CN104774612B - Double wave length fluorescent and the preparation method of dual wavelength electrogenerated chemiluminescence carbon quantum dot - Google Patents
Double wave length fluorescent and the preparation method of dual wavelength electrogenerated chemiluminescence carbon quantum dot Download PDFInfo
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000001378 electrochemiluminescence detection Methods 0.000 title claims abstract description 19
- 230000009977 dual effect Effects 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000498 ball milling Methods 0.000 claims abstract description 11
- 229910000831 Steel Inorganic materials 0.000 claims description 21
- 239000010959 steel Substances 0.000 claims description 21
- 229910001220 stainless steel Inorganic materials 0.000 claims description 14
- 239000010935 stainless steel Substances 0.000 claims description 14
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000006228 supernatant Substances 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 230000001186 cumulative effect Effects 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000001117 sulphuric acid Substances 0.000 claims description 3
- 238000001507 sample dispersion Methods 0.000 claims description 2
- 235000011149 sulphuric acid Nutrition 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 17
- 125000000524 functional group Chemical group 0.000 abstract description 7
- 229910052799 carbon Inorganic materials 0.000 abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 239000002096 quantum dot Substances 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 238000000108 ultra-filtration Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000007858 starting material Substances 0.000 abstract description 2
- 238000010189 synthetic method Methods 0.000 abstract description 2
- 230000005284 excitation Effects 0.000 description 9
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 4
- 239000011324 bead Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 150000001721 carbon Chemical class 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000006056 electrooxidation reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000006396 nitration reaction Methods 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
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- 230000009467 reduction Effects 0.000 description 2
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- 238000002835 absorbance Methods 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
A kind of double wave length fluorescent and the preparation method of dual wavelength electrogenerated chemiluminescence carbon quantum dot, belong to Novel Carbon Nanomaterials and preparing technical field thereof.The method be activated carbon is mixed with highly basic after ball milling, then obtain orange-yellow carbon quantum dot solution by ultra-filtration and separation, this quantum dot has double wave length fluorescent and dual wavelength electrogenerated chemiluminescence character.Advantage is: synthetic method is simply effective, and cheaper starting materials is easy to get, reaction condition gentleness and environmental friendliness, it is easy to large-scale production carbon quantum dot.It addition, the carbon quantum dot using the inventive method to prepare contains abundant oxygen-containing functional group, good water solubility, there is double wave length fluorescent and the character of dual wavelength electrogenerated chemiluminescence.
Description
Technical field
The invention belongs to carbon nanomaterial and preparing technical field thereof, particularly relate to one have double wave length fluorescent and
The preparation method of the carbon quantum dot of dual wavelength electrogenerated chemiluminescence character.
Background technology
Carbon quantum dot is that a kind of particle diameter is less than 10nm, has the torispherical nano-particle of good dispersion.Owing to it has
There are the advantages such as good water solublity, high fluorescent stability, low preparation cost, hypotoxicity and good biocompatibility,
Cause the extensive concern of people.Fluorescence that especially carbon quantum dot is unique and the character of electrogenerated chemiluminescence, make
It has broad prospect of application in fields such as bio-sensing and bio-imagings.
Preparation at present has the method for fluorescence and electrogenerated chemiluminescence character carbon quantum dot with microwave method, electrochemical oxidation
Method and chemical oxidization method are main.At document (1) Adv.Funct.Mater., in 2012,22,2971-2979, L.L.Li
Et al. under the conditions of nitration mixture, utilize microwave heating graphene oxide nanometer sheet solution, obtain that there is yellow green (before reduction)
With the carbon quantum dot of blue (after reduction) fluorescence, and the carbon quantum dot with yellow-green fluorescence also has electroluminescent chemistry
Luminosity.At document (2) J.Am.Chem.Soc., in 2009,131,4564-4565, L.Y.Zheng et al. profit
Prepare by the method for electrolytic graphite rod and there is fluorescence and the carbon quantum dot of electrogenerated chemiluminescence character.In document (3)
Carbon, in 2013,56,12-17, activated carbon is refluxed by Y.Q.Dong et al. with nitration acid heat, then through ultra-filtration and separation,
Obtain the carbon quantum dot with yellow fluorescence, and this carbon quantum dot forms electrogenerated chemiluminescence system with sulphite.
