CN107254309A - A kind of preparation method of carbon quantum dot - Google Patents
A kind of preparation method of carbon quantum dot Download PDFInfo
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- CN107254309A CN107254309A CN201710529302.1A CN201710529302A CN107254309A CN 107254309 A CN107254309 A CN 107254309A CN 201710529302 A CN201710529302 A CN 201710529302A CN 107254309 A CN107254309 A CN 107254309A
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- quantum dot
- carbon quantum
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- dispersion liquid
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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
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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
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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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
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
Abstract
The invention discloses one kind carbon quantum dot method is prepared using electrolysis tech.The present invention, as electrolyte, carbon quantum dot is can obtain by electrolysis and post processing using alcohols solvent and highly basic.Carbon quantum dot has that size uniformity, fluorescence be strong, yield is high, and dispersible different organic solvent, can long-time storage, have very big application prospect in the field such as luminescence generated by light and biomarker.
Description
Technical field
The present invention relates to a kind of method that utilization electrolysis tech prepares carbon quantum dot, and in particular to one kind uses alcohols solvent
With the method for highly basic electrosynthesis glyoxal carbon quantum dot, belong to carbon functional material synthesis field.
Background technology
The transition domain that the yardstick of nano material tends between cluster and macro object, its special knot with conventional solid material
There is notable difference in structure, nano material has many characteristic properties, such as skin effect, small-size effect, quantum size effect in itself
Should, macro quanta tunnel effect etc..Quantum dot is zero dimensional nanometer materials, by a small amount of atomic building.Quantum dot has as one kind
The novel nano-material of unique physical, causes the broad interest of domestic and international researcher, and its research contents is related to physics, change
, material etc. are multidisciplinary, it has also become an emerging cross discipline.Quantum dot has invented many different sides by scientists
Method is manufactured, and before illustrating in fields such as optical bio mark, solar cell, luminescent devices and being widely applied
Scape.Carbon quantum dot can be applied to evolving hydrogen reaction, catalysis, the field such as photoelectric device, energy storage and medical biotechnology imaging, and
Carbon quantum dot good biocompatibility, nontoxic pollution-free, with wide application space.Carbon quantum dot preparation method is a lot, including
Solvent-thermal method, high temperature sintering and microwave ultrasound technology.Simple, the with low cost and green carbon quantum dot of development technology can control
Preparation Method is the key for making it be able to promote in the application of each field.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the simple and green carbon quantum dot of low cost, technique.
The present invention, as electrolyte, carbon quantum dot is can obtain by electrolysis and post processing using alcohols solvent and highly basic,
Advantage is protruded in terms of the preparation of scale magnanimity.Gained carbon quantum dot has that size uniformity, fluorescence be strong, yield is high, and dispersible difference
Organic solvent, can long-time storage.
A kind of preparation method of carbon quantum dot, it is characterised in that step is this method successively：
1）Highly basic is dissolved in alcohols solvent, metal platinum and titanium sheet apply potential electrolysis and obtain forerunner's reactant as electrode；
2）By step 1）Products therefrom carries out sour neutralization, centrifugation, cleaning and redisperse and obtains carbon quantum dot dispersion liquid；
3）In step 1）By adding sulfur-bearing or nitrogen-containing compound in electrolyte, then through step 2）Processing, obtains sulphur or N doping
Carbon quantum dot.
Alcohols solvent of the present invention is methanol, ethanol or isopropanol, and highly basic is sodium hydroxide and potassium hydroxide.
Decomposition voltage of the present invention is 50-300V, and the time is 10-200min.
Sulfur-bearing or nitrogen-containing compound of the present invention are urea, thiocarbamide, thioacetamide and DMF
One kind.
The size for the carbon quantum dot that the present invention is obtained is 1-10nm.
The invention has the advantages that：
1）Material therefor is cheap, nontoxic, and cost is low；
2）Easy to operate controllable, easily doping is reproducible.
The effect benefit of the present invention：Carbon quantum dot is prepared there is provided a kind of simple scale, raw materials are prepared abundant, honest and clean
Valency is easy to get, environment-friendly, reproducible, stable and reliable product quality；Open a kind of preparation method of new carbon quantum dot, carbon
Quantum dot has very big application prospect in the field such as luminescence generated by light and biomarker.
