CN109068413A - The preparation method of graphite composite film, the graphite composite film being obtained by this method and its application - Google Patents
The preparation method of graphite composite film, the graphite composite film being obtained by this method and its application Download PDFInfo
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- CN109068413A CN109068413A CN201810810341.3A CN201810810341A CN109068413A CN 109068413 A CN109068413 A CN 109068413A CN 201810810341 A CN201810810341 A CN 201810810341A CN 109068413 A CN109068413 A CN 109068413A
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- Prior art keywords
- graphite
- composite film
- graphite composite
- microchip
- alcohol
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Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/145—Carbon only, e.g. carbon black, graphite
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
- H05B3/34—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater flexible, e.g. heating nets or webs
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
- H05B2203/013—Heaters using resistive films or coatings
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
- H05B2203/017—Manufacturing methods or apparatus for heaters
Abstract
The invention discloses a kind of preparation methods of graphite composite film, the application of the graphite composite film and the film that are prepared by this method.Graphite microchip dispersion liquid is made this method comprises: expanded graphite is removed, is separated and be dried to obtain graphite microchip；The graphite microchip and binder, medium and dispersing agent are mixed in a certain ratio to obtain graphite microchip suspension；Graphite composite film finally is made in resulting graphite microchip suspension.Compared with prior art, this method is formed a film using aqueous medium, at low cost, small pollution of the environment；Graphite microchip has the orientation of height in graphite composite film obtained, and graphite composite film has the characteristics that high flexibility and low-resistivity, resistivity are less than or equal to 0.2 Ω cm.The composite membrane can be driven by high-low voltage generates heat and realizes temperature control, can be used as exothermic material in heating clothes or heating device.
Description
Technical field
The present invention relates to carbon material field, more particularly to a kind of graphite composite film preparation method, be obtained by this method
Graphite composite film and its application.
Background technique
Currently, resistance heating is most popular Electric heating.The thermo electric material that resistance heating uses can be divided into
Two major classes: metallic resistance silk and ceramic heating material.However, metallic resistance silk has, density is big, oxidizable, heating efficiency is low,
The disadvantages of electromagnetic radiation is serious；The heating rate of ceramic heating material is slow, and brittleness is high, flexibility is poor.In addition, these two types of material ratios
It is great, not resistant to bending, it can not all meet the requirement of the fields to heating material such as wearable field or outdoor high and cold protection very well.
Chinese patent CN106003889A is disclosed one kind and is combined with graphene and carbon nanotube, multiple with organic elastomer matrix
Conductive film and the method as Electric radiant Heating Film is made in conjunction.The electric heating composite membrane being obtained by this method has light weight, flexible, bullet
Property high, fever stable and uniform the advantages that.However, the main preparation methods of graphene are oxidation-reduction method at present, this method is not only
It is with high costs, and need to use a large amount of heavily contaminateds in its production process and rich in corrosive chemicals, such as the concentrated sulfuric acid, hydrogen fluorine
Acid etc., these substances can aggravate environmental pollution.
Therefore, seeking a kind of thermo electric materials such as inexpensive, environmental-friendly, highly conductive, high flexibility becomes the urgent of this field
Demand.
Summary of the invention
In order to solve the problems in the existing technology, the invention proposes a kind of preparation method of graphite composite film, by
Graphite composite film made from the method and its application.
According to an aspect of the present invention, a kind of preparation method of graphite composite film is proposed, comprising the following steps:
S01: expanded graphite, surfactant and oxidant are added in the mixed solution of water or water and ethyl alcohol, are passed through
Graphite microchip dispersion liquid is made in ultrasound removing or mechanical stripping, and the dispersion liquid is separated and be dried to obtain graphite microchip；
S02: resulting graphite microchip and binder, medium and dispersing agent are mixed in a certain ratio, graphite microchip is obtained
Suspension；
S03: graphite composite film is made in resulting graphite microchip suspension.
Further, in step S01, the surfactant is carboxymethyl cellulose；The oxidant is hydrogen peroxide；Institute
The piece diameter for stating graphite microchip is 0.1~600 μm, with a thickness of 5~100nm；The binder be aqueous epoxy resins, acrylic acid,
One or more mixtures of silicone acrylic emulsion, aqueous polyurethane；The medium is the mixture of water, alcohol or water and alcohol, wherein
The alcohol is water-soluble monohydric alcohol, dihydric alcohol or polyalcohol, and the volume ratio of water and alcohol is 1:10~10:1；The stone
The weight percent that black microplate accounts for the medium is 0.1%~20%.
