CN108557874A - A method of different size vulcanized lead quantum dots are prepared by base exchange method - Google Patents
A method of different size vulcanized lead quantum dots are prepared by base exchange method Download PDFInfo
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- CN108557874A CN108557874A CN201810224049.3A CN201810224049A CN108557874A CN 108557874 A CN108557874 A CN 108557874A CN 201810224049 A CN201810224049 A CN 201810224049A CN 108557874 A CN108557874 A CN 108557874A
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Abstract
The invention discloses a kind of methods preparing different size vulcanized lead quantum dots by base exchange method, using lead salt as lead source, using cheap sulphur powder as sulphur source, cadmium oxide is cadmium source, octadecylene is solvent, oleic acid is ligand, and cadmiumsulfide quantum dot is prepared using hot note method, and the growth time by controlling cadmiumsulfide quantum dot prepares various sizes of cadmiumsulfide quantum dot.The absorption peak of vulcanized lead quantum dot prepared by the present invention is in 888nm~1213nm, and size is in 2nm~4nm.The present invention controls its size by controlling the Quantum Dots Growth of cadmium sulfide, it is exchanged by cation, to obtain the vulcanized lead quantum dot of different absorbing wavelengths, the preparation process is more environmentally protective as the building-up process of sulphur source relative to use TMS, and manufacturing cost is cheap.
Description
Technical field
The present invention relates to a kind of method preparing different size vulcanized lead quantum dots by base exchange method, vulcanized lead amounts
For the absorption peak of son point in 888nm~1213nm, size is 2nm~4nm.
Background technology
Vulcanized lead quantum dot is the direct band-gap semicondictor material for having sodium chloride cube rock salt phase structure, its delustring system
Number is very big, is now widely used in quantum dot photovoltaic hull cell device.The controllable vulcanized lead quantum of high quality, size
Point be organic phase (such as：Octadecylene) in by regulate and control vulcanized lead quantum dot nucleation and growth (pass through control reactant mole
Than realizations such as, reaction time) come what is reached.To prevent from occurring under high-temperature situation oxidation and the oxygen of organic solvent of reactant
Change, burning etc., reaction process needs are completed in the protections system such as nitrogen or inert gas.
Currently, the synthesis of vulcanized lead quantum dot is mainly completed using hot note method, the selection of sulphur source is mainly that activity is very high
TMS, but the toxicity of TMS, unstability, volatility etc., which cause it to place in air, can lead to active rapid drawdown.In addition, price
Costliness is but also synthesis cost improves；In addition, the size and monodispersity of vulcanized lead quantum dot are applied to the meaning for also having important
Justice, usual quantum dot photovoltaic film battery device, which absorbs peak position, should be less than 1100nm, and excessive quantum dot size can be serious
Influence battery performance.In view of problem above, the present invention, as sulphur source, is injected using sulphur powder that is cheap and stablizing by heat
Two-step method synthesizes vulcanized lead quantum dot, and the Quantum Dots Growth by controlling cadmium sulfide controls its size, is exchanged by cation, from
And obtain the vulcanized lead quantum dot of different absorbing wavelengths, the preparation process relative to using TMS as sulphur source building-up process more
To be environmentally protective, and manufacturing cost is cheap.
Invention content
The present invention is intended to provide a kind of method preparing different size vulcanized lead quantum dots by base exchange method, made
Standby vulcanized lead quantum dot size is controllable, and manufacturing cost is cheap, preparation process environmental protection.
