CN103607795B - A kind of preparation method of Graphene heating film - Google Patents
A kind of preparation method of Graphene heating film Download PDFInfo
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- CN103607795B CN103607795B CN201310637495.4A CN201310637495A CN103607795B CN 103607795 B CN103607795 B CN 103607795B CN 201310637495 A CN201310637495 A CN 201310637495A CN 103607795 B CN103607795 B CN 103607795B
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Abstract
The invention belongs to material with carbon element field, be specially a kind of preparation method of Graphene heating film.The methods such as ultrasonic and stirring are utilized to be dispersed in organic solvent by graphene powder, obtain the graphene solution that concentration is 0.05mg/ml ~ 0.5mg/ml, by the method for suction filtration, graphene uniform is covered on organic filter membrane or water system filter membrane, by the method for mechanical stripping, immersion or organic solvent dissolution, graphene film is separated with filter membrane again, obtain graphene film, graphene film adds top electrode, voltage is applied to it and can produce heat.The present invention utilizes the two-dimensional nanostructure of Graphene uniqueness, the characteristic of large radius-thickness ratio, high specific area, by above preparation technology, make between graphene sheet layer, to form the conductive network be evenly communicated with, applying can produce higher heat under lower voltage (1 ~ 10V).The advantages such as it is simple and easy to control that the present invention has preparation process, pollution-free, size adjustable, are applicable to large-scale production.
Description
Technical field
The invention belongs to material with carbon element field, be specially a kind of preparation method of Graphene heating film.
Background technology
Electric-heating technology has the remarkable advantages such as clean energy resource, thermal conversion efficiency is high, Pavement design is convenient, is widely used in fields such as modern architecture, heating engineering, decorations.For the inefficient shortcoming of traditional electric-heating technology, the high-performance carbon-based exothermic material of development low resistance, high-termal conductivity, high heat-resistant stability is just becoming the inexorable trend of future development.
Since first time in 2004 prepares Graphene, the physical property of Graphene excellence has attracted the extensive concern of numerous scholar.Graphene has excellent conductivity, and electron mobility is up to 2 × 10
5cm
2v
-1s
-1, about the material indium antimonide high twice more maximum than carrier mobility known at present.Meanwhile, the resistance value under Graphene room temperature only has 2/3rds of copper, and Graphene has very high radius-thickness ratio (up to more than 5000) and specific area, and (theoretical value is up to 2600m
2/ g), the two-dimension plane structure of Graphene makes it more easily form conductive network in the base than zero dimension or one-dimensional electric material.The performance of Graphene these excellences above-mentioned, makes it present good application prospect in field of electric heating, particularly transparent, pliable and tough thin film heater.
At present, the application report about graphene transparent conductive film display screen, vehicle window anti-icing equipment, heat insulation window and other heating systems out of doors has been had.Compared with carbon fiber felt heating element conventional at present, when graphene film is used for electric heating element, there is the machine-shaping characteristic of the resistivity of appropriateness, preferably thermal stability and excellence, more energy-efficient.The preparation technology that graphene film is conventional has hand brush, dipping, spraying, spin coating etc., but these complicated process of preparation and heating efficiency is low.
Summary of the invention
For existing conventional graphene film complicated process of preparation, shortcoming that heating efficiency is low; the object of the invention is a kind of preparation method of novel graphite alkene heating film; there is preparation process simple and easy to control, the advantages such as pollution-free, size adjustable, be applicable to large-scale production.
Technical scheme of the present invention is:
First a preparation method for Graphene heating film, is that raw material is made with Graphene, and graphene powder is in organic solvent dispersed, obtains the Graphene colloidal suspensions that concentration is 0.05mg/ml ~ 0.5mg/ml; Then, by the method for vacuum filtration, graphene uniform is covered on miillpore filter; Again by Graphene together with miillpore filter through natural drying or heat drying, then obtain uniform and stable Graphene heating film by the method for mechanical stripping, immersion or organic solvent dissolution; Graphene film adds top electrode, applies voltage and can produce heat.
The Graphene that described Graphene is intercalation stripping method, prepared by graphite oxidation reducing process or additive method.
The homodisperse method of described graphene powder is ultrasonic or stirs, and the ultrasonic disperse time is 5min ~ 80min.
Described organic solvent is DMF, ethanol, n-butanol, isopropyl alcohol or acetone.
