CN102634342A - Preparation method of water-soluble CdTe quantum dot - Google Patents
Preparation method of water-soluble CdTe quantum dot Download PDFInfo
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- CN102634342A CN102634342A CN2012100947996A CN201210094799A CN102634342A CN 102634342 A CN102634342 A CN 102634342A CN 2012100947996 A CN2012100947996 A CN 2012100947996A CN 201210094799 A CN201210094799 A CN 201210094799A CN 102634342 A CN102634342 A CN 102634342A
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Abstract
The invention discloses a preparation method of a water-soluble CdTe quantum dot, which includes: using cadmium salt as a cadmium source, tellurium dioxide as a tellurium source and sulfhydryl compound as stabilizer, and performing one-step preparation in a water phase system to directly synthetize high-fluorescence and water-soluble CdTe quantum dot. The preparation method has simple steps, used reagents are few, cost is low and the method is easy to implement. The whole production process meets the green and chemical requirements and is safe and environment-friendly. The prepared CdTe quantum dot has high quantum yield and high stability.
Description
Technical field
The present invention relates to the preparation method of inorganic semiconductor preparation of nanomaterials, particularly a kind of water-soluble CdTe quantum dots.
Background technology
Quantum dot is a kind of novel inorganic semiconductor nano material, because its excellent optical property has caused the extensive interest of academia.Quantum dot has excellent luminescent properties, such as the fluorescent emission of size adjustable, and narrow and symmetric emmission spectrum, wide and successive absorption spectrum, fabulous light stability makes him demonstrate great potential aspect biomarker and the bio-imaging.The CdTe quantum dot is the most extensively II-IV family quantum dot of the present maximum and application of studying, owing to it has great application prospect at biomarker with on forming images, so how easy synthetic CdTe quantum dot is the direction of researchist in effort always.The quantum dot of biologically using at present is still mainly from organic synthesis, and this method synthetic quantum dot has single dispersion, high quantum production rate and good advantages such as percent crystallinity; Shortcomings such as but also there is severe reaction conditions in this method, and synthetic cost is high, and toxicity is big, and product is water insoluble.1996, Rogach, A.L. proposed the synthetic CdTe quantum dot of water first, and were that stablizer has synthesized the CdTe quantum dot with the sulfhydryl compound.Because aqueous phase synthetic CdTe quantum dot has water-soluble and biocompatibility, thereby can directly be used for biological mark and detection.But to prepare telluretted hydrogen (H earlier usually in the method for the synthetic CdTe quantum dot of present water method
2Te) or sodium hydrogen telluride (NaHTe) as the tellurium source, the preparation process need distributes, and operates comparatively loaded down with trivial details.
Through existing literature is investigated; Find that Shen etc. has delivered the paper that is entitled as " Size-and shape-controlled synthesis of CdTe and PbTe nanocrystals using tellurium dioxide as the tellurium precursor " (" with the tellurous oxide for the controlled CdTe of the synthetic shape and size in tellurium source and the nano particle of PbTe ") on Chem.Mater (2010 the 22nd volume 4756-4761); Though adopting tellurous oxide is that the tellurium source is in operation; And the aspect of performance of quantum dot has been obtained improvement; But the synthesis condition of organic phase is still comparatively harsh, thereby has limited the greenization and the handiness of the operation of this method.
Summary of the invention
The preparation method of a kind of water-soluble CdTe quantum dots that the objective of the invention is to be directed against the deficiency of prior art and provide; This method is passed through with cadmium salt as the cadmium source; Tellurous oxide is as the tellurium source; Sulfhydryl compound is as stablizer, thereby realizes the directly synthetic high fluorescence of step preparation, water miscible CdTe quantum dot, and is convenient, simply synthesized the CdTe quantum dot.
