CN103100725A - Preparation method of silver/carbon quantum dot composite nanometer materials - Google Patents
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Abstract
The invention provides a preparation method of silver/carbon quantum dot composite nanometer materials. The specific preparation processes comprise the steps of adding a certain amount of silver nitrate solution to polyvinylpyrrolidone solution, adding a certain amount of carbon quantum dot solution to the polyvinylpyrrolidone solution, mixing for some time, transferring the solution into a reaction kettle, conducting a hydrothermal reaction at a certain temperature for some time, conducting centrifugal separation on a product, washing the product several times by using deionized water and ethanol, and obtaining the silver/carbon quantum dot composite nanometer materials after vacuum desiccation. The preparation method of the silver/carbon quantum dot composite nanometer materials is environment-friendly, high-efficient and easy to operate. Besides, the prepared silver/carbon quantum dot composite nanometer materials have good application prospects in the field of sensing, catalysis and the like.
Description
Technical field
The present invention relates to the preparation method of a kind of silver/carbon quantum dot composite nano materials, simple, the with low cost method of especially a kind of preparation technology.
Technical background
Metal nanoparticle is because of its unusual optics, electronics, magnetic property, and in the potential using value of the aspects such as catalysis, information storage, biomarker, SERS (SERS) spectrum and day by day receive people's concern, wherein silver nano-grain has superconductivity and widely than chromatic effect, thereby become one of the most attractive nano material, anisotropic silver nanostructured (such as bar-shaped, wire, nucleocapsid structure etc.) has unique application prospect at aspects such as SERS and nonlinear optical properties; Silver nano-grain is synthetic aqueous phase, and main method is under the existence of the stabilizing agents such as polyvinylpyrrolidone, softex kw, is obtained by traditional reducing agent reduction such as hydrazine hydrate, sodium borohydride, ascorbic acid, methyl alcohol; These reducing agents are often noxious material, can cause certain pollution to environment, and usually have the difficult shortcoming of separating, collecting of product; In recent years, the environmental friendliness shaped materials such as glucose and protein are widely used in the synthetic of metal nanoparticle, the core-shell structure nano particle that obtains; Wherein as the carbon-coating of shell, not only protected silver nano-grain not oxidized, and given the character of the new aspects such as optics of material, application prospect is good.
Recently, carbon group material has new development, is similar to luminous carbon quantum dot one appearance of semiconductor-quantum-point, namely with advantages such as good optical property, synthetic convenience, abundant raw material and toxicity are little, has been used for biomarker and life science; The people such as Li (Angewandte Chemie International Edition, 2010,49 (26): 4430-4434) composite of synthetic carbon quantum dot and titanium dioxide is as photochemical catalyst; The people such as Helena (Biosensors and Bioelectronics, 2010,26:1302-1306) prepared mensuration Hg
2+Carbon quantum dot sensor; The people such as Shi (Phys. Chem. Chem. Phys., 2012,14, the gold/carbon quantum dot composite nano materials that prepared 7360-7366) is used for SERS, yet the method for preparing gold/carbon quantum dot that this seminar adopts exists product to be difficult to separate, not to be suitable for the shortcomings such as large-scale production.
Up to now, still find no the human one step hydro thermal method and prepare silver/carbon quantum dot composite nano materials; The present invention adopts green grass to be carbon source, and with low cost, technique is simple, and prepared silver/carbon quantum dot composite nano materials has the applications well prospect in fields such as sensing, catalysis.
Summary of the invention
The object of the invention is to provide a kind of method of using new one step hydro thermal method to synthesize silver/carbon quantum dot composite nano materials.
The present invention realizes by following steps:
(1) preparation carbon quantum dot solution: carbon quantum dot pressed powder is with reference to Sun report (the Adv. Mater. 2012 of seminar, 24,2037 – 2041) method preparation, then use deionized water dissolved carbon quantum dot solid, being settled to concentration is the carbon quantum dot solution of 0.1g/L.
(2) prepare respectively polyvinylpyrrolidone (PVP) solution (dissolving 10gPVP in every 1L distilled water) and AgNO
3(concentration is 0.01～0.03mol/L) to solution, then measures above-mentioned two kinds of solution that volume ratio is 2:1, stirs after mixing; Again the carbon quantum dot solution is added in mentioned solution (wherein carbon quantum dot solution and AgNO
3The volume ratio of solution is 2:1), after magnetic agitation is even, be transferred to reactor.
(3) reactor being placed in the electronics baking oven, is under 140 ℃～180 ℃ in temperature, and reaction obtains taupe suspension after 4～8h, with distilled water, ethanol respectively centrifugal, wash products repeatedly post-drying obtain silver/carbon quantum dot composite nano materials.
(4) utilize X-ray diffractometer (XRD), transmission electron microscope (TEM), ultraviolet-uisible spectrophotometer (UV) to carry out micromorphology analysis to product.
The present invention has the characteristics of environmental protection, convenient and efficient, in preparation process, take green grass as the prepared carbon quantum dot solution of carbon source as reducing agent, one step hydro thermal method has synthesized silver/carbon quantum dot composite material, and silver/carbon quantum dot nano-particle presents nucleocapsid structure, is 60nm as the particle diameter of the silver-colored particle of core, is 2nm as the thickness of the ultra-thin carbon quantum dot layer of shell, the granule-morphology homogeneous, favorable dispersibility; The silver that this method is synthesized/carbon quantum dot composite nano materials has the applications well prospect in fields such as sensing, catalysis.
Description of drawings
Fig. 1 is the transmission electron microscope photo of embodiment 3 preparation carbon quantum dots, by the carbon quantum point grain diameter homogeneous that can find out preparation in photo (2～4nm), favorable dispersibility.
