CN108383112A - A kind of high heat graphene heating film and preparation method thereof - Google Patents
A kind of high heat graphene heating film and preparation method thereof Download PDFInfo
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- CN108383112A CN108383112A CN201810526754.9A CN201810526754A CN108383112A CN 108383112 A CN108383112 A CN 108383112A CN 201810526754 A CN201810526754 A CN 201810526754A CN 108383112 A CN108383112 A CN 108383112A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/24—Thermal properties
Abstract
The invention discloses a kind of high heat graphene heating films and preparation method thereof.Carbon nano-tube solution and graphene oxide solution are carried out ultrasonic disperse by the present invention respectively, it is made to be uniformly dispersed, and are then hybridly prepared into mixed aqueous solution, and naturally dry after solution film forming obtains graphene oxide carbon nano-tube compound film；Even application deionized water is carried out in gained composite film surface, surface swelling is allowed to, then multiple composite membrane through-thickness bonds together；It is placed on baking oven drying；Then by obtained composite membrane, high temperature heat-treats under inertia or reducing atmosphere protection, obtains high heat graphene heating film.The thickness of the high heat graphene heating film is 1 μm 20 μm, and 900 DEG C can be warming up in 30s, is had broad application prospects.
Description
Technical field
The invention belongs to thermo electric material technical field, a kind of high heat graphene heating film and its preparation are related in particular to
Method.
Background technology
Two dimensional crystal material-the graphene being made of single carbon atom layer, is most thin in known materials, is referred to as mystery
Material, started global research boom.Graphene has excellent electric property, heat conductivility outstanding, extraordinary ratio
Surface area, Young's modulus and fracture strength.The excellent electrical and thermal conductivity performance of graphene is well beyond metal, while graphene has
There is the advantages of corrosion-and high-temp-resistant, and its good mechanical performance and lower density more allow it to have in thermo electric material field
The potentiality of substituted metal.Since graphene large-scale processing is increasingly becoming reality, graphene film applies substituted metal material
Different fields.
Electrical resistor heating element in common electric heating system generally uses metal foil, film coating, resistance wire, metal mesh etc.
Material.Most commonly used heating element is nichrome.However, for nichrome, still seem in the following areas at present not
Foot：The density of nichrome is more than 8g/cm3, thickness has several millimeters when use；Resistivity is low, however it remains electric thermal conversion efficiency
Rate is low, and the rate of heat addition is small, and heating element does not have automatic constant-temperature and power back-off function so that electric heating system is complicated, and heat is used
Property it is big the deficiencies of place；Ferrum-chromium-aluminum is Alfer, and there are the high temperature of cold-shortness, 475 DEG C of brittleness and 1000 DEG C or more is crisp
Property, it is short to eventually lead to heating element service life since elevated temperature strength caused by high-temperature brittleness is low；The solderability of alloy is very poor, difficult
It repairs.On the whole, it is badly in need of the high heat membrane material that exploitation is efficient, high speed, low-density, stability are good, flexibility is good at present.
Invention content
It is an object of the invention to solve the above-mentioned problems in the prior art, a kind of system of graphene heating film is provided
Preparation Method, the present invention can greatly improve thermal conductivity, flexibility, electric conductivity and the stability of graphene heating film.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of preparation method of high heat graphene heating film, which is characterized in that the preparation method comprises the following steps：
(1) carbon nano-tube solution and graphene oxide solution are subjected to ultrasonic disperse respectively, it is made to be uniformly dispersed, then mixed
It closes, is configured to mixed aqueous solution, naturally dry after solution film forming obtains graphene oxide carbon nano-tube compound film；
(2) film surface obtained by step (1) carries out even application deionized water, is allowed to surface swelling, then answers multiple
Film through-thickness is closed to bond together；
(3) film obtained by step (2) is placed on baking oven drying；
(4) film for obtaining step (3) high temperature under inertia or reducing atmosphere protection heat-treats, and obtains high heat graphite
Alkene heating film.
The thickness for the graphene oxide carbon nano-tube compound film that the step (1) is prepared is 1 μm -20 μm.
A concentration of 1-10mg/ml of carbon nano-tube solution, a concentration of 1- of graphene oxide solution in the step (1)
15mg/ml。
The ultrasonic time is 20-120min, ultrasonic power 100-500W in the step (1).
The temperature of step (4) the high temperature thermal reduction is 800-1500 DEG C, and heat treatment time is 1-5 hours.
Inert atmosphere is argon gas, nitrogen or helium in the step (4), and reducing atmosphere is hydrogen.
A kind of high heat graphene heating film being prepared using above-mentioned preparation method, preparation-obtained high heat
Graphene heating film can be warming up to 900 DEG C in 30s.