The pressure limit of described vacuum filtration is 0.05MPa ~ 0.2MPa, and time range is 15min ~ 45min.
Described miillpore filter is organic filter membrane or water system filter membrane.
Described miillpore filter is Kynoar filter membrane, polyamide filter membrane, teflon membrane filter or mixed ester membranes, and the aperture of miillpore filter is 0.10 ~ 1.0 micron.
The surface density of described Graphene heating film is 10g/m
2~ 50g/m
2, thickness is 0.02mm ~ 0.20mm, and specific insulation is 0.005 Ω cm ~ 0.02 Ω cm, and surface resistivity is 0.5 Ω/sq ~ 3.0 Ω/sq.
Compared with prior art, tool of the present invention has the following advantages:
(1) the present invention is without the need to carrying out complicated process to raw material, and manufacture process is simple, is easy to operation, and product is more even simultaneously, good stability.And the size of product can be set according to actual needs.
(2) graphene film that prepared by the present invention is applied to field of electric heating, and compared with existing conventional material with carbon element Electric radiant Heating Film, heating is fast, and surface temperature is even and stable.
(3) the present invention adopts the method for suction filtration to prepare graphene film, compared with prior art, easy and simple to handle and heating efficiency is high, therefore has more advantage.
Accompanying drawing explanation
The electron scanning micrograph of Graphene of Fig. 1 for using in the embodiment of the present invention.
Fig. 2 is the electron scanning micrograph on the graphene film surface of preparation in the embodiment of the present invention 1 and embodiment 2.Wherein, (a) figure is embodiment 1; B () is embodiment 2.
Fig. 3 is the photo of graphene film prepared in the embodiment of the present invention 1.
The surface Scanning Electron microphotograph of carbon fiber felt of Fig. 4 for using in comparative example 1 of the present invention and comparative example 2.Wherein, (a) figure is comparative example 1; B () is comparative example 2.
Fig. 5 is the heating curve of comparative example 1, comparative example 2, embodiment 1 and embodiment 2 sample.Wherein, (a) figure is comparative example 1; B () is comparative example 2; C () figure is embodiment 1; D () is embodiment 2.
Embodiment
The preparation technology of Graphene heating film of the present invention is as follows: graphene powder is in organic solvent dispersed, and obtaining concentration is that 0.05mg/ml ~ 0.5mg/ml(is preferably 0.1mg/ml ~ 0.3mg/ml) Graphene colloidal suspensions; By the method for vacuum filtration, graphene uniform is covered on organic filter membrane or water system filter membrane, again after natural drying or heat drying, be separated graphene film and filter membrane by the method for mechanical stripping, immersion or organic solvent dissolution, obtain uniform and stable graphene film.Graphene film adds top electrode, applies voltage and can produce heat.
The present invention adopts conventional Vacuum filtration device, this device comprises: the filter flask of the Buchner funnel of 300ml, sintered glass filter, 1000ml ~ 2000ml and connect flexible pipe used, fixture, and vacuum pump used can be vacuum pump using circulatory water or oilless vacuum pump.Vacuum pump is connected with filter flask flexible pipe, miillpore filter is put on sintered glass filter, presses filter tunnel, clamp with clip, go up solution, connect vacuum-pump power supply, start suction filtration, the pressure limit of vacuum filtration is 0.05MPa ~ 0.2MPa, and the time is 15min ~ 45min.After suction filtration, first disconnect flexible pipe and put vacuum, then powered-down, and then take away filter flask.
As shown in Figure 1, the pattern feature of Graphene of the present invention and technical parameter as follows: Graphene has good laminated structure, because it has very large radius-thickness ratio (being greater than 1000), it is of a size of 0.5 ~ 50 μm, thickness 1 ~ 5nm, macroscopically show as shown in the figure curl form, be rendered as fluffy cluster-shaped.
The Graphene that described Graphene can be intercalation stripping method, prepared by graphite oxidation reducing process and additive method, the Graphene that the present invention uses is obtained through solid phase intercalation, high-temperature expansion by graphite powder, thickness 1 ~ 5nm, the number of plies≤10 layer, be of a size of 0.5 ~ 50 μm, purity >97%.Described organic solvent can be DMF, ethanol, n-butanol, isopropyl alcohol or acetone etc.Described preparation method is vacuum filtration, and described miillpore filter can be organic filter membrane or water system filter membrane.Described graphene film and the separation method of filter membrane can be the methods of mechanical stripping, immersion or organic solvent dissolution.
