CN108946708A - A kind of preparation method of high sensitivity graphene quantum dot ultraviolet detector - Google Patents

A kind of preparation method of high sensitivity graphene quantum dot ultraviolet detector Download PDF

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Publication number
CN108946708A
CN108946708A CN201810711089.0A CN201810711089A CN108946708A CN 108946708 A CN108946708 A CN 108946708A CN 201810711089 A CN201810711089 A CN 201810711089A CN 108946708 A CN108946708 A CN 108946708A
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China
Prior art keywords
quantum dot
graphene quantum
graphene
yield
fluorescence
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CN201810711089.0A
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Inventor
陈爱英
史羽隆
张轶辉
向俊明
马瑶
王现英
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/184Preparation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • 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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01JMEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J1/00Photometry, e.g. photographic exposure meter
    • G01J1/58Photometry, e.g. photographic exposure meter using luminescence generated by light

Abstract

The present invention provides a kind of preparation methods of graphene quantum dot ultraviolet detector, include the steps for preparing a graphene quantum dot, weigh citric acid, benzenediol, the molar ratio of citric acid and benzenediol is 1:0.5-5,15 ~ 35min of ultrasound after mixing, the hydro-thermal at 120-180 DEG C, is then cleaned with ethyl alcohol again, obtains the graphene quantum dot of different quantum yields;Choose the quantum dot of following different quantum yields, using a disk container, there are four independent spaces for the disk container tool, the graphene quantum dot of above-mentioned different quantum yields are encapsulated into respectively in four independent spaces to get graphene quantum dot ultraviolet detector is arrived.The graphene quantum dot of different quantum yields is fitted into special container by the present invention, is fabricated to ultraviolet detector, is applied in production and living through measurement uitraviolet intensity to have the function that pre- antiultraviolet.

