CN105752958B - A kind of synthetic method of carbon nano-cluster and its application - Google Patents

A kind of synthetic method of carbon nano-cluster and its application Download PDF

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Publication number
CN105752958B
CN105752958B CN201610118766.9A CN201610118766A CN105752958B CN 105752958 B CN105752958 B CN 105752958B CN 201610118766 A CN201610118766 A CN 201610118766A CN 105752958 B CN105752958 B CN 105752958B
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cluster
carbon nano
carbon
quantum dot
agar
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CN105752958A (en
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刘萍萍
周会娜
陈千思
翟妞
金立锋
郑庆霞
陈霞
张慧
王晨
徐国云
林福呈
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Zhengzhou Tobacco Research Institute of CNTC
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Zhengzhou Tobacco Research Institute of CNTC
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    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/65Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
    • 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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/51Particles with a specific particle size distribution
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/60Optical properties, e.g. expressed in CIELAB-values

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  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

A kind of synthetic method of carbon nano-cluster and its application, it is characterised in that:This method comprises the following steps:1)A certain amount of agar and ammonium sulfate are mixed;2)Deionized water is added in, is stirred evenly;3)Mixed solution is put into Muffle furnace reaction kettle and is reacted, 4)Solution takes out 15000 rpm centrifugations after reacting;5)0.22 μm of water phase filtering;6)Chloroform, ethyl acetate aqueous phase extracted, obtain carbon nanometer a small bundle of straw, etc. for silkworms to spin cocoons on namely carbon quantum dot after dialysis.It is demonstrated experimentally that the carbon quantum dot form of the method for the present invention synthesis is uniform, particle size distribution range is relatively narrow, and fluorescence intensity is high.The carbon nano-cluster that the present invention is synthesized is applied to technical field in terms of biomarker, identification, has many advantages, such as that stability is strong, bio-compatible is good, has a very broad application prospects.

Description

A kind of synthetic method of carbon nano-cluster and its application
Technical field
The present invention relates to bio-nanotechnology field, the synthetic method of specifically a kind of carbon nano-cluster and its in fluorescence mark Note, the application in ion identification field.
Background technology
Carbon nano-cluster is made of tens to hundreds of carbon atoms, usual 2nm of grain size or so.Since its grain size approaches Fermi's wavelength of electronics, therefore it has the optical property different from large-sized particle, chemical property and electrical properties.As A kind of novel fluorescence nano material, carbon nano-cluster have many advantages, such as that photostability is strong, bio-compatibility is good, have extremely wide answer Use prospect.
Invention content
The purpose of the present invention is based on above-mentioned prior art situation and provides a kind of synthetic method of new carbon nano-cluster And its fluorescent marker, ion identification field application application.
The purpose of the present invention is achieved through the following technical solutions:
A kind of synthetic method of carbon nano-cluster, comprises the following specific steps that:
1)A certain amount of agar and ammonium sulfate are mixed, the mass ratio of agar and ammonium sulfate is 1: 0.2-0.3;
2)Deionized water is added in, addition is agar and 30-50 times of ammonium sulfate gross mass, is stirred evenly;
3)Mixed solution is put into Muffle furnace reaction kettle and is reacted, 200-240 DEG C of temperature, time 10-15 hour;
4)Solution takes out 15000 rpm centrifugations after reacting, and collects centrifugate and abandons precipitation;
5)0.22 μm of water phase filtering;
6)Chloroform, ethyl acetate distinguish aqueous phase extracted successively, and carbon nanometer a small bundle of straw, etc. for silkworms to spin cocoons on namely carbon quantum dot are obtained after dialysis.
In the present invention, the dialysis molecular cut off is 1000 Da, i.e., retains 1000 more than Da's with bag filter.
Prepared carbon nanocluster size is 462 nm in 1-1.7nm, excitation wavelength 375nm, launch wavelength.
The carbon quantum dot is water solubility.
Utilize the application of carbon nanometer a small bundle of straw, etc. for silkworms to spin cocoons on prepared by the method for the present invention in terms of fluorescent marker, example identification response.
The advantage of the invention is that:Synthesized carbon quantum dot form is uniform, and particle distribution range is relatively narrow, fluorescence intensity It is high.The carbon nano-cluster of the invention synthesized is applied to biomarker, identification aspect technical field, it is strong, biological simultaneous with stability It has a very broad application prospects the advantages that having held.
Description of the drawings
Fig. 1 is the carbon quantum dot excitation wavelength of the present invention, emission wavelength spectra figure.
Fig. 2 is the transmission electron microscope picture of carbon nano-cluster.
Fig. 3 is the grain size distribution of carbon nano-cluster of the present invention.
Specific embodiment
The present invention is described further below in conjunction with specific experiment method:
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
The preparation method of carbon quantum dot used in following embodiments:
A kind of synthetic method of carbon nano-cluster, comprises the following specific steps that:
1)The ammonium sulfate of the agar of 0.4g and 0.08g are mixed;
2)20mL deionized waters are added in, are stirred evenly;
3)Mixed solution is put into Muffle furnace reaction kettle in 220 DEG C of reactions, 12 hours time;
4)Solution takes out 15000 rpm centrifugations after reacting, and collects centrifugate and abandons precipitation;
5)0.22 μm of water phase filtering;
6)Chloroform(About 20mL), ethyl acetate(About 20mL)Aqueous phase extracted is distinguished successively, and carbon nanometer a small bundle of straw, etc. for silkworms to spin cocoons on is obtained after dialysis That is carbon quantum dot.Dialysis molecular cut off is 1000 Da, i.e., retains 1000 more than Da's with bag filter.
The feature of prepared carbon nano-cluster is as follows:
1st, carbon nano-cluster is spherical shape;
2nd, the carbon nanocluster size is in 1-1.7nm;The carbon quantum dot is water solubility;
3rd, the excitation wavelength of the carbon nano-cluster is 375nm, and launch wavelength is 462 nm.
The characterization of carbon nano-cluster used in following embodiments:
Characterization:Above-mentioned quantum-dot structure is scanned transmission electron microscope and excitation spectrum and emission spectrum, as a result such as Fig. 1 institutes Show.
Transmission electron microscope picture shows that synthesized quantum dot is spherical in shape, and particle diameter distribution is uniform(Referring to Fig. 2,3).
Fluorescence spectrum characterization:Fluoremetry is carried out using luminoscope, first fixed transmission wavelength is 462 nm, and scanning fluorescence swashs Luminous spectrum obtains 375 nm of maximum excitation wavelength;Again using 375 nm as excitation wavelength, quantum dot fluorescence emission spectrum is scanned.
As a result:Fluorescence excitation spectrum shows that the quantum dot has wider excitation wavelength range, from 300 nm to 450 nm; Fluorescence emission wavelengths are in 462 nm or so.Obtained carbon quantum dot product is clear solution, has good water solubility.
Application example:The carbon nano-cluster that the present invention is synthesized is applied to technical field in terms of biomarker, identification, stability By force, bio-compatible is good.

