CN102211207A - Nano gold/graphene oxide composite material and preparation method thereof - Google Patents
Nano gold/graphene oxide composite material and preparation method thereof Download PDFInfo
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- CN102211207A CN102211207A CN2011101480498A CN201110148049A CN102211207A CN 102211207 A CN102211207 A CN 102211207A CN 2011101480498 A CN2011101480498 A CN 2011101480498A CN 201110148049 A CN201110148049 A CN 201110148049A CN 102211207 A CN102211207 A CN 102211207A
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Abstract
The invention relates to a nano gold/graphene oxide composite material and a preparation method thereof, which are used for enhancing the conductivity of a material. The preparation method of the nano gold/graphene oxide composite material is as follows: based on graphene oxide dispersed in a water phase as a carrier, nano gold particles with even particle distribution are generated through in situ direct reduction of chloroauric acid on the surface of the carrier so as to obtain the nano gold/graphene oxide composite material; and preferably, sodium borohydride is added in a dispersion obtained by fully mixing the graphene oxide with HAuCl4 under the severe stirring condition so that HAuCl4 is reduced, so as to obtain the nano gold/graphene oxide composite material. According to the invention, experiment conditions are simple, an operation method is simple and easy, and a protective agent is not added in the experiment process; the vast majority of prepared nano gold particles are modified on the surface of graphene oxide (GO), the shape is regular, the state is stable, particle size is evenly distributed, and the conductivity and biocompatibility of GO can be enhanced by modifying the nano gold on the surface of GO.
Description
Technical field
The present invention relates to a kind of nm of gold/graphene oxide composite and preparation method thereof.
Background technology
Graphene (Graphene), just mono-layer graphite is a kind of monolayer carbon atomic plane material that separates from graphite material, its thickness has only 0.335 nanometer.It is a kind of perfect monolayer carbon atom two dimensional crystal, is made up of the carbon atom of one deck hexagon cellular shape, and carbon atom can be by sp
2Covalent bond closely is connected to form the lamellar structure of two dimension.Graphene has the hexaplanar network structure, three sp in the hexaplanar
2Hybridized orbit is mutually hexagonal angle and arranges, and forms covalent bond with adjacent carbon atom.Each carbon atom links to each other with other three carbon atoms, and six carbon atom forms orthohexagonal ring at grade, stretches to form lamellar structure.Graphene is high owing to structure uniqueness, excellent performance, theoretical research are worth, having a extensive future receives much concern.
Yet Graphene also because extremely strong hydrophobicity can not be dispersed in aqueous phase, has limited its application in the bio-sensing field greatly except being difficult to preparation.Graphene oxide (GO) is to contain the Graphene derivative that enriches oxygen-containing functional group, can peel off cheap graphite by chemical oxidation and get, and handles can be made into Graphene subsequently by reduction.Therefore, utilize GO to become the important channel that low cost, magnanimity prepare Graphene through reduction preparation Graphene again, the magnanimity that promotes Graphene is used be significant.GO has good water-solubility, is easy to film forming, and common lab just can be produced in enormous quantities, is widely used in the bio-sensing field, and its shortcoming is that electric conductivity is poor than Graphene.
Summary of the invention
The invention provides the preparation method of a kind of nm of gold/graphene oxide composite, with the electric conductivity of reinforcing material.
The present invention also provides the nm of gold/graphene oxide composite of above-mentioned preparation method's gained.
The preparation method of described nm of gold/graphene oxide composite is, with the graphene oxide that is dispersed in aqueous phase is carrier, directly reduce gold chloride on its surface by original position and generate the nanogold particle of even particle distribution, obtain nm of gold/graphene oxide composite.
