CN103607795A - Preparation method for graphene heating film - Google Patents
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- CN103607795A CN103607795A CN201310637495.4A CN201310637495A CN103607795A CN 103607795 A CN103607795 A CN 103607795A CN 201310637495 A CN201310637495 A CN 201310637495A CN 103607795 A CN103607795 A CN 103607795A
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Abstract
The invention belongs to the field of carbon materials, and particularly relates to a preparation method for a graphene heating film. Graphene powder is evenly scattered in an organic solvent by using an ultrasonic method, a stirring method and other methods to obtain a graphene solution with the concentration of 0.05mg/ml to 0.5mg/ml, the graphene evenly covers an organic filter film or a water-attributed filter film through a suction filtration method, the grapheme film and the filter film are separated through a mechanical stripping method or a soaking method or an organic solvent dissolving method, the graphene thin film is obtained, electrodes are added to the graphene thin film, and heat can be generated by applying voltages on the graphene thin film. According to the preparation method for the graphene heating film, the unique two-dimensional nano-structure, the characteristic of the large ratio of thickness to radial dimension and the characteristic of the high specific surface area of the graphene are utilized, through the preparation technology, evenly communicated conductive networks are formed among graphene sheet layers, and much heat can be generated by applying low voltages (1-10V). The preparation method for the graphene heating film has the advantages that the preparation process is simple and easy to control and free of pollution, and the size is adjustable, and the preparation method for the graphene heating film is suitable for 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, in fields such as modern architecture, heating engineering, decorations, is widely used.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 2004 prepare Graphene for the first time, the physical property of Graphene excellence has attracted numerous scholars' extensive concern.Graphene has good conductivity, and electron mobility is up to 2 * 10
5cm
2v
-1s
-1, than the high twice of the material indium antimonide of at present known carrier mobility maximum left and right.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 than zero dimension or one-dimensional electric material, more easily form conductive network in matrix.Above-mentioned these the excellent performances of Graphene, make it in field of electric heating, represent good application prospect, particularly transparent, pliable and tough thin film heater.
At present, relevant for the graphene transparent conductive film application report of display screen, vehicle window anti-icing equipment, heat insulation window and other heating systems out of doors.Compare with at present conventional carbon fiber felt heating element, when graphene film is used for electric heating element, there is appropriate resistivity, good thermal stability and excellent machine-shaping characteristic, more energy-efficient.The preparation technology that graphene film is conventional has hand brush, dipping, spraying, spin coating etc., yet these complicated process of preparation and heating efficiency are low.
Summary of the invention
For existing conventional graphene film complicated process of preparation, shortcoming that heating efficiency is low; the preparation method who the object of the invention is a kind of novel graphite alkene heating film; have preparation process simple and easy to control, the advantage such as pollution-free, size is adjustable, is applicable to large-scale production.
Technical scheme of the present invention is:
A preparation method for Graphene heating film, first, the Graphene of take is made as raw material, and graphene powder is dispersed in organic solvent, and obtaining concentration is the Graphene colloidal suspensions of 0.05mg/ml～0.5mg/ml; Then, the method by vacuum filtration is covered in graphene uniform on miillpore filter; Again Graphene is passed through to natural drying or heat drying together with miillpore filter, then obtain uniform and stable Graphene heating film by the method for mechanical stripping, immersion or organic solvent dissolution; On graphene film, add top electrode, apply voltage and can produce heat.
Described Graphene is Graphene prepared by intercalation stripping method, graphite oxidation reducing process or additive method.
The homodisperse method of described graphene powder is ultrasonic or stirring, and ultrasonic jitter 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 carrying out complicated processing to raw material, and manufacture process is simple, easy operating, and product is more even simultaneously, good stability.And can set according to actual needs the size of product.
(2) graphene film that prepared by the present invention is applied to field of electric heating, compares with existing conventional material with carbon element Electric radiant Heating Film, and 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
Fig. 1 is the electron scanning micrograph of the Graphene that uses 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) be embodiment 2.
Fig. 3 is the photo of graphene film prepared in the embodiment of the present invention 1.
Fig. 4 is the surface scan electron micrograph of the carbon fiber felt that uses in comparative example 1 of the present invention and comparative example 2.Wherein, (a) figure is comparative example 1; (b) be comparative example 2.
Fig. 5 is the heating curve of comparative example 1, comparative example 2, embodiment 1 and embodiment 2 samples.Wherein, (a) figure is comparative example 1; (b) be comparative example 2; (c) figure is embodiment 1; (d) be embodiment 2.
