CN108467728A - A kind of preparation method of water-soluble phosphorus, nitrogen co-doped carbon quantum dot - Google Patents
A kind of preparation method of water-soluble phosphorus, nitrogen co-doped carbon quantum dot Download PDFInfo
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- CN108467728A CN108467728A CN201810247054.6A CN201810247054A CN108467728A CN 108467728 A CN108467728 A CN 108467728A CN 201810247054 A CN201810247054 A CN 201810247054A CN 108467728 A CN108467728 A CN 108467728A
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- quantum dot
- carbon quantum
- water
- doped carbon
- nitrogen
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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
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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
- C09K11/0883—Arsenides; Nitrides; Phosphides
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- 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
- G01N21/6486—Measuring fluorescence of biological material, e.g. DNA, RNA, cells
Abstract
The present invention relates to a kind of water-soluble phosphorus, the preparation method of nitrogen co-doped carbon quantum dot, 1) hair is placed in quartz boat, it is warming up to 120 200 DEG C under nitrogen protection, be carbonized 0.8~1.2h at 120 200 DEG C, then cools to room temperature；Obtained black product is with being continuously milled into black powder in agateware；2) with phenoxy group ring phosphonitrile in mass ratio 2:1 mills after mixing in agateware, is put into quartz boat, is warming up to 350~600 DEG C under nitrogen protection, and 1.5~2.5h is calcined at 350~600 DEG C, is cooled to room temperature；3) the product 0.2g after high-temperature calcination is added into 50~300ml of distilled water, 0.5~1.5h of ultrasound under 300~800W in ultrasonic cleaner, 5min is centrifuged under the conditions of 400~600rpm, dialyzate is obtained with 48~96h of bag filter dialysis, dialyzate is finally carried out to constant temperature rotary evaporation in constant temperature Rotary Evaporators to get to water-soluble phosphorus, nitrogen co-doped carbon quantum dot at 50~70 DEG C.
Description
Technical field
The present invention relates to the preparations that biological developing agent material technical field more particularly to a kind of Water-soluble carbon quantum dot are given birth to
Method.
Background technology
The Sun Yaping of Clemson University of the U.S. in 2006 has found carbon quantum dot for the first time, is after carbon nanotube, nanometer Buddha's warrior attendant
The novel nano-carbon material of one kind occurred after stone, fullerene and graphene.Carbon quantum dot have it is excellent optically and electrically
Performance is compared with traditional semiconductor-quantum-point, has many advantages, such as that cytotoxicity is low, synthesis cost is low, good light stability, therefore
It has a wide range of applications in fields such as biological developing imaging, sensing and probes.
Existing carbon quantum dot quantum efficiency is low, and the carbon quantum dot quantum efficiency of document report is usually no more than 10 ﹪.It is another
Aspect, the upward reverse ability that carbon quantum dot absorbs long-wavelength excitation light and launches short wavelength's (visible light) is also weaker, cannot
Across thicker tissue, use receives limitation.
Invention content
The technical problem to be solved by the present invention is to provide one kind for the present situation of the prior art to absorb near infrared light
Line has the relatively strong water-soluble phosphorus for reversing ability upwards, the preparation method of nitrogen co-doped carbon quantum dot.
Technical solution is used by the present invention solves above-mentioned technical problem：The water-soluble phosphorus, nitrogen co-doped carbon quantum dot
Preparation method, it is characterised in that include the following steps：
1) 10g hairs are placed in quartz boat, 120- is warming up to the rate of 0.5~1.5 DEG C/min under nitrogen protection
200 DEG C, be carbonized 0.8~1.2h at 120-200 DEG C, then cools to room temperature；Obtained black product, is connected in agateware
It is continuous to mill 30~60min into black powder；
2) by the black powder and phenoxy group ring phosphonitrile in mass ratio 5:1~1:1 mills mixing in agateware
It after even, is put into quartz boat, is warming up to 350~600 DEG C under nitrogen protection with the rate of 1~2 DEG C/min, at 350~600 DEG C
1.5~2.5h of lower calcining, is cooled to room temperature；
3) add 50~300ml of distilled water in ultrasonic cleaner under 300~800W the product 0.2g after high-temperature calcination
0.5~1.5h of ultrasound centrifuges 5min extracting centrifugal liquids under the conditions of 400~600rpm, and the bag filter with shearing molecular weight 1000 is saturating
48~96h of analysis obtains dialyzate, and dialyzate is finally carried out in constant temperature Rotary Evaporators at 50~70 DEG C to constant temperature rotary evaporation,
Obtained solid powder is water-soluble phosphorus, nitrogen co-doped carbon quantum dot.