Preferably, under intense agitation, at graphene oxide and HAuCl
4In the well-mixed dispersion liquid, add sodium borohydride, make HAuCl
4Reduction obtains nm of gold/graphene oxide composite.Sodium borohydride reduction HAuCl
4Obtaining nanogold particle is a kind of known response, and reaction is carried out in alkaline environment (generally adding potash regulates) usually, and needs to add protective agent.But applicant's discovery, under the situation that graphene oxide exists, sodium borohydride reduction HAuCl
4Obtain nm of gold and there is following difference in above-mentioned known reaction conditions: need not to add potash conditioned reaction system and be alkalescence; Need not to add protective agent.
More preferably, under intense agitation, be that graphene oxide dispersion liquid and the 0.1-0.5mL concentration of 1mg/mL is 10mg/mL HAuCl in 0.1-0.5mL concentration
4In the well-mixed dispersion liquid of solution, add the sodium borohydride aqueous solution of 0.035-0.17mg, reduction HAuCl
4Generate nm of gold, reaction at room temperature can be finished rapidly, prepares nm of gold/graphene oxide composite fast.
The invention has the beneficial effects as follows:
React according to technique scheme: experiment condition is simple, method of operating is simple and easy, does not add protective agent in the experimentation; Trace NaBH
4Add as reducing agent, can impel the formation of nanogold particle rapidly; The nanogold particle overwhelming majority for preparing all is modified at the GO surface, and regular shape, in stable condition, particle diameter be evenly distributed, and decorated by nano-gold can strengthen electric conductivity and the biocompatibility of GO on the GO surface.
Description of drawings
Fig. 1 is the transmission electron microscope picture of embodiment 1 gained nm of gold/graphene oxide composite;
Fig. 2 is that embodiment 1 gained nm of gold/(curve a) is modified the scan round voltammogram of platinum electrode (curve b) in potassium ferrocyanide solution with blank graphene oxide to graphene oxide composite modification platinum electrode.
Fig. 3 is the transmission electron microscope picture of embodiment 2 gained nm of gold/graphene oxide composite.
The specific embodiment
Embodiment 1
A kind of preparation method of nm of gold/graphene oxide may further comprise the steps:
1) take by weighing 1mg GO, be dissolved in the 1mL redistilled water, the GO solution of configuration 1mg/mL,
2) take by weighing 1g HAuCl
4, be dissolved in the 100mL volumetric flask HAuCl of configuration 1%
4Solution,
3) in the round-bottomed flask that contains 20mL distilled water, add 0.2mL 1mg/mLGO solution, stir after 10 minutes, add the HAuCl of 0.1mL 1% rapidly
4Solution continued vigorous stirring 10 minutes, added 0.035mg NaBH
4The last composite that promptly obtained modified nano gold on GO in 20 minutes that stirs again.
In the present embodiment, GO and HAuCl
4Mass ratio be 1: 5.Product perspective Electronic Speculum figure as shown in Figure 1.Nanogold particle on the GO is shaped as regular spherical about diameter 5nm, in stable condition, particle diameter is evenly distributed.
Fig. 2 is that embodiment 1 gained nm of gold/(curve a) is modified the scan round voltammogram of platinum electrode (curve b) in potassium ferrocyanide solution with blank graphene oxide to graphene oxide composite modification platinum electrode.
Concrete experiment condition is as follows: the preparation of (1) working electrode: get 5 μ L 1mg/mL nm of gold/graphene oxide composites and 1mg/mL GO drips of solution respectively and be coated in the platinum electrode surface that diameter is 3mm, under room temperature, dry naturally, obtain nm of gold/graphene oxide composite respectively and modify platinum electrode and blank graphene oxide modification platinum electrode; (2) experiment of scan round volt-ampere is carried out on electrochemical workstation (CHI660B), adopts traditional three-electrode system, and promptly above-mentioned modification platinum electrode is as working electrode, and saturated calomel electrode is as reference electrode, and the platinum filament conduct is to electrode.The 1mM potassium ferrocyanide is as electroactive probe, and 0.1M potassium chloride is as supporting electrolyte, and sweep speed is 100mV/s, from 0 to 0.5 volt of sweep limits.
