CN111908435A - Preparation method of CdTe nanocrystal based on halogen-like in-situ passivation method - Google Patents
Preparation method of CdTe nanocrystal based on halogen-like in-situ passivation method Download PDFInfo
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- 239000002159 nanocrystal Substances 0.000 title claims abstract description 64
- 229910004613 CdTe Inorganic materials 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000002161 passivation Methods 0.000 title claims abstract description 11
- -1 ammonium tetrafluoroborate Chemical compound 0.000 claims abstract description 19
- SOIFLUNRINLCBN-UHFFFAOYSA-N ammonium thiocyanate Chemical compound [NH4+].[S-]C#N SOIFLUNRINLCBN-UHFFFAOYSA-N 0.000 claims abstract description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- OOQZNLPSEKLHJX-UHFFFAOYSA-N 3,3,3-tris(sulfanyl)propanoic acid Chemical compound OC(=O)CC(S)(S)S OOQZNLPSEKLHJX-UHFFFAOYSA-N 0.000 claims description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims description 12
- 238000011049 filling Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 10
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 8
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 6
- 239000012279 sodium borohydride Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
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- 239000007790 solid phase Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
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- 238000002156 mixing Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 238000010979 pH adjustment Methods 0.000 claims description 2
- 150000003863 ammonium salts Chemical class 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 4
- 239000002243 precursor Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 230000006798 recombination Effects 0.000 abstract description 2
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M thiocyanate group Chemical group [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 abstract description 2
- 238000005215 recombination Methods 0.000 abstract 1
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- RWSXRVCMGQZWBV-WDSKDSINSA-N glutathione Chemical compound OC(=O)[C@@H](N)CCC(=O)N[C@@H](CS)C(=O)NCC(O)=O RWSXRVCMGQZWBV-WDSKDSINSA-N 0.000 description 2
- IZFHEQBZOYJLPK-SSDOTTSWSA-N (R)-dihydrolipoic acid Chemical compound OC(=O)CCCC[C@@H](S)CCS IZFHEQBZOYJLPK-SSDOTTSWSA-N 0.000 description 1
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 description 1
- 108010024636 Glutathione Proteins 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
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- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052950 sphalerite Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
The invention provides a preparation method of CdTe nano crystal based on a halogen-like in-situ passivation method, belonging to the technical field of nano crystal. According to the technical scheme, halogen-like ammonium salts (ammonium thiocyanate, ammonium tetrafluoroborate and ammonium hexafluorophosphate) are introduced into a precursor solution for preparing the CdTe nanocrystal, and halogen-like groups (namely thiocyanate groups, tetrafluoroborate groups and hexafluorophosphate groups) introduced in situ can effectively passivate the surface defects of the CdTe nanocrystal and reduce non-radiative recombination centers, so that the fluorescence performance and stability of the CdTe nanocrystal are effectively improved. The CdTe nanocrystal prepared by the method has high fluorescence performance and good stability; meanwhile, the method has the advantages of simple process, easily controlled preparation parameters and good repeatability, and provides a new way for preparing the high-brightness stable CdTe nanocrystal.
Description
Technical Field
The invention relates to the technical field of nanocrystals, in particular to a preparation method of CdTe nanocrystals based on a halogen-like in-situ passivation method.
Background
In recent years, CdTe nanocrystals have the advantages of narrow excitation spectrum, continuous distribution of excitation wavelength, large exciton Bohr radius, good photochemical stability and the like, and show wide application prospects in the fields of biological detection, solar cells, laser devices, photocatalysis, optical sensors and the like. At present, researchers have prepared CdTe nanocrystals with higher fluorescence quantum yield and adjustable luminescence performance by adopting different preparation methods, optimizing synthesis conditions and other measures. However, the CdTe nanocrystal has a large specific surface area, a large number of surface defects exist on the surface of the CdTe nanocrystal, and the CdTe nanocrystal is easily oxidized, so that the fluorescence performance and stability of the CdTe nanocrystal are seriously deteriorated. To actually apply the CdTe nanocrystals, it is still a challenge to further improve the fluorescence properties and stability.
In order to improve the fluorescence property and stability of CdTe nanocrystals, researchers have adopted different methods and strategies, such as surface coating with small molecule sulfhydryl compounds such as dihydrolipoic acid, mercaptopropionic acid, glutathione, etc., or formation of core-shell structures. Researches show that the measures can effectively improve the stability of the CdTe nanocrystal, but the methods still have the defects, such as: the need for specific ligands or complex process steps, etc. Therefore, it is important to explore a simple and efficient method for realizing the preparation of the CdTe nanocrystal with high brightness and stability.