Compared with prior art, the carbon quantum dot biological developing agent tool prepared by the present invention has the advantage that：
1, yield is high, size dispersion is uniform；
2, low cytotoxicity, it is soluble easily in water, it can be used for the fields such as cell imaging or living imaging；
3, obtained carbon quantum dot can enter cell, and the glimmering of different colours can be inspired under different excitation wavelengths
Light especially inspires long wavelength's light source, is used as biological developing agent, thicker tissue can be passed through, in tissue
Development has stronger practicability.
Description of the drawings
Fig. 1 is the carbon quantum dot diameter distribution profile that embodiment 1 is prepared；
Fig. 2 is the fluorescence spectrum for the carbon quantum dot that embodiment 1 is prepared；
Fig. 3 is that carbon quantum dot cell developing photo is prepared in embodiment 1 in HELA cells.
Specific implementation mode
Below in conjunction with attached drawing embodiment, present invention is further described in detail.
10g hairs are placed in quartz boat, are warming up to 180 DEG C under nitrogen protection with the rate of 1 DEG C/min, constant temperature 1 is small
When, carry out low-temperature carbonization；It then cools to room temperature, obtains black product.
Black product is continuously milled 40min with being ground into fine powder in agateware, at black powder.
By above-mentioned black powder and phenoxy group ring phosphonitrile in mass ratio 2:1 mixing, mills uniformly mixed in agateware
After be put into quartz boat, under nitrogen protection, with the rate of 1.5 DEG C/min be warming up to 380 DEG C calcining 2h, be subsequently cooled to room
Temperature.
50ml distilled water is added into the product after high-temperature calcination, the ultrasonic cleaning machine ultrasound 1h through 300w takes after centrifugation
Liquid is dialysed 72 hours with the bag filter of shearing molecular weight 1000 and obtains dialyzate；Dialyzate is finally carried out to perseverance at 60 DEG C
Warm rotary evaporation, obtained solid powder are water-soluble phosphorus, nitrogen co-doped carbon quantum dot.
Test the grain size of carbon quantum dot
Pass through transmission electron microscope (TEM) and high resolution transmission electron microscopy (HR-TEM, FEI Tecnai G2 S-
Twin) acquisition statistics obtains the grain size of carbon quantum dot, collection voltages 200kV, and grain size distribution is shown in Fig. 1.
As seen from Figure 1, the grain size of carbon quantum dot is in relatively narrow distribution, and size is 4.9nm or so.
Test the fluorescence emission spectrum of carbon quantum dot
Carbon quantum dot is configured to the carbon quantum dot aqueous solution of 1mg/ml concentration, using SENS-9000 spectrometer collections, inspection
320nm~460nm, the fluorescence emission spectrum of the lower carbon quantum dot obtained of different wave length excitation are surveyed.As shown in Figure 2.
As seen from Figure 2, carbon quantum dot has higher fluorescent emission in 650nm~900nm near infrared regions, has fine
Upward reverse luminous power.Fluorescence quantum efficiency is measured using the subsidiary integration sphere light source system of SENS-9000 spectrometers.It measures
Quantum efficiency is 23.5%.
Cell developing detects
Cell culture medium presses 9 by DMEM and fetal calf serum:1 ratio is allocated.Condition of culture is 37 DEG C, and carbon dioxide contains
Amount 5%.Hela cells are cultivated 24 hours on porous plate first, and density is 1 × 105A/hole.Prepared carbon amounts is added later
Son point solution, the aqueous solution of a concentration of 1mg/ml of carbon quantum dot are fixed after incubation in 4 hours with paraformaldehyde, and phosphorus is used
Phthalate buffer, which rinses three times, removes extra carbon quantum dot；It is imaged under Olympus FV1000CLSM Laser Scanning Confocal Microscopes,
As shown in Figure 3.Excitation light source used is 360nm, power 2.5mW, and it is 320nm to 650nm to measure and choose wave-length coverage.
