CN113621367A - Preparation method of rice-grain-shaped lead sulfide quantum dots - Google Patents
Preparation method of rice-grain-shaped lead sulfide quantum dots Download PDFInfo
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- CN113621367A CN113621367A CN202110658746.1A CN202110658746A CN113621367A CN 113621367 A CN113621367 A CN 113621367A CN 202110658746 A CN202110658746 A CN 202110658746A CN 113621367 A CN113621367 A CN 113621367A
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- XCAUINMIESBTBL-UHFFFAOYSA-N lead(ii) sulfide Chemical compound [Pb]=S XCAUINMIESBTBL-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002096 quantum dot Substances 0.000 claims abstract description 52
- 239000002243 precursor Substances 0.000 claims abstract description 21
- 229940056932 lead sulfide Drugs 0.000 claims abstract description 13
- 229910052981 lead sulfide Inorganic materials 0.000 claims abstract description 13
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 8
- 239000011593 sulfur Substances 0.000 claims abstract description 8
- 239000002159 nanocrystal Substances 0.000 claims abstract 2
- 239000000243 solution Substances 0.000 claims description 27
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 10
- 229920000642 polymer Polymers 0.000 claims description 10
- 239000002707 nanocrystalline material Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- 235000007164 Oryza sativa Nutrition 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 235000009566 rice Nutrition 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 239000002245 particle Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 21
- 230000001681 protective effect Effects 0.000 abstract 2
- 239000002861 polymer material Substances 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 241000209094 Oryza Species 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 3
- 239000005642 Oleic acid Substances 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 3
- 229910000464 lead oxide Inorganic materials 0.000 description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 3
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003346 selenoethers Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
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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
- C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
- C09K11/661—Chalcogenides
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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
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
- C01G21/21—Sulfides
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/30—Particle morphology extending in three dimensions
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biophysics (AREA)
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Abstract
A method for preparing rice-shaped lead sulfide quantum dots. The preparation method comprises the following steps: providing the components and the proportion of the lead sulfide quantum dot precursor, the template polymer material, the concentration and the solvent; providing process conditions of the preparation process: controlling the temperature and the protective gas to prepare a lead precursor, adding a sulfur precursor, controlling the temperature and the protective gas to prepare the rice-shaped lead sulfide nanocrystal, and separating the rice-shaped lead sulfide quantum dots.
Description
Technical Field
The invention relates to a preparation method of inorganic quantum dots with special shapes, belonging to the application fields of quantum dot sensitized solar energy, photoelectric detection and the like.
Background
The inorganic narrow-band semiconductor quantum dot material (such as sulfide or selenide) is in a visible-near infrared band for a corresponding light region of a solar spectrum, and has the advantages of easy preparation, electron mobility, adjustability of a band gap energy level and the like, so that the inorganic narrow-band semiconductor quantum dot material becomes a widely used solar light capturing agent and is applied to the fields of solar cells, photoelectric detection field effect transistors, photoluminescence devices and the like. In order to improve the photoresponse range and the structural stability of the inorganic quantum dots and aim at different application fields, researchers change the energy band structure by doping modification and a method for preparing the core-shell structure quantum dots; meanwhile, researchers at home and abroad explore a plurality of quantum dot preparation methods, including on-line methods, such as a continuous ion-sheath adsorption reaction method; off-line methods, such as thermal injection methods, regulate the shape and size of the quantum dots in different ways to regulate performance.
For example, the shape and size greatly affect the position and surface performance of quantum dots, and then affect the processes of carrier injection and recombination in quantum dot sensitized solar cell application, and the like, and have a significant effect on the apparent photovoltaic performance of the device. Reports show that the rod-shaped quantum dots are more beneficial to improving the photoelectric conversion efficiency of the battery device compared with spherical and irregular quantum dots. However, researchers are focusing on adjusting the size direction of the quantum dots, that is, changing the sizes of various quantum dots by different preparation methods and process conditions and post-treatment conditions. Relatively little research has been done on the shape control of quantum dots.
In summary, there is a great need for and a need to solve the technical problem of researching a quantum dot preparation method for simply and effectively regulating and controlling the shape of quantum dots.
Disclosure of Invention
The invention aims to provide a method for preparing a lead sulfide quantum dot in a rice grain shape, and an inorganic quantum dot nanocrystalline material in other shapes meeting different requirements is prepared according to the method.
According to the method provided by the invention, the PDPPPTD template polymer is added before the lead precursor is prepared, the mass ratio of the PDPPPTD template polymer to the lead precursor is 1.0-1.1, and the lead sulfide quantum dots in a rice-grain shape can be synthesized. When the mass ratio of the PDPPPTD template polymer to the lead precursor exceeds 1, all the synthesized lead sulfide quantum dots are in a rice grain shape.
