CN108675279A - A kind of preparation method with fluorescence vesicle structure nano-particle - Google Patents
A kind of preparation method with fluorescence vesicle structure nano-particle Download PDFInfo
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- CN108675279A CN108675279A CN201810637387.XA CN201810637387A CN108675279A CN 108675279 A CN108675279 A CN 108675279A CN 201810637387 A CN201810637387 A CN 201810637387A CN 108675279 A CN108675279 A CN 108675279A
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Abstract
The invention discloses a kind of preparation method with fluorescence vesicle structure nano-particle, this method includes：A) graphite powder and potassium carbonate are placed on together in mortar and are ground so that they are sufficiently mixed uniformly, it adds mixture to and carries out ball milling in the ball grinder containing bead, then add deionized water, stir, take solution and be centrifuged off potassium carbonate obtain doped with carboxyl graphite solid precipitation；Solid precipitation is added in potassium hydroxide solution again, ball milling takes out solution again, and the pH value of solution is transferred to neutrality.It is centrifuged off precipitation and obtains graphene solution；B) graphene solution being prepared is dried, the graphene after drying is taken to be ground in mortar fully with potassium nitrate and sodium nitrate solid, then it is calcined in Muffle furnace, distilled water is added in obtained solid, ultrasound, then decompression filters, and obtains the vesicle structure nano-particle with fluorescence property.The present invention is easy to operate, of low cost, and obtained particle has good fluorescence property.
Description
Technical field
The present invention relates to chemical synthetic material technical fields, specifically by the method for melting salt oxidation, graphene
Oxidation is carried out in fused salt to prepare the nano-particle with fluorescence property and for vesicle structure.
Background technology
Carbon quantum dot (CQDs) is that a kind of lateral dimension found recently is less than the zero dimension carbon nano-particles of 100 nm.With biography
System semiconductor-quantum-point is compared, they have chemical inertness, be readily produced, fast light drift, the low, good biocompatibility of cytotoxicity etc.
Advantage has broad application prospects in sensor, bio-imaging, opto-electronic device etc..In addition, it is similar with graphene,
CQDs has that large specific surface area, diameter are big, the pi-conjugated networks of π-or surface group is utilized to carry out the specific physicals such as fine surface grafting
Characteristic.In addition, the carboxyl and hydroxyl at their edges allow them to show excellent water solubility and are suitable for various organic, nothings
The continuous function of machine, polymerization or biological species, can be applicable to different field.
Currently, preparing the method for CQDs, there are many kind, such as hydro-thermal method, the sides such as electrochemical process and electron beam lithography
Method.Wherein hydro-thermal method has used the acid of strong oxidizing property and has made preparation process than relatively hazardous, while handling useless caused by reaction
Liquor ratio is cumbersome.Electrochemical process is prepared CQDs and to clean, for example obtained CQDs solution contains Various Complex particle,
Continuous purification process is wanted to obtain pure CQDs.Electron beam lithography preparation CQDs is of high cost, low output.
Invention content
The purpose of the present invention is the methods by melting salt oxidation, prepare a kind of nano-particle with special construction, and should
Particle has fluorescence property.This method is with graphite, and potassium carbonate, sodium hydroxide, potassium nitrate and sodium nitrate are raw material, by fused salt oxygen
Change acts on, and has obtained the nano-particle of vesicle structure, which has good fluorescence property.