Claims (1)
1. the preparation method of a kind of water-soluble phosphorus, nitrogen co-doped carbon quantum dot, it is characterised in that include the following steps：
1) 10g hairs are placed in quartz boat, 120-200 is warming up to the rate of 0.5~1.5 DEG C/min under nitrogen protection
DEG C, be carbonized 0.8~1.2h at 120-200 DEG C, then cools to room temperature；Obtained black product, with continuous in agateware
30~60min mill into black powder；
2) by the black powder and phenoxy group ring phosphonitrile in mass ratio 2:1 mills after mixing in agateware, is put into
In quartz boat, 350~600 DEG C are warming up to the rate of 1~2 DEG C/min under nitrogen protection, 1.5 are calcined at 350~600 DEG C
~2.5h, is cooled to room temperature；
3) by the product 0.2g after high-temperature calcination add 50~300ml of distilled water in ultrasonic cleaner under 300~800W it is ultrasonic
0.5~1.5h centrifuges 5min, extracting centrifugal liquid, with the bag filter dialysis 48 of shearing molecular weight 1000 under the conditions of 400~600rpm
~96h obtains dialyzate, and dialyzate is finally carried out in constant temperature Rotary Evaporators at 50~70 DEG C to constant temperature rotary evaporation, gained
Solid powder is water-soluble phosphorus, nitrogen co-doped carbon quantum dot.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109674676A (en) * | 2018-11-20 | 2019-04-26 | 安康德美（中山）纳米科技有限公司 | A kind of environmentally protective hair styling finishing agent and preparation method and application |
| CN111721933A (en) * | 2019-09-17 | 2020-09-29 | 中国科学院上海微***与信息技术研究所 | Kit, tumor cell detection method and application thereof |
| CN111808610A (en) * | 2020-03-19 | 2020-10-23 | 广东两山科技有限公司 | Carbon nitride-like phosphorus-rich quantum dot fluorescent probe and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896251A (en) * | 2014-04-04 | 2014-07-02 | 宁波工程学院 | Preparation method of water-soluble carbon quantum dot biological developing agent |
-
2018
- 2018-03-23 CN CN201810247054.6A patent/CN108467728A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896251A (en) * | 2014-04-04 | 2014-07-02 | 宁波工程学院 | Preparation method of water-soluble carbon quantum dot biological developing agent |
Non-Patent Citations (3)
| Title |
|---|
| JING-HUI ZHANG ET AL.: "In vivo characterization of hair and skin derived carbon quantum dots with high quantum yield as longterm bioprobes in zebrafish", 《SCIENTIFIC REPORTS》 * |
| SI-SI LIU ET AL.: "Hair-derived carbon dots toward versatile multidimensional fluorescent materials", 《JOURNAL OF MATERIALS CHEMISTRY C》 * |
| YONGMING GUO ET AL.: "Thermal treatment of hair for the synthesis of sustainable carbon quantum dots and the applications for sensing Hg2+", 《SCIENTIFIC REPORTS》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109674676A (en) * | 2018-11-20 | 2019-04-26 | 安康德美（中山）纳米科技有限公司 | A kind of environmentally protective hair styling finishing agent and preparation method and application |
| CN109674676B (en) * | 2018-11-20 | 2021-07-09 | 安康德美（中山）纳米科技有限公司 | Green and environment-friendly hair styling finishing agent, and preparation method and application thereof |
| CN111721933A (en) * | 2019-09-17 | 2020-09-29 | 中国科学院上海微***与信息技术研究所 | Kit, tumor cell detection method and application thereof |
| CN111808610A (en) * | 2020-03-19 | 2020-10-23 | 广东两山科技有限公司 | Carbon nitride-like phosphorus-rich quantum dot fluorescent probe and preparation method and application thereof |
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