The objective of the invention is to realize like this:
A kind of preparation method of water-soluble CdTe quantum dots; It is characterized in that this method adopts tellurous oxide as the tellurium source; Cadmium salt is as the cadmium source, and sulfhydryl compound is realized the directly synthetic high fluorescence of step preparation, water miscible CdTe quantum dot as stablizer at aqueous phase system; The concrete operations step is following:
Method one
(1) under the room temperature, to concentration be 0.5～5.0 mmole/liter cadmium salt soln in add sulfhydryl compound, the mol ratio of cadmium salt and sulfhydryl compound is 1:1.3～2.4, obtains the precursor solution of cadmium;
(2) in the precursor solution of the cadmium that step (1) makes, add tellurous oxide, the mol ratio of cadmium salt and tellurous oxide is 1:0.1～0.5, and be adjusted to pH=8～12.5 with sodium hydroxide with it with solution acidity this moment;
(3) in the solution that step (2) makes, feed nitrogen; Again to wherein adding reductive agent, 80～105 ℃ of reflux 30 minutes to 30 hours, the mol ratio of tellurous oxide and reductive agent was 1:1.5～3; Adition process is carried out under magnetic agitation, makes the CdTe quantum dot solution;
(4) the CdTe quantum dot solution that step (3) is made is centrifugal with 8000 rev/mins rotating speed, the gained precipitation is dispersed in the acetone soln after removing supernatant liquid, spinning 2～4 times, at last with the gained resolution of precipitate in water, water-soluble CdTe quantum dots;
Method two
(1) under the room temperature, to concentration be 0.5～5.0 mmole/liter cadmium salt soln in add sulfhydryl compound, the mol ratio of cadmium salt and sulfhydryl compound is 1:1.3～2.4, obtains the precursor solution of cadmium;
(2) in the precursor solution of the cadmium that step (1) makes, add tellurous oxide, the mol ratio of cadmium salt and tellurous oxide is 1:0.1～0.5, and be adjusted to pH=8～12.5 with sodium hydroxide with it with solution acidity this moment;
(3) in the solution that step (2) makes, feed nitrogen, 80～105 ℃ of reflux 30 minutes to 30 hours, adition process was carried out under magnetic agitation, makes the CdTe quantum dot solution;
(4) the CdTe quantum dot solution that step (3) is made is centrifugal with 8000 rev/mins rotating speed, the gained precipitation is dispersed in the acetone soln after removing supernatant liquid, spinning 2～4 times, at last with the gained resolution of precipitate in water, water-soluble CdTe quantum dots; Wherein:
Said sulfhydryl compound structure is:
N=0-10 in the formula; P=1-10; M=0-10; R and R ' are identical or different, and R and R ' are COOH, NH
2Or OH;
Said cadmium salt is a Cadmium chloride fine powder, cadmium perchlorate, cadmium acetate; Reductive agent is NaBH
4, NH
2NH
2
Preparation process of the present invention is simple, and agents useful for same quantity is few, and cost is low, and is easy to implement; Whole process of preparation satisfies the requirement of Green Chemistry, safety, environmental protection; Prepared CdTe quantum dot has higher quantum yield, well stability.
Description of drawings
Fig. 1 is the fluorescence spectrum figure of the embodiment of the invention 1 obtained CdTe quantum dot;
Fig. 2 is the ultraviolet-visible absorption spectrum figure of the embodiment of the invention 1 obtained CdTe quantum dot;
Fig. 3 is the fluorescence spectrum figure of the embodiment of the invention 2 obtained CdTe quantum dots;
Fig. 4 is the ultraviolet-visible absorption spectrum figure of the embodiment of the invention 2 obtained CdTe quantum dots;
Fig. 5 is the fluorescence spectrum figure of the embodiment of the invention 3 obtained CdTe quantum dots;
Fig. 6 is the ultraviolet-visible absorption spectrum figure of the embodiment of the invention 3 obtained CdTe quantum dots;
Fig. 7 is the fluorescence spectrum figure of the embodiment of the invention 4 obtained CdTe quantum dots;
Fig. 8 is the ultraviolet-visible absorption spectrum figure of the embodiment of the invention 4 obtained CdTe quantum dots;
Fig. 9 is the fluorescence spectrum figure of the embodiment of the invention 5 obtained CdTe quantum dots;
Figure 10 is the ultraviolet-visible absorption spectrum figure of the embodiment of the invention 5 obtained CdTe quantum dots;
Figure 11 is the fluorescence spectrum figure of the embodiment of the invention 6 obtained CdTe quantum dots;
Figure 12 is the ultraviolet-visible absorption spectrum figure of the embodiment of the invention 6 obtained CdTe quantum dots;
Figure 13 is the fluorescence spectrum figure of the embodiment of the invention 7 obtained CdTe quantum dots;
Figure 14 is the ultraviolet-visible absorption spectrum figure of the embodiment of the invention 7 obtained CdTe quantum dots.
Embodiment
Below in conjunction with specific embodiment the present invention is further specified, embodiment provided the process of embodiment, but protection scope of the present invention is not limited thereto being to implement under the prerequisite with technical scheme of the present invention.
The fluorescence pattern of the CdTe quantum of the present invention's preparation is gathered by spectrophotofluorometer PerkinElmer LS55 and is obtained, and ultraviolet-visible light extinction spectrum is obtained by unic 2802 series ultraviolet visible spectrophotometer collections.
