CN102816567A - Method for preparing high-yield carbon quantum dots - Google Patents
Method for preparing high-yield carbon quantum dots Download PDFInfo
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- CN102816567A CN102816567A CN2012102991866A CN201210299186A CN102816567A CN 102816567 A CN102816567 A CN 102816567A CN 2012102991866 A CN2012102991866 A CN 2012102991866A CN 201210299186 A CN201210299186 A CN 201210299186A CN 102816567 A CN102816567 A CN 102816567A
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 21
- 229910052799 carbon Inorganic materials 0.000 claims description 20
- 239000002096 quantum dot Substances 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 9
- YXVFQADLFFNVDS-UHFFFAOYSA-N diammonium citrate Chemical compound [NH4+].[NH4+].[O-]C(=O)CC(O)(C(=O)O)CC([O-])=O YXVFQADLFFNVDS-UHFFFAOYSA-N 0.000 claims description 6
- -1 Hydrocerol A ammonium salt Chemical class 0.000 claims description 5
- BWKOZPVPARTQIV-UHFFFAOYSA-N azanium;hydron;2-hydroxypropane-1,2,3-tricarboxylate Chemical group [NH4+].OC(=O)CC(O)(C(O)=O)CC([O-])=O BWKOZPVPARTQIV-UHFFFAOYSA-N 0.000 claims description 4
- KLOIYEQEVSIOOO-UHFFFAOYSA-N carbocromen Chemical compound CC1=C(CCN(CC)CC)C(=O)OC2=CC(OCC(=O)OCC)=CC=C21 KLOIYEQEVSIOOO-UHFFFAOYSA-N 0.000 claims description 3
- 238000006862 quantum yield reaction Methods 0.000 abstract description 14
- 239000002994 raw material Substances 0.000 abstract description 5
- 239000000090 biomarker Substances 0.000 abstract description 3
- 238000000197 pyrolysis Methods 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000005485 electric heating Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000003384 imaging method Methods 0.000 abstract 1
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 230000003013 cytotoxicity Effects 0.000 description 3
- 231100000135 cytotoxicity Toxicity 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 238000002161 passivation Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000004083 survival effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000004500 asepsis Methods 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- ZHNFLHYOFXQIOW-LPYZJUEESA-N quinine sulfate dihydrate Chemical compound [H+].[H+].O.O.[O-]S([O-])(=O)=O.C([C@H]([C@H](C1)C=C)C2)C[N@@]1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OC)C=C21.C([C@H]([C@H](C1)C=C)C2)C[N@@]1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OC)C=C21 ZHNFLHYOFXQIOW-LPYZJUEESA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
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Abstract
The invention discloses a method for preparing high-yield carbon quantum dots, which comprises the following steps that: (1) ammonium citrate is put into an electric heating furnace, the temperature rises at a heating rate of 5 to 50 DEG C/min, and the reaction is carried out for 2-4h at a temperature of 150 to 250 DEG C to obtain a pyrolysis product; (2) the pyrolysis product is milled into powder and added with ethanol to be stirred and centrifuged to remove insolubles to obtain a brown ethanol solution containing carbon quantum dots; and (3) the drying is carried out to obtain the carbon quantum dots. The process is simple to operate, the source of raw materials is wide, the cost of raw materials is low, the preparation conditions has low requirements and are relatively mild, the yield of obtained carbon quantum dots and the quantum yield are higher, the problems that the carbon quantum dots can not be produced on the scale and the fluorescence quantum yield of the obtained carbon quantum dots is low due to the limit of the process and the raw materials in the traditional preparation method of the carbon quantum dots can be solved, and the method can be applied to the fields such as biomarker, bio-imaging, a photovoltaic device, and a biosensor.
Description
Technical field
The present invention relates to carbon quantum dot preparing technical field, be specifically related to a kind of preparation method of high yield carbon quantum dot.
Background technology
The investigator had chanced on the carbon quantum dot in purification carbon nanotube process in 2004.With respect to traditional semiconductor-quantum-point, the carbon quantum dot has following advantage: particle diameter is generally less than 10nm, stable photoluminescence performance, the excitation wavelength range of broad, characteristic, excellent biocompatibility and the asepsis environment-protecting etc. that emission wavelength relies on excitation wavelength.Therefore, the carbon quantum dot is expected to replace semiconductor-quantum-point and is applied to fields such as biomarker, biological image, optoelectronic equipment and biosensor, is the research focus of carbon current field of nanometer material technology.