Further, in step S02, the dispersing agent is hydroxypropyl methyl cellulose, hydroxymethyl cellulose, polyethylene pyrrole
One or more mixtures of pyrrolidone, the weight percent that the dispersing agent accounts for the graphite microchip is 0.1%~6%.
Further, in step S03, by solvent evaporation, solution coating, curtain coating, spray, brush one of or it is a variety of
Method prepares graphite composite film on substrate, and the substrate is polyethylene terephthalate, polypropylene, polyethylene, polyamides
Imines, polytetrafluoroethylene (PTFE) or nylon substrate.
According to another aspect of the present invention, it proposes a kind of graphite composite film, is prepared by one of aforementioned method
's.
Further, the graphite microchip in the graphite composite film be in height-oriented arrangement, composite film thickness be 0.6~
2000 μm, resistivity is less than or equal to 0.2 Ω cm.
According to a further aspect of the invention, a kind of graphite composite film heater is proposed comprising heating layer, use are aforementioned
The graphite composite film of method preparation is as exothermic material；Electrode layer is located at the surface or inside of the heating layer；Waterproof layer,
The two sides of the heating layer, electrode outside are set；Protective layer is arranged on the outside of waterproof layer.
Further, the material of the electrode layer is elargol, wire, metal foil, one kind or more of conductive metal adhesive tape
Kind；The material of the waterproof layer be silica gel, epoxy resin, polyurethane it is one or more；The material of the protective layer is nonwoven
Cloth, leather, cloth, resin film it is one or more.
According to a further aspect of the invention, propose graphite composite film heater described above as fever temperature regulating device
Application, the fever temperature regulating device be used for heating clothes or heating and heat-insulating device.
Graphite composite film preparation method proposed by the present invention, has the advantage that compared with prior art
(1) the use of expanded graphite is raw material, graphite microchip is prepared by physical separation methods, using graphite microchip as electric heating
Conducting medium in film, it is this method simple process, low in cost, and high pollution chemicals is not used, it is environmentally friendly；It uses
Oxidant moderately aoxidizes graphite microchip, forms chemical bond with binder, performance is more excellent.
(2) aqueous medium, the method phase with existing organic solvent as medium are used in the preparation process of graphite composite film
Than lower to the adverse effect of environment；
(3) dispersing agent is added in the preparation process of Electric radiant Heating Film, graphite microchip can control by the addition of dispersing agent and exist
Height-oriented layered arrangement is formed in film, mutually overlap joint forms continuous conductive path each other, it is ensured that composite membrane has
Excellent electric conductivity.If graphite microchip does not have height-oriented layered arrangement, it is difficult to form low-resistivity that (resistivity is small
In equal to 0.2 Ω cm) composite membrane.
(4) the method for the present invention preparation graphite composite film have high conductivity and high flexibility, it is light, be easy to cut processing,
It is resistant to bending, various shape is made with can be convenient, meets the requirement of different use occasions；
(5) lower voltage (lower than 36V) and high voltage can be used in the heater based on the preparation of above-mentioned graphite composite film
(220V) driving, low-voltage are safe to the human body；And low energy consumption, fever is uniform and can pass through for graphite composite film heater
It controls voltage and realizes temperature control, wearable or transportable heating device requirement can be met well.
Detailed description of the invention
Fig. 1 is the flow chart of graphite composite film preparation method of the invention.
Fig. 2 is the stereoscan photograph of the graphite composite film of one embodiment of the invention preparation.
Fig. 3 is the graphite composite film heating element structure of one embodiment of the invention preparation.
Specific embodiment
Specific embodiments of the present invention are described more fully below, it should be noted that the embodiments described herein is served only for illustrating
Illustrate, is not intended to restrict the invention.In the following description, in order to provide a thorough understanding of the present invention, a large amount of spies are elaborated
Determine details.It will be apparent, however, to one skilled in the art that, it is not necessary to this hair is carried out using these specific details
It is bright.In other instances, in order to avoid obscuring the present invention, well known structure, circuit, material or method are not specifically described.
Throughout the specification, meaning is referred to " one embodiment ", " embodiment ", " example " or " example "
, a particular feature, structure, or characteristic described in conjunction with this embodiment or example is comprised at least one embodiment of the invention.
Therefore, the phrase " in one embodiment ", " in embodiment ", " example " occurred in each place of the whole instruction
Or " example " is not necessarily all referring to the same embodiment or example.Furthermore, it is possible in any suitable combination and/or sub-portfolio will be specific
Feature, structure or characteristic combine in one or more embodiment or examples.The present invention is carried out below with reference to attached drawing specific
Description.