Embodiment 1
(1) under the room temperature with zero(ppm) water with 1.24 milliliter of 80.7 mmole/liter dichloride cadmium be diluted to 88.76 milliliters, add 21.34 ul MPA;
(2) solution in step (1) adds 8.0 mg TeO
2, utilize sodium hydroxide to transfer pH value of solution to 11.5 then;
(3) solution to step (2) led to nitrogen 5～30 minutes, stirred down, added 5.8 milligrams of Peng Qinghuanas, and then added 5 ml distilled waters, made Peng Qinghuana get in the solution fully;
(4) solution with step 3 is heated to 100 ℃; Between measure appearance at regular intervals, thereby the situation of carrying out of monitoring reaction;
(5) solution that step (4) is made is centrifugal with 8000 rev/mins rotating speed, the gained precipitation is dispersed in the acetone soln after removing supernatant liquid, spinning 2～4 times, at last with the gained resolution of precipitate in water, water-soluble CdTe quantum dots.
The present embodiment material molar ratio is CdCl
2: MPA:TeO
2=1:2.4:0.5.
Fig. 1, Fig. 2 are the fluorescence spectrum figure and the ultraviolet-visible absorption spectrum collection of illustrative plates of embodiment 1 gained water-soluble CdTe quantum dots.
Embodiment 2
The consumption of preparation process and dichloride cadmium is identical with embodiment 1, and material molar ratio is CdCl
2: MPA:TeO
2=1:1.3:0.5.
Fig. 3, Fig. 4 are the fluorescence spectrum figure and the ultraviolet-visible absorption spectrum figure of embodiment 2 gained water-soluble CdTe quantum dots.
The consumption of preparation process and dichloride cadmium is identical with embodiment 1, and material molar ratio is CdCl
2: MPA:TeO
2=1:1.3:0.2.
Fig. 5, Fig. 6 are the fluorescence spectrum figure and the ultraviolet-visible absorption spectrum figure of embodiment 3 gained water-soluble CdTe quantum dots.
Embodiment 4
The consumption of preparation process and dichloride cadmium is identical with embodiment 1, material molar ratio CdCl
2: MPA:TeO
2=1:1.3:0.1.
Fig. 7, Fig. 8 are the fluorescence spectrum figure and the ultraviolet-visible absorption spectrum figure of embodiment 4 gained water-soluble CdTe quantum dots.
Embodiment 5
The consumption of preparation process and dichloride cadmium is identical with embodiment 1, and material molar ratio is CdCl
2: MPA:TeO
2=1:1.7:0.5.
Fig. 9, Figure 10 are the fluorescence spectrum figure and the ultraviolet-visible absorption spectrum figure of embodiment 5 gained water-soluble CdTe quantum dots.
Embodiment 6
The consumption of preparation process and dichloride cadmium is identical with embodiment 1, and material molar ratio is CdCl
2: MPA:TeO
2=1:1.7:0.3.
Figure 11, Figure 12 are the fluorescence spectrum figure and the ultraviolet-visible absorption spectrum figure of embodiment 6 gained water-soluble CdTe quantum dots.
Embodiment 7
The consumption of preparation process and dichloride cadmium is identical with embodiment 1, and material molar ratio is CdCl
2: MPA:TeO
2=1:1.7:0.1.
Figure 13, Figure 14 are the fluorescence spectrum figure and the ultraviolet-visible absorption spectrum collection of illustrative plates of embodiment 7 gained water-soluble CdTe quantum dots.
The fluorescence emission peak scope of the CdTe quantum of the present invention's preparation is that the position of 480～880nm emission peak can be regulated and control through the control experiment condition as required.
Claims (1)
1. the preparation method of a water-soluble CdTe quantum dots; It is characterized in that this method adopts tellurous oxide as the tellurium source; Cadmium salt is as the cadmium source, and sulfhydryl compound is realized the directly synthetic high fluorescence of step preparation, water miscible CdTe quantum dot as stablizer at aqueous phase system; The concrete operations step is following:
(1) under the room temperature, to concentration be 0.5～5.0 mmole/liter cadmium salt soln in add sulfhydryl compound, the mol ratio of cadmium salt and sulfhydryl compound is 1:1.3～2.4, obtains the precursor solution of cadmium;
(2) in the precursor solution of the cadmium that step (1) makes, add tellurous oxide, the mol ratio of cadmium salt and tellurous oxide is 1:0.1～0.5, and be adjusted to pH=8～12.5 with sodium hydroxide with it with solution acidity this moment;
(3) in the solution that step (2) makes, feed nitrogen; Again to wherein adding reductive agent, 80～105 ℃ of reflux 30 minutes to 30 hours, the mol ratio of tellurous oxide and reductive agent was 1:1.5～3; Adition process is carried out under magnetic agitation, makes the CdTe quantum dot solution;