Realizing the specific technical solution of the object of the invention is：
A kind of preparation method with fluorescence vesicle structure nano-particle, this method include step in detail below：
Step 1：Graphite powder and potassium carbonate are placed on 30 ~ 60 min of grinding in mortar together so that graphite powder and potassium carbonate are abundant
It is uniformly mixed, the mass ratio of graphite powder and potassium carbonate is 1:10；Uniformly mixed mixture is added to containing ZrO2Bead
In polytetrafluoroethyltank tank, with 300 ~ 400 rpm rotating speed 20 ~ 40h of ball milling, then add deionized water, stir, take solution and
It carries out centrifugation 3000 ~ 5000rpm, 10 ~ 30 min removing potassium carbonate and obtains the graphite solid precipitation doped with carboxyl；Again solid
Precipitation is added in the potassium hydroxide solution of 3 ~ 5 mol/L；The added graphite solid doped with carboxyl and potassium hydroxide solution matter
Amount Wei 1:100~200；
It continuously adds containing ZrO2In the polytetrafluoroethyltank tank of bead, with 300 ~ 400 rpm rotating speeds ball milling, 30 ~ 40 h；It takes out
The pH value of solution is transferred to neutrality by solution；Centrifugation 3000 ~ 5000rpm, 60 ~ 120min are carried out again；Precipitation is removed, graphite is obtained
Alkene solution；
Step 2：The graphene solution being prepared is dried, the graphene solid after drying and potassium nitrate and nitric acid are taken out
Sodium solid is ground fully in mortar, wherein graphene is=0.2 ~ 1 with sodium nitrate and potassium nitrate mass ratio: 1: 1；Then
In Muffle furnace, temperature calcines 1 ~ 5 h under the conditions of being 250 DEG C, and distilled water, the matter of added distilled water are added in obtained solid
The ratio between amount and solid masses are 10 ~ 50:1, ultrasound, then decompression filter, obtain color be flaxen clear transparent solutions i.e.
There is fluorescence vesicle structure nano-particle to be described.
Beneficial effects of the present invention
（1）The nano-particle with special vesicle structure has been prepared by the method for melting salt oxidation.
（2）The particle being prepared has good fluorescence property.
Description of the drawings
Fig. 1 is the ultraviolet-visible absorption spectroscopy figure for the vesicle structure particle solution that the embodiment of the present invention 1 obtains；
Fig. 2 is the fluorescence emission spectrogram of compound for the vesicle structure particle that the embodiment of the present invention 1 obtains；
Fig. 3 is the transmission electron microscope picture of graphene and vesicle structure particle that the embodiment of the present invention 1 obtains.
Specific implementation mode
Embodiment 1
Step 1：First weigh 0.5g graphite powders（99.95%）, then 5.0g potassium carbonate is weighed, it is placed in mortar grinds 30 together
Min so that graphite powder and potassium carbonate are sufficiently mixed uniformly, and it is 2 mm ZrO to be then added to 500ml to contain 300g radiuses2Bead
Polytetrafluoroethyltank tank in, with 300rpm rotating speed ball milling 20h, then add ionized water, take solution and centrifuged
3000rpm removes potassium carbonate and obtains solid precipitation, is then added in the KOH solution of 50ml 5mol/L solid precipitation,
It continuously adds 500ml and contains 300g, radius is 2mm ZrO2In the polytetrafluoroethyltank tank of bead, with 300rpm rotating speed ball millings
20h takes out solution, then is neutralized, and the pH value of solution is transferred to neutrality, then carry out centrifugation 3000rpm, 60min, and it is heavy to remove
It forms sediment, obtains graphene solution.
Step 2：By the graphene being prepared, 0.1g and 0.3g KNO are taken after dry3With 0.3g NaNO3In mortar
Grinding is abundant, and then in Muffle furnace, temperature calcines 3h under the conditions of being 250 DEG C, and distilled water 10ml is added in obtained solid, surpasses
Then sound depressurizes suction filtration, it is flaxen clear transparent solutions to obtain color.
Fig. 1 shows be the vesicle solution being prepared UV-vis absorption spectrum.What Fig. 2 was indicated is vesicle structure
Particle solution, can respectively in the fluorescence emission spectrogram of compound that 365nm, 405nm, 450nm, 500nm and 532nm are excitation wavelength
To find out gradually increasing with excitation wavelength, the wavelength corresponding to maximum fluorescence intensity gradually increases.Fig. 3 left figures indicate
The transmission electron microscope picture of graphene is prepared in ball milling under alkaline condition, and right figure indicates the transmission electron microscope picture of vesicle structure particle.