The preparation method of carbon current quantum dot has multiple, for example: arc process, laser method, electrochemical oxidation process, burning/thermal decomposition method, microwave method or the like.But above method often needs the material or the instrument of strict experiment condition, costliness, and process step is loaded down with trivial details, and cost is higher, and the yield of carbon quantum dot is very low.And aforesaid method synthetic carbon quantum dot generally all needs strong acid or surface passivation agent further to modify processing, to obtain certain fluorescent properties and solubility property, so be difficult to the popularization of accomplishing scale production in the short period of time.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art exists, a kind of preparation method of high yield carbon quantum dot is provided.
Technical scheme of the present invention is summarized as follows:
A kind of preparation method of high yield carbon quantum dot comprises the steps:
(1) the Hydrocerol A ammonium salt being put into electrothermal oven, is that 5～50 ℃/min heats up with temperature rise rate, and at 150～250 ℃, reaction 2～4h obtains split product;
(2) said split product is milled into powder, the ratio adding ethanol stirring 5-8h in 1g/100ml with the centrifugal 10-15min of the speed of 4000～6000rpm, removes insolubles, obtains the ethanolic soln of brown carbon containing quantum dot;
(3) with the ethanolic soln oven dry of said carbon containing quantum dot, obtain the carbon quantum dot.
The Hydrocerol A ammonium salt is ammonium dihydrogen citrate, diammonium hydrogen citrate or ammonium citrate.
Electrothermal oven is preferably retort furnace, electric tube furnace or baking oven.
Advantage of the present invention:
(1) the present invention is simple to operate, does not need follow-up strong acid or surface passivation agent to handle, and single stage method can obtain the carbon quantum dot.
(2) starting material Hydrocerol A ammonium salt and purification reagent alcohol are general reagent, wide material sources, low price.
(3) production unit only needs electrothermal oven, the stove temperature rise rate is required lower, and all can be heated to more than 150 ℃ stove all can, do not have any particular requirements such as protective atmosphere, vacuum tightness.
(4) the preparation temperature scope of carbon quantum dot is comparatively wide in range, and preparation temperature is relatively gentle, and minimum preparation temperature only needs 150 ℃.
(5) yield of carbon quantum dot is higher, generally between 2.1%～17.5%.
(6) quantum yield of carbon quantum dot is higher, is object of reference with Quinine Sulphate Di HC (quantum yield 54%), and the relative quantum productive rate of gained carbon quantum dot is generally between 22.9%～26.1%.
In a word; Technological operation of the present invention is simple; Extensive and the low price of raw material sources, preparation condition is less demanding and gentle relatively, and gained carbon quantum dot yield and quantum yield are all higher; Having solved existing carbon quantum dot preparation method can't large-scale production because of the restriction of technology and raw material and obtain the lower problem of fluorescence quantum yield of carbon quantum dot, can be applicable to fields such as biomarker, biological image, optoelectronic equipment and biosensor.
Description of drawings
Fig. 1 is the infrared spectrogram of different preparation temperature gained carbon quantum dots among the present invention.
Fig. 2 is the high power transmission electron microscope picture (a) and the size distribution figure (b) of carbon quantum dot among the present invention.
Fig. 3 is the shows fluorescent microscopy images of carbon quantum dot aqueous solution droplets among the present invention.
Fig. 4 is the cytotoxicity result under the carbon quantum dot different concns condition among the present invention.
Embodiment
In order to make those skilled in the art person understand technical scheme of the present invention better, the present invention is done further detailed description below in conjunction with accompanying drawing and embodiment.