Advantage of the invention is that：
1, in the graphene heat conducting film for preparing of the present invention can effective dispersed graphite alkene lamella, good heat conductivity；
2, graphene heat conducting film raw material sources prepared by the present invention are abundant, and the membrane material of preparation is at low cost, ultralight ultra-thin, easily
Processing meets various sizes requirement, at low cost without carrying out high temperature cabonization, graphitization processing；
3, the thickness of high heat graphene heating film prepared by the present invention is 1 μm -20 μm, and 900 can be warming up in 30s
DEG C, temperature tolerance is good, there is certain flexibility, there is huge application prospect.
Specific implementation mode
Embodiment 1
A kind of preparation method of high heat graphene heating film, which is characterized in that the preparation method comprises the following steps：
(1) carbon nano-tube solution and graphene oxide solution are subjected to ultrasonic disperse respectively, it is made to be uniformly dispersed, then mixed
It closes, is configured to mixed aqueous solution, naturally dry after solution film forming obtains graphene oxide carbon nano-tube compound film；
(2) film surface obtained by step (1) carries out even application deionized water, is allowed to surface swelling, then answers multiple
Film through-thickness is closed to bond together；
(3) film obtained by step (2) is placed on baking oven drying；
(4) film for obtaining step (3) high temperature under inertia or reducing atmosphere protection heat-treats, and obtains high heat graphite
Alkene heating film.
The thickness for the graphene oxide carbon nano-tube compound film that the step (1) is prepared is 1 μm.The step (1)
A concentration of 1mg/ml of middle carbon nano-tube solution, a concentration of 1mg/ml of graphene oxide solution.It is ultrasonic in the step (1)
Time is 20min, ultrasonic power 100W.The temperature of step (4) the high temperature thermal reduction is 800 DEG C, heat treatment time 1
Hour.Inert atmosphere is argon gas in the step (4), and reducing atmosphere is hydrogen.
The high heat graphene heating film being prepared using above-mentioned preparation method can be warming up to 900 DEG C in 30s.
Embodiment 2
A kind of preparation method of high heat graphene heating film, which is characterized in that the preparation method comprises the following steps：
(1) carbon nano-tube solution and graphene oxide solution are subjected to ultrasonic disperse respectively, it is made to be uniformly dispersed, then mixed
It closes, is configured to mixed aqueous solution, naturally dry after solution film forming obtains graphene oxide carbon nano-tube compound film；
(2) film surface obtained by step (1) carries out even application deionized water, is allowed to surface swelling, then answers multiple
Film through-thickness is closed to bond together；
(3) film obtained by step (2) is placed on baking oven drying；
(4) film for obtaining step (3) high temperature under inertia or reducing atmosphere protection heat-treats, and obtains high heat graphite
Alkene heating film.
The thickness for the graphene oxide carbon nano-tube compound film that the step (1) is prepared is 20 μm.The step (1)
A concentration of 10mg/ml of middle carbon nano-tube solution, a concentration of 15mg/ml of graphene oxide solution.It is ultrasonic in the step (1)
Time be 120min, ultrasonic power 500W.The temperature of step (4) high temperature thermal reduction is 1500 DEG C, when heat treatment
Between be 5 hours.Inert atmosphere is argon gas in the step (4), and reducing atmosphere is hydrogen.
The high heat graphene heating film being prepared using above-mentioned preparation method can be warming up to 900 DEG C in 30s.
Embodiment 3
A kind of preparation method of high heat graphene heating film, which is characterized in that the preparation method comprises the following steps：
(1) carbon nano-tube solution and graphene oxide solution are subjected to ultrasonic disperse respectively, it is made to be uniformly dispersed, then mixed
It closes, is configured to mixed aqueous solution, naturally dry after solution film forming obtains graphene oxide carbon nano-tube compound film；
(2) film surface obtained by step (1) carries out even application deionized water, is allowed to surface swelling, then answers multiple
Film through-thickness is closed to bond together；
(3) film obtained by step (2) is placed on baking oven drying；
(4) film for obtaining step (3) high temperature under inertia or reducing atmosphere protection heat-treats, and obtains high heat graphite
Alkene heating film.
The thickness for the graphene oxide carbon nano-tube compound film that the step (1) is prepared is 10 μm.The step (1)
A concentration of 5mg/ml of middle carbon nano-tube solution, a concentration of 10mg/ml of graphene oxide solution.It is ultrasonic in the step (1)
Time be 80min, ultrasonic power 300W.The temperature of step (4) the high temperature thermal reduction is 1000 DEG C, heat treatment time
It is 3 hours.Inert atmosphere is argon gas in the step (4), and reducing atmosphere is hydrogen.
The high heat graphene heating film being prepared using above-mentioned preparation method can be warming up to 900 DEG C in 30s.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (7)
1. a kind of preparation method of high heat graphene heating film, which is characterized in that the preparation method comprises the following steps：
(1) carbon nano-tube solution and graphene oxide solution are subjected to ultrasonic disperse respectively, it are made to be uniformly dispersed, then mixed,
It is configured to mixed aqueous solution, naturally dry after solution film forming obtains graphene oxide carbon nano-tube compound film；
(2) film surface obtained by step (1) carries out even application deionized water, surface swelling is allowed to, then by multiple composite membranes
Through-thickness bonds together；
(3) film obtained by step (2) is placed on baking oven drying；
(4) film for obtaining step (3) high temperature under inertia or reducing atmosphere protection heat-treats, and obtains high heat graphene hair
Hotting mask.