But use the methods such as microwave method, electrochemical oxidation process and chemical oxidization method to prepare carbon quantum dot and there is certain office
Sex-limited, as cost of material is high, carbon quantum dot quantum yield is low, last handling process is complicated, is the most all difficult to scale
Produce carbon quantum dot.
Summary of the invention
It is an object of the invention to provide a kind of double wave length fluorescent and the preparation side of dual wavelength electrogenerated chemiluminescence carbon quantum dot
Method.The method be activated carbon is mixed with highly basic after ball milling, then obtain orange-yellow carbon quantum by ultra-filtration and separation
Point solution, this quantum dot has double wave length fluorescent and the character of dual wavelength electrogenerated chemiluminescence.Concrete technology step is such as
Under:
(1) with the ratio that mass ratio is 1:1～1:2 of highly basic according to activated carbon the two is mixed and this biased sample is put
Enter in stainless cylinder of steel, weigh stainless steel ball according to the ratio that mass ratio is 1:50～1:70 of biased sample Yu stainless steel ball
And stainless steel ball is added in stainless cylinder of steel, biased sample accounts for rustless steel tank volume with the cumulative volume of stainless steel ball
1/4～1/2, with the rotating speed ball millings 40 of 400～600 revs/min～70 hours.Wherein, described highly basic be potassium hydroxide or
Any one in sodium hydroxide.
(2) after the ball milling that step (1) is obtained sample dispersion in deionized water, wherein sample and deionization after ball milling
The mass ratio of water is 1:40～1:60, ultrasonic disperse 10～30 minutes, and being then neutralized to pH with strong acid solution is 7.0,
With the rotating speeds of 5000～9000 revs/min, (this rotating speed is equivalent to the acceleration of gravity of 2795～9055 times, generally represents
Be 2795～9055 × g) centrifugal 5～10 minutes, take supernatant in super filter tube, with high molecular cut off super filter tube from
The heart separates, and takes filtrate with the further centrifugation of low catching molecular super filter tube, and adds deionized water wash 5～8
Secondary, until filtrate is become colorless by yellow, take and retain part for orange-yellow carbon quantum dot solution.Wherein, described by force
Acid is any one in nitric acid, hydrochloric acid or sulphuric acid, and its concentration is 0.1～0.3mol L-1；Described high molecular cut off
The molecular cut off of super filter tube is 30,50 or one in 100kDa, retaining point of low catching molecular super filter tube
Son amount is the one in 3 or 10kDa, and high molecular cut off super filter tube and low catching molecular super filter tube are carried out group
Close, to obtain various sizes of carbon quantum dot.