According to the method provided by the invention, the molar ratio of the molecules of the complexing agent of the lead precursor solution to the atoms of lead of the lead source substance is 1.1-1.5.
According to the method provided by the invention, the lead precursor solution containing PDPPPTD is placed into a three-mouth bottle, vacuum pumping is carried out for 40 minutes, nitrogen is introduced at the temperature of 100-110 ℃, and the solution is stirred and reacted for 40 minutes, and then the temperature of the solution is reduced to 60 ℃.
According to the method provided by the invention, when the quantum dots are synthesized, the molar ratio of sulfur atoms to lead atoms of the sulfur precursor solution relative to the lead precursor solution is 1.1-1.2.
According to the method provided by the invention, when the quantum dots are synthesized, the sulfur precursor solution is added for three times, 2ml each time, and the interval is seven minutes.
According to the method provided by the invention, the prepared quantum dot solution is stored at minus 5-6 ℃ in a liquid form after being cooled to room temperature by adding an n-hexane dispersing agent at the temperature of 60 ℃.
According to the method provided by the invention, the prepared quantum dot solution is prepared by adding an acetone precipitator at room temperature, taking the lower layer liquid, drying in vacuum and storing in a powder form in a dark place.
The method provided by the invention has two key points, one is that the adding amount of the PDPPPTD polymer template determines the proportion of the lead sulfide rice grain-shaped quantum dots and the spherical quantum dots in the preparation system of the quantum dots, and when the mass ratio of the PDPPPTD template polymer to the lead precursor exceeds 1, all the synthesized lead sulfide quantum dots are rice grain-shaped; secondly, the process conditions are strictly controlled in the process of preparing the quantum dots, the size and the shape of the lead sulfide quantum dots are controlled under the process conditions, the diameter of the spherical quantum dots is 3-15nm, the minor axis of the rice-shaped quantum dots is 2-6 nm, and the major axis of the rice-shaped quantum dots is 10-30 nm. They are all nano-polymorphs.
Drawings
FIG. 1 is TEM photograph of rice-shaped lead sulfide quantum dots, and FIG. 2 is electron diffraction spectrum of the rice-shaped quantum dots;
FIG. 3 is a TEM photograph of spherical lead sulfide quantum dots; fig. 4 is a TEM photograph of two shapes of quantum dots coexisting.
Detailed Description
Example 1
Adding 500mg of lead oxide and 1ml of oleic acid into 5 g of PDPPPTD solution to prepare a solution, and placing the solution into a three-mouth bottle; vacuumizing for 40 minutes, introducing nitrogen at the temperature of 110 ℃, simultaneously stirring and reacting for 40 minutes, and then reducing the temperature of the solution to 60 ℃; adding simple substance sulfur into hexamethyl dithiosilane in an argon atmosphere at the temperature of 120 ℃, and stirring for 30 minutes; adding the prepared solution into three-mouth bottles for 3 times at 60 ℃, wherein each time is 2ml, and the interval is 7 minutes; adding 5ml of n-hexane at the temperature of 60 ℃, cooling to room temperature, and storing at the temperature of minus 5-6 ℃. All the prepared quantum dots are rice-grain-shaped lead sulfide quantum dots, as shown in a TEM photograph of FIG. 2.
Example 2
Adding 500mg of lead oxide and 1.5ml of oleic acid into 1g of PDPPPTD solution to prepare a solution, and placing the solution into a three-mouth bottle; vacuumizing for 40 minutes, introducing nitrogen at the temperature of 100 ℃, simultaneously stirring for reacting for 40 minutes, and then reducing the temperature of the solution to 60 ℃; adding simple substance sulfur into hexamethyl dithiosilane in an argon atmosphere at the temperature of 120 ℃, and stirring for 30 minutes; adding the prepared solution into three-mouth bottles for 3 times at 60 ℃, wherein each time is 2ml, and the interval is 7 minutes; adding 5ml of n-hexane at the temperature of 60 ℃, cooling to room temperature, and storing at the temperature of minus 5-6 ℃. Part of the prepared quantum dots are rice-grain-shaped lead sulfide quantum dots, and part of the prepared quantum dots are spherical quantum dots, as shown in a TEM photograph of fig. 4.