Experimental result shows: electroactive probe is modified on the platinum electrode than modify platinum electrode at blank graphene oxide at nm of gold/graphene oxide composite has bigger response current and less OR spike potential poor, illustrates that decorated by nano-gold can strengthen the electric conductivity of GO on the GO surface.
Embodiment 2
A kind of preparation method of nm of gold/graphene oxide may further comprise the steps:
1) take by weighing 1mg GO, be dissolved in the 1mL redistilled water, the GO solution of configuration 1mg/mL,
2) take by weighing 1g HAuCl
4, be dissolved in the 100mL volumetric flask HAuCl of configuration 1%
4Solution,
3) in the round-bottomed flask that contains 20mL distilled water, add 0.2mL 1mg/mLGO solution, stir after 10 minutes, add the HAuCl of 0.2mL 1% rapidly
4Solution continued vigorous stirring 10 minutes, 0.07mg NaBH
4The last composite that promptly obtained modified nano gold on GO in 20 minutes that stirs again.
In the present embodiment, employed GO and HAuCl
4Mass ratio be 1: 10.Product perspective Electronic Speculum figure as shown in Figure 2.Nanogold particle on the GO is shaped as regular spherical about diameter 5nm, in stable condition, particle diameter is evenly distributed.
Claims (4)
1. the preparation method of nm of gold/graphene oxide composite, it is characterized in that, with the graphene oxide that is dispersed in aqueous phase is carrier, directly reduces gold chloride on its surface by original position and generates the nanogold particle of even particle distribution, obtains nm of gold/graphene oxide composite.
2. the preparation method of nm of gold as claimed in claim 1/graphene oxide composite is characterized in that, under intense agitation, at graphene oxide and HAuCl
4In the well-mixed dispersion liquid, add sodium borohydride, make HAuCl
4Reduction obtains nm of gold/graphene oxide composite.
3. the preparation method of nm of gold as claimed in claim 2/graphene oxide composite is characterized in that, under intense agitation, is that graphene oxide dispersion liquid and the 0.1-0.5mL concentration of 1mg/mL is 10mg/mLHAuCl in 0.1-0.5mL concentration
4In the well-mixed dispersion liquid of solution, add the sodium borohydride of 0.035-0.17mg, make HAuCl
4Reduction obtains nm of gold/graphene oxide composite.
4. the nm of gold of each preparation method's gained/graphene oxide composite among the claim 1-3.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102385938A (en) * | 2011-11-10 | 2012-03-21 | 电子科技大学 | Metal matrix graphene composite electrical contact material and preparation method thereof |
| CN102513533A (en) * | 2011-12-30 | 2012-06-27 | 北京交通大学 | Single-layer graphene/gold nanoparticle composite and preparation method for same |
| CN103551194A (en) * | 2013-11-14 | 2014-02-05 | 厦门大学 | Graphene-heme and nanogold ternary composite material, preparation method and application |
| CN103668141A (en) * | 2012-08-30 | 2014-03-26 | 中国科学院上海微***与信息技术研究所 | Method for growing noble metal nanocrystal on graphene oxide surface |
| CN104900723A (en) * | 2014-03-05 | 2015-09-09 | 株式会社东芝 | Transparent conductor and device |
| CN105062299A (en) * | 2015-07-15 | 2015-11-18 | 延平区鑫东来新型导电材料加工厂 | Modified graphene conductive coating and preparation method thereof |
| CN105750558A (en) * | 2016-04-12 | 2016-07-13 | 同济大学 | Method for synthesizing gold nano-rod/graphene oxide composite material with one-pot process |
| CN106076361A (en) * | 2016-06-03 | 2016-11-09 | 济南大学 | A kind of nickel foam/graphene/nanometer metal/composite material and preparation method thereof |