Description

A kind of preparation method of high sensitivity graphene quantum dot ultraviolet detector
Technical field:
The invention belongs to chemical fields, are related to a kind of preparation method of graphene quantum dot, specifically a kind of Gao Ling The preparation method of sensitivity graphene quantum dot ultraviolet detector.
Background technique:
Under no safeguard procedures, ultraviolet light easily causes huge harm human body.If exposed skin is exposed to one Under the ultraviolet light for determining intensity, less serious case will appear redness, pain is itched, furfur;Severe one even can cause canceration, skin neoplasin etc..Meanwhile It is also " the stealthy killer " of eyes, can cause conjunctiva, corneal inflammation, long-term irradiation may result in cataract.
Grapheme material is as the big hot spot in terms of material scientific research at present, and graphene quantum dot be even more have it is unique Performance, such as luminescence generated by light behavior.The photoluminescence property of graphene quantum dot, so that graphene quantum dot is under ultraviolet light irradiation Fluorescence can be issued, due to modified graphene quantum dot preparation process very simple, stability is relatively high, and quantum yield is higher etc. Advantage can be used for production ultraviolet detector.
Summary of the invention:
The present invention provides a kind of preparation method of highly sensitive graphene quantum dot ultraviolet detector, this height The method that the preparation method of sensitivity graphene quantum dot ultraviolet detector will solve to detect ultraviolet light in the prior art is complicated, at This high technical problem.
The present invention provides a kind of preparation methods of graphene quantum dot ultraviolet detector, include the following steps:
1) prepare graphene quantum dot the step of, citric acid, benzenediol are weighed, the benzenediol is catechol Either any one in hydroquinone or resorcinol, the molar ratio of the citric acid and benzenediol are 1:0.5-5, are mixed It closes 15~35min of ultrasound, the hydro-thermal 4-20h at 120-180 DEG C after stirring then to be cleaned 2~5 times with ethyl alcohol again, obtain different The graphene quantum dot of quantum yield and fluorescence color;
2) quantum dot for choosing following different quantum yields, is added water or organic solvent makes the dense of the quantum dot Degree is 10 μ g/L-20mg/L;
(a) the quantum yield 10-20% of graphene quantum dot;
(b) the quantum yield 30-40% of graphene quantum dot;
(c) the quantum yield 50-60% of graphene quantum dot;
(d) the quantum yield 60-80% of graphene quantum dot;
Using a disk container, there are four independent spaces for the disk container tool, by above-mentioned different quantum yields Graphene quantum dot be encapsulated into four independent spaces respectively to get to graphene quantum dot ultraviolet detector.
Further,
(a) when the quantum yield of graphene quantum dot is 10-20%, when detecting ultraviolet light, which is displayed in red glimmering Light;
(b) when the quantum yield of graphene quantum dot is 30-40%, when detecting ultraviolet light, region display green is glimmering Light;
(c) when the quantum yield of graphene quantum dot is 50-60%, when detecting ultraviolet light, which shows that yellow is glimmering Light;
(d) when the quantum yield of graphene quantum dot is 60-80%, when detecting ultraviolet light, which is displayed in blue glimmering Light.
Specifically, the organic solvent is ethyl alcohol.
The present invention includes the steps that the graphene quantum dot of the different quantum yields of a synthesis, by hydro-thermal method, changes real Condition is tested to obtain the graphene quantum dot of different quantum yields;The graphene quantum dot of different quantum yields is packed into specific appearance The step of device to get arrive graphene quantum dot ultraviolet detector.
Inventive principle of the invention is: the power of ultraviolet light, benefit are shown using the graphene quantum dot of different quantum yields Uv damage degree is warned with different fluorescence colors.
After tested, the graphene quantum dot of different quantum yields shows the glimmering of different colours to the present invention under ultraviolet light Light, when the fluorescence that can issue different colours, varying strength under ultraviolet irradiation, quantum yield is higher, and fluorescence is stronger. Using its ultraviolet photoluminescence characteristic, we are used for production ultraviolet detector, apply and pass through measurement in production and living Uitraviolet intensity is to have the function that pre- antiultraviolet.We according to the quantum yield of graphene quantum dot size order by its It is put into a discoid different zones, when uitraviolet intensity is very low, when substantially harmless to human body, each area of detector Domain does not issue fluorescence, and with the increase of uitraviolet intensity, and quantum yield is highest to issue fluorescence at first, uitraviolet intensity after Continuous to increase, then the region for issuing fluorescence is increased in succession.
The present invention makes ultraviolet detector using graphene quantum dot, produces purple using different graphene quantum dot solutions External detector, the ultraviolet detector has the characteristics that visualization, cheap, can spread in the life of ordinary people, subtract Few harm being subject to by ultraviolet light.People can be allowed whether easily to detect to home with the presence of ultraviolet light.It can accomplish to shift to an earlier date Prevention avoids the direct projection for being in ultraviolet light for a long time from causing disease.
The present invention is compared with prior art, and technological progress is significant.Present invention visualization: can be clear with eyes It observes with the presence or absence of ultraviolet light, the power and degree of danger of ultraviolet light.The present invention is low in cost;Graphene quantum dot it is dense Degree is very low, and dosage is few, at low cost.Detector preparation of the present invention is simple, encapsulation.
Detailed description of the invention:
The PL figure that Fig. 1 is GQDs in embodiment 1.
The PL figure that Fig. 2 is GQDs in embodiment 2.
Fig. 3 is the picture of graphene quantum dot ultraviolet detector under visible light in embodiment 4.
Fig. 4 is the fluorescence picture of graphene quantum dot ultraviolet detector under ultraviolet light in embodiment 4.
Embodiment 1
Graphene quantum dot preparation method:
1) using citric acid and resorcinol as raw material, molar ratio 1:3, ultrasound 20min, the hydro-thermal at 180 DEG C after stirring 8h.Ethyl alcohol cleans three times.The graphene quantum dot of different quantum yields and fluorescence color can be prepared.Quantum yield is 63%. Fluorescence color is blue, sees that attached drawing 1PL is composed.
2) this quantum dot solution is chosen, it is 15 μ g/L that distilled water, which is added, and obtains the concentration of quantum dot, takes 25ml, encloses circle In disc shaped container.
Embodiment 2
Graphene quantum dot preparation method:
1) using citric acid and catechol as raw material, molar ratio 1:5, ultrasound 20min, the hydro-thermal at 120 DEG C after stirring 4h.Ethyl alcohol cleans three times.The graphene quantum dot of different quantum yields and fluorescence color can be prepared.Quantum yield is 56%. Fluorescence color is yellow, sees that 2 PL of attached drawing is composed.
2) this quantum dot solution is chosen, it is 1mg/L that distilled water, which is added, and obtains the concentration of quantum dot, takes 25 ml, encloses disk In shape container.
Embodiment 3
Graphene quantum dot preparation method:
1) using citric acid and hydroquinone as raw material, molar ratio 1:0.5, ultrasound 20min, is lauched at 160 DEG C after stirring Hot 6h.Ethyl alcohol cleans three times.The graphene quantum dot of different quantum yields and fluorescence color can be prepared.Quantum yield is 34%.Fluorescence color is green.
2) this quantum dot solution is chosen, the concentration of quantum dot is 100 μ g/L, takes 25ml, encloses in discoid container.
Embodiment 4
Graphene quantum dot preparation method:
1) using citric acid and hydroquinone as raw material, molar ratio 1:4, ultrasound 20min, the hydro-thermal at 180 DEG C after stirring 18h.Ethyl alcohol cleans three times.The graphene quantum dot of different quantum yields and fluorescence color can be prepared.Quantum yield is 14%. Fluorescence color is red.
2) this quantum dot solution is chosen, it is 20mg/L that alcohol solvent, which is added, and obtains the concentration of quantum dot, takes 25ml, encloses circle In disc shaped container.The detector figure prepared under visible light is shown in attached drawing 3.Under ultraviolet light, the color of detector is shown in attached drawing 4.
Under the ultraviolet light irradiation of 365nm, when the graphene quantum dot ultraviolet lamp distance of red fluorescence is 4m, naked eyes red color visible Fluorescence.Green fluorescence graphene quantum dot away from ultraviolet lamp be 6m when, naked eyes visible green fluorescence.The graphene quantum of yellow fluorescence When point away from ultraviolet lamp is 8m, naked eyes visible yellow color fluorescence.The graphene quantum dot of blue-fluorescence away from be 10m away from ultraviolet lamp When, naked eyes visible blue fluorescence.The power of ultraviolet light is judged by fluorescence color and colour developing distance, and is warned.For example, molten When liquid issues blue-fluorescence, illustrates to exist in environment there are faint ultraviolet light but intensity is not high, do not cause to seriously endanger.But When issuing red fluorescence, illustrates uitraviolet intensity height, human injury can be caused, provide and warn, it is dangerous, it not continue close to purple External source.