In order to be illustrated more clearly in technical scheme of the present invention, be described in further detail below in conjunction with embodiment and accompanying drawing.
Embodiment 1
The graphene powder taking 9.375mg is put in beaker, adds absolute ethyl alcohol reagent 50mL, ultrasonic disperse 1h, obtains the Graphene colloidal suspensions that concentration is the isotropic stable of 0.1875mg/mL.Be placed on the miillpore filter of Vacuum filtration device by Graphene colloidal suspensions, employing aperture is the Kynoar filter membrane of 0.45 μm, and the pressure of vacuum filtration is 0.08MPa, and the time is 15min.After suction filtration completes, graphene film is placed in 45 DEG C of dry 24h of drying box together with filter membrane, then adopts the method for mechanical stripping, obtain graphene film.As can be seen from Fig. 2 (a) and Fig. 3: the graphene film surface uniform that vacuum filtration obtains is smooth, lamella overlap joint closely.
The surface density of the graphene film utilizing the method to obtain is 15g/m
2, thickness is 0.05mm, and specific insulation is 0.0160 Ω cm, and surface resistivity is 2.0 Ω/sq.
Embodiment 2
Difference from Example 1 is, the graphene powder taking 18.750mg is put in beaker, adds DMF reagent 100mL, ultrasonic disperse 1h, obtains the Graphene colloidal suspensions that concentration is the isotropic stable of 0.1875mg/mL.Be placed on the miillpore filter of Vacuum filtration device by Graphene colloidal suspensions, employing aperture is the teflon membrane filter of 0.45 μm, and the pressure of vacuum filtration is 0.15MPa, and the time is 35min.After suction filtration completes, graphene film is placed in 100 DEG C of dry 38h of drying box together with filter membrane, then adopts the method for mechanical stripping, obtain graphene film, as can be seen from Fig. 2 (b): the graphene film surface uniform obtained is smooth, lamella overlap joint closely.
The surface density of the graphene film utilizing the method to obtain is 30g/m
2, thickness is 0.10mm, and specific insulation is 0.0090 Ω cm, and surface resistivity is 1.0 Ω/sq.
Embodiment 3
Difference from Example 1 is, the graphene powder taking 12.80mg is put in beaker, adds isopropyl alcohol reagent 100mL, ultrasonic disperse 1h, obtains the Graphene colloidal suspensions that concentration is the isotropic stable of 0.1280mg/mL.Graphene colloidal suspensions is placed on the miillpore filter of Vacuum filtration device, employing aperture is conventional mixed ester membranes (the CN-CA film of 0.22 μm, be made up of PAA-CN-CA, as: the WX type mixed cellulose ester microporous membrane of Shanghai Yan Sheng biochemical reagents Co., Ltd), the pressure of vacuum filtration is 0.10MPa, and the time is 25min.After suction filtration completes, graphene film is placed in 40 DEG C of dry 12h of drying box together with filter membrane, then adopts the method that acetone soln dissolves, obtain graphene film.
The surface density of the graphene film utilizing the method to obtain is 20.50g/m
2, thickness is 0.08mm, and specific insulation is 0.0120 Ω cm, and surface resistivity is 1.5 Ω/sq.
Embodiment 4
Difference from Example 1 is, the graphene powder taking 21.50mg is put in beaker, adds DMF reagent 100mL, ultrasonic disperse 1h, obtains the Graphene colloidal suspensions that concentration is the isotropic stable of 0.2150mg/mL.Be placed on the miillpore filter of Vacuum filtration device by Graphene colloidal suspensions, employing aperture is the teflon membrane filter of 0.45 μm, and the pressure of vacuum filtration is 0.20MPa, and the time is 45min.After suction filtration completes, graphene film is placed in 100 DEG C of dry 38h of drying box together with filter membrane, then adopts the method for mechanical stripping, obtain graphene film.
The surface density of the graphene film utilizing the method to obtain is 34.40g/m
2, thickness is 0.15mm, and specific insulation is 0.008 Ω cm, and surface resistivity is 2.3 Ω/sq.
Comparative example 1
Commercially available carbon fiber felt is shown in Fig. 4 (a), and mass area ratio is 15g/m
2.The thickness of carbon fiber felt is 0.34mm, and specific insulation is 0.3570 Ω cm, and surface resistivity is 10.5 Ω/sq.
