CN106675556B - A kind of novel fluorescence c-based nanomaterial and its preparation method and application - Google Patents

A kind of novel fluorescence c-based nanomaterial and its preparation method and application Download PDF

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CN106675556B
CN106675556B CN201710009189.4A CN201710009189A CN106675556B CN 106675556 B CN106675556 B CN 106675556B CN 201710009189 A CN201710009189 A CN 201710009189A CN 106675556 B CN106675556 B CN 106675556B
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metal ion
based nanomaterial
fcnms
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CN106675556A (en
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王忠霞
王伟
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Yangcheng Institute of Technology
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    • C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N2021/6432—Quenching

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Abstract

Application the invention discloses a kind of fluorescence c-based nanomaterial and preparation method thereof and in terms of colorimetric detection metal ion, the fluorescence c-based nanomaterial are spherulite configuration, and partial size is 5~7nm, containing C, N and O element, a length of 330nm of optimum excitation wave.The present invention synthesizes evenly dispersed FCNMs using simple hydro-thermal method, effectively increase the catalytic performance of c-based nanomaterial, be conducive to the application for making it in catalytic field, it solves FCNMs and only carries out this technical problem of fluorescence detection metal ion, realize metal ion in simple colorimetric detection water body.Fluorescence and colorimetric test show the FCNMs in H2O2Under the action of there is excellent color developing to various metals ion, and be able to achieve H2O2Wide linearity test.Product obtained by the present invention cannot be only used for some substances of fluorescence detection, while apply also for metal ion in colorimetric analysis water body, and be applied to catalytic field as catalyst.