The method that the present invention prepares different size vulcanized lead quantum dots by base exchange method, includes the following steps：
Step 1：0.28g cadmium oxides, 1.5ml oleic acid and 18ml octadecylenes are added in three-necked bottle, is placed in heating mantle and stirs
Heating is mixed, 300 DEG C are to slowly warm up in the environment of argon gas, with the raising of reaction temperature, cadmium oxide reacts with oleic acid,
Oleic acid is as ligand and Cd2+In conjunction with cation precursor is formed, the color of reaction solution becomes faint yellow from brown, obtains the forerunner of cadmium
Liquid solution；
Step 2：0.032g sulphur powder heating stirrings are dissolved in 10ml octadecylenes, obtain anionic pre-cursors, for use；
Step 3：When the temperature of reaction solution in step 1 reaches 280-300 DEG C, the anionic pre-cursors that step 2 is prepared are added
In the precursor solution for entering cadmium, ice-water bath prepares various sizes of cadmium sulfide quantum by controlling the reaction time (1-5 minutes)
Point；
Step 4：Use successively ethyl alcohol and n-butylamine mixed liquor (4mL+0.1mL, the addition of n-butylamine be make aliphatic acid and
Carboxylate is preferably dissolved into ethyl alcohol phase to achieve the purpose that removal), the mixed liquor (1mL+4mL, into one of n-hexane and ethyl alcohol
Step carries out precipitation separation to cadmiumsulfide quantum dot), mixed liquor (1mL+0.1mL+3mL, the chlorine of n-hexane, chloroform and acetone
Imitative is added to octadecylene solution being retained in polarity acetone phase, to achieve the purpose that removal), n-hexane and acetone
Mixed liquor (realizing being completely separated for cadmiumsulfide quantum dot and solvent) is washed and is centrifuged to cadmiumsulfide quantum dot prepared by step 3
(4000 revs/min, centrifuge 10 minutes), cadmium sulfide powder is obtained after dry；
Step 5：The cadmium sulfide powder heating that step 4 obtains is dissolved in octadecylene, the sulphur source of 30-40mg/ml is configured to
Solution；
Step 6：Lead salt and oleyl amine mixed solution are added in three-necked bottle, is placed in heating mantle and is heated with stirring to 80 DEG C and goes forward side by side
Row vacuumizes water removal, and subsequent breaking vacuum environment is passed through argon gas, is warming up to 140 DEG C and keeps the temperature half an hour, obtains white latex
Shape solution, as lead source solution；
Step 7：The sulphur source solution that step 5 is prepared is injected into rapidly in the lead source solution that step 6 obtains, the face of reaction solution
Color becomes black from milky immediately, closes heating source, toluene, oil are separately added into when reacting liquid temperature is down to 70 DEG C, 40 DEG C
Acid continues cooling down to room temperature to dissolve the lead salt that the reaction was complete and the weaker oleyl amine ligand of quantum dot surface binding force
Acetone is added afterwards and carries out separating-purifying, obtained precipitation is vulcanized lead quantum dot, is dissolved in toluene and storing.
In step 6, the lead salt is plumbi nitras or lead chloride.
In step 7, the ratio of lead source and sulphur source is with Pb/S molar ratio computings for 2：1.
For the absorption peak of vulcanized lead quantum dot prepared by the present invention in 888nm~1213nm, size is 2nm~4nm.
Compared with the prior art, beneficial effects of the present invention are embodied in：
1, the present invention uses sulphur powder instead of the poor TMS of expensive, volatile, toxic, stability as sulphur source.
2, the method for the present invention is at low cost extensively using raw material sources, and apparatus and process is simple, and operability is strong.
3, the present invention can synthesize various sizes of vulcanized lead quantum dot by controlling the change of cadmiumsulfide quantum dot concentration.
4, the present invention can synthesize various sizes of vulcanized lead quantum dot by exchanging various sizes of cadmium sulfide.
Description of the drawings
Fig. 1 is the cleaning detailed process of cadmiumsulfide quantum dot in embodiment 1, and bottom solution is to centrifuge bottom of the tube after centrifugation
Remaining solution.
Fig. 2 is the absorption spectrum for the cadmiumsulfide quantum dot that embodiment 1 obtains, and absorption peak is in the position of 374nm.
Fig. 3 is the absorption spectrum for the vulcanized lead quantum dot that embodiment 1 obtains, and absorption peak is in the position of 888nm.
Fig. 4 is the absorption spectrum for the vulcanized lead quantum dot that embodiment 2 obtains, and absorption peak is in the position of 1020nm.
Fig. 5 is the absorption spectrum for the cadmiumsulfide quantum dot that embodiment 3 obtains, and absorption peak is in the position of 395nm.
Fig. 6 is the absorption spectrum for the vulcanized lead quantum dot that embodiment 3 obtains, and absorption peak is in the position of 982nm.
Fig. 7 is the absorption spectrum for the vulcanized lead quantum dot that embodiment 4 obtains, and absorption peak is in the position of 1213nm.
Fig. 8 is the high-resolution transmission electron microscopy figure for the vulcanized lead quantum dot that embodiment 1 obtains.
Fig. 9 is the high-resolution transmission electron microscopy figure for the vulcanized lead quantum dot that embodiment 2 obtains.
Figure 10 is the high-resolution transmission electron microscopy figure for the vulcanized lead quantum dot that embodiment 4 obtains.