Example 3
500mg of lead oxide, 1.5ml of oleic acid and 25ml of octadecene are prepared into a solution and placed into a three-necked bottle; vacuumizing for 40 minutes, introducing nitrogen at the temperature of 120 ℃, simultaneously stirring and reacting for 40 minutes, and then reducing the temperature of the solution to 60 ℃; adding simple substance sulfur into hexamethyl dithiosilane in an argon atmosphere at the temperature of 120 ℃, and stirring for 30 minutes; adding the prepared solution into three-mouth bottles for 3 times at 60 ℃, wherein each time is 2ml, and the interval is 7 minutes; adding 5ml of n-hexane at the temperature of 60 ℃, cooling to room temperature, and storing at the temperature of minus 5-6 ℃. The whole part of the prepared quantum dots is spherical quantum dots, as shown in a TEM picture of FIG. 3.
Claims (9)
1. Based on the traditional inorganic quantum dot thermal injection preparation principle, PDPPPTD (polymer dispersed phase dispersed particle) is adopted, (C)15H218N6O6S4) The n polymer is used as a template to prepare a rice grain-shaped lead sulfide quantum dot nanocrystalline material different from a common spherical shape.
2. The inorganic quantum dots with other shapes than the conventional spherical shape according to claim 1, which are prepared by adding the polymer-type template material before preparing the precursor.
3. The rice-shaped lead sulfide quantum dot nanocrystalline material according to claim 1, added before preparation of a lead precursorPDPPPTD, (C15H218N6O6S4) n template polymer.
4. The rice-grain-shaped lead sulfide quantum dot nanocrystalline material according to claim 1, wherein the mass ratio of the PDPPPTD template polymer to the lead precursor is 1.0-1.1 before the lead precursor is prepared, so that the rice-grain-shaped lead sulfide quantum dot can be synthesized.
5. The rice-shaped lead sulfide quantum dot nanocrystalline material according to claim 1, wherein the mass ratio of the PDPPPTD template polymer to the lead precursor is more than 1 before the lead precursor is prepared, and all the synthesized lead sulfide quantum dots are rice-shaped.
6. The rice-shaped lead sulfide quantum dot nanocrystalline material according to claim 1, wherein the lead precursor solution containing PDPPPTD is placed in a three-mouth bottle, vacuum pumping is performed for 40 minutes, nitrogen is introduced at the temperature of 100-110 ℃, the stirring reaction is performed for 40 minutes, and then the temperature of the solution is reduced to 60 ℃.
7. The rice-shaped lead sulfide quantum dot nanocrystal material of claim 1, wherein the sulfur precursor solution is added in 3 times at intervals of 7 minutes when the quantum dots are synthesized.
8. The rice-shaped lead sulfide quantum dot nanocrystalline material according to claim 1, wherein a molar ratio of sulfur precursor solution to lead precursor solution is between 1.1 and 1.2 when the quantum dot is synthesized.
9. The rice-shaped lead sulfide quantum dot nanocrystalline material according to claim 1, wherein n-hexane is added at a temperature of 60 ℃, and the material is stored at a temperature of-5 to 6 ℃ after being cooled to room temperature.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1522953A (en) * | 2003-09-05 | 2004-08-25 | 同济大学 | Preparation method of metal sulfide semiconductor nanocrystalline |
| CN101941735A (en) * | 2010-09-09 | 2011-01-12 | 长春理工大学 | Short rod-like and peony-like lead sulfide nano-structure material and preparation method thereof |
| CN102633299A (en) * | 2010-09-09 | 2012-08-15 | 长春理工大学 | Short-rod-shaped lead sulfide nanostructured material and preparation method thereof |
| CN109850937A (en) * | 2019-01-25 | 2019-06-07 | 深圳扑浪创新科技有限公司 | A kind of preparation method of vulcanized lead quantum dot fluorescence powder |
| CN110312573A (en) * | 2016-12-30 | 2019-10-08 | 纳米2D材料有限公司 | Synthesis is assisted using the template of the 2D nanometer sheet of nanoparticle template |
-
2021
- 2021-06-15 CN CN202110658746.1A patent/CN113621367A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1522953A (en) * | 2003-09-05 | 2004-08-25 | 同济大学 | Preparation method of metal sulfide semiconductor nanocrystalline |
| CN101941735A (en) * | 2010-09-09 | 2011-01-12 | 长春理工大学 | Short rod-like and peony-like lead sulfide nano-structure material and preparation method thereof |
| CN102633299A (en) * | 2010-09-09 | 2012-08-15 | 长春理工大学 | Short-rod-shaped lead sulfide nanostructured material and preparation method thereof |
| CN110312573A (en) * | 2016-12-30 | 2019-10-08 | 纳米2D材料有限公司 | Synthesis is assisted using the template of the 2D nanometer sheet of nanoparticle template |
| CN109850937A (en) * | 2019-01-25 | 2019-06-07 | 深圳扑浪创新科技有限公司 | A kind of preparation method of vulcanized lead quantum dot fluorescence powder |
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