CN103183340A - Ultra-high-modulus and high-strength oxidized graphene film and preparation method thereof - Google Patents
Ultra-high-modulus and high-strength oxidized graphene film and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of nano function materials, and relates to an ultra-high-modulus and high-strength oxidized graphene film and a preparation method thereof. Oxidized graphene film is prepared from at least the following three raw materials: oxidized graphene, a treating agent with a catechol structure and a cross-linking agent; and oxidized graphene can also contain other components. The oxidized graphene film has the characteristics of macroscopic size, ultra high modulus and high strength. The raw materials of oxidized graphene are obtained by using the modified Hummers method; the treating agent is a small molecule substance with the catechol structure, such as dopamine; and the cross-linking agent is substance with multiple reactive groups, such as polyetherimide. The method has the advantages that oxidized graphene is cheap and easy to get, and has biocompatibility; and the obtained enhanced film has an excellent mechanics property, and has wide application prospects in aspects of packaging, separating, supercapacitors, electric conduction and heat conduction and the like.
Description
Technical field
The invention belongs to the nano-functional material technical field, relate to a kind of ultra high modulus and high-intensity graphene oxide film and preparation method thereof, at least obtained by following three kinds of feedstock production: graphene oxide, contain the agent of catechol structure treatment, linking agent, also can contain other components.The characteristics of this graphene oxide film are the size macroscopic view, and have ultra high modulus and high strength.
Background technology
Thin-film material is the indispensable part of modern science and technology, is widely used in separation, electronic apparatus and fields such as micro-nano electron device, protective layer and adhesion layer.Based on the inorganic thin film material of nano components successful commercial applications, be mainly used in aspects such as high-temperature adhesives, protective layer, high heat-conductivity conducting, as peel off the film of quartz plate.
Graphene oxide (Graphene Oxide) is a kind of monolayer carbon atom two-dimensional material that contains multiple oxy radical, by sp
2A large amount of oxy radicals on hydridization carbon atom conjugate planes and surface thereof and the edge (hydroxyl, carboxyl, epoxy group(ing) etc.) are formed, it has specific surface area and the excellent mechanical property of super large, the existing application widely at aspects such as polymer composites, electromagnetism device, biological medicines.
Graphene oxide mainly is the graphite oxide that obtains by the strong acid graphite oxide, graphite layers is apart from being increased to 7 ~ 10 by 3.35 before the oxidation in the graphite oxide, and show as wetting ability, through heating or in water ultrasonic peeling off, be easy to form the graphene oxide laminated structure of separation.
The graphene oxide sheet of individual layer has extremely high Young's modulus (200-500 GPa) and breaking tenacity (63 GPa), still, the limitation of size of its Nano grade it as the application of macroscopic material.Recent study finds that graphene oxide can form macroscopical graphene oxide film by simple suction filtration or in the liquid-gas interface self-assembly.Because the hydrogen bond action of graphene oxide sheet interlayer, pure graphene oxide film itself has certain mechanical property.But, the various graphene oxide films of reporting in the present document, Young's modulus is usually at 6-42 GPa, and tensile strength well below mono-layer graphite oxide alkene sheet, can't embody its performance advantage at 76-293 MPa.Therefore, the mechanical property by chemistry or physical crosslinking method enhancing graphene oxide film is a kind of suitable, efficient manner.
Summary of the invention
The present invention relates to a kind of ultra high modulus and high-intensity graphene oxide film and preparation method thereof, obtained by following three kinds of feedstock production at least: graphene oxide, contain the agent of catechol structure treatment, linking agent also can contain other components.The characteristics of this graphene oxide film are the size macroscopic view, and have ultra high modulus and high strength.Employed graphene oxide among the present invention, be from expanded graphite, utilizing the Hummers method oxidation of modification to prepare gained, also can be the graphene oxide that utilizes other method such as Brodie method, Staudenmaier method, Hummers method and carry out improved prepared in various methods on this basis.
Contain the agent of catechol structure treatment among the present invention, for having the catechol small molecules derivative of adjacent diphenol structure, be specially the derivative of hydrochloride, suprarenin, chlorogenic acid or the above-mentioned substance of Dopamine HCL.The catechol structure is become the quinoid structure by airborne dioxygen oxidation under alkaline condition, simultaneously, benzene ring structure forms free radical, concurrently is conigenous poly-ly, is coated on the graphene oxide surface, and the quinoid structure becomes the catechol structure again after the acidity washing.