Description

A kind of novel fluorescence c-based nanomaterial and its preparation method and application
Technical field
It is examined the invention belongs to detection field more particularly to a kind of fluorescence c-based nanomaterial and preparation method thereof and in colorimetric Survey metal ion and quantitative detection H2O2The application of aspect.
Background technique
In nature, contaminant metal ions in environment due to can accumulate in vivo enrichment thus increasingly by To the attention of people.If people the organism containing high-concentration metallic ions is eaten for a long time or in containing metal ion and its In the environment of compound, it also may cause some important diseases of the mankind, including certain reproductive systems, nervous system, angiocarpy Chronic disease and some developmental disorders are especially also possible to that some serious child growth problems can be caused.
Fluorescence c-based nanomaterial (FCNMs) makes it in bio-imaging, catalysis, sensing due to its unique optical property Device and optical electro-chemistry etc. are widely used in fields, and especially the FCNMs with certain given activity sites can be with metal The inorganic ions such as cation specifically bind or react and cause under external force the concern of numerous researchers.Currently, sharp Detection technique of fluorescence is mainly used with FCNMs detection metal ion, method therefor needs fluorescence detection equipment, to seriously affect The development of its detection technique.
Summary of the invention
The purpose of the present invention is to provide a kind of novel fluorescence c-based nanomaterials, and provide the preparation method of above-mentioned material With the application in terms of colorimetric detection metal ion.
To achieve the goals above, the invention adopts the following technical scheme: a kind of novel fluorescence c-based nanomaterial, described Fluorescence c-based nanomaterial is spherulite configuration, and partial size is 5~7nm, and containing C, N and O element, optimum excitation wave is a length of 330nm。
The fluorescence c-based nanomaterial is prepared using hydro-thermal method.
A kind of preparation method of novel fluorescence c-based nanomaterial, is prepared using hydro-thermal method, by 1- (3- dimethylamino third Base) -3- ethyl-carbodiimide hydrochloride is placed in a beaker, water and ethyl alcohol is then gradually added, at room temperature ultrasound 30min, then Gained precursor liquid is transferred in the pyroreaction kettle of polytetrafluoroethylene (PTFE), after reacting 8.0h under the conditions of 180 DEG C, is naturally cooled to Room temperature, obtained yellow solution carry out eccentric cleaning, and supernatant saves at 4 DEG C, obtain product.
A kind of application of novel fluorescence c-based nanomaterial in terms of colorimetric detection metal ion, comprising the following steps:
(1) measuring 10.0 μ L concentration is 1.0mg mL-1Fluorescence c-based nanomaterial is placed in the centrifuge tube of 1.5mL, successively The Tris-HNO of 65 μ L 50mmol/L is added3Buffer solution is then respectively adding different metal ion standard solution, hatching 3 ~it is separately added into the hydrogen peroxide of 500mmol/L after ten minutes, its constant volume to 100 μ L is finally stood into reaction 20min with secondary water Afterwards, the variation for observing its solution colour records the color of solution corresponding to different metal ions；
(2) metal ion solution to be measured is detected referring to step 1, observes the variation of its solution colour, according to the color of solution Determine the species of metal ion of metal ion solution to be measured.
Further, Tris-HNO3Buffer solution pH is 6.0.
Further, the concentration of standard solution is 100 μm of ol/L.
A kind of novel fluorescence c-based nanomaterial is in fluorescence detection H2O2The application of aspect, comprising the following steps:
(1) measuring 10.0 μ L concentration is 1.0mg mL-1Fluorescence c-based nanomaterial is placed in the centrifuge tube of 2.0mL, successively The Tris-HNO of 50 μ L 50mM pH 6.0 is added3Buffer solution, 50 μ L copper ion titers, the H of various concentration2O2Standard is molten Liquid, hatching 3~after ten minutes with secondary water by its constant volume to 500 μ L, after finally standing reaction 20min, be in excitation wavelength Under conditions of 330nm, excitation and transmite slit width are 5nm, the variation of its FCNMs maximum fluorescence intensity is surveyed, then according to glimmering The fluorescent quenching degree of light c-based nanomaterial draws standard curve [(FL0-FL)/FL0]；
(2) sample to be tested is tested referring to step 1, according to the mark of the fluorescent quenching degree of test sample to be tested and above-mentioned drafting Directrix curve comparison, obtains corresponding sample to be tested concentration.
Further, the concentration of copper ion titer is 1mmol/L.
FCNMs is synthesized using hydro-thermal method, since a large amount of-COOH ,-OH ,-O- and-NH are contained in surface2Equal hydrophilic groups Group, so that it be made to be dispersed in water phase.
Effectively increase the application range of FCNMs.Fluorometric investigation the result shows that, prepared FCNMs have it is very stable Optical property, the partial size of particle are that the synthesized FCNMs of about 6nm, EDS and XPS characterization mainly contains tri- kinds of elements of C, N, O, and In the presence of hydrogen peroxide, there can be developing response to six metal ion species, and be able to achieve H2O2Quantitative fluorescence detection, effectively improve The application range of doping FCNMs.
By the way that certain density H is added into the fluorescent carbon point mixed liquor containing metal ion in chromogenic reaction2O2, can To carry out the metal ion in effective colorimetric analysis water body, metal ion includes Co2+、Mn2+、Cu2+、Fe2+、Fe3+And Cr3+Deng Six metal ion species.
The invention has the advantages that the present invention synthesizes evenly dispersed FCNMs using simple hydro-thermal method, carbon is effectively increased The catalytic performance of based nano-material is conducive to the application for making it in catalytic field, solves FCNMs and only carries out fluorescence detection gold Belong to this technical problem of ion, realizes metal ion in simple colorimetric detection water body.Fluorescence and colorimetric test show this FCNMs is in H2O2Under the action of there is excellent color developing to various metals ion, and be able to achieve H2O2Wide linearity test.This The obtained product of invention cannot be only used for some substances of fluorescence detection, at the same apply also in colorimetric analysis water body metal from Son, and it is applied to catalytic field as catalyst.