Embodiment 2
Step 1：First weigh 0.5g graphite powders（99.95%）, then 5.0g potassium carbonate is weighed, it is placed in mortar grinds 30 together
Min so that graphite powder and potassium carbonate are sufficiently mixed uniformly, and it is 2 mm ZrO to be then added to 500ml to contain 300g radiuses2Bead
Polytetrafluoroethyltank tank in, with 300rpm rotating speed ball milling 20h, then add ionized water, take solution and centrifuged
3000rpm removes potassium carbonate and obtains solid precipitation, is then added in the KOH solution of 4 mol/L of 50ml solid precipitation,
It continuously adds 500ml and contains 300g, radius is 2mm ZrO2In the polytetrafluoroethyltank tank of bead, with 300rpm rotating speed ball millings
20h takes out solution, then is neutralized, and the pH value of solution is transferred to neutrality, then carry out centrifugation 3000rpm, 60min, and it is heavy to remove
It forms sediment, obtains graphene solution.
Step 2：By the graphene being prepared, 0.1g and 0.1g KNO are taken after dry3With 0.1g NaNO3In mortar
Grinding is abundant, and then in Muffle furnace, temperature calcines 3h under the conditions of being 250 DEG C, and 8 ml of distilled water is added in obtained solid, surpasses
Then sound depressurizes suction filtration, it is flaxen clear transparent solutions to obtain color.
Embodiment 3
Step 1：First weigh 0.5g graphite powders（99.95%）, then 5.0g potassium carbonate is weighed, it is placed in mortar grinds 30 together
Min so that graphite powder and potassium carbonate are sufficiently mixed uniformly, and it is 2 mm ZrO to be then added to 500ml to contain 300g radiuses2Bead
Polytetrafluoroethyltank tank in, with 300rpm rotating speed ball milling 20h, then add ionized water, take solution and centrifuged
3000rpm removes potassium carbonate and obtains solid precipitation, is then added in the KOH solution of 50ml 5mol/L solid precipitation,
It continuously adds 500ml and contains 300g, radius is 2mm ZrO2In the polytetrafluoroethyltank tank of bead, with 300rpm rotating speed ball millings
20h takes out solution, then is neutralized, and the pH value of solution is transferred to neutrality, then carry out centrifugation 3000rpm, 60min, and it is heavy to remove
It forms sediment, obtains graphene solution.
Step 2：By the graphene being prepared, 0.05g and 0.2g KNO are taken after dry3With 0.2g NaNO3In mortar
Middle grinding is abundant, and then in Muffle furnace, temperature calcines 5 h under the conditions of being 250 DEG C, and distilled water is added in obtained solid
10ml, then decompression filters ultrasound, and it is flaxen clear transparent solutions to obtain color.
Embodiment 4
Step 1：First weigh 0.5g graphite powders（99.95%）, then 5.0g potassium carbonate is weighed, it is placed in mortar grinds 30 together
Min so that graphite powder and potassium carbonate are sufficiently mixed uniformly, and it is 2 mm ZrO to be then added to 500ml to contain 300g radiuses2Bead
Polytetrafluoroethyltank tank in, with 300rpm rotating speed ball milling 20h, then add ionized water, take solution and centrifuged
3000rpm removes potassium carbonate and obtains solid precipitation, then in the KOH solution for solid precipitation being added to 3 mol/L of 100ml
In, it continuously adds 500ml and contains 300g, radius is 2mm ZrO2In the polytetrafluoroethyltank tank of bead, with 300rpm rotating speed balls
20h is ground, solution is taken out, then neutralized, the pH value of solution is transferred to neutrality, then carry out centrifugation 3000rpm, 60min, it is heavy to remove
It forms sediment, obtains graphene solution.