Specific implementation mode
Embodiment 1：
The method for preparing different size vulcanized lead quantum dots in the present embodiment by base exchange method is as follows：
1,0.28g cadmium oxides, 1.5ml oleic acid and 18ml octadecylenes are added in three-necked bottle, are placed in stirring in heating mantle and add
Heat is to slowly warm up to 300 DEG C in the environment of argon gas, and with the raising of reaction temperature, cadmium oxide reacts with oleic acid, oleic acid
As ligand and Cd2+In conjunction with cation precursor is formed, the color of reaction solution becomes faint yellow from brown, and the presoma for obtaining cadmium is molten
Liquid；
2,0.032g sulphur powder heating stirrings are dissolved in 10ml octadecylenes, obtain anionic pre-cursors, for use；
3, when the temperature of reaction solution in step 1 reaches 280-300 DEG C, cadmium is added in the anionic pre-cursors that step 2 is prepared
Precursor solution in, reaction 1 minute after, room temperature is cooled to using ice-water bath soon, prepares cadmiumsulfide quantum dot；
4, the mixed liquor (4mL+0.1mL) of ethyl alcohol and n-butylamine, the mixed liquor (1mL+ of n-hexane and ethyl alcohol are used successively
4mL), the mixed liquor of the mixed liquor (1mL+0.1mL+3mL) of n-hexane, chloroform and acetone, n-hexane and acetone is to step 3
Preparation cadmiumsulfide quantum dot cleaning purification, centrifuge and be absorbed after drying peak 374nm cadmiumsulfide quantum dot powder；From
Heart rotating speed is 4000 revs/min, and centrifugation time is 10 minutes.
5, the cadmium sulfide powder heating that step 4 obtains is dissolved in octadecylene, is configured to the sulphur source solution of 30mg/ml；
6, lead salt and oleyl amine mixed solution are added in three-necked bottle with the molar ratio of Pb/S=2 in lead source and sulphur source, are placed in
It is heated with stirring to 80 DEG C in heating mantle and carries out vacuumizing water removal half an hour, subsequent breaking vacuum environment is passed through argon gas, is warming up to
140 DEG C and half an hour is kept the temperature, obtains white latex shape solution, as lead source solution；
7, the sulphur source solution that step 5 is prepared is injected into rapidly in the lead source solution that step 6 obtains, the color of reaction solution is vertical
Become black from milky, close heating source, toluene is separately added into when reacting liquid temperature is down to 70 DEG C, 40 DEG C, oleic acid is used
With the weaker oleyl amine ligand of dissolving the lead salt and quantum dot surface binding force that the reaction was complete, add after continuing cooling down to room temperature
Enter acetone and carry out separating-purifying, obtained precipitation is vulcanized lead quantum dot, and absorption peak is located at 888nm, is dissolved in toluene and storing up
It deposits；The lead salt is plumbi nitras.
Embodiment 2：
The method for preparing different size vulcanized lead quantum dots in the present embodiment by base exchange method is as follows：
Step 1-4, with embodiment 1.
5, the cadmium sulfide powder heating that step 4 obtains is dissolved in octadecylene, is configured to the sulphur source solution of 40mg/ml；
6, lead salt and oleyl amine mixed solution are added in three-necked bottle with the molar ratio of Pb/S=2 in lead source and sulphur source, are placed in
It is heated with stirring to 80 DEG C in heating mantle and carries out vacuumizing water removal half an hour, subsequent breaking vacuum environment is passed through argon gas, is warming up to
140 DEG C and half an hour is kept the temperature, obtains white latex shape solution, as lead source solution；
7, the sulphur source solution that step 5 is prepared is injected into rapidly in the lead source solution that step 6 obtains, the color of reaction solution is vertical
Become black from milky, close heating source, toluene is separately added into when reacting liquid temperature is down to 70 DEG C, 40 DEG C, oleic acid is used
With the weaker oleyl amine ligand of dissolving the lead salt and quantum dot surface binding force that the reaction was complete, add after continuing cooling down to room temperature
Enter acetone and carry out separating-purifying, obtained precipitation is vulcanized lead quantum dot, and absorption peak is located at 1020nm, is dissolved in toluene and storing up
It deposits；The lead salt is plumbi nitras.