In the description carried out below in conjunction with attached drawing to technical solution of the present invention, size, the ratio of each element of attached middle school
And positional relationship is only exemplary, the connection type between illustrated each element is also intended merely to be illustrated, not
For limiting the present invention.
Embodiment 1
The preparation method of graphite composite film is shown referring to Fig.1.It the use of natural flake graphite is raw material, after intercalation processing
Obtain expanded graphite.It weighs a certain amount of expanded graphite to be dispersed in water, appropriate carboxymethyl cellulose and hydrogen peroxide is added, ultrasound
Graphite microchip dispersion liquid is obtained after processing.The dispersion liquid is separated, is dried to obtain graphite microchip, analysis shows that, gained graphite is micro-
The average piece diameter of piece is 12 μm, average thickness 30nm.
Graphite microchip is added in the mixed solution of water and ethyl alcohol together with acrylic resin, while methylol fibre is added
Dimension element is used as dispersing agent.Wherein, the volume ratio of water and ethyl alcohol is 8:1, and graphite microchip accounts for the 8% of mixed solution weight, methylol
Cellulose accounts for the 2% of graphite microchip weight.Said mixture is sufficiently stirred, graphite microchip suspension is obtained.The suspension is equal
Even stabilization can stand 1 week or more without obvious sedimentation.
Above-mentioned suspension is coated on pet substrate, forms graphite composite film through drying.
The graphite composite film prepared by the above method, average thickness are~30 μm.Referring to fig. 2, scanning electron microscope is shown,
Graphite microchip preferably remains original laminated structure in graphite composite film, and in height-oriented, it is folded to be parallel to substrate surface
Layer dense arrangement simultaneously mutually overlaps.Measurement display, the resistivity of the graphite composite film are 0.02 Ω cm.The film has good
Flexibility, electric conductivity is not decreased obviously after repeatedly rubbing, and required shape can be easily cut into tool, such as rectangular
Shape block.
As shown in figure 3, after cropped, in the both ends connection electrode of graphite composite film 301, after being encapsulated with silica gel 302,302 '
Adhesive epoxy resin cured sheets 303,303 ' are used as insulating layer on the outside again, and graphite composite film heater 300 is made.Gained is sent out
Hot body heat is pressed among timber floor.Measurement display, under the driving of 220V voltage, the electric current of heating floor is 0.2A, power
44.0W, mean temperature have uniform and good heating effect up to 34.6 DEG C.
Embodiment 2
The preparation process of graphite composite film is substantially the same manner as Example 1.It the use of natural flake graphite is raw material, by intercalation
Expanded graphite is obtained after processing.It weighs a certain amount of expanded graphite to be dispersed in water, appropriate carboxymethyl cellulose and dioxygen is added
Water handles to obtain graphite microchip dispersion liquid through homogenizer.The dispersion liquid separated, dry after obtain graphite microchip, analysis shows that,
The average piece diameter of gained graphite microchip is 8 μm, average thickness 15nm.
Graphite microchip is added to the water together with aqueous epoxy resins, while polyvinylpyrrolidone is added as dispersion
Agent.Wherein, graphite microchip accounts for the 18% of water weight, and polyvinylpyrrolidone accounts for the 5.5% of graphite microchip weight.By above-mentioned mixing
Object is sufficiently stirred, and obtains graphite microchip suspension.The uniform suspension is stablized, and can stand 1 week or more without obvious sedimentation.
Above-mentioned suspension is coated on polyimide substrate using the tape casting, forms graphite composite film through drying.
The graphite composite film prepared by the above method, average thickness is 60 μm, and the graphite in graphite composite film
Microplate preferably remains original laminated structure, in height-oriented, is parallel to substrate surface lamination dense arrangement and phase interconnection
It connects.Measurement display, the resistivity of the graphite composite film are 0.05 Ω cm.The film has good flexibility, by repeatedly rubbing
Electric conductivity is not decreased obviously after stranding, and required shape, such as palm shaped can be easily cut into tool.
After cropped, in graphite composite film surface layout electrode, after being encapsulated using polyurethane again outer side bonds leather as
Graphite composite film heater is made in insulating layer.By the centre of the palm and the back of the hand two sides of gained heater filling gloves, fever hand is made
Set.Measurement display, the gloves have uniform and good fever and heat insulation effect, increase voltage, and gloves temperature correspondinglys increase.