Employed linking agent among the present invention, for molecular weight be 500-50000 have a polyamino oligopolymer linking agent, be specially polyetherimide amine oligomer, polypropylene amine oligopolymer etc.The catechol structure is oxidized to the quinoid structure under alkaline condition, with amino Mike's that addition or schiff base reaction take place easily, thereby form the chemical bond crosslinking structure, plays enhancement.
In the material of the present invention, also can use various other auxiliary agents, as pH buffer reagent, oxygenant, reductive agent etc., not influence the performance of institute's invention material, and use according to practical situation.Dispersiveness after several main components composition (mass parts) ratios are handled by graphene oxide among the present invention and the mechanical strength of graphene oxide film determine.
The ratio of quality and the number of copies of graphene oxide, catechol structure class treatment agent and linking agent is for example following:
100 parts of graphene oxides,
Contain catechol structure treatment agent 0.01-100 part,
Linking agent 0.01-200 part.
On the preparation method, following steps are arranged:
(1) expanded graphite is made the dispersion graphene oxide; Utilize the Hummers method oxidation of modification to make graphene oxide expanded graphite, (Tris, 10mM) ultra-sonic dispersion 30 minutes in the buffered soln obtains stable dispersion system to get the Tutofusin tris that a certain amount of graphene oxide (GO) places pH8.5.
(2) with graphene oxide with containing catechol structure treatment agent dispersion treatment; In ice-water bath, add and contain the agent of catechol structure treatment, dissolving in ultrasonic 10 minutes, transposition magnetic agitation 24h again, suction filtration, earlier be washed to neutrality again with pickling, place the dry acquisition of 25 ℃ of vacuum drying ovens through containing the graphene oxide (PGO) that the agent of catechol structure treatment is handled.
(3) graphene oxide (PGO) through containing catechol structure treatment agent processing that step (2) is obtained mixes in pH neutral buffered soln with linking agent; Get a certain amount of PGO at phosphoric acid salt (PBS, the 0.2M Na of pH7.0
2HPO
4/ 0.2M NaH
2PO
4=19/31) ultra-sonic dispersion 1h in the buffered soln obtains stable dispersion system.Adding pH7.0 is dissolved with the PBS buffered soln of polyetherimide (Polyetherimide, PEI, molecular weight 600), and ultrasonic mixing 1h, suction filtration obtain uncrosslinked PGO+PEI composite membrane.
(4) with the PGO+PEI composite membrane crosslinked graphene oxide film that makes enhancing under the ealkaline buffer condition that obtains in the step (3); Composite membrane is placed the Tris buffered soln of pH8.5, make PEI with contain the agent of catechol structure treatment take place crosslinked, the graphene oxide film that is enhanced.
Embodiment
The present invention is further elaborated by the following examples, wherein forms umber, content all by weight.
Embodiment 1
100 parts of graphene oxides (GO) are placed the Tutofusin tris of pH8.5, and (Tris 10mM) in the buffered soln ultrasonic 30 minutes, is configured to the stable dispersion that concentration is 0.5 mg/mL.In ice-water bath, add 50 parts of dopamine hydrochlorides, dissolving in ultrasonic 10 minutes, transposition magnetic agitation 24h again, suction filtration is washed to neutrality again with pickling earlier, places that 25 ℃ of vacuum drying ovens are dry to obtain the graphene oxide (PGO) that Dopamine HCLs are handled.Get 92.5 parts of PGO at phosphoric acid salt (PBS, the 0.2M Na of pH7.0
2HPO
4/ 0.2M NaH
2PO
4=19/31) ultra-sonic dispersion 1h in the buffered soln obtains stable dispersion system.Adding pH7.0 is dissolved with the PBS buffered soln of 7.5 parts of polyetherimides (Polyetherimide, PEI, molecular weight 600), and ultrasonic mixing 1h, suction filtration obtain uncrosslinked PGO+PEI composite membrane.Place the Tris buffered soln of pH8.5 to soak 30 minutes composite membrane, it is crosslinked that PEI and poly-Dopamine HCL are taken place, the graphene oxide film that is enhanced.Film is cut into rectangular specimen carries out Elongation test, with respect to pure graphene oxide suction filtration film, the modulus of this enhanced film and intensity have improved 159.5% and 44.9% respectively.
