CN103525412B - Method for one-step synthesis of fluorescent carbon nano-particle solution - Google Patents
Method for one-step synthesis of fluorescent carbon nano-particle solution Download PDFInfo
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- CN103525412B CN103525412B CN201310435760.0A CN201310435760A CN103525412B CN 103525412 B CN103525412 B CN 103525412B CN 201310435760 A CN201310435760 A CN 201310435760A CN 103525412 B CN103525412 B CN 103525412B
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Abstract
The invention discloses a method for one-step synthesis of a fluorescent carbon nano-particle solution, relating to a method for synthesizing a carbon particle solution. According to the method, glycol is used as a solvent and ammonium oxalate and saccharide or organic acid are used as a carbon source to synthesize fluorescent carbon nano-particles through co-heating, and more than two types of carbon source substances are used during synthesis. The method comprises the following steps of: firstly, comminuting ammonium oxalate and carbon source raw materials, and dissolving the raw materials in glycol to prepare a solution; then transferring the solution into a reaction kettle, heating the reaction kettle in a constant temperature box, and reacting to generate the carbon nano-particle solution, wherein the obtained solution has fluorescence and is a fluorescent carbon nano-particle solution. The raw materials used in the method are easy to obtain, the method is simple, less equipment is needed, reagents are cheap, the synthesis speed is high, strong acid and strong alkali are not used, and the obtained carbon nano-particles are nontoxic and can be conveniently used for biological markers. The carbon nano-particle solution synthesized by the method does not need passivation and separation, has a good fluorescent characteristic and can be directly used.
Description
Technical field
The present invention relates to the method for synthesis carbon particles solution, particularly relate to a kind of method of one-step synthesis fluorescent carbon nano-particles solution.
Background technology
Carbon nano-particles (CNPs) is a kind of novel fluorescence nano material, has high chemical stability, and light stability and special optical property, be widely used in fields such as sensing, imaging, sun power, photoelectric devices.CNPs has the fluorescence property similar to quantum dot, as strong in fluorescence and stablize, excitation wavelength and emission wavelength controllable, upper conversion performance, have excellent visible region fluorescent emission.Compared with other fluorescent nano particles, because its surface has abundant oxygen element, fluorescent carbon nano-particles has good water-soluble and biocompatibility and is easy to the advantage such as surface-functionalized.Fluorescent carbon nano-particles is at biomarker, and particularly the Related Research Domain such as in vivo marker is with a wide range of applications.Because there is electron hole on fluorescent carbon nano-particles surface, it be excellent electron acceptor(EA) and give body, also have wide application prospects at semiconductor applications, catalytic field.The preparation method of fluorescent carbon nano-particles can be divided into from top to bottom the method for (Top-down) and (Bottom-up) from bottom to top.Top-to-bottom method is exactly that the carbon material of bulk is divided into nanoparticle, mainly contains arc discharge, laser ablation method, electrochemical synthesis.The method of (Top-down) is ascending preparation method from bottom to top, namely generates short grained carbon nano-particles with carbon source material, reassociates into required carbon nano-particles.The equipment requirements of laser ablation, electrochemical production nano material is higher, and the concentrated acid oxidation style time response time generally needs tens hours, there is environmental pollution, equipment corrosion, time tediously long shortcoming.The most of fluorescence property of carbon nano-particles prepared by traditional method is not high, cannot be used for biological marker, and needing further passivation to modify just can have good fluorescence.Modifier mainly contains Macrogol 200, polyethylene glycol 1500, polymine (PEI) and some tensio-active agents etc., and reagent price is high, chronic to the modification reaction of carbon nano-particles, about tens hours.
Summary of the invention
The object of the present invention is to provide a kind of method of one-step synthesis fluorescent carbon nano-particles solution, what the method adopted is organic carbon method, the time of the fluorescent carbon nano-particles of preparation is short, equipment is corrosion-free, prepared carbon nano-particles does not need to modify passivation just good fluorescence property, achieve a step and complete reaction, save reactions steps.