Jeol Ltd. JEM-2100F type high resolution transmission electron microscopy (HRTEM) is used to characterize this carbon
The pattern of quantum dot, test result is as it is shown in figure 1, product size is more uniform, and particle diameter is at about 2.2nm.Use
Brooker company Vertex 70V type Fourier transform infrared spectroscopy of Germany (FTIR) characterizes this carbon quantum dot, such as Fig. 2
Shown in, show that this carbon quantum dot contains abundant hydroxyl and carboxyl functional group.Use Rigaku company D/MAX
2500VB2+/PC type x-ray diffractometer (XRD) characterizes this carbon quantum dot, as it is shown on figure 3, the crystalline substance of carbon quantum dot
Compartment is away from for 0.403nm, and more slightly larger than the spacing of lattice of Graphene, analysis is that carbon quantum dot contains abundant surface official
Can group support big caused by interlamellar spacing.Use U.S.'s Perkinelmer Inc. Lambda 35 type UV, visible light spectrophotometric
Its ultraviolet-visible absorption spectroscopy surveyed by meter (UV-Vis), as shown in Figure 4, product without obvious ultraviolet and visible absorption peak, but
There is the widest absorption band at below 550nm, illustrate that this carbon quantum dot contains abundant oxygen-containing functional group.Use Japan
Its fluorescence (PL) spectrum under different excitation wavelengths surveyed by Shimadzu RF-5301PC type spectrofluorophotometer, such as Fig. 5
Shown in.This carbon quantum dot, in the excitation wavelength range of 290～390nm, has two parts under each excitation wavelength
Overlapping emission peak.From figure 5 it can be seen that first emission peak does not moves along with the change of excitation wavelength,
Emission maximum peak position is at 490nm, and second emission peak is along with the increase of excitation wavelength and red shift.Use auspicious stepping
Its electrogenerated chemiluminescence character surveyed by the Electrochemiluminescprocess process instrument of analytical tool company, then by successively by Single wavelength
Infiltration type optical filter (wavelength is respectively 425,440,460,475,490,505,520,535,555,575,590,620,
640,665,690,715,740 and 765nm) it is positioned over bottom reaction tank, after covering photomultiplier tube, carries out electroluminescentization
Learning luminous detection and obtain its electrogenerated chemiluminescence (ECL) spectrogram, as shown in Figure 6, this carbon quantum dot has dual wavelength electricity
Cause chemiluminescence character.
Feature and the advantage of the present invention are: use high-energy ball milling method to prepare carbon quantum dot, and synthetic method is simply effective,
Cheaper starting materials is easy to get, reaction condition gentleness and environmental friendliness, it is easy to large-scale production carbon quantum dot.It addition, use this
Carbon quantum dot prepared by inventive method contains abundant oxygen-containing functional group, good water solubility, has double wave length fluorescent with double
Wavelength electrogenerated chemiluminescence character.
Accompanying drawing explanation
The HRTEM photo of the carbon quantum dot that Fig. 1 provides for the embodiment of the present invention 1.
The carbon quantum dot FTIR spectrogram that Fig. 2 provides for the embodiment of the present invention 1.Wherein, abscissa is wave number, unit
For: centimetre-1(cm-1), vertical coordinate is light transmittance, and unit is: percent (%).
The XRD spectra of the carbon quantum dot that Fig. 3 provides for the embodiment of the present invention 1.Wherein, abscissa is angle 2 θ,
Unit is: degree (°)；Vertical coordinate is diffracted intensity, and unit is: absolute unit (a.u.).
The UV-Vis spectrogram of the carbon quantum dot that Fig. 4 provides for the embodiment of the present invention 1.Wherein, abscissa is wavelength,
Unit is: nanometer (nm), vertical coordinate is absorbance, without unit.
The PL spectrogram of the carbon quantum dot that Fig. 5 provides for the embodiment of the present invention 1 (excitation wavelength by 250nm to 530nm,
Step-length 20nm).Wherein, abscissa is wavelength, and unit is: nanometer (nm), and vertical coordinate is peak intensity, and unit is:
Absolute unit (a.u.).
The ECL spectrogram of the carbon quantum dot that Fig. 6 provides for the embodiment of the present invention 1.Wherein, abscissa is wavelength, single
Position is: nanometer (nm), vertical coordinate is peak intensity, and unit is: absolute unit (a.u.).