Brief description of the drawings
Fig. 1 is gained carbon quantum dot dispersion liquid photoluminescence spectrum in the embodiment of the present invention 1.
Embodiment
Embodiment 1
Sodium hydroxide powder 1g will be added in 200ml alcohol solvents, be stirred well to and be completely dissolved, using platinum electrode and Titanium
Piece applies 80V voltages as electrolysis electrode, is electrolysed 150min, can obtain dark brown precursor liquid.Precursor liquid is subjected to hydrochloric acid
Neutralize, centrifugation and distilled water cleaning, carbon quantum dot dispersion liquid can be obtained by being finally scattered in ethanol, DMF.
Fig. 1 is the luminescence generated by light spectrogram of carbon quantum dot/DMF dispersion liquid, and exciting light is 365nm, maximum emission intensity
At 460nm.Gained carbon quantum dot passes through transmission electron microscope（TEM）Analysis, size is distributed homogeneous in 5nm or so.
Embodiment 2
Sodium hydroxide powder 0.8g will be added in 200ml alcohol solvents, be stirred well to and be completely dissolved, using platinum electrode and metal
Titanium sheet applies 120V voltages as electrolysis electrode, is electrolysed 30min, can obtain dark brown precursor liquid.Precursor liquid is subjected to salt
Acid is neutralized, centrifugation and distilled water cleaning, and carbon quantum dot/alcohol dispersion liquid can be obtained by being finally scattered in ethanol.Carbon quantum dot chi
Very little distribution is homogeneous, and by atomic force microscope observation, size is in 5nm or so.
Embodiment 3
Potassium hydroxide powder 0.5g will be added in 100ml alcohol solvents, be stirred well to and be completely dissolved, using platinum electrode and metal
Titanium sheet applies 250V voltages as electrolysis electrode, is electrolysed 30min, can obtain precursor liquid.Precursor liquid is carried out in hydrochloric acid
With, centrifugation and distilled water cleaning, carbon quantum dot/N, N- dimethyl formyls can be obtained by being finally scattered in DMF
Amine dispersion liquid.Carbon quantum dot dispersion liquid fluorescence intensity is high, passes through transmission electron microscope（TEM）Analysis understands that size is 3nm or so, point
Cloth is homogeneous.
Embodiment 4
Potassium hydroxide powder 0.5g will be added in 100ml alcohol solvents, be stirred well to and be completely dissolved, using platinum electrode and metal
Titanium sheet applies 100V voltages as electrolysis electrode, is electrolysed 80min, can obtain precursor liquid.Precursor liquid is carried out in hydrochloric acid
With, centrifugation and distilled water cleaning, carbon quantum dot/N, N- dimethyl formyls can be obtained by being finally scattered in DMF
Amine dispersion liquid.Carbon quantum dot dispersion liquid fluorescence intensity is high, passes through transmission electron microscope（TEM）Analysis understands that size is 3nm or so, point
Cloth is homogeneous.
Embodiment 5
Sodium hydroxide powder 1.5g will be added in 200ml methanol solvates, be stirred well to and be completely dissolved, using platinum electrode and metal
Titanium sheet applies 150V voltages as electrolysis electrode, is electrolysed 100min, can obtain precursor liquid.Precursor liquid is carried out in hydrochloric acid
With, centrifugation and distilled water cleaning, carbon quantum dot/N, N- dimethyl formyls can be obtained by being finally scattered in DMF
Amine dispersion liquid.Carbon quantum dot dispersion liquid fluorescence intensity is high, passes through transmission electron microscope（TEM）Analysis understands that size is 5nm or so, point
Cloth is homogeneous.
Embodiment 6
Potassium hydroxide powder 1.5g will be added in 200ml methanol solvates, be stirred well to and be completely dissolved, using platinum electrode and metal
Titanium sheet applies 250V voltages as electrolysis electrode, is electrolysed 100min, can obtain precursor liquid.Precursor liquid is carried out in hydrochloric acid
With, centrifugation and distilled water cleaning, be finally scattered in methanol, ethanol or DMF can obtain corresponding carbon quantum
Point dispersion liquid.Pass through transmission electron microscope（TEM）Analysis understands that size is 5nm or so, is distributed homogeneous.