2. preparation method according to claim 1, which is characterized in that the graphene oxide that the step (1) is prepared
The thickness of carbon nano-tube compound film is 1 μm -20 μm.
3. preparation method as described in claim 1, which is characterized in that carbon nano-tube solution is a concentration of in the step (1)
1-10mg/ml, a concentration of 1-15mg/ml of graphene oxide solution.
4. preparation method as described in claim 1, which is characterized in that the ultrasonic time is 20- in the step (1)
120min, ultrasonic power 100-500W.
5. preparation method as described in claim 1, which is characterized in that the temperature of step (4) high temperature thermal reduction is
800-1500 DEG C, heat treatment time is 1-5 hours.
6. preparation method as described in claim 1, which is characterized in that in the step (4) inert atmosphere be argon gas, nitrogen or
Helium, reducing atmosphere are hydrogen.
7. a kind of high heat graphene heating film being prepared using claim 1-6 any one of them preparation methods,
It is characterized in that, preparation-obtained high heat graphene heating film can be warming up to 900 DEG C in 30s.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2018103209322 | 2018-04-11 | ||
| CN201810320932 | 2018-04-11 |
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| CN108383112A true CN108383112A (en) | 2018-08-10 |
Family
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| CN201810526754.9A Pending CN108383112A (en) | 2018-04-11 | 2018-05-29 | A kind of high heat graphene heating film and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109330058A (en) * | 2018-12-20 | 2019-02-15 | 四川省安德盖姆石墨烯科技有限公司 | A kind of graphene heating knee pad |
| CN111601407A (en) * | 2020-05-08 | 2020-08-28 | 安徽宇航派蒙健康科技股份有限公司 | Graphene heating film for electric heating picture and preparation method thereof |
| CN111609454A (en) * | 2020-05-08 | 2020-09-01 | 安徽宇航派蒙健康科技股份有限公司 | Electric heating picture and preparation method thereof |
| CN111654929A (en) * | 2020-05-08 | 2020-09-11 | 安徽宇航派蒙健康科技股份有限公司 | Graphene heating body for electric heating picture and preparation method thereof |
| CN111978931A (en) * | 2020-08-27 | 2020-11-24 | 清华大学深圳国际研究生院 | Graphene composite slurry, graphite heat dissipation film structure and preparation method thereof |
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| CN102674315A (en) * | 2012-04-25 | 2012-09-19 | 浙江大学 | Graphene-carbon nano tube composite all-carbon ultra-light elastic aerogel and preparation method thereof |
| CN103725263A (en) * | 2013-12-17 | 2014-04-16 | 张家港康得新光电材料有限公司 | Film made from graphene-carbon nanotube composite material and preparation method of film |
| CN105826571A (en) * | 2016-05-26 | 2016-08-03 | 江苏深苏电子科技有限公司 | Method for preparing flexible high-conductivity graphene and carbon nano tube composite current collector |
| CN107140619A (en) * | 2017-05-27 | 2017-09-08 | 杭州高烯科技有限公司 | A kind of graphene thick film of high heat conduction and preparation method thereof |
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| CN102674315A (en) * | 2012-04-25 | 2012-09-19 | 浙江大学 | Graphene-carbon nano tube composite all-carbon ultra-light elastic aerogel and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109330058A (en) * | 2018-12-20 | 2019-02-15 | 四川省安德盖姆石墨烯科技有限公司 | A kind of graphene heating knee pad |
| CN111601407A (en) * | 2020-05-08 | 2020-08-28 | 安徽宇航派蒙健康科技股份有限公司 | Graphene heating film for electric heating picture and preparation method thereof |
| CN111609454A (en) * | 2020-05-08 | 2020-09-01 | 安徽宇航派蒙健康科技股份有限公司 | Electric heating picture and preparation method thereof |
| CN111654929A (en) * | 2020-05-08 | 2020-09-11 | 安徽宇航派蒙健康科技股份有限公司 | Graphene heating body for electric heating picture and preparation method thereof |
| CN111609454B (en) * | 2020-05-08 | 2022-04-08 | 安徽宇航派蒙健康科技股份有限公司 | Electric heating picture and preparation method thereof |
| CN111654929B (en) * | 2020-05-08 | 2022-07-29 | 安徽宇航派蒙健康科技股份有限公司 | Graphene heating body for electric heating picture and preparation method thereof |
| CN111601407B (en) * | 2020-05-08 | 2023-02-17 | 安徽宇航派蒙健康科技股份有限公司 | Graphene heating film for electric heating picture and preparation method thereof |
| CN111978931A (en) * | 2020-08-27 | 2020-11-24 | 清华大学深圳国际研究生院 | Graphene composite slurry, graphite heat dissipation film structure and preparation method thereof |
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Application publication date: 20180810 |