Embodiment
The preparation technology of Graphene heating film of the present invention is as follows: graphene powder is dispersed in organic solvent, and obtaining concentration is that 0.05mg/ml～0.5mg/ml(is preferably 0.1mg/ml～0.3mg/ml) Graphene colloidal suspensions; Method by vacuum filtration is covered in graphene uniform on organic filter membrane or water system filter membrane, again after natural drying or heat drying, the separated graphene film of method and filter membrane by mechanical stripping, immersion or organic solvent dissolution, obtain uniform and stable graphene film.On graphene film, add top electrode, apply 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, glass sand core filter, 1000ml～2000ml and connect flexible pipe used, fixture, vacuum pump used can be vacuum pump using circulatory water or oilless vacuum pump.Vacuum pump is connected with flexible pipe with filter flask, miillpore filter is put on glass sand core filter, press filter tunnel, with clip, clamp, go up solution, connect vacuum-pump power supply, start suction filtration, the pressure limit of vacuum filtration is 0.05MPa～0.2MPa, 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, pattern feature and the technical parameter of Graphene of the present invention are 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 μ m, thickness 1～5nm, in macroscopic view, show as the form of curling as shown in the figure, be rendered as fluffy cluster-shaped.
Described Graphene can be Graphene prepared by intercalation stripping method, graphite oxidation reducing process and additive method, the Graphene that the present invention uses is to be made 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 μ m, 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, below in conjunction with embodiment and accompanying drawing, be described in further detail.
The graphene powder that takes 9.375mg is put in beaker, adds absolute ethyl alcohol reagent 50mL, ultrasonic dispersion 1h, and obtaining concentration is the stable Graphene colloidal suspensions of homogeneous of 0.1875mg/mL.Graphene colloidal suspensions is placed on the miillpore filter of vacuum filtration device, adopting aperture is the Kynoar filter membrane of 0.45 μ m, and the pressure of vacuum filtration is 0.08MPa, and the time is 15min.After suction filtration completes, graphene film is placed in to the dry 24h of 45 ℃ of drying boxes together with filter membrane, then adopts the method for mechanical stripping, obtain graphene film.From Fig. 2 (a) and Fig. 3, can find out: the graphene film surface uniform that vacuum filtration obtains is smooth, lamella overlap joint closely.
Utilizing the surface density of the graphene film that the method makes is 15g/m
2, thickness is 0.05mm, and specific insulation is 0.0160 Ω cm, and surface resistivity is 2.0 Ω/sq.
Difference from Example 1 is, the graphene powder that takes 18.750mg is put in beaker, adds DMF reagent 100mL, ultrasonic dispersion 1h, and obtaining concentration is the stable Graphene colloidal suspensions of homogeneous of 0.1875mg/mL.Graphene colloidal suspensions is placed on the miillpore filter of vacuum filtration device, adopting aperture is the teflon membrane filter of 0.45 μ m, and the pressure of vacuum filtration is 0.15MPa, and the time is 35min.After suction filtration completes, graphene film is placed in to the dry 38h of 100 ℃ of drying boxes together with filter membrane, then adopts the method for mechanical stripping, obtain graphene film, from Fig. 2 (b), can find out: the graphene film surface uniform obtaining is smooth, lamella overlap joint closely.
Utilizing the surface density of the graphene film that the method makes is 30g/m
2, thickness is 0.10mm, and specific insulation is 0.0090 Ω cm, and surface resistivity is 1.0 Ω/sq.
Difference from Example 1 is, the graphene powder that takes 12.80mg is put in beaker, adds isopropyl alcohol reagent 100mL, ultrasonic dispersion 1h, and obtaining concentration is the stable Graphene colloidal suspensions of homogeneous of 0.1280mg/mL.Graphene colloidal suspensions is placed on the miillpore filter of vacuum filtration device, adopting aperture is conventional mixed ester membranes (the CN-CA film of 0.22 μ m, by PAA-CN-CA, made, 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 to the dry 12h of 40 ℃ of drying boxes together with filter membrane, the method that then adopts acetone soln to dissolve, obtains graphene film.
Utilizing the surface density of the graphene film that the method makes 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.
Difference from Example 1 is, the graphene powder that takes 21.50mg is put in beaker, adds DMF reagent 100mL, ultrasonic dispersion 1h, and obtaining concentration is the stable Graphene colloidal suspensions of homogeneous of 0.2150mg/mL.Graphene colloidal suspensions is placed on the miillpore filter of vacuum filtration device, adopting aperture is the teflon membrane filter of 0.45 μ m, and the pressure of vacuum filtration is 0.20MPa, and the time is 45min.After suction filtration completes, graphene film is placed in to the dry 38h of 100 ℃ of drying boxes together with filter membrane, then adopts the method for mechanical stripping, obtain graphene film.