(4) the CdTe quantum dot solution that step (3) is made is centrifugal with 8000 rev/mins rotating speed, the gained precipitation is dispersed in the acetone soln after removing supernatant liquid, spinning 2～4 times, at last with the gained resolution of precipitate in water, water-soluble CdTe quantum dots;
Perhaps
(1) under the room temperature, to concentration be 0.5～5.0 mmole/liter cadmium salt soln in add sulfhydryl compound, the mol ratio of cadmium salt and sulfhydryl compound is 1:1.3～2.4, obtains the precursor solution of cadmium;
(2) in the precursor solution of the cadmium that step (1) makes, add tellurous oxide, the mol ratio of cadmium salt and tellurous oxide is 1:0.1～0.5, and be adjusted to pH=8～12.5 with sodium hydroxide with it with solution acidity this moment;
(3) in the solution that step (2) makes, feed nitrogen, 80～105 ℃ of reflux 30 minutes to 30 hours, adition process was carried out under magnetic agitation, makes the CdTe quantum dot solution;
(4) the CdTe quantum dot solution that step (3) is made is centrifugal with 8000 rev/mins rotating speed, the gained precipitation is dispersed in the acetone soln after removing supernatant liquid, spinning 2～4 times, at last with the gained resolution of precipitate in water, water-soluble CdTe quantum dots; Wherein:
Said sulfhydryl compound structure is:
N=0-10 in the formula; P=1-10; M=0-10; R is identical with R ' or inequality, and R and R ' are COOH, NH
2Or OH;
Said cadmium salt is a Cadmium chloride fine powder, cadmium perchlorate, cadmium acetate; Reductive agent is NaBH
4, NH
2NH
2
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011095A (en) * | 2012-12-29 | 2013-04-03 | 湖南科技大学 | Rapid preparation method of cadmium telluride quantum dot |
| CN103552999A (en) * | 2013-10-25 | 2014-02-05 | 湖南科技大学 | Method for preparing quantum dots at low temperature |
| CN103979506A (en) * | 2014-05-26 | 2014-08-13 | 合肥工业大学 | Preparation method of hyperfluorescent cadmium telluride quantum dot |
| CN104357059A (en) * | 2014-11-28 | 2015-02-18 | 湖南科技大学 | Preparation method of near-infrared CdTe quantum dots |
| CN106053787A (en) * | 2016-06-06 | 2016-10-26 | 上海师范大学 | Fluorescent immunochromatography test strip for detecting furazolidone metabolites as well as preparation and application |
| CN108774512A (en) * | 2018-06-07 | 2018-11-09 | 太仓萃励新能源科技有限公司 | A kind of method of synthesis in water ZnSe@ZnS quantum dots |
Citations (1)
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|---|---|---|---|---|
| CN101870459A (en) * | 2010-06-11 | 2010-10-27 | 山东大学 | Method for preparing water-soluble CdTe quantum dots |
-
2012
- 2012-03-31 CN CN2012100947996A patent/CN102634342A/en active Pending
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| CN101870459A (en) * | 2010-06-11 | 2010-10-27 | 山东大学 | Method for preparing water-soluble CdTe quantum dots |
Non-Patent Citations (3)
| Title |
|---|
| 王益林等: "一锅合成绿色到近红外发射的CdTe量子点", 《无机化学学报》, 31 January 2012 (2012-01-31) * |
| 王益林等: "以TeO2为碲源水相合成CdTe量子点及其表征", 《化工学报》, 31 March 2011 (2011-03-31) * |
| 王益林等: "颜色可调的高荧光CdTe量子点的水相合成", 《高等学校化学学报》, 31 December 2011 (2011-12-31) * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011095A (en) * | 2012-12-29 | 2013-04-03 | 湖南科技大学 | Rapid preparation method of cadmium telluride quantum dot |
| CN103011095B (en) * | 2012-12-29 | 2014-10-29 | 湖南科技大学 | Rapid preparation method of cadmium telluride quantum dot |
| CN103552999A (en) * | 2013-10-25 | 2014-02-05 | 湖南科技大学 | Method for preparing quantum dots at low temperature |
| CN103552999B (en) * | 2013-10-25 | 2015-06-17 | 湖南科技大学 | Method for preparing quantum dots at low temperature |
| CN103979506A (en) * | 2014-05-26 | 2014-08-13 | 合肥工业大学 | Preparation method of hyperfluorescent cadmium telluride quantum dot |
| CN104357059A (en) * | 2014-11-28 | 2015-02-18 | 湖南科技大学 | Preparation method of near-infrared CdTe quantum dots |
| CN104357059B (en) * | 2014-11-28 | 2016-04-06 | 湖南科技大学 | A kind of preparation method of near infrared CdTe quantum |
| CN106053787A (en) * | 2016-06-06 | 2016-10-26 | 上海师范大学 | Fluorescent immunochromatography test strip for detecting furazolidone metabolites as well as preparation and application |
| CN108774512A (en) * | 2018-06-07 | 2018-11-09 | 太仓萃励新能源科技有限公司 | A kind of method of synthesis in water ZnSe@ZnS quantum dots |
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Application publication date: 20120815 |