The object of the invention is to be achieved through the following technical solutions:
The method of one-step synthesis fluorescent carbon nano-particles solution, said method comprising the steps of:
(1) dissolving of material: take 0.5 gram of carbon source material and 0.05-0.5 gram of ammonium oxalate mixing, porphyrize in mortar, pours the mixture of porphyrize into beaker, add ethylene glycol 20 milliliters, put into magneton, be placed on magnetic stirrer and stir, until solid dissolves completely, obtain colourless transparent solution;
(2) fluorescent carbon nano-particles generates: poured into by above-mentioned colourless transparent solution in the reactor of liner Teflon, tighten reactor kettle cover, reactor is placed in thermostatic drying chamber in 140-180 DEG C of heating 3 hours, then from thermostatic drying chamber, take out reactor naturally cool to room temperature, in reactor, solution is brown color, and the liquid of gained is fluorescent carbon nano-particles solution.
The method of described one-step synthesis fluorescent carbon nano-particles solution, described carbon source material is glucose, vitamins C, tartrate, oxysuccinic acid, citric acid, fumaric acid.
The method of described one-step synthesis fluorescent carbon nano-particles solution, the carbon nano-particles of described glucose prepared by carbon source has blue-green fluorescent, and vitamins C is that the carbon nano-particles solution of raw material has green fluorescence, and all the other are sky blue fluorescence.
Advantage of the present invention and effect are:
The present invention take ethylene glycol as solvent, and ammonium oxalate and carbon source material are presoma, altogether thermal synthesis fluorescent carbon nano-particles solution, and have raw material supply abundance, cost is low, and equipment is simple and easy to the advantage purchased, and whole flow operations is simple.Feasibility is comparatively large, magnanimity can produce, meet commercial application in laboratory.The brightness of gained fluorescent carbon nano-particles solution fluorescence is high, and good water solubility can widely use in actual applications.Carbon nano-particles solution synthesized by present method does not need other passivation to modify, and is rare one-step synthesis.Carbon nano-particles synthesized by present method does not use toxic substance, and toxicity is extremely low, and fluorescence property is good, may be used for living organisms mark.
Accompanying drawing explanation
Fig. 1 is fluorescence excitation-emission spectrum and the uv absorption spectra of the carbon nanomaterial aqueous solution
Fig. 2 is the fluorescence spectrum figure of the carbon nanomaterial aqueous solution under different wave length optical excitation
Fig. 3 is the XRD spectrum figure of carbon nanomaterial
Embodiment
Below in conjunction with accompanying drawing illustrated embodiment, the invention will be further described.
The present invention is a kind of method of one-step synthesis fluorescent carbon nano-particles solution.The present invention take ethylene glycol as solvent, and ammonium oxalate and carbohydrate or organic acid are carbon source thermal synthesis fluorescent carbon nano-particles altogether, employ two or more carbon source materials in synthesis.First by ammonium oxalate and carbon source raw material porphyrize, be dissolved in ethylene glycol and make solution, then transfer in reactor, be placed in thermostat container and heat, through reaction Formed nano-particle solution, gained solution has fluorescence, and this solution is fluorescence nano carbon particles solution.The present invention is raw materials used to be easy to get, and method is simple, and required equipment is few, and reagent is cheap, and resultant velocity is fast, and do not use strong acid, highly basic, gained carbon nano-particles is nontoxic, convenient for biological marker.Synthesized by present method, carbon nano-particles solution does not need passivation, without the need to being separated and having good fluorescent characteristic, can directly use.
For technical scheme of the present invention is described better, spy provides following examples, but enforcement of the present invention is not limited in this.
Embodiment 1
(1) dissolving of material: take 0.5 gram of citric acid and 0.1 gram of ammonium oxalate mixing, porphyrize in mortar, pours the mixture of porphyrize into beaker, add ethylene glycol 20 milliliters, put into magneton, be placed on magnetic stirrer and stir, until solid dissolves completely, obtain colourless transparent solution.
(2) fluorescent carbon nano-particles generates: poured into by above-mentioned solution in the reactor of liner Teflon, tighten reactor kettle cover, be placed in thermostatic drying chamber in 170 DEG C of heating 3 hours, then from thermostatic drying chamber, take out reactor naturally cool to room temperature, in still, solution is brown color, and the liquid of gained is fluorescent carbon nano-particles solution.