A kind of preparation method of high yield carbon quantum dot may further comprise the steps:
(1) is that the ammonium citrate of 0.5g is put into retort furnace with quality, is set at 10 ℃/min with temperature rise rate and heats up that at 150 ℃, reaction 2.5h obtains split product;
(2) split product is milled into powder, adds 50ml ethanol and stir 6h,, remove insolubles, obtain the ethanolic soln of brown carbon containing quantum dot with the centrifugal 12min of the speed of 4500rpm;
(3) with the ethanolic soln oven dry of said carbon containing quantum dot, obtain the carbon quantum dot.Yield is 17.5%, and quantum yield is 26.1%;
Embodiment 2
A kind of preparation method of high yield carbon quantum dot may further comprise the steps:
(1) is that the ammonium dihydrogen citrate of 0.5g is put into retort furnace with quality, is set at 10 ℃/min with temperature rise rate and heats up that at 200 ℃, reaction 4h obtains split product;
(2) split product is milled into powder, adds 50ml ethanol and stir 5h,, remove insolubles, obtain the ethanolic soln of brown carbon containing quantum dot with the centrifugal 15min of the speed of 4000rpm;
(3) with the ethanolic soln oven dry of said carbon containing quantum dot, obtain the carbon quantum dot.Yield is 13.5%, and quantum yield is 23.7%;
A kind of preparation method of high yield carbon quantum dot may further comprise the steps:
(1) is that the ammonium citrate of 0.5g is put into electric tube furnace with quality, is set at 50 ℃/min with temperature rise rate and heats up that at 250 ℃, reaction 2h obtains split product;
(2) split product is milled into powder, adds 50ml ethanol and stir 5h,, remove insolubles, obtain the ethanolic soln of brown carbon containing quantum dot with the centrifugal 10min of the speed of 6000rpm;
(3) with the ethanolic soln oven dry of said carbon containing quantum dot, obtain the carbon quantum dot.Yield is 2.1%, and quantum yield is 22.9%;
A kind of preparation method of high yield carbon quantum dot may further comprise the steps:
(1) is that the ammonium citrate of 0.5g is put into baking oven with quality, is set at 5 ℃/min with temperature rise rate and heats up that at 150 ℃, reaction 3h obtains split product;
(2) split product is milled into powder, adds 50ml ethanol and stir 8h,, remove insolubles, obtain the ethanolic soln of brown carbon containing quantum dot with the centrifugal 13min of the speed of 4500rpm;
(3) with the ethanolic soln oven dry of said carbon containing quantum dot, obtain the carbon quantum dot.Yield is 16.8%, and quantum yield is 25.9%;
A kind of preparation method of high yield carbon quantum dot may further comprise the steps:
(1) is that the ammonium citrate of 0.5g is put into baking oven with quality, is set at 5 ℃/min with temperature rise rate and heats up that at 200 ℃, reaction 3h obtains split product;
(2) split product is milled into powder, adds 50ml ethanol and stir 6h,, remove insolubles, obtain the ethanolic soln of brown carbon containing quantum dot with the centrifugal 13min of the speed of 4500rpm;
(3) with the ethanolic soln oven dry of said carbon containing quantum dot, obtain the carbon quantum dot.Yield is 12.1%, and quantum yield is 24.2%;
A kind of preparation method of high yield carbon quantum dot may further comprise the steps:
(1) is that the ammonium dihydrogen citrate of 0.5g is put into retort furnace with quality, is set at 10 ℃/min with temperature rise rate and heats up that at 200 ℃, reaction 2.5h obtains split product;
(2) split product is milled into powder, adds 50ml ethanol and stir 6h,, remove insolubles, obtain the ethanolic soln of brown carbon containing quantum dot with the centrifugal 13min of the speed of 4500rpm;
(3) with the ethanolic soln oven dry of said carbon containing quantum dot, obtain the carbon quantum dot.Yield is 11.6%, and quantum yield is 21.8%;
A kind of preparation method of high yield carbon quantum dot may further comprise the steps:
(1) is that the diammonium hydrogen citrate of 0.5g is put into baking oven with quality, is set at 5 ℃/min with temperature rise rate and heats up that at 200 ℃, reaction 3h obtains split product;
(2) split product is milled into powder, adds 50ml ethanol and stir 6h,, remove insolubles, obtain the ethanolic soln of brown carbon containing quantum dot with the centrifugal 13min of the speed of 4500rpm;
(3) with the ethanolic soln oven dry of said carbon containing quantum dot, obtain the carbon quantum dot.Yield is 14.7%, and quantum yield is 22.4%;
Quartz colorimetric utensil fills the carbon quantum dot aqueous solution, is positioned on the ultraviolet transmission platform, after the 365nm excitation light source excites, sends blue-fluorescence.