Detailed description of the invention
Fig. 1 is TEM (A), the HRTEM (B) and SAED (C) figure of FCNMs.
Fig. 2 is the EDS figure of FCNMs.
Fig. 3 is the launching light spectrogram of the ultraviolet spectrogram and FCNMs of FCNMs under 330nm excitation.
Fig. 4 is the excitation wavelength optimization figure of FCNMs.
Fig. 5 is FCNMs to pH, ionic strength and storage time fluorescence Quality Research.
Fig. 6 is FCNMs detection metal ion pH optimization figure.
Fig. 7 is FCNMs detection H2O2Ion.
Fig. 8 is FCNMs detection H2O2The investigation of selectivity.
Specific embodiment
The present invention is further elaborated with specific embodiment with reference to the accompanying drawing, and the present invention is not limited thereto.
(1) hydro-thermal method prepares novel FCNMs: weighing 0.55g 1- (3- dimethylamino-propyl) -3- ethyl carbodiimide salt Hydrochlorate (EDC) is placed in 50mL beaker, 12.5mL water and 12.5mL ethyl alcohol is then gradually added, at room temperature ultrasound 30min, then Gained precursor liquid is transferred in the pyroreaction kettle of polytetrafluoroethylene (PTFE), after reacting 8.0h under the conditions of 180 DEG C, is naturally cooled to Room temperature (25 DEG C).Obtained yellow solution carries out eccentric cleaning, and eccentric cleaning revolving speed is 10,000rpm, and centrifugation time is 20min, supernatant save at 4 DEG C, obtain the excellent FCNMs of fluorescence property.
(2) pH value optimizes: the optimum experimental condition in order to obtain highly sensitive detection metal ion, to the pH value of reaction solution It is optimized.Measure the Tris-HNO that 10.0 μ L FCNMs are added sequentially to 50 μ L difference pH value3In buffer solution, then divide It Jia Ru not 500 μM of H2O2, after incubation 20min, it is separately added into the Cu of same concentrations2+Ion is finally determined with secondary water Hold 500 μ L.Under conditions of excitation wavelength is that 330nm, excitation and transmite slit width are 5nm, its FCNMs maximum fluorescence is surveyed The variation of intensity.
(3) novel FCNMs colorimetric analysis metal ion: a kind of process of typical case's colorimetric estimation metal ion is as follows: Measuring 10.0 μ L concentration is 1.0mg mL-1FCNMs is placed in the centrifuge tube of 1.5mL, sequentially adds 65 μ L 50mmol/L's Tris-HNO3Buffer solution is then respectively adding the different metal ion standard solution of 100 μm of ol/L, after hatching 3-10 minutes It is separately added into the hydrogen peroxide of 500mM, its constant volume to 100 μ L is finally observed into its solution after standing reaction 20min with secondary water The variation of color.Referring to above-mentioned steps, changes metal ion standard solution into metal ion solution to be measured, observe its solution colour Variation, the species of metal ion of metal ion solution to be measured is determined according to the color of solution.I.e. according to the color of solution come really What determine that metal ion contained in aqueous solution.
(4) novel FCNMs fluorescence analysis H2O2: a kind of Representative fluorescence measurement H2O2Process it is as follows: measure 10.0 μ L Concentration is 1.0mg mL-1FCNMs is placed in the centrifuge tube of 2.0mL, sequentially adds the Tris-HNO of 50 μ L 50mM pH 6.03It is slow Rush solution, 50 μ L copper ion titers (1mM), the H of various concentration2O2Standard solution, hatching 3-10 minutes after with secondary water by its Constant volume is to 500 μ L, is the item that 330nm, excitation and transmite slit width are 5nm in excitation wavelength after finally standing reaction 20min Under part, the variation of its FCNMs maximum fluorescence intensity is surveyed, then according to the fluorescent quenching degree ([(FL of FCNMs0-FL)/FL0]) draw Standard curve processed, when testing sample to be tested, according to the fluorescent quenching degree ([(FL of test sample to be tested0-FL)/FL0]) with it is above-mentioned The standard curve of drafting compares, and obtains corresponding sample to be tested concentration.
The transmission electron microscope picture (TEM) of obtained FCNMs see Figure 1A, the visible FCNMs of Figure 1A be monodispersed and partial size compared with Uniform spherical particle, HRTEM (interior illustration, B) and electronic diffraction structure (SAED schemes C) are analysis shows that go out to use party's legal system Standby FCNMs is crystal configuration, and partial size is about 5~7nm (interior illustration).
Fig. 2 proves that prepared FCNMs mainly contains tri- kinds of elements of C, N and O.
The ultraviolet spectrogram and transmitting fluorescence spectra that Fig. 3 is FCNMs.
Fig. 4 has found that optimal excitation wavelength is at 330nm by the optimization to FCNMs excitation wavelength.
Fig. 5 has studied FCNMs and is studied ionic strength, pH value of solution and storage time, research shows that synthesis FCNMs has good optical stability under various conditions.
The pH that Fig. 6 detects metal ion to it is optimized, and optimum results show that optimal pH is 6.0.FCNMs is in pH= 6.0Tris-HNO3The ratio colour response of different metal ions and corresponding fluorescence photo are shown in buffer solution: FCNMs pairs Co2+、Mn2+、Cu2+、Fe2+、Fe3+And Cr3+Six metal ion species have apparent developing response.
Fig. 7 is FCNMs in pH=6.0Tris-HNO3To various concentration H in buffer solution2O2Fluorescence response, as a result table Bright FCNMs is to H2O2With the wider range of linearity.
Fig. 8 is (Tris-HNO under the conditions of same detection3, pH=6.0) and H that it is constructed2O2Sensor is selected Property investigation, as the result is shown based on FCNMs to H2O2Detection has selectivity well, the above result shows that, FCNMs is to H2O2 And Cu2+Ion has good fluorescence response.
The above is only preferred embodiments of the invention, not does any type of limitation to the present invention.It is all according to According to technology and methods essence of the invention to any simple modification, equivalent change and modification made by above example, still fall within In the range of technology and methods scheme of the invention.