To having carried out fluorescence, UV spectrum sign after the carbon nano-particles solution dilution of this example.See Fig. 1.Best excitation peak is at 354nm as seen from the figure, and optimum transmit peak is at 439nm.Under 365nm ultraviolet lamp, this nanomaterial solution is sky blue, and emission peak and the perfection of excitation peak shape, illustrate nanoparticle uniform particles.Ultra-violet absorption spectrum has strong absorption at 200-300nm, has a broad peak at about 350nm, and consistent at 354nm with best excitation peak, this peak meets carbon nanomaterial feature.
Embodiment 2,
(1) dissolving of material: take 0.5 gram of glucose and 0.05 gram of ammonium oxalate mixing, porphyrize in mortar, pour the mixture of porphyrize into beaker, add ethylene glycol 20 milliliters, put into magneton, be placed on magnetic stirrer and stir, until solid dissolves completely, the liquid of gained is fluorescent carbon nano-particles solution.
(2) fluorescent carbon nano-particles generates: poured into by above-mentioned solution in the reactor of liner Teflon, tighten reactor kettle cover, be placed in thermostatic drying chamber in 140 DEG C of heating 3 hours, then from thermostatic drying chamber, take out reactor naturally cool to room temperature, in still, solution is brown color, and the liquid of gained is fluorescent carbon nano-particles solution.
XRD sign is carried out, as Fig. 4 to this routine carbon nano-particles: a ° appearance broad peak in 2 θ=20, this peak is the characteristic peak of agraphitic carbon, illustrates that this sample is carbon nano-particles.
Embodiment 3
(1) dissolving of material: take 0.5 gram, tartrate and 0.2 gram of ammonium oxalate mixing, porphyrize in mortar, pour the mixture of porphyrize into beaker, add ethylene glycol 20 milliliters, put into magneton, be placed on magnetic stirrer and stir, until solid dissolves completely, the liquid of gained is fluorescent carbon nano-particles solution.
(2) fluorescent carbon nano-particles generates: poured into by above-mentioned solution in the reactor of liner Teflon, tighten reactor kettle cover, be placed in thermostatic drying chamber in 180 DEG C of heating 3 hours, then from thermostatic drying chamber, take out reactor naturally cool to room temperature, in still, solution is brown color, and the liquid of gained is fluorescent carbon nano-particles solution.
Fluorescent Characterization has been carried out to after the carbon nano-particles solution dilution of this example.See Fig. 3, within the scope of excitation wavelength 340-440nm, this sample has good fluorescence property, along with excitation wavelength increases, the obvious red shift of emission peak, has some strength, this fluorescent excellent property is described, particularly also there is stronger VISIBLE LIGHT EMISSION in excited by visible light district, has multicolor property, has potential function.
Claims (2)
1. the method for one-step synthesis fluorescent carbon nano-particles solution, is characterized in that, said method comprising the steps of:
(1) dissolving of material: take 0.5 gram of carbon source material and 0.05-0.5 gram of ammonium oxalate mixing, porphyrize in mortar, pours the mixture of porphyrize into beaker, add ethylene glycol 20 milliliters, put into magneton, be placed on magnetic stirrer and stir, until solid dissolves completely, obtain colourless transparent solution;
(2) fluorescent carbon nano-particles generates: poured into by above-mentioned colourless transparent solution in the reactor of liner Teflon, tighten reactor kettle cover, reactor is placed in thermostatic drying chamber in 140-180 DEG C of heating 3 hours, then from thermostatic drying chamber, take out reactor naturally cool to room temperature, in reactor, solution is brown color, and the liquid of gained is fluorescent carbon nano-particles solution; Described carbon source material is glucose, vitamins C, tartrate, oxysuccinic acid, citric acid, fumaric acid.
2. the method for one-step synthesis fluorescent carbon nano-particles solution according to claim 1, it is characterized in that, the carbon nano-particles of described glucose prepared by carbon source has blue-green fluorescent, and vitamins C is that the carbon nano-particles solution of raw material has green fluorescence, and all the other are sky blue fluorescence.
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