CN107033893A - Preparation method with double centre of luminescence fluorescent carbon points - Google Patents
Preparation method with double centre of luminescence fluorescent carbon points Download PDFInfo
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- CN107033893A CN107033893A CN201710414174.6A CN201710414174A CN107033893A CN 107033893 A CN107033893 A CN 107033893A CN 201710414174 A CN201710414174 A CN 201710414174A CN 107033893 A CN107033893 A CN 107033893A
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- fluorescent carbon
- carbon point
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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
- C09K11/70—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus
Abstract
There is pair preparation method of centre of luminescence fluorescent carbon points the invention discloses a kind of, this method is using diammonium hydrogen phosphate as composition adjusting control agent, ethanol is passivator, is modified using solvent-thermal method and etches the fluorescent carbon point that coal is obtained through hydrogen peroxide oxidation, final to obtain dual wavelength luminous fluorescent carbon point.Dual color light emitting carbon point obtained by preparation method disclosed by the invention has containing two kinds of heterogeneous element groups such as N, P, the property with visible absorption, with advantages such as colorimetric pH value detection properties.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of to have pair preparation side of centre of luminescence fluorescent carbon points
Method.
Background technology
Due to it is good it is water-soluble, be easy to surface-functionalized, good biocompatibility and the spy such as excellent luminescence generated by light
Property, fluorescent carbon point, particularly multicolor fluorescence transmitting carbon point, biological detection, fluorescence labeling, pharmaceutical carrier, fluorescent optical sensor,
The fields such as photocatalysis, solar energy conversion have important application value.For a long time, fluorescent carbon point is mostly ultra-blue-light, green glow
Deng based on, it is difficult to obtain the adjustable fluorescent emission of polychrome.Research is found recently, by controlling nitrogen, oxygen containing in fluorescent carbon point
Amount and combination result in the carbon point lighted with longer wavelength, such as gold-tinted, orange light, feux rouges carbon point.But, control
Nitrogen processed, the oxygen method and combination of content in fluorescent carbon point not only need to select the organic molecule system of specific structure
Standby, in addition it is also necessary to strict contrived experiment condition, therefore, the preparation cost of current multicolor fluorescence carbon point is very high, so that limiting it
Extensive use.Inorganic salts are cheap and are easily obtained, and adjust the composition in fluorescent carbon point to realize multicolor fluorescence with it
Transmitting is expected to that product cost is greatly reduced, and still, corresponding effective ways is still lacked at present.
Fluorescent material with dual color light emitting center, which is contemplated that in colorimetric fluorescence probe field, has highly important application.
But colorimetric fluorescence probe is this mode by being combined obtained from the material of two kinds of different glow colors or wavelength mostly at present
Obtaining colorimetric fluorescence probe, not only combined coefficient is low, process is cumbersome, and cost height, not transreplication.
The content of the invention
It is contemplated that overcoming current multicolor fluorescence carbon point to prepare, cost is high, colorimetric fluorescence probe combined coefficient is low, cost
It is high, not transreplication the shortcomings of, disclose a kind of utilization inorganic salts regulation carbon point composition has pair system of centre of luminescence fluorescent carbon points
Preparation Method.
The present invention is achieved by the following technical solutions：
Preparation method with double centre of luminescence fluorescent carbon points uses following steps：
(1) the m milliliters of blue emission fluorescent carbon point solution prepared with dioxygen water etching coal and n milliliters of absolute ethyl alcohols are taken
Solution is mixed, wherein m:N=0.9-1.2；
(2) toward the diammonium hydrogen phosphate solid particle of w grams of addition in the mixed solution of step (1), and made by ultrasonic vibration
It is completely dissolved, and the molar concentration of diammonium hydrogen phosphate is 2-7g/L after dissolving；
(3) mixed solution obtained in step (2) is transferred in polytetrafluoroethyllining lining reactor, then dried in air blast
In case at 150~220 DEG C, 10~15 hours are incubated；Again after cooling, the fluorescent carbon point with red, yellow two glow peaks is obtained
Solution.
Ethanol solution in step (1) can be replaced absolute methanol solution.
The present invention compared with prior art, resulting dual color light emitting carbon point have containing two kinds of heterogeneous element groups such as N, P,
Property with visible absorption, with the colorimetric pH value detection advantage such as property.
Brief description of the drawings
Fig. 1 is the transmission electron microscope photo of the luminous carbon point of double-colored wavelength prepared by the present invention；
Fig. 2 is luminous luminescence generated by light spectrogram of the carbon point under different excitation wavelengths of the double-colored wavelength of the invention prepared；
Fig. 3 is the optical absorption spectrogram of the luminous carbon point of double-colored wavelength prepared by the present invention；
Fig. 4 is the infrared spectrogram of the luminous carbon point of double-colored wavelength prepared by the present invention；
Fig. 5 is the x-ray photoelectron spectroscopy figure of the luminous carbon point of double-colored wavelength prepared by the present invention；
Dual color light emitting peaks of the Fig. 6 for the luminous carbon point of the double-colored wavelength of the invention prepared at various ph values.
Fig. 7 is the luminous carbon point dual color light emitting peak intensity ratio of the double-colored wavelength of the invention prepared and the linear relationship of pH value.