Claims (3)

1. a kind of synthetic method of carbon nano-cluster, it is characterised in that:This method comprises the following steps:
1)A certain amount of agar and ammonium sulfate are mixed, the mass ratio of agar and ammonium sulfate is 1: 0.2-0.3
2)Deionized water is added in, addition is agar and 30-50 times of ammonium sulfate gross mass, is stirred evenly;
3)Mixed solution is put into Muffle furnace reaction kettle and is reacted, 200-240 DEG C of temperature, time 10-15 hour;
4)Solution takes out 15000 rpm centrifugations after reacting, and collects centrifugate and abandons precipitation;
5)0.22 μm of water phase filtering;
6)Chloroform, ethyl acetate distinguish aqueous phase extracted successively, and carbon nano-cluster namely carbon quantum dot, dialysis retention are obtained after dialysis Molecular weight is 1000 Da;Prepared carbon nanocluster size is in 1-1.7nm, excitation wavelength 375nm, launch wavelength 462 nm。
2. the synthetic method of carbon nano-cluster according to claim 1, it is characterised in that:The carbon quantum dot is water solubility.
3. a kind of application of carbon nano-cluster prepared using claim 1 the method in terms of fluorescent marker ion identification.
CN201610118766.9A 2016-03-03 2016-03-03 A kind of synthetic method of carbon nano-cluster and its application Active CN105752958B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102942170A (en) * 2012-10-22 2013-02-27 上海交通大学 Preparation method of carbon quantum dots based on atmospheric pressure micro-plasma technology
CN103361047A (en) * 2012-03-28 2013-10-23 中国科学院大连化学物理研究所 Functional fluorescence carbon nanoparticles based on natural saccharide materials and preparation method and application thereof
CN103708447A (en) * 2013-12-27 2014-04-09 中国科学院上海微***与信息技术研究所 Method for purifying graphene oxide quantum dots
CN105154076A (en) * 2015-10-15 2015-12-16 青岛大学 Method for preparing fluorescent carbon quantum dots by using hydrothermal method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103361047A (en) * 2012-03-28 2013-10-23 中国科学院大连化学物理研究所 Functional fluorescence carbon nanoparticles based on natural saccharide materials and preparation method and application thereof
CN102942170A (en) * 2012-10-22 2013-02-27 上海交通大学 Preparation method of carbon quantum dots based on atmospheric pressure micro-plasma technology
CN103708447A (en) * 2013-12-27 2014-04-09 中国科学院上海微***与信息技术研究所 Method for purifying graphene oxide quantum dots
CN105154076A (en) * 2015-10-15 2015-12-16 青岛大学 Method for preparing fluorescent carbon quantum dots by using hydrothermal method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
One-step hydrothermal approach to fabricate carbon dots from apple juice for imaging of mycobacterium and fungal cells;Vaibhavkumar N. Mehtaa et al.;《Sensors and Actuators B: Chemical》;20150303;第213卷;434-443 *

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