Claims (2)

1. a kind of preparation method of graphene quantum dot ultraviolet detector, it is characterised in that include the following steps:
1) citric acid, benzenediol are weighed prepare graphene quantum dot the step of, the benzenediol be catechol or The molar ratio of any one in hydroquinone or resorcinol, the citric acid and benzenediol is 1:0.5-5, and mixing is stirred After mixing then 15~35min of ultrasound, the hydro-thermal 4-20h at 120-180 DEG C are cleaned 2~5 times again with ethyl alcohol, obtain different quantum The graphene quantum dot of yield and fluorescence color;
2) quantum dot for choosing following different quantum yields, is added water or organic solvent makes the concentration of the quantum dot to be 10μg/L-20mg/L;
(a) the quantum yield 10-20% of graphene quantum dot;
(b) the quantum yield 30-40% of graphene quantum dot;
(c) the quantum yield 50-60% of graphene quantum dot;
(d) the quantum yield 60-80% of graphene quantum dot;
Using a disk container, there are four independent spaces for the disk container tool, by the stone of above-mentioned different quantum yields Black alkene quantum dot is encapsulated into four independent spaces to arrive graphene quantum dot ultraviolet detector respectively.
2. a kind of preparation method of graphene quantum dot ultraviolet detector according to claim 1, it is characterised in that:
(a) when the quantum yield of graphene quantum dot is 10-20%, when detecting ultraviolet light, which is displayed in red fluorescence;
(b) when the quantum yield of graphene quantum dot is 30-40%, when detecting ultraviolet light, which shows green fluorescence;
(c) when the quantum yield of graphene quantum dot is 50-60%, when detecting ultraviolet light, which shows yellow fluorescence;
(d) when the quantum yield of graphene quantum dot is 60-80%, when detecting ultraviolet light, which is displayed in blue fluorescence.
CN201810711089.0A 2018-07-02 2018-07-02 A kind of preparation method of high sensitivity graphene quantum dot ultraviolet detector Pending CN108946708A (en)

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CN110697691A (en) * 2019-09-04 2020-01-17 西安交通大学 Graphene quantum dot material with high ultraviolet absorption characteristic and lipophilicity and preparation method thereof
CN111234817A (en) * 2020-03-02 2020-06-05 太原理工大学 Carbon dots with high thermal stability and preparation method thereof

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN110697691A (en) * 2019-09-04 2020-01-17 西安交通大学 Graphene quantum dot material with high ultraviolet absorption characteristic and lipophilicity and preparation method thereof
CN110697691B (en) * 2019-09-04 2020-08-28 西安交通大学 Graphene quantum dot material with high ultraviolet absorption characteristic and lipophilicity and preparation method thereof
CN111234817A (en) * 2020-03-02 2020-06-05 太原理工大学 Carbon dots with high thermal stability and preparation method thereof
CN111234817B (en) * 2020-03-02 2020-11-06 太原理工大学 Carbon dots with high thermal stability and preparation method thereof

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