Embodiment 7
Sodium hydrate solid powder 2g and thiocarbamide 0.3g will be added in 200ml isopropanol solvents, be stirred well to and be completely dissolved.Adopt
With platinum electrode and metal titanium sheet as electrolysis electrode, apply 60V voltages, be electrolysed 140min, can obtain precursor liquid.By precursor liquid
Body carries out sour neutralization, centrifugation and distilled water cleaning, is finally scattered in isopropanol, ethanol, DMF equal solvent,
Sulfur doping carbon quantum dot dispersion liquid can be obtained.
Embodiment 8
Potassium hydroxide solid powder 2g and urea 0.3g will be added in 200ml alcohol solvents, be stirred well to and be completely dissolved.Using
Platinum electrode and metal titanium sheet apply 100V voltages as electrolysis electrode, are electrolysed 80min, can obtain precursor liquid.By precursor liquid
Sour neutralization, centrifugation and distilled water cleaning are carried out, ethanol, DMF equal solvent is finally scattered in, you can obtain
Nitrogen-doped carbon quantum dot dispersion liquid.
Embodiment 9
Potassium hydroxide solid powder will be added in 200ml alcohol solvents（2g）And thioacetamide（0.3g）, it has been stirred well to
Fully dissolved.Using platinum electrode and metal titanium sheet as electrolysis electrode, apply 100V voltages, be electrolysed 100min, can obtain precursor liquid
Body.Precursor liquid is subjected to sour neutralization, centrifugation and distilled water cleaning, ethanol, DMF etc. is finally scattered in
Solvent, you can obtain sulfur doping carbon quantum dot dispersion liquid.
Embodiment 10
10ml DMFs will be added in 200ml alcohol solvents, and take potassium hydroxide powder 2g to be dissolved in above-mentioned mixing
Solvent, is stirred well to and is completely dissolved.Using platinum electrode and metal titanium sheet as electrolysis electrode, apply 100V voltages, electrolysis
100min, can obtain precursor liquid.Precursor liquid is subjected to sour neutralization, centrifugation and distilled water cleaning, be finally scattered in ethanol,
DMF equal solvent, you can obtain nitrogen-doped carbon quantum dot dispersion liquid.
Claims (4)
1. a kind of preparation method of carbon quantum dot, it is characterised in that step is this method successively：
1）Highly basic is dissolved in alcohols solvent, metal platinum and titanium sheet apply potential electrolysis and obtain forerunner's reactant as electrode；
2）By step 1）Products therefrom carries out sour neutralization, centrifugation, cleaning and redisperse and obtains carbon quantum dot dispersion liquid；
3）In step 1）By adding sulfur-bearing or nitrogen-containing compound in electrolyte, then through step 2）Processing, obtains sulphur or N doping
Carbon quantum dot.
2. the method as described in claim 1, it is characterised in that alcohols solvent is methanol, ethanol or isopropanol, and highly basic is hydrogen-oxygen
Change sodium and potassium hydroxide.
3. the method as described in claim 1, it is characterised in that decomposition voltage is 50-300V, the time is 10-200min.