Fig. 2 is the transmission electron microscope photo of embodiment 3 preparation silver/carbon quantum dot composite nano materials, by finding out in photo that prepared silver/carbon quantum dot composite nano materials presents nucleocapsid structure, particle diameter as the silver-colored particle of core is 60nm, thickness as the ultra-thin carbon quantum dot layer of shell is 2nm, the granule-morphology homogeneous, favorable dispersibility has the applications well prospect in fields such as sensing, catalysis.
Fig. 3 is the XRD diffraction spectrogram of embodiment 3 preparation silver/carbon quantum dot composite nano materials, the surface the successful preparation of silver/carbon quantum dot composite nano materials.
Fig. 4 is the ultraviolet-visible spectrogram of embodiment 3 preparation silver/carbon quantum dot composite nano materials, by observing at 450cm in spectrogram
-1A wider absworption peak occurs, further proved the successful preparation of silver/carbon quantum dot composite material.
Embodiment 1
0.1g PVP is dissolved in 10mL distilled water, measures 5mL AgNO
3(0.03mol/L) join in above-mentioned PVP solution, after stirring at room 10min, the 10mL carbon quantum dot solution (0.1g/L) for preparing is joined in above-mentioned mixed liquor, after continuing to stir 20min, reactant liquor is transferred in the 50mL water heating kettle, is placed in 140 ℃, electronics baking oven, reaction 8h; After reaction is completed, with the products therefrom centrifugation, and clean repeatedly with distilled water, ethanol respectively, be placed in vacuum drying oven and dry.
Embodiment 2
0.1g PVP is dissolved in 10mL distilled water, measures 5mL AgNO
3(0.02mol/L) join in above-mentioned PVP solution, after stirring at room 10min, the 10ml carbon quantum dot solution (0.1g/L) for preparing is joined in above-mentioned mixed liquor, after continuing to stir 20min, reactant liquor is transferred in the 50mL water heating kettle, is placed in 160 ℃, electronics baking oven, reaction 4h; After reaction is completed, with the products therefrom centrifugation, and clean repeatedly with distilled water, ethanol respectively, be placed in vacuum drying oven and dry.
Embodiment 3
0.1g PVP is dissolved in 10mL distilled water, measures 5mL AgNO
3(0.02mol/L) join in above-mentioned PVP solution, after stirring at room 10min, the 10mL carbon quantum dot solution (0.1g/L) for preparing is joined in above-mentioned mixed liquor, after continuing to stir 20min, reactant liquor is transferred in the 50mL water heating kettle, is placed in 180 ℃, electronics baking oven, reaction 4h; After reaction is completed, with the products therefrom centrifugation, and clean repeatedly with distilled water, ethanol respectively, be placed in vacuum drying oven and dry.
Embodiment 4
0.1g PVP is dissolved in 10mL distilled water, measures 5mL AgNO
3(0.01mol/L) join in above-mentioned PVP solution, after stirring at room 10min, the 10mL carbon quantum dot solution (0.1g/L) for preparing is joined in above-mentioned mixed liquor, after continuing to stir 20min, reactant liquor is transferred in the 50mL water heating kettle, is placed in 180 ℃, electronics baking oven, reaction 8h; After reaction is completed, with the products therefrom centrifugation, and clean repeatedly with distilled water, ethanol respectively, be placed in vacuum drying oven and dry.
Claims (2)
1. the preparation method of silver/carbon quantum dot composite nano materials,, be 60nm as the particle diameter of the silver-colored particle of core, be 2nm as the thickness of the ultra-thin carbon quantum dot layer of shell, the granule-morphology homogeneous, favorable dispersibility is characterized in that comprising the steps:
(1) preparation carbon quantum dot solution: with deionized water dissolved carbon quantum dot solid, being settled to concentration is the carbon quantum dot solution of 0.1g/L;
(2) prepare respectively polyvinylpyrrolidone (PVP) solution, dissolve 10gPVP in every 1L distilled water; Concentration is the AgNO of 0.01～0.03mol/L
3Solution, then measure above-mentioned two kinds of solution, polyvinylpyrrolidone (PVP) solution and AgNO
3The volume ratio of solution is 2:1, stirs after mixing; Again the carbon quantum dot solution is added in mentioned solution, wherein carbon quantum dot solution and AgNO
3The volume ratio of solution is 2:1, after magnetic agitation is even, is transferred to reactor;
(3) reactor being placed in the electronics baking oven, is under 140 ℃～180 ℃ in temperature, and reaction obtains taupe suspension after 4～8h, with distilled water, ethanol respectively centrifugal, wash products repeatedly post-drying obtain silver/carbon quantum dot composite nano materials.
2. a kind of silver as claimed in claim 1/carbon quantum dot composite nano materials preparation method, is characterized in that, wherein the molecular weight of step (2) PVP used is between 4000～160000 K-30.
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| CN103785853A (en) * | 2014-01-24 | 2014-05-14 | 太原理工大学 | Preparation method of hybrid carbon silver composite material |
| CN104046353A (en) * | 2014-04-25 | 2014-09-17 | 安徽师范大学 | Assembly object for fluorescence enhancement and preparation method and application thereof |
| CN104477967A (en) * | 2014-11-18 | 2015-04-01 | 江苏大学 | Method for preparing cuprous oxide microcrystals by taking carbon quantum dots as reducing agent |
| CN105664966A (en) * | 2015-12-31 | 2016-06-15 | 丽王化工(南通)有限公司 | Preparation method and application of metal/cuprous oxide composite nano material |
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