Embodiment 3：
The method for preparing different size vulcanized lead quantum dots in the present embodiment by base exchange method is as follows：
1,0.28g cadmium oxides, 1.5ml oleic acid and 18ml octadecylenes are added in three-necked bottle, are placed in stirring in heating mantle and add
Heat is to slowly warm up to 300 DEG C in the environment of argon gas, and with the raising of reaction temperature, cadmium oxide reacts with oleic acid, oleic acid
As ligand and Cd2+In conjunction with cation precursor is formed, the color of reaction solution becomes faint yellow from brown, and the presoma for obtaining cadmium is molten
Liquid；
2,0.032g sulphur powder heating stirrings are dissolved in 10ml octadecylenes, obtain anionic pre-cursors, for use；
3, when the temperature of reaction solution in step 1 reaches 280-300 DEG C, cadmium is added in the anionic pre-cursors that step 2 is prepared
Precursor solution in, reaction after five minutes, room temperature is cooled to using ice-water bath soon, prepares cadmiumsulfide quantum dot；
4, the mixed liquor (4mL+0.1mL) of ethyl alcohol and n-butylamine, the mixed liquor (1mL+ of n-hexane and ethyl alcohol are used successively
4mL), the mixed liquor of the mixed liquor (1mL+0.1mL+3mL) of n-hexane, chloroform and acetone, n-hexane and acetone is to step 3
Preparation cadmiumsulfide quantum dot cleaning purification, centrifuge and be absorbed after drying peak 395nm cadmiumsulfide quantum dot powder；From
Heart rotating speed is 4000 revs/min, and centrifugation time is 10 minutes.
5, the cadmium sulfide powder heating that step 4 obtains is dissolved in octadecylene, is configured to the sulphur source solution of 30mg/ml；
6, lead salt and oleyl amine mixed solution are added in three-necked bottle with the molar ratio of Pb/S=2 in lead source and sulphur source, are placed in
It is heated with stirring to 80 DEG C in heating mantle and carries out vacuumizing water removal half an hour, subsequent breaking vacuum environment is passed through argon gas, is warming up to
140 DEG C and half an hour is kept the temperature, obtains white latex shape solution, as lead source solution；
7, the sulphur source solution that step 5 is prepared is injected into rapidly in the lead source solution that step 6 obtains, the color of reaction solution is vertical
Become black from milky, close heating source, toluene is separately added into when reacting liquid temperature is down to 70 DEG C, 40 DEG C, oleic acid is used
With the weaker oleyl amine ligand of dissolving the lead salt and quantum dot surface binding force that the reaction was complete, add after continuing cooling down to room temperature
Enter acetone and carry out separating-purifying, obtained precipitation is vulcanized lead quantum dot, and absorption peak is located at 982nm, is dissolved in toluene and storing up
It deposits；The lead salt is plumbi nitras.
Embodiment 4：
The method for preparing different size vulcanized lead quantum dots in the present embodiment by base exchange method is as follows：
Step 1-4, with embodiment 3.
5, the cadmium sulfide powder heating that step 4 obtains is dissolved in octadecylene, is configured to the sulphur source solution of 40mg/ml；
6, lead salt and oleyl amine mixed solution are added in three-necked bottle with the molar ratio of Pb/S=2 in lead source and sulphur source, are placed in
It is heated with stirring to 80 DEG C in heating mantle and carries out vacuumizing water removal half an hour, subsequent breaking vacuum environment is passed through argon gas, is warming up to
140 DEG C and half an hour is kept the temperature, obtains white latex shape solution, as lead source solution；
7, the sulphur source solution that step 5 is prepared is injected into rapidly in the lead source solution that step 6 obtains, the color of reaction solution is vertical
Become black from milky, close heating source, toluene is separately added into when reacting liquid temperature is down to 70 DEG C, 40 DEG C, oleic acid is used
With the weaker oleyl amine ligand of dissolving the lead salt and quantum dot surface binding force that the reaction was complete, add after continuing cooling down to room temperature
Enter acetone and carry out separating-purifying, obtained precipitation is vulcanized lead quantum dot, and absorption peak is located at 1213nm, is dissolved in toluene and storing up
It deposits；The lead salt is plumbi nitras.