Embodiment 2
Other are with embodiment 1, and the ratio of GO and Dopamine HCL treatment agent changes 100 parts and 80 parts into, and the final crosslinked film that obtains is with respect to pure graphene oxide suction filtration film, and modulus and intensity have improved 202% and 35% respectively.
Embodiment 3
Other are with embodiment 1, and the ratio of PGO and PEI changes 85 parts and 15 parts into, and with respect to pure graphene oxide suction filtration film, the modulus of this enhanced film and intensity have improved 297.7% and 50.8% respectively.
Embodiment 4
Other are with embodiment 1, and the ratio of PGO and PEI changes 70 parts and 30 parts into, and with respect to pure graphene oxide suction filtration film, the modulus of this enhanced film and intensity have improved 437% and 83.5% respectively.
Embodiment 5
Other are with embodiment 1, and the ratio of PGO and PEI changes 55 parts and 45 parts into, and with respect to pure graphene oxide suction filtration film, the modulus of this enhanced film and intensity have improved 373.9% and 73.8% respectively.
Embodiment 6
100 parts of GO are placed ultrasonic 30 minutes of the Tris buffered soln of pH8.5, be configured to the stable dispersion that solubility is 0.5 mg/mL.In ice-water bath, add 50 parts of dopamine hydrochlorides, dissolving in ultrasonic 10 minutes, transposition magnetic agitation 24h again, suction filtration, first pickling is washed to neutrality again, places the dry PGO of acquisition of 25 ℃ of vacuum drying ovens.Get 70 parts of PGO ultra-sonic dispersion 1h in the PBS of pH7.0 buffered soln, obtain stable dispersion system.Adding pH7.0 is dissolved with the PBS buffered soln of 30 parts of PEI, and ultrasonic mixing 1h, suction filtration obtain uncrosslinked PGO+PEI composite membrane.The Tris buffered soln that adds an amount of pH8.5 again carries out suction filtration, depresses certain outer that PEI and Dopamine HCL are taken place is crosslinked, obtains surpassing the graphene oxide film of enhancing.The Elongation test result shows that with respect to pure graphene oxide suction filtration film, the modulus of this enhanced film and intensity have improved 554% and 115% respectively.
Embodiment 7
100 parts of GO are placed ultrasonic 30 minutes of the Tris buffered soln of pH8.5, be configured to the stable dispersion that solubility is 0.5 mg/mL.In ice-water bath, add 50 parts of dopamine hydrochlorides, dissolving in ultrasonic 10 minutes, transposition magnetic agitation 24h again, suction filtration, first pickling is washed to neutrality again, places the dry PGO of acquisition of 25 ℃ of vacuum drying ovens.Get 100 parts of PGO ultra-sonic dispersion 1h in the PBS of pH7.0 buffered soln, obtain stable dispersion system, suction filtration obtains the PGO composite membrane.The Elongation test result shows that with respect to pure graphene oxide suction filtration film, the modulus of PGO composite membrane and intensity have improved 93.7% and 19.6% respectively.
Embodiment 8
100 parts of GO are placed ultrasonic 30 minutes of the Tris buffered soln of pH8.5, be configured to the stable dispersion that solubility is 0.5 mg/mL.In ice-water bath, add 50 parts of dopamine hydrochlorides, dissolving in ultrasonic 10 minutes, transposition magnetic agitation 24h again, suction filtration, first pickling is washed to neutrality again, places the dry PGO of acquisition of 25 ℃ of vacuum drying ovens.Get 92.5 parts of PGO ultra-sonic dispersion 1h in the PBS of pH7.0 buffered soln, obtain stable dispersion system.Adding pH7.0 is dissolved with the PBS buffered soln of 7.5 parts of PEI, and ultrasonic mixing 1h, suction filtration obtain uncrosslinked PGO+PEI composite membrane.The Elongation test result shows that with respect to pure graphene oxide suction filtration film, modulus and the intensity of the PGO+PEI composite membrane that this is uncrosslinked have improved 94% and 19.5% respectively.
Embodiment 9
Other are with embodiment 8, and the ratio of PGO and PEI changes 85 parts and 15 parts into, and with respect to pure graphene oxide suction filtration film, modulus and the intensity of the PGO+PEI composite membrane that this is uncrosslinked have improved 93.4% and 19.1% respectively.