Disclosure of Invention
The invention aims to provide a preparation method of CdTe nanocrystal based on halogen-like in-situ passivation method aiming at overcoming the technical problem that the fluorescence performance and stability of CdTe nanocrystal prepared by the conventional method are to be improved.
The invention also aims to solve the technical problem of how to expand the preparation method of the CdTe nanocrystal.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a preparation method of CdTe nanocrystal based on halogen-like in-situ passivation method comprises the following steps:
1) under nitrogen atmosphere, 0.2X 10-3mixing mmol tellurium powder with excessive sodium borohydride, injecting 1.2-1.5mL of deionized water, and reacting at normal temperature until black tellurium powder completely disappears to obtain NaHTe;
2) with said NaHThe molar quantity of Te in Te is a scalar quantity; adding cadmium acetate into a three-neck flask according to the molar weight of Cd being 1:1.2, injecting 200-250mL of deionized water, adding trimercaptopropionic acid into the flask according to the molar weight of trimercaptopropionic acid being 1:2.4, and adding SCN according to the scalar weight-Adding ammonium thiocyanate according to the molar weight of 1: 2.5-7.5, adjusting the pH to 9-10, turning to a nitrogen atmosphere, adding the NaHTe, and refluxing for 50-60 minutes at 100 ℃; adding 10-20mL of isopropanol, then carrying out solid-liquid separation to obtain a solid phase, washing with ethanol, and drying to obtain the CdTe nanocrystal.
Preferably, the scalar quantity SCN is-Adding ammonium thiocyanate into the mixture according to the molar weight of 1: 2.5-7.5, and replacing the ammonium thiocyanate with the mixture: according to scalar BF4Adding ammonium tetrafluoroborate into the mixture according to the molar weight ratio of 1: 2.5-7.5.
Preferably, the scalar quantity SCN is-Adding ammonium thiocyanate into the mixture according to the molar weight of 1: 2.5-7.5, and replacing the ammonium thiocyanate with the mixture: according to scalar quantity of PF6Ammonium hexafluorophosphate is added in a molar ratio of 1: 2.5-7.5.
Preferably, in the step 1), the mixing place is a branch bottle; the nitrogen atmosphere is constructed by the following method: and filling nitrogen into the branch mouth bottle for 8-10min, and removing the air in the branch mouth bottle.
Preferably, in the step 1), the injection of 1.2-1.5mL of deionized water is realized by using an injector.
Preferably, in step 2), the pH adjustment is performed by using NaOH or KOH.
Preferably, in the step 2), the conversion to the nitrogen atmosphere includes the following steps: and filling nitrogen into the three-neck flask for 30-40 minutes.
Preferably, in step 2), the solid phase is taken by solid-liquid separation, and the precipitate is taken by centrifugation at 8000r/min for 5 min.
Preferably, in the step 2), the ethanol washing is performed by washing with ethanol, centrifuging and repeating for three times.
Preferably, in step 2), the drying method is vacuum drying.
In the process of preparing the CdTe nanocrystal, the invention discovers that when halogen-like ammonium salt (comprising ammonium thiocyanate, ammonium tetrafluoroborate and ammonium hexafluorophosphate) is introduced into a precursor solution in situ, the prepared CdTe nanocrystal has enhanced fluorescence property and improved stability. Based on the beneficial discovery, the invention develops a halogen-like in-situ passivation method for preparing the CdTe nanocrystal with high and stable brightness, namely, in the process of preparing the CdTe nanocrystal, halogen-like ammonium salt (comprising ammonium thiocyanate, ammonium tetrafluoroborate and ammonium hexafluorophosphate) is introduced into a precursor solution in situ to prepare the CdTe nanocrystal.
The result of the invention shows that the halogen-like ammonium salt (comprising ammonium thiocyanate, ammonium tetrafluoroborate and ammonium hexafluorophosphate) is introduced into the precursor solution for preparing the CdTe nanocrystal, and the halogen-like groups (namely thiocyanate groups, tetrafluoroborate groups and hexafluorophosphate groups) introduced in situ can effectively passivate the surface defects of the CdTe nanocrystal and reduce the non-radiative recombination center, thereby effectively improving the fluorescence performance and stability of the CdTe nanocrystal. The invention provides a new method for preparing the CdTe nanocrystal with high brightness and stability.