Step 2：By the graphene being prepared, 0.1g and 0.5g KNO are taken after dry3With 0.5g NaNO3In mortar
Grinding is abundant, and then in Muffle furnace, temperature calcines 5h under the conditions of being 250 DEG C, and distilled water 15ml is added in obtained solid, surpasses
Then sound depressurizes suction filtration, it is flaxen clear transparent solutions to obtain color.
Claims (1)
1. a kind of preparation method with fluorescence vesicle structure nano-particle, which is characterized in that this method includes walking in detail below
Suddenly：
Step 1：Graphite powder and potassium carbonate are placed on 30 ~ 60 min of grinding in mortar together so that graphite powder and potassium carbonate are abundant
It is uniformly mixed, the mass ratio of graphite powder and potassium carbonate is 1:10；Uniformly mixed mixture is added to containing ZrO2Bead
In polytetrafluoroethyltank tank, with 300 ~ 400 rpm rotating speed 20 ~ 40h of ball milling, then add deionized water, stir, take solution and
It carries out centrifugation 3000 ~ 5000rpm, 10 ~ 30 min removing potassium carbonate and obtains the graphite solid precipitation doped with carboxyl；Again solid
Precipitation is added in the potassium hydroxide solution of 3 ~ 5 mol/L；The added graphite solid doped with carboxyl and potassium hydroxide solution matter
Amount Wei 1:100~200；
It continuously adds containing ZrO2In the polytetrafluoroethyltank tank of bead, with 300 ~ 400 rpm rotating speeds ball milling, 30 ~ 40 h；It takes out molten
The pH value of solution is transferred to neutrality by liquid；Centrifugation 3000 ~ 5000rpm, 60 ~ 120min are carried out again；Precipitation is removed, graphene is obtained
Solution；
Step 2：The graphene solution being prepared is dried, the graphene solid after drying and potassium nitrate and nitric acid are taken out
Sodium solid is ground fully in mortar, wherein graphene is=0.2 ~ 1 with sodium nitrate and potassium nitrate mass ratio: 1: 1；Then
In Muffle furnace, temperature calcines 1 ~ 5 h under the conditions of being 250 DEG C, and distilled water, the matter of added distilled water are added in obtained solid
The ratio between amount and solid masses are 10 ~ 50:1, ultrasound, then decompression filter, obtain color be flaxen clear transparent solutions i.e.
There is fluorescence vesicle structure nano-particle to be described.
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| CN102225759A (en) * | 2011-04-14 | 2011-10-26 | 温州医学院 | Low-temperature preparation method of hydroxy-functionalized graphene |
| CN103382026A (en) * | 2012-05-02 | 2013-11-06 | 中国科学院上海硅酸盐研究所 | Low-cost mass preparation method of high-quality graphene |
| CN103011143B (en) * | 2012-12-20 | 2015-04-29 | 中国科学院宁波材料技术与工程研究所 | Graphene and fabrication method thereof and super capacitor |
| KR20150084295A (en) * | 2014-01-13 | 2015-07-22 | 인하대학교 산학협력단 | Manufacturing method of graphene oxide nanopowder |
| CN105112022A (en) * | 2015-09-01 | 2015-12-02 | 刘义林 | Functionalized graphene composite fused salt |
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- 2018-06-20 CN CN201810637387.XA patent/CN108675279B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817516A (en) * | 2010-05-21 | 2010-09-01 | 哈尔滨工业大学 | Method for preparing graphene or graphene oxide by using high-efficiency and low-cost mechanical stripping |
| CN102225759A (en) * | 2011-04-14 | 2011-10-26 | 温州医学院 | Low-temperature preparation method of hydroxy-functionalized graphene |
| CN103382026A (en) * | 2012-05-02 | 2013-11-06 | 中国科学院上海硅酸盐研究所 | Low-cost mass preparation method of high-quality graphene |
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| 辛国祥: "碳基超级电容器电极材料的研究", 《中国博士学位论文全文数据库·工程科技I辑》 * |
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