Detailed description of the invention
Embodiment 1:
Weigh 2g activated carbon and 4g potassium hydroxide in stainless cylinder of steel, add the stainless of 9 a diameter of 20mm
The big ball of steel, the rustless steel bead (mixing of ball and 50 a diameter of 6mm in the rustless steel of 20 a diameter of 10mm
Sample is 1:70 with the mass ratio of stainless steel ball), biased sample accounts for rustless steel tank volume with the cumulative volume of stainless steel ball
1/2, with the rotating speed ball milling 50h of 500rpm.Take 0.6g milled sample, add 30mL deionized water, ultrasonic point
Dissipate 10min, be 0.2mol L by concentration-1Nitric acid is neutralized to pH=7, and 5000 revs/min (2795 × g) is centrifuged 10min,
Discard precipitation, obtain the orange-yellow supernatant.The supernatant is loaded in the super filter tube of 30kDa, centrifugation,
Take filtrate.Again filtrate is loaded in the super filter tube of 3kDa, centrifugation, add deionized water and clean 6 times extremely
Filtrate is become colorless by yellow, takes and retains part, i.e. obtains orange-yellow carbon quantum dot solution.
Fig. 1 is the HRTEM photo of above-mentioned carbon quantum dot, it can be seen that product size is more uniform, and grain
Footpath is at about 2.2nm.Fig. 2 is the FTIR spectrogram of above-mentioned carbon quantum dot, it can be seen that this carbon quantum
Point is containing abundant hydroxyl and carboxyl functional group.Fig. 3 is the XRD spectra of above-mentioned carbon quantum dot, can from figure
Going out, the spacing of lattice of this carbon quantum dot is 0.403nm, more slightly larger than the spacing of lattice of Graphene, and analysis is due to carbon
Quantum dot contains abundant surface functional group, has supportted big caused by interlamellar spacing.Fig. 4 is the UV-Vis of above-mentioned carbon quantum dot
Spectrogram, it can be seen that this carbon quantum dot is without obvious ultraviolet and visible absorption peak, but has at below 550nm
The widest absorption band, illustrates that this carbon quantum dot contains abundant oxygen-containing functional group.Fig. 5 is the PL of above-mentioned carbon quantum dot
Spectrogram, it can be seen that this carbon quantum dot is in the excitation wavelength range of 290 to 390nm, each excites
Two partly overlapping emission peaks are had under wavelength.Further, first emission peak not along with excitation wavelength change and
Mobile, emission maximum peak position is at 490nm, and the red shift along with the increase of excitation wavelength of second emission peak.Figure
6 is the ECL spectrogram of above-mentioned carbon quantum dot, it can be seen that this carbon quantum dot has the electroluminescent chemistry of dual wavelength
Luminous character.
Embodiment 2:
Weigh 2g activated carbon and 2g potassium hydroxide in stainless cylinder of steel, add the stainless of 7 a diameter of 20mm
The big ball of steel, the rustless steel bead (mixing of ball and 50 a diameter of 6mm in the rustless steel of 10 a diameter of 10mm
Sample is 1:60 with the mass ratio of stainless steel ball), biased sample accounts for rustless steel tank volume with the cumulative volume of stainless steel ball
1/3, with the rotating speed ball milling 40h of 600rpm.Take 0.6g milled sample, add 24mL deionized water, ultrasonic point
Dissipate 20min, be 0.1mol L by concentration-1Sulphuric acid is neutralized to pH=7, and 9000 revs/min (9055 × g) is centrifuged 5min,
Discard precipitation, obtain the orange-yellow supernatant.The supernatant is loaded in the super filter tube of 100kDa, centrifugal point
From, take filtrate.Again filtrate is loaded in the super filter tube of 10kDa, centrifugation, add deionized water and clean 8
Secondary, until filtrate is become colorless by yellow, take and retain part, i.e. obtain orange-yellow carbon quantum dot solution.
