resin forming process.
Example 5
A graphene paper composite material comprises graphene paper and a glass fiber epoxy resin prepreg which are arranged in a stacked mode; the glass fiber epoxy resin prepreg is divided into two layers; the graphene paper is positioned between the two layers of glass fiber epoxy resin prepreg.
And (3) curing the graphene paper composite material at 140 ℃, and cutting the graphene paper composite material into a dumbbell shape of 5cm multiplied by 1cm after curing for mechanical property testing. The tensile machine used was an E44.104 tensile machine of MTS company, and changes in the internal structure of the graphene paper composite were monitored by observing changes in the resistance of the graphene paper composite during the tensile test, with the results shown in fig. 6. As can be seen from fig. 6: with the increase of the deformation, the resistance of the graphene paper composite material is increased; after the maximum deformation is reached, the graphene paper composite material is broken, and the resistance is infinite; therefore, the deformation of the internal structure of the graphene paper composite material can be predicted according to the tensile resistance change of the graphene paper composite material, and the purpose of monitoring the health of the resin structure is further achieved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (2)
1. Use of a graphene paper composite for monitoring resin moulding, the use comprising the steps of:
the graphene paper composite material is formed by positioning graphene paper in the middle of a glass fiber epoxy resin prepreg; connecting electrodes on two sides of the graphene paper and introducing current to cure the glass fiber epoxy resin prepreg; the total curing time of the glass fiber epoxy resin prepreg is different due to different flowing time before the glass fiber epoxy resin prepreg is molded at different temperatures, so that the time distribution of resistance change of the graphene paper is different due to the curing time of the glass fiber epoxy resin prepreg, and the resin molding process is monitored;
the preparation method of the graphene paper composite material comprises the following steps: embedding graphene paper into resin prepreg layers for co-curing to obtain the graphene paper composite material; the curing comprises oven curing or joule heating self-curing; when the material of the resin layer is thermosetting resin prepreg or thermoplastic resin prepreg, the graphene paper composite material is obtained by co-curing graphene paper and the resin prepreg; the step of joule heating self-curing comprises: connecting electrodes on two sides of the graphene paper, introducing current to enable the graphene paper to self-heat, and curing the thermoplastic resin prepreg or the thermosetting resin prepreg through heat conduction;
the graphene paper composite material consists of a graphene paper layer and a resin layer which are arranged in a stacked mode;
the graphene paper layer is positioned among the multiple resin layers;
the material of the resin layer comprises thermosetting resin prepreg or thermoplastic resin prepreg;
the material of the resin layer comprises fiber epoxy resin prepreg;
the fiber in the fiber epoxy resin prepreg is glass fiber;
the preparation method of the graphene paper comprises the following steps: reducing the polyimide paper by adopting laser induction to obtain graphene paper; the laser focusing distance induced by the laser is 33.1-43.1 mm; the laser induced power is 0.25-25W; the scanning speed of the laser induction is 2.54-254 mm/s; the laser-induced printing resolution is 10-1000.
2. Use of a graphene paper composite in resin structure health monitoring, the use comprising the steps of:
the graphene paper composite material is formed by positioning graphene paper between two layers of glass fiber epoxy resin prepreg; curing the graphene paper composite material in an oven to obtain a formed graphene paper composite material; cutting the graphene paper composite material into a dumbbell shape, applying tension on two sides of the dumbbell-shaped graphene paper composite material, and monitoring the health condition of a resin structure by observing the resistance change of the graphene paper composite material; the resistance of the graphene paper is increased along with the increase of the deformation applied to the graphene paper composite material, after the maximum deformation is reached, the graphene paper composite material is broken, the resistance of the graphene paper composite material is infinite, the change of the internal structure of the resin is predicted according to the change of the deformation and the resistance, and the method is effectively used for monitoring the health of the resin structure;
the preparation method of the graphene paper composite material comprises the following steps: embedding graphene paper into resin prepreg layers for co-curing to obtain the graphene paper composite material; the curing comprises oven curing or joule heating self-curing; when the material of the resin layer is thermosetting resin prepreg or thermoplastic resin prepreg, the graphene paper composite material is obtained by co-curing graphene paper and the resin prepreg; the step of joule heating self-curing comprises: connecting electrodes on two sides of the graphene paper, introducing current to enable the graphene paper to self-heat, and curing the thermoplastic resin prepreg or the thermosetting resin prepreg through heat conduction;
the graphene paper composite material consists of a graphene paper layer and a resin layer which are arranged in a stacked mode;
the graphene paper layer is positioned among the multiple resin layers;
the material of the resin layer comprises thermosetting resin prepreg or thermoplastic resin prepreg;
the material of the resin layer comprises fiber epoxy resin prepreg;
the fiber in the fiber epoxy resin prepreg is glass fiber;
the preparation method of the graphene paper comprises the following steps: reducing the polyimide paper by adopting laser induction to obtain graphene paper; the laser focusing distance induced by the laser is 33.1-43.1 mm; the laser induced power is 0.25-25W; the scanning speed of the laser induction is 2.54-254 mm/s; the laser-induced printing resolution is 10-1000.
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| CN109734468A (en) * | 2019-02-26 | 2019-05-10 | 航天材料及工艺研究所 | A kind of graphene paper enhancing carbon/carbon compound material and preparation method thereof |
| CN110068595B (en) * | 2019-05-20 | 2021-03-09 | 北京航空航天大学 | Liquid sensor and preparation method and application thereof |
| CN112694930A (en) * | 2019-10-23 | 2021-04-23 | 广州顺倬能源科技有限公司 | Method for producing engine oil additive |
| CN112694935A (en) * | 2019-10-23 | 2021-04-23 | 广州顺倬能源科技有限公司 | Engine oil additive |
| CN111432507B (en) * | 2020-03-30 | 2022-03-04 | 北京航空航天大学 | Adjustable laser-induced graphene paper heater and application thereof |
| CN111923438B (en) * | 2020-06-16 | 2021-09-14 | 北京航空航天大学 | Preparation method of self-converted multifunctional graphene composite material |
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