CN107055522A - The preparation method of Alkali Metal Rb doped graphene composite - Google Patents

The preparation method of Alkali Metal Rb doped graphene composite Download PDF

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Publication number
CN107055522A
CN107055522A CN201710176285.8A CN201710176285A CN107055522A CN 107055522 A CN107055522 A CN 107055522A CN 201710176285 A CN201710176285 A CN 201710176285A CN 107055522 A CN107055522 A CN 107055522A
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China
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graphene
doped
dimethoxy
ethanes
preparation
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CN201710176285.8A
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Inventor
李小荣
严向玉
吴怡瑾
宋洁
赵朴素
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Huaiyin Normal University
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Huaiyin Normal University
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00Structure or properties of graphene
    • C01B2204/20Graphene characterized by its properties
    • C01B2204/22Electronic properties
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/80Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/85Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/04Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM

Abstract

The invention discloses a kind of preparation method of Alkali Metal Rb doped graphene composite, the preparation method is:Graphene under vacuum condition using mode of heating lead to N2Except O2;1,2 dimethoxy-ethanes lead to N2Except O2After be placed in container as reaction dissolvent;The Rb of two times of graphene amounts is scattered in 1,2 dimethoxy-ethanes until dissolving;In 1,2 dimethoxy-ethanes that graphene dispersion dissolves in Rb, magnetic agitation obtains the dispersion liquid of Rb doped graphenes;Stand, Rb doped graphene dispersion liquids are layered, and pour out upper strata settled solution;Remainder is cleaned through ethanol, centrifuged to remove the Rb of weak binding, and is dried under vacuum, obtains stable Rb doped graphenes.The present invention, to obtain the Rb doped graphenes of " clean ", is given full play to its electricity, mechanics and chemical property, has potential application value in terms of performance excellent electron device is developed by direct interaction formation chemical bond between carbon atom and metallic atom.

Description

The preparation method of Alkali Metal Rb doped graphene composite
Technical field
The present invention relates to room temperature wet chemical synthesis, and in particular to a kind of Alkali Metal Rb(Rb)Doped graphene composite wood The preparation method of material.
Background technology
Chemical doping is inherently to modify the effective ways of host material property using hetero atom, such as electricity, magnetics with And chemistry and engineering properties etc..For carbon material, chemical doping is a kind of abundant carrier density, strengthens electricity and thermal conductivity The prefered method of performance.Recently, chemical doping graphene has been achieved for the achievement attracted people's attention.For example, by using oxygen Etch process, graphene is etched simultaneously, and surface is oxidized and is doped;By using nitrogen plasma treatment method, Exposure graphene obtains the graphene of N doping in nitrogen plasma.More importantly the theory of metal-doped graphene is ground Study carefully the possibility for also having foretold that fermi level change and p-type are intersected to n-type.Recently, the alkali in various dopants Metal Rb be considered as it is a kind of can be used in the superior element of carbon material chemical doping, thus it is expected that it can improve graphene Electrical properties.So far, researcher obtains Rb doped graphenes and mainly utilizes chemical vapour deposition technique, and this method needs Completed under high temperature, high vacuum condition, thus easily graphene can be caused to accumulate again.In addition, this method poor controllability, and And power consumption is high, cost is high.Accordingly, it would be desirable to develop alternative doping method.In previous studies, room temperature chemistry K doping Interacted by π-π and be successfully used to improve the characteristic of CNT and graphene, such as add its metalline, influenceed Its lattice array, and have adjusted its electricity, mechanically and chemically property.But this method is added in building-up process Organic reagent, has had a strong impact on giving full play to for its electrical properties.
The content of the invention
It is an object of the invention to:A kind of preparation method of simple alkali metal Rb doped graphenes at room temperature is provided, should Method forms chemical bond to obtain the Rb doped graphenes of " clean " by direct interaction between carbon atom and metallic atom Composite, further enhances its metallicity, gives full play to its electricity, mechanics and chemical property, excellent in exploitation performance There is potential application value in terms of good electronic device.
The present invention technical solution be:Graphene under vacuum condition using mode of heating lead to N2Except O2Afterwards in case should With;1,2- dimethoxy-ethanes lead to N2Except O2Afterwards, it is placed in container, is used as reaction dissolvent;The Rb of two times of graphene amounts is in magnetic force It is scattered under stirring in 1,2- dimethoxy-ethanes, until being completely dissolved;The 1,2- bis- that graphene dispersion dissolves in above-mentioned Rb In Ethyl Methyl Ether, magnetic agitation obtains Rb doped graphites by the ionic bond interaction between metallic atom and carbon atom Alkene dispersion liquid;Stand, Rb doped graphene dispersion liquids are layered, and pour out upper strata settled solution;Remainder cleans through ethanol, Centrifugation is dried under vacuum with removing the Rb of weak binding, obtains black powder, and as stable Rb doped graphenes are answered Condensation material.
The present invention has advantages below:
1st, according to the theoretical research of metal-graphite alkene, the metal of the first main group to the 3rd main group, between metallic atom and carbon atom Form ionic bond.It is theoretical using this, the Rb doped graphenes of " clean " are designed and synthesized, are existed without any protective agent Under, the optkmal characteristics of composite are given full play to by the synergy between each material, this is in nano electron device and urges Change field has important scientific meaning.
2nd, the synthesis of Rb doped graphenes of the invention is operated in the Simple hand casing of anhydrous and oxygen-free, and room temperature is wet Chemical synthesis process is safe and reliable, simple to operate, and material is easy to get, and reaction is gentle, and post processing is easy.
3rd, Rb doped graphenes are formed ionic bond by Rb atoms and carbon atom direct interaction and obtained, with prior art Compare, the preparation method that the present invention is provided is simple, using one-step synthesis, and without heating and add any other addition Agent, is solved due to the problem of the presence of high temperature and additional agents influences composite property.
Brief description of the drawings
Fig. 1 synthesizes the TEM of Rb doped graphenes for wet chemistry method at room temperature(A)And HR-TEM(B)Image and EDAX power spectrums (C)The main component for showing Rb doped graphenes is C, O and Rb.
Embodiment
Technical scheme is further illustrated with reference to embodiment, but is not to be construed as the limit to technical scheme System.
Embodiment 1:20 mg graphenes under vacuum condition using mode of heating lead to N2Except O2Afterwards in case using;150 mL 1,2- dimethoxy-ethanes(99.5%)Logical N2Except O2Afterwards, it is placed in 250 mL round-bottomed flasks, is used as reaction dissolvent;40 mg Rb It is scattered under magnetic stirring in 150 mL 1,2- dimethoxy-ethanes, until being completely dissolved;20 mg graphene dispersions are in upper State 40 mg Rb dissolving 1,2- dimethoxy-ethanes in, the h of magnetic agitation 48, by between metallic atom and carbon atom from Sub-key interacts, and obtains Rb doped graphene dispersion liquids;Stand after a period of time, Rb doped graphene dispersion liquids divide Layer, pours out upper strata settled solution;Remainder is cleaned through ethanol, centrifuged to remove the Rb of weak binding, and is done under vacuum It is dry, obtain black powder, as stable Rb doped graphene composites.
The Rb doped graphenes of above-mentioned gained have following electricity, mechanics and chemical property:(1)Rb doping Effective Regulation stones The band structure of black alkene, makes it have excellent electron mobility and the excellent electric property such as high free carrier density, enters And the electric conductivity of graphene is improved, for the research in terms of ultracapacitor, fuel cell and sensor.(2)Rb is doped into One step strengthens the stability of two-dimensional graphene, Young's modulus with basic mechanical performances such as intensity, brilliant in microelectronic component, field-effect The fields such as body pipe have very important application value.(3)After Rb doping there are substantial amounts of defect sites in graphenic surface, increase Its adsorption and various atoms and molecule are desorbed, it is shown the chemical property such as excellent catalytic activity and response characteristic, This graphene chemical modification and strengthen there is very big potential in the application of graphene composite material.