Claims (5)
1. a kind of method preparing different size vulcanized lead quantum dots by base exchange method, it is characterised in that including walking as follows
Suddenly：
Step 1：0.28g cadmium oxides, 1.5ml oleic acid and 18ml octadecylenes are added in three-necked bottle, stirring in heating mantle is placed in and adds
Heat is to slowly warm up to 300 DEG C in the environment of argon gas, and with the raising of reaction temperature, the color of reaction solution becomes light from brown
Yellow obtains the precursor solution of cadmium；
Step 2：0.032g sulphur powder heating stirrings are dissolved in 10ml octadecylenes, obtain anionic pre-cursors, for use；
Step 3：When the temperature of reaction solution in step 1 reaches 280-300 DEG C, cadmium is added in the anionic pre-cursors that step 2 is prepared
Precursor solution in, ice-water bath, by control the reaction time prepare various sizes of cadmiumsulfide quantum dot；
Step 4：Use successively ethyl alcohol and the mixed liquor of n-butylamine, the mixed liquor of n-hexane and ethyl alcohol, n-hexane, chloroform and
The cadmiumsulfide quantum dot that the mixed liquor of the mixed liquor of acetone, n-hexane and acetone prepares step 3 is washed and is centrifuged, it is dry after
To cadmium sulfide powder；
Step 5：The cadmium sulfide powder heating that step 4 obtains is dissolved in octadecylene, the sulphur source solution of 30-40mg/ml is configured to；
Step 6：Lead salt and oleyl amine mixed solution are added in three-necked bottle, is placed in heating mantle and is heated with stirring to 80 DEG C and is taken out
Vaccum dewatering, subsequent breaking vacuum environment are passed through argon gas, are warming up to 140 DEG C and keep the temperature half an hour, it is molten to obtain white latex shape
Liquid, as lead source solution；
Step 7：The sulphur source solution that step 5 is prepared is injected into rapidly in the lead source solution that step 6 obtains, the color of reaction solution is vertical
Become black from milky, close heating source, toluene is separately added into when reacting liquid temperature is down to 70 DEG C, 40 DEG C, oleic acid is used
With the weaker oleyl amine ligand of dissolving the lead salt and quantum dot surface binding force that the reaction was complete, add after continuing cooling down to room temperature
Enter acetone and carry out separating-purifying, obtained precipitation is vulcanized lead quantum dot, is dissolved in toluene and storing.
2. according to the method described in claim 1, it is characterized in that：
In step 3, the ice-water bath lower reaction time is 1-5 minutes.
3. according to the method described in claim 1, it is characterized in that：
In step 6, the lead salt is plumbi nitras or lead chloride.
4. according to the method described in claim 1, it is characterized in that：
In step 7, the ratio of lead source and sulphur source is with Pb/S molar ratio computings for 2：1.
5. according to the method described in claim 1, it is characterized in that：
For the absorption peak of the vulcanized lead quantum dot of preparation in 888nm~1213nm, size is 2nm~4nm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109301008A (en) * | 2018-10-31 | 2019-02-01 | 深圳清华大学研究院 | Quantum dot light electric explorer and preparation method thereof |
| CN110707177A (en) * | 2019-09-25 | 2020-01-17 | 江苏大学 | Gold nanorod-lead sulfide quantum dot light detector and preparation method thereof |
| CN111682118A (en) * | 2020-06-24 | 2020-09-18 | 合肥福纳科技有限公司 | Preparation method of quantum dot, photosensitive layer and solar cell device |
| CN114015442A (en) * | 2021-11-17 | 2022-02-08 | 北京工业大学 | Vacuum-assisted large-size lead sulfide quantum dot large-batch multi-injection synthesis method |
-
2018
- 2018-03-19 CN CN201810224049.3A patent/CN108557874A/en active Pending
Non-Patent Citations (1)
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| 姚旭东: ""硫化铅量子点的合成及其新型异质结光伏器件的研究"", 《中国博士学位论文全文数据库 工程科技I辑》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109301008A (en) * | 2018-10-31 | 2019-02-01 | 深圳清华大学研究院 | Quantum dot light electric explorer and preparation method thereof |
| CN110707177A (en) * | 2019-09-25 | 2020-01-17 | 江苏大学 | Gold nanorod-lead sulfide quantum dot light detector and preparation method thereof |
| CN111682118A (en) * | 2020-06-24 | 2020-09-18 | 合肥福纳科技有限公司 | Preparation method of quantum dot, photosensitive layer and solar cell device |
| CN111682118B (en) * | 2020-06-24 | 2023-06-09 | 合肥福纳科技有限公司 | Quantum dot preparation method, photosensitive layer and solar cell device |
| CN114015442A (en) * | 2021-11-17 | 2022-02-08 | 北京工业大学 | Vacuum-assisted large-size lead sulfide quantum dot large-batch multi-injection synthesis method |
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Application publication date: 20180921 |