Fig. 1 is the infrared spectrogram of different preparation temperature gained carbon quantum dots among the present invention, on the carbon quantum dot surface of preparation below 250 ℃ more carboxyl and amino is arranged all, and is consistent with its higher quantum yield result.
Fig. 2 is the high power transmission electron microscope picture (a) and the size distribution figure (b) of carbon quantum dot among the present invention, and the median size of carbon quantum dot is about 6nm.(embodiment 1 preparation)
Fig. 3 is the shows fluorescent microscopy images of carbon quantum dot aqueous solution droplets among the present invention.Wherein, a is a water white drop under the natural light condition; B is that ultraviolet source excites down the drop that is blue; C is that blue-light source excites down greeny drop; D is that green light source excites down the drop that takes on a red color.(embodiment 1 preparation)
Fig. 4 is the cytotoxicity result under the carbon quantum dot different concns condition among the present invention, and the carbon quantum dot is below 350mg/ml concentration, and mtt assay detects the survival rate of L929 cell more than 80%.(embodiment 1 preparation)
The median size that experiment showed, the carbon quantum dot of embodiment 2-7 preparation is about 6nm.The fluorescence of carbon quantum dot aqueous solution droplets, water white drop under the natural light condition; Excite the drop that is blueness down at ultraviolet source; Excite greeny drop down at blue-light source; Excite the drop that takes on a red color down at green light source.Cytotoxicity result under the different concns condition, the carbon quantum dot is below 350mg/ml concentration, and mtt assay detects the survival rate of L929 cell all more than 80%.
Claims (3)
1. the preparation method of one kind high yield carbon quantum dot is characterized in that, may further comprise the steps:
(1) the Hydrocerol A ammonium salt being put into electrothermal oven, is that 5～50 ℃/min heats up with temperature rise rate, and at 150～250 ℃, reaction 2～4h obtains split product;
(2) said split product is milled into powder, the ratio adding ethanol stirring 5-8h in 1g/100ml with the centrifugal 10-15min of the speed of 4000～6000rpm, removes insolubles, obtains the ethanolic soln of brown carbon containing quantum dot;
(3) with the ethanolic soln oven dry of said carbon containing quantum dot, obtain the carbon quantum dot.
2. the preparation method of a kind of high yield carbon quantum dot according to claim 1 is characterized in that: said Hydrocerol A ammonium salt is ammonium dihydrogen citrate, diammonium hydrogen citrate or ammonium citrate.
3. the preparation method of a kind of high yield carbon quantum dot according to claim 1 is characterized in that: said electrothermal oven is retort furnace, electric tube furnace or baking oven.
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| CN103382389A (en) * | 2013-07-11 | 2013-11-06 | 中山大学 | Fluorescent carbon quantum dot, its light-emitting polymer based composite material and preparation method |
| CN103497762A (en) * | 2013-06-26 | 2014-01-08 | 上海交通大学 | Method for synthesizing nitrogen doped carbon quantum dot based on one-step monocomponent hydro-thermal synthesis |
| CN103834397A (en) * | 2014-03-11 | 2014-06-04 | 太原理工大学 | Method for preparing water-soluble fluorescent carbon dots |
| CN104555978A (en) * | 2013-10-17 | 2015-04-29 | 中国科学院理化技术研究所 | Preparation method of photoluminescence carbon quantum dots |
| CN104927849A (en) * | 2015-07-08 | 2015-09-23 | 安徽工业大学 | Green synthetic method for blue fluorescence carbon quantum dots with high fluorescence quantum yield |
| CN104946251A (en) * | 2015-06-05 | 2015-09-30 | 沈阳大学 | Method for direct thermal decomposition synthesis of nitrogen-doped carbon nanoparticles |
| CN105018082A (en) * | 2015-07-10 | 2015-11-04 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing carbon quantum dot labeled probe for silk fibroin extracted cell development |
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| CN105838364A (en) * | 2016-04-29 | 2016-08-10 | 济南大学 | Method for preparing fluorescent carbon dots by pyrolyzing ammonium carboxylate |
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| CN112018439A (en) * | 2020-08-31 | 2020-12-01 | 天津大学 | Preparation and application of solid electrolyte based on polyvinyl benzene sulfonic acid lithium-citric acid carbon dots |
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