Comparative example 2
Commercially available carbon fiber felt is shown in Fig. 4 (b), and mass area ratio is 30g/m
2.The thickness of carbon fiber felt is 0.51mm, and specific insulation is 0.3315 Ω cm, and surface resistivity is 6.5 Ω/sq.
Graphene used is in the above-described embodiments that Sichuan Jinlu Group Co., Ltd produces, the Graphene (Fig. 1) obtained through solid phase intercalation, high-temperature expansion by graphite powder.Carbon fiber felt used in comparative example is that Shenyang Yu Heng carbon fiber Co., Ltd produces (Fig. 4).Method of testing with reference to GB/T7287-2008, JG-T286-2010 measures the heating data of sample, and specimen size is that 25mm × 25mm(is as Fig. 3).The voltage that sample applies is 1V ~ 4V, as can be seen from Fig. 5 (a): comparative example 1(surface density is 15g/m
2carbon fiber felt) caloric value under applied voltage is less, when voltage is 4V, surface temperature is only 39 DEG C; As can be seen from Fig. 5 (b): comparative example 2(surface density is 30g/m
2carbon fiber felt) caloric value under applied voltage is still less relative to the graphene film prepared by the present invention, when voltage is 4V, surface temperature is only 60.5 DEG C; As can be seen from Fig. 5 (c): embodiment 1(surface density is 15g/m
2graphene film) surface temperature with the rule of curved rising heating time.At the energising initial stage, the surface temperature climbing speed of heater is very fast, along with the increase of conduction time, the surface temperature climbing speed change of heater reduces gradually, no longer change after reaching a certain stable temperature, when voltage is 4V, the stable temperature that embodiment 1 sample reaches is 96 DEG C; As can be seen from Fig. 5 (d): embodiment 2(surface density is 30g/m
2graphene film), its temperature changing regularity is similar with embodiment 1, and when voltage is 4V, the stable temperature reached is higher, is 118 DEG C.
Embodiment result shows, the present invention utilizes the two-dimensional nanostructure of Graphene uniqueness, the characteristic of large radius-thickness ratio, high specific area, by above preparation technology, make between graphene sheet layer, to form the conductive network be evenly communicated with, applying can produce higher heat under lower voltage (1 ~ 10V).The advantages such as it is simple and easy to control that the present invention has preparation process, pollution-free, size adjustable, are applicable to large-scale production.
Claims (7)
1. a preparation method for Graphene heating film, is characterized in that: first, is that raw material is made with Graphene, and graphene powder is in organic solvent dispersed, obtains the Graphene colloidal suspensions that concentration is 0.05mg/ml ~ 0.5mg/ml; Then, by the method for vacuum filtration, graphene uniform is covered on miillpore filter; Again by Graphene together with miillpore filter through natural drying or heat drying, then obtain uniform and stable Graphene heating film by the method for mechanical stripping, immersion or organic solvent dissolution; Graphene film adds top electrode, applies voltage and can produce heat; The surface density of described Graphene heating film is 10g/m
2~ 50g/m
2, thickness is 0.02mm ~ 0.20mm, and specific insulation is 0.005 Ω cm ~ 0.02 Ω cm, and surface resistivity is 0.5 Ω/sq ~ 3.0 Ω/sq.
2. according to the preparation method of Graphene heating film according to claim 1, it is characterized in that, described Graphene is Graphene prepared by intercalation stripping method or graphite oxidation reducing process.
3. according to the preparation method of Graphene heating film according to claim 1, it is characterized in that, the homodisperse method of described graphene powder is ultrasonic or stirs, and the ultrasonic disperse time is 5min ~ 80min.
4. according to the preparation method of Graphene heating film according to claim 1, it is characterized in that, described organic solvent is DMF, ethanol, n-butanol, isopropyl alcohol or acetone.
5. according to the preparation method of Graphene heating film according to claim 1, it is characterized in that, the pressure limit of described vacuum filtration is 0.05MPa ~ 0.2MPa, and time range is 15min ~ 45min.
6. according to the preparation method of Graphene heating film according to claim 1, it is characterized in that, described miillpore filter is organic filter membrane or water system filter membrane.
7. according to the preparation method of Graphene heating film according to claim 1, it is characterized in that, described miillpore filter is Kynoar filter membrane, polyamide filter membrane, teflon membrane filter or mixed ester membranes, and the aperture of miillpore filter is 0.10 ~ 1.0 micron.
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