Utilizing the surface density of the graphene film that the method makes 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 that Sichuan Jinlu Group Co., Ltd produces in the above-described embodiments, the Graphene being made through solid phase intercalation, high-temperature expansion by graphite powder (Fig. 1).In comparative example, carbon fiber felt used is that Shenyang Yu Heng carbon fiber Co., Ltd produces (Fig. 4).The heating data of measuring sample with reference to the method for testing of GB/T7287-2008, JG-T286-2010, specimen size is that 25mm * 25mm(is as Fig. 3).The voltage that sample applies is 1V～4V, by Fig. 5 (a), can be found out: 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 ℃; By Fig. 5 (b), can be found out: comparative example 2(surface density is 30g/m
2carbon fiber felt) caloric value under the applied voltage graphene film prepared with respect to the present invention be still less, when voltage is 4V, surface temperature is only 60.5 ℃; By Fig. 5 (c), can be found out: 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 of heater changes and reduces gradually, after reaching a certain stable temperature, no longer change, when voltage is 4V, the stable temperature that embodiment 1 sample reaches is 96 ℃; By Fig. 5 (d), can be found out: embodiment 2(surface density is 30g/m
2graphene film), its temperature changing regularity is similar with embodiment 1, when voltage is 4V, the stable temperature reaching is higher, is 118 ℃.
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 being evenly communicated with, can produce higher heat applying under lower voltage (1～10V).The advantages such as it is simple and easy to control that the present invention has preparation process, and pollution-free, size is adjustable, are applicable to large-scale production.
Claims (8)
1. a preparation method for Graphene heating film, is characterized in that: first, the Graphene of take is made as raw material, and graphene powder is dispersed in organic solvent, and obtaining concentration is the Graphene colloidal suspensions of 0.05mg/ml～0.5mg/ml; Then, the method by vacuum filtration is covered in graphene uniform on miillpore filter; Again Graphene is passed through to natural drying or heat drying together with miillpore filter, then obtain uniform and stable Graphene heating film by the method for mechanical stripping, immersion or organic solvent dissolution; On graphene film, add top electrode, apply voltage and can produce heat.
2. according to the preparation method of Graphene heating film claimed in claim 1, it is characterized in that, described Graphene is Graphene prepared by intercalation stripping method, graphite oxidation reducing process or additive method.
3. according to the preparation method of Graphene heating film claimed in claim 1, it is characterized in that, the homodisperse method of described graphene powder is ultrasonic or stirring, and ultrasonic jitter time is 5min～80min.
4. according to the preparation method of Graphene heating film claimed in 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 claimed in 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 claimed in 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 claimed in 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.
8. according to the preparation method of Graphene heating film claimed in claim 1, it is characterized in that, 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.
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| CN109152113B (en) * | 2018-09-20 | 2022-02-01 | 广东烯创科技有限公司 | Graphene-based electrothermal film, preparation method thereof, electric heating sheet and electric heating equipment |
| CN110089801B (en) * | 2019-05-24 | 2021-07-02 | 湖南云亭烯新材料科技有限公司 | Graphite alkene pressure-sensitive shoes that generate heat |
| CN110089801A (en) * | 2019-05-24 | 2019-08-06 | 湖南云亭烯新材料科技有限公司 | A kind of pressure-sensitive heating shoes of graphene |
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| CN110473670A (en) * | 2019-07-09 | 2019-11-19 | 广东工业大学 | A kind of manufacturing method of nano conductive film |
| CN111432508A (en) * | 2020-04-15 | 2020-07-17 | 威海无缝新材料有限公司 | Graphene fast heating film and preparation method thereof |
| CN112291868A (en) * | 2020-09-14 | 2021-01-29 | 兰州大学 | Self-annealing graphene self-supporting high-temperature electrothermal film and preparation method thereof |
| CN112291868B (en) * | 2020-09-14 | 2021-12-14 | 兰州大学 | Self-annealing graphene self-supporting high-temperature electrothermal film and preparation method thereof |
| CN112804775A (en) * | 2021-01-18 | 2021-05-14 | 安徽宇航派蒙健康科技股份有限公司 | Method for preparing electrothermal film by adopting transparent graphene |
| CN115849361A (en) * | 2023-01-10 | 2023-03-28 | 南京信息工程大学 | Graphene oxide felt and preparation method thereof |
| CN115849361B (en) * | 2023-01-10 | 2024-04-30 | 南京信息工程大学 | Graphene oxide felt and preparation method thereof |
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