| CN107096926A (en) * | 2017-04-20 | 2017-08-29 | 华南理工大学 | A kind of supercritical CO2The method that original position prepares Au/ graphene nanocomposite materials |
| CN107973621A (en) * | 2017-11-03 | 2018-05-01 | 东南大学 | A kind of reaction island based on graphene/nanometer gold plating and its preparation method and application |
| CN109260963A (en) * | 2018-10-11 | 2019-01-25 | 青岛大学 | A kind of redox graphene/gold nano combined filtration film and its preparation and application |
| CN109590482A (en) * | 2018-12-07 | 2019-04-09 | 信阳师范学院 | A kind of modified graphene oxide, modified graphene oxide load gold nano grain and preparation method thereof |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102385938B (en) * | 2011-11-10 | 2013-06-12 | 电子科技大学 | Metal matrix graphene composite electrical contact material and preparation method thereof |
| CN102385938A (en) * | 2011-11-10 | 2012-03-21 | 电子科技大学 | Metal matrix graphene composite electrical contact material and preparation method thereof |
| CN102513533A (en) * | 2011-12-30 | 2012-06-27 | 北京交通大学 | Single-layer graphene/gold nanoparticle composite and preparation method for same |
| CN102513533B (en) * | 2011-12-30 | 2013-07-03 | 北京交通大学 | Single-layer graphene/gold nanoparticle composite and preparation method for same |
| CN103668141B (en) * | 2012-08-30 | 2015-12-16 | 中国科学院上海微***与信息技术研究所 | In the method for surface of graphene oxide growth noble metal nanocrystalline |
| CN103668141A (en) * | 2012-08-30 | 2014-03-26 | 中国科学院上海微***与信息技术研究所 | Method for growing noble metal nanocrystal on graphene oxide surface |
| CN103551194A (en) * | 2013-11-14 | 2014-02-05 | 厦门大学 | Graphene-heme and nanogold ternary composite material, preparation method and application |
| CN104900723A (en) * | 2014-03-05 | 2015-09-09 | 株式会社东芝 | Transparent conductor and device |
| US9763320B2 (en) | 2014-03-05 | 2017-09-12 | Kabushiki Kaisha Toshiba | Transparent conductor and device |
| US10306752B2 (en) | 2014-03-05 | 2019-05-28 | Kabushiki Kaisha Toshiba | Transparent conductor and device |
| CN105062299A (en) * | 2015-07-15 | 2015-11-18 | 延平区鑫东来新型导电材料加工厂 | Modified graphene conductive coating and preparation method thereof |
| CN105750558A (en) * | 2016-04-12 | 2016-07-13 | 同济大学 | Method for synthesizing gold nano-rod/graphene oxide composite material with one-pot process |
| CN106076361A (en) * | 2016-06-03 | 2016-11-09 | 济南大学 | A kind of nickel foam/graphene/nanometer metal/composite material and preparation method thereof |
| CN106076361B (en) * | 2016-06-03 | 2019-04-05 | 济南大学 | A kind of nickel foam/graphene/nanometer metal/composite material and preparation method thereof |
| CN107096926A (en) * | 2017-04-20 | 2017-08-29 | 华南理工大学 | A kind of supercritical CO2The method that original position prepares Au/ graphene nanocomposite materials |
| CN107973621A (en) * | 2017-11-03 | 2018-05-01 | 东南大学 | A kind of reaction island based on graphene/nanometer gold plating and its preparation method and application |
| CN109260963A (en) * | 2018-10-11 | 2019-01-25 | 青岛大学 | A kind of redox graphene/gold nano combined filtration film and its preparation and application |
| CN109590482A (en) * | 2018-12-07 | 2019-04-09 | 信阳师范学院 | A kind of modified graphene oxide, modified graphene oxide load gold nano grain and preparation method thereof |
| CN109590482B (en) * | 2018-12-07 | 2021-02-05 | 信阳师范学院 | Modified graphene oxide, modified graphene oxide-loaded gold nanoparticles and preparation method thereof |
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Application publication date: 20111012 |