Embodiment 3:
Weigh 2g activated carbon and 4g sodium hydroxide in stainless cylinder of steel, add the stainless of 7 a diameter of 20mm
The big ball of steel, the rustless steel bead (mixing of ball and 30 a diameter of 6mm in the rustless steel of 10 a diameter of 10mm
Sample is 1:50 with the mass ratio of stainless steel ball), biased sample accounts for rustless steel tank volume with the cumulative volume of stainless steel ball
1/4, with the rotating speed ball milling 70h of 400rpm.Take 0.6g milled sample, add 36mL deionized water, ultrasonic point
Dissipate 30min, be 0.3mol L by concentration-1Hydrochloric acid is neutralized to pH=7,7000 revs/min (5478 × g) centrifugal 7
Min, discards precipitation, obtains the orange-yellow supernatant.The supernatant is loaded in the super filter tube of 50kDa, from
The heart separates, and takes filtrate.Again filtrate is loaded in the super filter tube of 3kDa, centrifugation, add deionized water clear
Wash 5 times, until filtrate is become colorless by yellow, take and retain part, i.e. obtain orange-yellow carbon quantum dot solution.
Examples detailed above is the citing of the present invention, although disclose for illustrative purposes highly preferred embodiment of the present invention and
Accompanying drawing, but be not intended to limit the present invention, any those of ordinary skill in the art, without departing from the present invention and
In appended spirit and scope by the claims, various replacements, to change and modifications be all possible.Therefore, this
Bright should not be limited to most preferred embodiment and accompanying drawing disclosure of that.
Claims (2)
1. a double wave length fluorescent and the preparation method of dual wavelength electrogenerated chemiluminescence carbon quantum dot, it is characterised in that work
Skill step is:
(1) with the ratio that mass ratio is 1:1～1:2 of highly basic according to activated carbon the two is mixed and this biased sample is put into
In stainless cylinder of steel, weigh stainless steel ball according to the ratio that mass ratio is 1:50～1:70 of biased sample Yu stainless steel ball and incite somebody to action
Stainless steel ball adds in stainless cylinder of steel, and wherein biased sample accounts for rustless steel tank volume with the cumulative volume of stainless steel ball
1/4～1/2, with the rotating speed ball millings 40 of 400～600 revs/min～70 hours；
(2) after ball milling step (1) obtained, sample dispersion is in deionized water, wherein, after ball milling sample with go from
The mass ratio of sub-water is 1:40～1:60, ultrasonic disperse 10～30 minutes, and being then neutralized to pH with strong acid solution is 7.0,
With the rotating speed of 5000～9000 revs/min, take supernatant in super filter tube, with high molecular cut off super filter tube centrifugation,
Take filtrate with the further centrifugation of low catching molecular super filter tube, and add deionized water wash 5～8 times, until filter
Liquid is become colorless by yellow, takes and retains part for orange-yellow carbon quantum dot solution；
Highly basic described in step (1) is any one in potassium hydroxide or sodium hydroxide；
The molecular cut off of high molecular cut off super filter tube described in step (2) is 30,50 or one in 100kDa,
The molecular cut off of low catching molecular super filter tube is the one in 3 or 10kDa, by high molecular cut off super filter tube and
Low catching molecular super filter tube is combined, to obtain various sizes of carbon quantum dot.
Preparation method the most according to claim 1, it is characterised in that described in step (2), strong acid is nitric acid, salt
Acid or sulphuric acid in any one, its concentration is 0.1～0.3mol L-1。
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| CN101973541A (en) * | 2010-10-11 | 2011-02-16 | 福州大学 | Method for extracting carbon quantum dots from activated carbon |
| CN103265020A (en) * | 2013-05-27 | 2013-08-28 | 中国科学院上海微系统与信息技术研究所 | Method for preparing graphene quantum dot powder on large scale |
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| CN101973541A (en) * | 2010-10-11 | 2011-02-16 | 福州大学 | Method for extracting carbon quantum dots from activated carbon |
| CN103265020A (en) * | 2013-05-27 | 2013-08-28 | 中国科学院上海微系统与信息技术研究所 | Method for preparing graphene quantum dot powder on large scale |
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| Carbon Nanotubols from Mechanochemical Reaction;Hualong Pan等;《Nano Lett.》;20031231;第3卷;29-32 * |
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