CN102166844B - Graphene/graphene oxide composite membrane and preparation method thereof - Google Patents
Graphene/graphene oxide composite membrane and preparation method thereof Download PDFInfo
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- CN102166844B CN102166844B CN 201010607319 CN201010607319A CN102166844B CN 102166844 B CN102166844 B CN 102166844B CN 201010607319 CN201010607319 CN 201010607319 CN 201010607319 A CN201010607319 A CN 201010607319A CN 102166844 B CN102166844 B CN 102166844B
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Abstract
The invention provides a graphene/graphene oxide composite membrane which is composed of a graphene layer and a graphene oxide layer, wherein the thickness of each layer is 50 nanometers-1 millimeter. The preparation method of the graphene/graphene oxide composite membrane comprises the following steps of: putting a graphene oxide solution into a container for filtering or evaporating to obtain a graphene oxide membrane; and putting a graphene solution into the container containing the graphene oxide membrane for filtering or evaporating to obtain the graphene/graphene oxide composite membrane. The membrane has excellent mechanical properties and has a very strong response characteristic to temperature or humidity; and by the characteristic, the graphene//graphene oxide composite membrane can be applied on a micro-actuator or sensor.
Description
Technical field
The invention belongs to the rare material technology of graphite field, relate in particular to a kind of graphene/graphene oxide composite membrane and preparation method thereof.
Background technology
The appearance of CNT and Graphene has stimulated people its physics and mechanical property to be applied to the very big interest of device.Confirmed that in theory and experimentally they have very high hardness and intensity.Also have in addition very high electrical conductivity and thermal conductivity.Unique mechanics and physical property make them obtain widely research in device miscellaneous.
Many research groups are obtaining remarkable achievement aspect the microactrator of CNT, but the research based on the microactrator of full grapheme material and sensor aspect is relatively less, Small 2009,6,210 have introduced a kind of material that comprises CNT/graphene oxide composite membrane, and this material demonstrates good humiture sensitivity.But carbon nanotube layer is comprised of nano-material, and the graphene oxide layer is comprised of the nano flake material, thereby the associativity of materials at two layers is poor, and electrical conductivity is not high.
Summary of the invention
Goal of the invention:In order to solve the poor shortcoming of associativity of the materials at two layers that prior art exists, the purpose of this invention is to provide a kind of graphene/graphene oxide composite membrane and preparation method thereof, because materials at two layers is graphene-based material, the composite membrane associativity of preparation is good.
Technical scheme:A kind of graphene/graphene oxide composite membrane is composited by graphene layer and graphene oxide layer, and every layer thickness is between 50 nanometers-1 millimeter.
The preparation method who prepares described graphene/graphene oxide composite membrane, concrete steps are:
The first step: get graphite oxide 1 mass parts and be dissolved in 10～100000 mass parts solvents, ultrasonic or stirred 0.2～5 hour, obtain graphene oxide solution.Described solvent is any one in water, alcohol or the chloroform.
Second step: place container filtration or evaporation to obtain into the graphene oxide film graphene oxide solution.Filter type is during negative pressure leaching or normal pressure filter.The formula of described evaporation side is atmospheric evaporation or negative pressure evaporation; The temperature range of described evaporation is 0-100 degree centigrade.The implication of normal pressure is an atmospheric pressure.
The 3rd step: the graphene solution of getting mass parts 10～100000 places the container that the graphene oxide film is housed, through filtering or evaporation acquisition graphene/graphene oxide composite membrane.The atomic ratio of carbon ratio oxygen is greater than 3 in the composition of described Graphene.The mass percent concentration of described graphene solution is 0.01% ~ 10%.
Beneficial effect:Compared with prior art, the present invention has following characteristics:
The present invention utilizes suction filtration or evaporation to obtain the composite membrane of graphene/graphene oxide, and this film has good mechanical performance, simultaneously has very strong response characteristic for temperature or humidity, and the crimp force that causes owing to high temperature or high humility is quite large; The amount of crimp that different temperature or humidity cause is also different large.When temperature or humidity reduction, the flattening gradually of this film has good repeatability in addition.This characteristic so that Graphene can be applied on microactrator or the sensor.