In addition to vest and gloves, specific shape can also be made in graphite composite film heater of the invention, and then be used for
Different types of clothing and fever product are sewed, such as knee-pad, waist support, socks, cap, scarf, insole, underwear, earflap, trousers, window
Curtain, wallpaper, quilt, cushion etc. can also need to be made Portable heating/attemperator according to different occasions.
Although exemplary embodiment describes the present invention with reference to several, it is to be understood that, term used is explanation and shows
Example property, term and not restrictive.The spirit or reality that can be embodied in a variety of forms due to the present invention without departing from invention
Matter, it should therefore be appreciated that above-described embodiment is not limited to any of the foregoing details, and the spirit defined by appended claims
It all should be accompanying power with the whole change and modification widely explained, therefore fallen into claim or its equivalent scope in range
Benefit requires to be covered.
Claims (9)
1. a kind of preparation method of graphite composite film, comprising the following steps:
S01: expanded graphite, surfactant and oxidant are added in the mixed solution of water or water and ethyl alcohol, pass through ultrasound
Graphite microchip dispersion liquid is made in removing or mechanical stripping, and the dispersion liquid is separated and be dried to obtain graphite microchip；
S02: resulting graphite microchip and binder, medium and dispersing agent are mixed in a certain ratio, and obtain graphite microchip suspension
Liquid；
S03: graphite composite film is made in resulting graphite microchip suspension.
2. according to the method described in claim 1, it is characterized by:
In step S01, the surfactant is carboxymethyl cellulose；The oxidant is hydrogen peroxide；The graphite microchip
Piece diameter is 0.1~600 μm, with a thickness of 5~100nm；The binder is aqueous epoxy resins, acrylic acid, silicone acrylic emulsion, aqueous
One or more mixtures of polyurethane；The medium is the mixture of water, alcohol or water and alcohol, wherein the alcohol is to dissolve in
Monohydric alcohol, dihydric alcohol or the polyalcohol of water, and the volume ratio of water and alcohol is 1:10~10:1；The graphite microchip, which accounts for, to be given an account of
The weight percent of matter is 0.1%~20%.
3. according to the method described in claim 1, it is characterized by:
In step S02, the dispersing agent is hydroxypropyl methyl cellulose, one kind of hydroxymethyl cellulose, polyvinylpyrrolidone
Or a variety of mixtures, the weight percent that the dispersing agent accounts for the graphite microchip is 0.1%~6%.
4. according to the method described in claim 1, it is characterized by:
In step S03, through one of solvent evaporation, solution coating, curtain coating, spray, brushing or a variety of methods on substrate
Graphite composite film is prepared, the substrate is polyethylene terephthalate, polypropylene, polyethylene, polyimides, polytetrafluoroethyl-ne
Alkene or nylon substrate.
5. a kind of graphite composite film, it is characterised in that:
The graphite composite film is prepared by the method for one of Claims 1-4.
6. graphite composite film according to claim 5, it is characterised in that:
Graphite microchip in the graphite composite film is in height-oriented arrangement, and composite film thickness is 0.6~2000 μm, and resistivity is small
In equal to 0.2 Ω cm.
7. a kind of graphite composite film heater, comprising:
Heating layer uses the graphite composite film of claim 5 or 6 as exothermic material；Electrode layer is located at the table of the heating layer
Face or inside；The two sides of the heating layer, electrode outside is arranged in waterproof layer；Protective layer is arranged on the outside of waterproof layer.
8. according to the graphite composite film heater of claim 7 or 8, it is characterised in that:
The material of the electrode layer be elargol, wire, metal foil, conductive metal adhesive tape it is one or more；
The material of the waterproof layer be silica gel, epoxy resin, polyurethane it is one or more；
The material of the protective layer be non-woven fabrics, leather, cloth, resin film it is one or more.
9. application of the graphite composite film heater of one of such as claim 7 to 9 as fever temperature regulating device, which is characterized in that
The fever temperature regulating device is used for heating clothes or heating and heat-insulating device.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114591526A (en) * | 2022-01-12 | 2022-06-07 | 哈尔滨工业大学（威海） | Graphite nanosheet-based composite membrane driver, preparation method and application thereof |
| CN117098259A (en) * | 2023-10-17 | 2023-11-21 | 哈尔滨工业大学（威海） | Manufacturing method of flexible high-strength waterproof insulating heating device |
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| CN117098259B (en) * | 2023-10-17 | 2024-03-19 | 哈尔滨工业大学（威海） | Manufacturing method of flexible high-strength waterproof insulating heating device |
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