Embodiment 10
Other are with embodiment 8, and the ratio of PGO and PEI changes 77.5 parts and 22.5 parts into, and with respect to pure graphene oxide suction filtration film, modulus and the intensity of the PGO+PEI composite membrane that this is uncrosslinked have improved 93.4% and 19.5% respectively.
Embodiment 11
Other are with embodiment 1, and the treatment agent of used graphene oxide is chlorogenic acid.The final crosslinked film that obtains is with respect to pure graphene oxide suction filtration film, and modulus and intensity have improved 325.5% and 40.6% respectively.
Embodiment 12
Other are with embodiment 1, and the treatment agent of used graphene oxide is suprarenin.The final crosslinked film that obtains is with respect to pure graphene oxide suction filtration film, and modulus and intensity have improved 300.5% and 50.6% respectively.
Embodiment 13
Other are with embodiment 1, and used linking agent is polypropylene amine oligopolymer (Polyallylamine, PAA, molecular weight about 3000).The final crosslinked film that obtains is with respect to pure graphene oxide suction filtration film, and modulus and intensity have improved 393.8% and 75.1% respectively.
The modulus of the various graphene oxide films of table 1 and intensity
Claims (8)
1. graphene oxide film with ultra high modulus and intensity, this graphene oxide film size macroscopic view, and have ultra high modulus and high strength, it is characterized in that this graphene oxide film comprises following three kinds of compositions at least: graphene oxide, contain catechol body structure surface treatment agent and linking agent, also can contain other auxiliary agent
Wherein, the ratio of quality and the number of copies of graphene oxide, the treatment agent that contains the catechol structure and linking agent is for example down:
100 parts of graphene oxides,
Contain catechol structure treatment agent 0.01-100 part,
Linking agent 0.01-200 part.
2. graphene oxide film according to claim 1, it is characterized in that described graphene oxide is for being raw material with graphite, utilize Brodie method, Staudenmaier method or Hummers method to reach the graphene oxide that carries out improved prepared in various methods on this basis, or the graphene oxide of the various degree of oxidations of other any means preparation.
3. graphene oxide film according to claim 1 is characterized in that described to contain the agent of catechol structure treatment be for having the catechol small molecules derivative of adjacent diphenol structure.
4. according to claim 3ly contain the derivative that the agent of catechol structure treatment is specially hydrochloride, suprarenin, chlorogenic acid or the above-mentioned substance of Dopamine HCL.
5. graphene oxide film according to claim 1, what it is characterized in that described linking agent is molecular weight at 500-50000 has a polyamino oligopolymer linking agent.
6. linking agent according to claim 5 is specially polyetherimide amine oligomer or polypropylene amine oligopolymer.
7. described graphene oxide film according to claim 1 is characterized in that described other auxiliary agent, is pH buffer reagent, oxygenant or reductive agent.
8. preparation method with graphene oxide film of ultra high modulus and intensity as claimed in claim 1 is characterized in that the preparation method is as follows:
(1) expanded graphite is made the dispersion graphene oxide;
(2) with graphene oxide with containing catechol structure treatment agent dispersion treatment;
(3) the graphene oxide PGO through containing catechol structure treatment agent dispersion treatment that step (2) is obtained mixes in pH neutral buffered soln with linking agent, obtains uncrosslinked PGO+PEI composite membrane;
(4) with the PGO+PEI composite membrane crosslinked graphene oxide film that makes enhancing under the ealkaline buffer condition that obtains in the step (3).
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| CN103407997A (en) * | 2013-07-19 | 2013-11-27 | 北京航空航天大学 | Macro preparation method of macroscopic three-dimensional graphene aerogel adsorption material used for indoor air purification |
| CN103464013A (en) * | 2013-07-25 | 2013-12-25 | 烟台绿水赋膜材料有限公司 | High-performance hybrid separation membrane and preparation method thereof |
| CN103480278A (en) * | 2013-09-06 | 2014-01-01 | 烟台绿水赋膜材料有限公司 | Preparation method and application of anti-pollution hydrophilic separating membrane |
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| CN103407997A (en) * | 2013-07-19 | 2013-11-27 | 北京航空航天大学 | Macro preparation method of macroscopic three-dimensional graphene aerogel adsorption material used for indoor air purification |
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