Description of drawings
Fig. 1 is structural representation of the present invention, and 1 is graphene layer among the figure, and 2 is the graphene oxide layer.
The specific embodiment
The invention will be further described below in conjunction with example:
A kind of graphene/graphene oxide composite membrane is composited by graphene layer 1 and graphene oxide layer 2, and every layer thickness is between 50 nanometers-1 millimeter.
Embodiment 1
The first step takes by weighing 0.01 gram graphite oxide, puts into the beaker that fills 1000 gram water, ultrasonic 30 minutes, obtains uniform graphite oxide solution.
Second step places pumping and filtering device with gained graphite oxide aqueous solution, utilizes negative pressure to filter, and obtains the graphene oxide film.
The 3rd step, get carbon-to-oxygen ratio and be 5, mass concentration is the 0.02%(Graphene) Graphene chloroformic solution 100 grams place the above-mentioned suction filtration device that the graphene oxide film is housed, utilize negative pressure leaching, obtain the graphene/graphene oxide film, the thickness of two membranes is 10 microns.Through test, this film to response time of humiture all less than 1 second, but repeated flex stretches more than 1000 times.
Embodiment 2
The first step takes by weighing 1 gram graphite oxide, puts into the beaker that fills 10 gram alcohol, and ultrasonic 5h obtains uniform graphite oxide solution.
Second step places the glass culture dish atmospheric evaporation with gained graphene oxide alcoholic solution, and 100 degrees centigrade of evaporating temperatures obtain the graphene oxide film.
The 3rd step, get carbon-to-oxygen ratio and be 20, mass concentration is the 10%(Graphene) graphene aqueous solution 10 grams place the above-mentioned culture dish that the graphene oxide film is housed, utilize negative pressure evaporation, obtain the graphene/graphene oxide film, the thickness of two membranes is respectively 0.8 millimeter and 0.4 millimeter.Through test, this film to response time of humiture all less than 1.5 seconds, but repeated flex stretches more than 1000 times.
Embodiment 3
The first step takes by weighing 0.5 gram graphite oxide, puts into the beaker that fills 50 gram chloroforms, ultrasonic 10 minutes, obtains uniform graphite oxide solution.
Second step places normal atmosphere filter with gained graphene oxide chloroformic solution, obtains the graphene oxide film.
The 3rd step, get carbon-to-oxygen ratio and be 50, mass concentration is the 1%(Graphene) Graphene alcoholic solution 10 grams place the above-mentioned filter that the graphene oxide film is housed, utilize atmospheric evaporation, obtain the graphene/graphene oxide film, the thickness of two membranes is respectively 100 microns and 50 microns.Through test, this film to response time of humiture all less than 0.8 second, but repeated flex stretches more than 1000 times.
Claims (5)
1. prepare the method for graphene/graphene oxide composite membrane, it is characterized in that, concrete steps are:
The first step: get graphene oxide 1 mass parts and be dissolved in 10～100000 mass parts solvents, ultrasonic or stirred 0.2～5 hour, obtain graphene oxide solution;
Second step: place container to filter or evaporation acquisition graphene oxide film graphene oxide solution;
The 3rd step: the graphene solution of getting mass parts 10～100000 places the container that the graphene oxide film is housed, through filtering or evaporation acquisition graphene/graphene oxide composite membrane, described graphene/graphene oxide composite membrane, be composited by graphene layer (1) and graphene oxide layer (2), every layer thickness is between 50 nanometers-1 millimeter.
2. prepare as claimed in claim 1 the method for graphene/graphene oxide composite membrane, it is characterized in that: solvent is any one in water, alcohol or the chloroform in the step 1.
3. prepare as claimed in claim 1 the method for graphene/graphene oxide composite membrane, it is characterized in that: filter type is that negative pressure leaching or normal pressure filter.
4. prepare as claimed in claim 1 the method for graphene/graphene oxide composite membrane, it is characterized in that: evaporation mode is atmospheric evaporation or negative pressure evaporation, and the evaporating temperature scope is 0-100 degree centigrade.
5. prepare as claimed in claim 1 the method for graphene/graphene oxide composite membrane, it is characterized in that: the atomic ratio of carbon ratio oxygen is greater than 3 in the Graphene; The mass percent concentration of graphene solution is 0.01% ~ 10%.
