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 PDFInfo
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- 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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- 239000002096 quantum dot Substances 0.000 title claims abstract description 79
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 230000035945 sensitivity Effects 0.000 title description 4
- 238000006862 quantum yield reaction Methods 0.000 claims abstract description 42
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 235000019441 ethanol Nutrition 0.000 claims abstract description 9
- 238000002604 ultrasonography Methods 0.000 claims abstract description 7
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 8
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000005259 measurement Methods 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 description 5
- 230000006378 damage Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000003086 colorant Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005424 photoluminescence Methods 0.000 description 2
- 238000012800 visualization Methods 0.000 description 2
- 208000002177 Cataract Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000000795 conjunctiva Anatomy 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 125000005909 ethyl alcohol group Chemical group 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 206010023332 keratitis Diseases 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 201000005111 ocular hyperemia Diseases 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J1/00—Photometry, e.g. photographic exposure meter
- G01J1/58—Photometry, 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
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.
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Cited By (2)
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 |
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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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 |
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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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