Embodiment
Detailed technology scheme of the present invention is introduced below in conjunction with accompanying drawing：
Preparation method with double centre of luminescence fluorescent carbon points uses following steps：
(1) the m milliliters of blue emission fluorescent carbon point solution prepared with dioxygen water etching coal and n milliliters of absolute ethyl alcohols are taken
Solution is mixed, wherein m:N=0.9-1.2；
(2) toward the diammonium hydrogen phosphate solid particle of w grams of addition in the mixed solution of step (1), and made by ultrasonic vibration
It is completely dissolved, and the molar concentration of diammonium hydrogen phosphate is 2-7g/L after dissolving；
(3) mixed solution obtained in step (2) is transferred in polytetrafluoroethyllining lining reactor, then dried in air blast
In case at 150~220 DEG C, 10~15 hours are incubated；Again after cooling, the fluorescent carbon point with red, yellow two glow peaks is obtained
Solution.
The method for preparing blue emission fluorescent carbon point solution with dioxygen water etching coal is shown in granted patent
(ZL201510417503.3)。
Ethanol solution in step (1) can be replaced absolute methanol solution.
Embodiment 1
Preparation method with double centre of luminescence fluorescent carbon points uses following steps：
(1) take 100 milliliters of blue emission fluorescent carbon point solution prepared with dioxygen water etching coal and 90 milliliters it is anhydrous
Ethanol solution is mixed；
(2) toward the diammonium hydrogen phosphate solid particle of 0.76 gram of addition in the mixed solution of step (1), and ultrasonic vibration is passed through
It is completely dissolved it, the molar concentration of diammonium hydrogen phosphate is 4g/L after dissolving；
(3) mixed solution obtained in step (2) is transferred in polytetrafluoroethyllining lining reactor, then dried in air blast
In case at 200 DEG C, 12 hours are incubated；Again after cooling, the fluorescent carbon point solution with red, yellow two glow peaks is obtained.
Embodiment 2
Preparation method with double centre of luminescence fluorescent carbon points uses following steps：
(1) take 100 milliliters of blue emission fluorescent carbon point solution prepared with dioxygen water etching coal and 90 milliliters it is anhydrous
Methanol solution is mixed；
(2) toward the diammonium hydrogen phosphate solid particle of 0.76 gram of addition in the mixed solution of step (1), and ultrasonic vibration is passed through
It is completely dissolved it, the molar concentration of diammonium hydrogen phosphate is 4g/L after dissolving；
(3) mixed solution obtained in step (2) is transferred in polytetrafluoroethyllining lining reactor, then dried in air blast
In case at 200 DEG C, 12 hours are incubated；Again after cooling, the fluorescent carbon point solution with red, yellow two glow peaks is obtained.
Embodiment 3
Preparation method with double centre of luminescence fluorescent carbon points uses following steps：
(1) 50 milliliters of blue emission fluorescent carbon point solution prepared with dioxygen water etching coal and 50 milliliters of anhydrous second are taken
Alcoholic solution is mixed；
(2) toward the diammonium hydrogen phosphate solid particle of 0.6 gram of addition in the mixed solution of step (1), and ultrasonic vibration is passed through
It is completely dissolved it, the molar concentration of diammonium hydrogen phosphate is 6g/L after dissolving；
(3) mixed solution obtained in step (2) is transferred in polytetrafluoroethyllining lining reactor, then dried in air blast
In case at 180 DEG C, 14 hours are incubated；Again after cooling, the fluorescent carbon point solution with red, yellow two glow peaks is obtained.
Claims (2)
1. the preparation method with double centre of luminescence fluorescent carbon points, it is characterised in that：Using following steps：
(1) the m milliliters of blue emission fluorescent carbon point solution prepared with dioxygen water etching coal and n milliliters of ethanol solutions are taken
Mixing, wherein m:N=0.9-1.2；
(2) toward the diammonium hydrogen phosphate solid particle of w grams of addition in the mixed solution of step (1), and make its complete by ultrasonic vibration
The molar concentration of diammonium hydrogen phosphate is 2-7g/L after fully dissolved, dissolving；
(3) mixed solution obtained in step (2) is transferred in polytetrafluoroethyllining lining reactor, then in convection oven
At 150~220 DEG C, 10~15 hours are incubated；Again after cooling, the fluorescent carbon point solution with red, yellow two glow peaks is obtained.
2. according to claim 1 have pair preparation method of centre of luminescence fluorescent carbon points, it is characterised in that：Step (1)
In ethanol solution can be replaced absolute methanol solution.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109019560A (en) * | 2018-10-16 | 2018-12-18 | 吕梁学院 | A kind of preparation method of coal-based carbon point |
| CN109097035A (en) * | 2018-08-31 | 2018-12-28 | 中国石油大学(北京) | Carbon quantum dot and its preparation and application with high fluorescent characteristic |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109097035A (en) * | 2018-08-31 | 2018-12-28 | 中国石油大学(北京) | Carbon quantum dot and its preparation and application with high fluorescent characteristic |
| CN109097035B (en) * | 2018-08-31 | 2020-11-10 | 中国石油大学(北京) | Carbon quantum dot with high fluorescence characteristic and preparation and application thereof |
| CN109019560A (en) * | 2018-10-16 | 2018-12-18 | 吕梁学院 | A kind of preparation method of coal-based carbon point |
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