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| CN 201010607319 CN102166844B (en) | 2010-12-28 | 2010-12-28 | Graphene/graphene oxide composite membrane and preparation method thereof |
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| CN 201010607319 CN102166844B (en) | 2010-12-28 | 2010-12-28 | Graphene/graphene oxide composite membrane and preparation method thereof |
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| CN102166844A CN102166844A (en) | 2011-08-31 |
| CN102166844B true CN102166844B (en) | 2013-02-27 |
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| GB201214565D0 (en) | 2012-08-15 | 2012-09-26 | Univ Manchester | Membrane |
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| CN103779081A (en) * | 2012-10-23 | 2014-05-07 | 海洋王照明科技股份有限公司 | Graphene/graphene oxide thin film and preparation method thereof, and usage |
| CN103779082A (en) * | 2012-10-23 | 2014-05-07 | 海洋王照明科技股份有限公司 | Graphene/graphene oxide thin film and preparation method thereof, and super capacitor |
| CN103253655B (en) * | 2013-04-15 | 2015-04-29 | 中国科学院宁波材料技术与工程研究所 | Compound graphene with scattering scale and preparation method thereof |
| CN103349919A (en) * | 2013-07-09 | 2013-10-16 | 福州大学 | Graphene-semiconductor particle compound filter membrane with self-cleaning function |
| CN103639084B (en) * | 2013-12-16 | 2015-09-30 | 电子科技大学 | A kind of rush-harvesting and rush-planting based on the non-functional material that dissolves each other sprays composite film preparation technology altogether |
| CN104383879B (en) * | 2014-11-20 | 2016-11-09 | 东南大学 | Preparation method based on the functional extrusion coating paper that graphene oxide is modified |
| CN106145094B (en) * | 2015-03-13 | 2019-06-14 | 中国科学院上海应用物理研究所 | A kind of graphene-inorganic nanoparticles composite membrane and preparation method thereof |
| TWI642621B (en) * | 2015-05-29 | 2018-12-01 | National Taiwan University Of Science And Technology | Composite carbon material and method of preparing the same |
| CN105136860A (en) * | 2015-07-24 | 2015-12-09 | 浙江大学 | Humidity sensor based on graphene oxide/graphene/silicon and preparation method thereof |
| CN105582751B (en) * | 2015-12-17 | 2018-05-22 | 常州碳星科技有限公司 | Filter core and its preparation method and application |
| CN105883781B (en) * | 2016-03-09 | 2018-10-30 | 王祉豫 | A kind of preparation method of large area redox graphene film |
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| CN106082199B (en) * | 2016-06-21 | 2018-07-31 | 山东赛帝格新材料有限责任公司 | A kind of graphene composite film and preparation method thereof |
| CN106587016A (en) * | 2016-12-08 | 2017-04-26 | 南京信息职业技术学院 | Oxidized graphene humidity response actuator and preparation method thereof |
| CN106698405A (en) * | 2017-01-12 | 2017-05-24 | 东南大学 | Method for preparing large-area graphene paper by utilizing hydroiodic acid |
| CN107010617B (en) * | 2017-04-27 | 2019-06-21 | 北京化工大学 | A kind of preparation method of pair of temperature, humidity quick response Janus structure graphite alkene film |
| CN208078031U (en) | 2017-12-29 | 2018-11-09 | 云谷（固安）科技有限公司 | Encapsulating structure and display device including encapsulating structure |
| CN108900111A (en) * | 2018-08-07 | 2018-11-27 | 同天（福建）石墨烯科技有限公司 | A kind of preparation method of graphene-based twin crystal state microactrator |
| CN110449039B (en) * | 2019-08-16 | 2021-08-03 | 宁波石墨烯创新中心有限公司 | Graphene/graphene oxide-based separation membrane and preparation method thereof |
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| CN201941193U (en) * | 2010-12-28 | 2011-08-24 | 东南大学 | Graphene/graphene oxide compound film |
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| US8574681B2 (en) * | 2007-05-14 | 2013-11-05 | Northwestern University | Ceramic composite thin films |
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