Claims (1)

1. the preparation method of Alkali Metal Rb doped graphene composite, it is characterized in that the preparation method of the graphene composite material It is:Graphene under vacuum condition using mode of heating lead to N2Except O2Afterwards in case using;1,2- dimethoxy-ethanes lead to N2Except O2 Afterwards, it is placed in container, is used as reaction dissolvent;The Rb of two times of graphene amounts is scattered in 1,2- dimethoxy second under magnetic stirring In alkane, until being completely dissolved;Graphene dispersion is in 1, the 2- dimethoxy-ethanes that above-mentioned Rb dissolves, and magnetic agitation passes through gold The ionic bond interaction belonged between atom and carbon atom obtains Rb doped graphene dispersion liquids;Stand, Rb doped graphenes Dispersion liquid is layered, and pours out upper strata settled solution;Remainder cleans through ethanol, centrifuge to remove the Rb of weak binding, and Dried under vacuum condition, obtain black powder, as stable Rb doped graphene composites.
CN201710176285.8A 2017-03-23 2017-03-23 The preparation method of Alkali Metal Rb doped graphene composite Pending CN107055522A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102414124A (en) * 2009-04-24 2012-04-11 丰田自动车株式会社 Carbon material and method for producing same
CN103097287A (en) * 2010-08-10 2013-05-08 大学共同利用机关法人自然科学研究机构 Carbon nanostructure, metal-supported carbon nanostructure, lithium ion secondary battery, process for production of carbon nanostructure, and process for production of metal-supported carbon nanostructure
CN103717529A (en) * 2011-08-04 2014-04-09 贝克休斯公司 Method of preparing functionalized graphene

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102414124A (en) * 2009-04-24 2012-04-11 丰田自动车株式会社 Carbon material and method for producing same
CN103097287A (en) * 2010-08-10 2013-05-08 大学共同利用机关法人自然科学研究机构 Carbon nanostructure, metal-supported carbon nanostructure, lithium ion secondary battery, process for production of carbon nanostructure, and process for production of metal-supported carbon nanostructure
CN103717529A (en) * 2011-08-04 2014-04-09 贝克休斯公司 Method of preparing functionalized graphene

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