Claims (7)

1. a kind of fluorescence c-based nanomaterial, it is characterised in that: the fluorescence c-based nanomaterial is spherulite configuration, partial size For 5~7nm, containing C, N and O element, a length of 330nm of optimum excitation wave；
The fluorescence c-based nanomaterial is prepared using hydro-thermal method；Specific targets method is as follows: by 1- (3- dimethylamino third Base) -3- ethyl-carbodiimide hydrochloride is placed in a beaker, water and ethyl alcohol is then gradually added, at room temperature ultrasound 30min, then Gained precursor liquid is transferred in the pyroreaction kettle of polytetrafluoroethylene (PTFE), after reacting 8.0h under the conditions of 180 DEG C, is naturally cooled to Room temperature, obtained yellow solution carry out eccentric cleaning, and supernatant saves at 4 DEG C, obtain product.
2. a kind of preparation method of fluorescence c-based nanomaterial according to claim 1, it is characterised in that: use hydro-thermal legal system It is standby, 1- (3- dimethylamino-propyl) -3- ethyl-carbodiimide hydrochloride is placed in a beaker, water and ethyl alcohol is then gradually added, Gained precursor liquid, is then transferred in the pyroreaction kettle of polytetrafluoroethylene (PTFE) by ultrasound 30min at room temperature, under the conditions of 180 DEG C After reacting 8.0h, cooled to room temperature, obtained yellow solution carries out eccentric cleaning, and supernatant is saved at 4 DEG C, that is, made Obtain product.
3. a kind of application of the fluorescence c-based nanomaterial in terms of colorimetric detection metal ion according to claim 1, special Sign be the following steps are included:
(1) measuring 10.0 μ L concentration is 1.0mg mL-1Fluorescence c-based nanomaterial is placed in the centrifuge tube of 1.5mL, is sequentially added The Tris-HNO of 65 μ L 50mmol/L3Buffer solution is then respectively adding different metal ion standard solution, hatching 3~10 The hydrogen peroxide of 500mmol/L is separately added into after minute, finally with secondary water by its constant volume to 100 μ L, after standing reaction 20min, The variation for observing its solution colour records the color of solution corresponding to different metal ions；
(2) metal ion solution to be measured is detected referring to step 1, observes the variation of its solution colour, determined according to the color of solution The species of metal ion of metal ion solution to be measured, the metal ion are Co2+、Mn2+、Cu2+、Fe2+、Fe3+Or Cr3+。
4. application according to claim 3, it is characterised in that: the Tris-HNO3Buffer solution pH is 6.0.
5. application according to claim 3, it is characterised in that: the concentration of the standard solution is 100 μm of ol/L.
6. a kind of fluorescence c-based nanomaterial according to claim 1 is in fluorescence detection H2O2The application of aspect, it is characterised in that The following steps are included:
(1) measuring 10.0 μ L concentration is 1.0mg mL-1Fluorescence c-based nanomaterial is placed in the centrifuge tube of 2.0mL, is sequentially added The Tris-HNO of 50 μ L 50mM pH 6.03Buffer solution, 50 μ L copper ion titers, the H of various concentration2O2Standard solution is incubated Change 3~and after ten minutes with secondary water by its constant volume to 500 μ L, after finally standing reaction 20min, it is 330nm, swashs in excitation wavelength Under conditions of hair and transmite slit width are 5nm, the variation of its FCNMs maximum fluorescence intensity is surveyed, is then received according to fluorescence is carbon-based The fluorescent quenching degree of rice material draws standard curve [(FL0-FL)/FL0]；
(2) sample to be tested is tested referring to step 1, the standard according to the fluorescent quenching degree of test sample to be tested and above-mentioned drafting is bent Line comparison, obtains corresponding sample to be tested concentration.
7. application according to claim 6, it is characterised in that: the concentration of the copper ion titer is 1mmol/L.
CN201710009189.4A 2017-01-06 2017-01-06 A kind of novel fluorescence c-based nanomaterial and its preparation method and application Expired - Fee Related CN106675556B (en)

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CN105802621A (en) * 2016-04-05 2016-07-27 南京理工大学 N-CQDs (nitrogen-doped carbon quantum dots) with high fluorescence quantum yield as well as preparation method and application of N-CQDs

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CN105802621A (en) * 2016-04-05 2016-07-27 南京理工大学 N-CQDs (nitrogen-doped carbon quantum dots) with high fluorescence quantum yield as well as preparation method and application of N-CQDs

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Highly Luminescent N-Doped Carbon Quantum Dots as an Effective Multifunctional Fluorescence Sensing Platform;Zhaosheng Qian et al.;《Chem. Eur. J.》;20140121;第20卷;2254-2263

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