4. the method as described in claim 1, it is characterised in that sulfur-bearing or nitrogen-containing compound are urea, thiocarbamide, thioacetamide
And one kind of DMF.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108085711A (en) * | 2017-12-21 | 2018-05-29 | 西安科技大学 | A kind of preparation method of the carbon quantum dot to glow |
| CN108550829A (en) * | 2018-05-10 | 2018-09-18 | 中南大学 | One kind having rose shape vanadium disulfide/carbon quantum dot composite material and preparation method and application |
| CN109266339A (en) * | 2018-11-07 | 2019-01-25 | 福建工程学院 | The reflux preparation method of nitrogen-doped carbon quantum dot and its application in electrocatalytic hydrogen evolution |
| CN109988570A (en) * | 2019-01-28 | 2019-07-09 | 华中科技大学 | A kind of preparation facilities and preparation method of carbon quantum dot |
| CN110975913A (en) * | 2019-10-22 | 2020-04-10 | 上海电力大学 | Electrocatalyst for electrocatalytic hydrogen production and preparation method thereof |
| CN113046767A (en) * | 2021-03-22 | 2021-06-29 | 华东交通大学 | Method for rapidly preparing graphene in batches |
| CN113466015A (en) * | 2021-07-20 | 2021-10-01 | 湖南智享未来生物科技有限公司 | Staining reagent for distinguishing normal cells from cancer cells and preparation method and application thereof |
| CN113801659A (en) * | 2021-09-28 | 2021-12-17 | 华东交通大学 | Preparation method of water-soluble antimony-carbon quantum dot, prepared antimony-carbon quantum dot, application of antimony-carbon quantum dot and corrosion-resistant composite material |
| CN115029715A (en) * | 2022-07-05 | 2022-09-09 | 中国石油大学(华东) | Preparation method of carbon quantum dot, carbon quantum dot and application |
Citations (3)
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|---|---|---|---|---|
| CN103436905A (en) * | 2013-08-27 | 2013-12-11 | 湖南师范大学 | Electrochemical preparation method of nitrogen-doped fluorescent carbon dots (NC-dots) with up-conversion and down-conversion functions |
| CN104312582A (en) * | 2014-09-18 | 2015-01-28 | 中国石油大学(北京) | Sulfur doped carbon quantum dot with high fluorescent quantum yield, and preparation method and application thereof |
| CN106504906A (en) * | 2016-12-01 | 2017-03-15 | 中国石油大学(华东) | Carbon quantum dot/nickel hydroxide electrochemical energy storage materials, synthetic method and application |
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Patent Citations (3)
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| CN103436905A (en) * | 2013-08-27 | 2013-12-11 | 湖南师范大学 | Electrochemical preparation method of nitrogen-doped fluorescent carbon dots (NC-dots) with up-conversion and down-conversion functions |
| CN104312582A (en) * | 2014-09-18 | 2015-01-28 | 中国石油大学(北京) | Sulfur doped carbon quantum dot with high fluorescent quantum yield, and preparation method and application thereof |
| CN106504906A (en) * | 2016-12-01 | 2017-03-15 | 中国石油大学(华东) | Carbon quantum dot/nickel hydroxide electrochemical energy storage materials, synthetic method and application |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108085711A (en) * | 2017-12-21 | 2018-05-29 | 西安科技大学 | A kind of preparation method of the carbon quantum dot to glow |
| CN108550829A (en) * | 2018-05-10 | 2018-09-18 | 中南大学 | One kind having rose shape vanadium disulfide/carbon quantum dot composite material and preparation method and application |
| CN108550829B (en) * | 2018-05-10 | 2020-12-25 | 中南大学 | Rose-shaped vanadium disulfide/carbon quantum dot composite material and preparation method and application thereof |
| CN109266339A (en) * | 2018-11-07 | 2019-01-25 | 福建工程学院 | The reflux preparation method of nitrogen-doped carbon quantum dot and its application in electrocatalytic hydrogen evolution |
| CN109988570A (en) * | 2019-01-28 | 2019-07-09 | 华中科技大学 | A kind of preparation facilities and preparation method of carbon quantum dot |
| CN110975913A (en) * | 2019-10-22 | 2020-04-10 | 上海电力大学 | Electrocatalyst for electrocatalytic hydrogen production and preparation method thereof |
| CN113046767A (en) * | 2021-03-22 | 2021-06-29 | 华东交通大学 | Method for rapidly preparing graphene in batches |
| CN113466015A (en) * | 2021-07-20 | 2021-10-01 | 湖南智享未来生物科技有限公司 | Staining reagent for distinguishing normal cells from cancer cells and preparation method and application thereof |
| CN113466015B (en) * | 2021-07-20 | 2024-03-22 | 湖南智享未来生物科技有限公司 | Staining reagent for distinguishing normal cells from cancer cells, and preparation method and application thereof |
| CN113801659A (en) * | 2021-09-28 | 2021-12-17 | 华东交通大学 | Preparation method of water-soluble antimony-carbon quantum dot, prepared antimony-carbon quantum dot, application of antimony-carbon quantum dot and corrosion-resistant composite material |
| CN115029715A (en) * | 2022-07-05 | 2022-09-09 | 中国石油大学(华东) | Preparation method of carbon quantum dot, carbon quantum dot and application |
| CN115029715B (en) * | 2022-07-05 | 2023-07-07 | 中国石油大学(华东) | Preparation method of carbon quantum dot, carbon quantum dot and application |
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Application publication date: 20171017 |