The invention has the beneficial effects that: the CdTe nanocrystal prepared by the method has high fluorescence performance and good stability; meanwhile, the method has the advantages of simple process, easily controlled preparation parameters and good repeatability, and provides a new way for preparing the high-brightness stable CdTe nanocrystal.
Drawings
FIG. 1 is a transmission electron micrograph of CdTe nanocrystal prepared in example 1.
FIG. 2 is an X-ray diffraction pattern of the CdTe nanocrystal prepared in example 1.
FIG. 3 is the UV-visible absorption spectrum of the CdTe nanocrystal prepared in example 1.
FIG. 4 is the fluorescence spectrum of CdTe nanocrystal prepared in example 1.
FIG. 5 is a TEM photograph of the CdTe nanocrystal prepared in example 2.
FIG. 6 is a TEM photograph of the CdTe nanocrystal prepared in example 3.
Detailed Description
Hereinafter, specific embodiments of the present invention will be described in detail. Well-known structures or functions may not be described in detail in the following embodiments in order to avoid unnecessarily obscuring the details. Approximating language, as used herein in the following examples, may be applied to identify quantitative representations that could permissibly vary in number without resulting in a change in the basic function. Unless defined otherwise, technical and scientific terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
A halogen-like in-situ passivation method for preparing CdTe nano crystal with high brightness and stability includes the following steps:
(1) preparation of NaHTe:
weighing 0.2 × 10-3mmol tellurium powder, weighing slightly excessive sodium borohydride (NaBH)4) Filling nitrogen for 8-10min in a bottle with a branch mouth to remove air, injecting 1.2-1.5mL of deionized water by using a syringe, and reacting at normal temperature until the black tellurium powder completely disappears.
(2) Preparing CdTe nano crystal:
weighing cadmium acetate with corresponding mass according to the molar ratio of Cd to Te being 1:1.2, adding 200-250mL deionized water, adding trimercaptopropionic acid (MPA) according to the proportion of Te to MPA being 1:2.4, and adding Te to SCN according to the proportion of Te to SCN-Adding halogen-like ammonium salt (comprising ammonium thiocyanate, ammonium tetrafluoroborate and ammonium hexafluorophosphate) according to the molar ratio of 1: 2.5-7.5, adjusting the pH to about 9-10 by using NaOH or KOH, then filling nitrogen for 30-40 minutes, injecting the prepared NaHTe into a three-neck bottle, and refluxing for 50-60 minutes at 100 ℃ to obtain a clear transparent solution. Adding 10-20mL of isopropanol into the obtained clear transparent solution to remove excessive MPA and salt, centrifuging the nanocrystal solution for 5min at 8000r/min, removing supernatant, taking precipitate, washing with ethanol, centrifuging for three times, and vacuum drying to obtain CdTe nanocrystal.
Example 1
Weighing 0.026mg of tellurium powder, 0.009mg of sodium borohydride in a bottle with a branch mouth, and filling 10min of nitrogen to remove air in the bottle with the branch mouth. Injecting 1.2mL of deionized water by using an injector, and reacting at normal temperature until the black tellurium powder completely disappears to obtain a colorless transparent solution.
0.044mg of cadmium acetate is weighed into a three-neck flask, 200mL of deionized water is injected, trimercaptopropionic acid (MPA) is added according to the proportion of Te to MPA being 1:2.4, and Te to SCN-Adding ammonium thiocyanate according to the ratio of 1:2.5, adjusting the pH value to be about 9 by using NaOH, then filling nitrogen for 30min, injecting the prepared NaHTe into a three-neck bottle, and refluxing at 100 ℃ for 55min to obtain a clear and transparent solution. Adding 20mL of isopropanol into the obtained clear transparent solution to remove redundant MPA and salt, then centrifuging the CdTe nanocrystal solution for 5min at 8000r/min, removing supernatant, taking precipitate, then washing with ethanol, centrifuging for three times, and then performing vacuum drying to obtain CdTe nanocrystals.
FIGS. 1-4 are respectively a transmission electron microscope photograph, an X-ray diffraction pattern, an ultraviolet-visible absorption spectrum and a fluorescence spectrum of the prepared CdTe nanocrystal. As can be seen from the figure, the prepared CdTe nanocrystal has a particle size of about 4.1 nm, is a sphalerite structure, and has a light emission peak at 542 nm. The aqueous solution of CdTe nanocrystal can be stored stably for more than 4 weeks.
Example 2
Weighing 0.026mg of tellurium powder, 0.009mg of sodium borohydride in a bottle with a branch mouth, and filling 10min of nitrogen to remove air in the bottle with the branch mouth. Injecting 1.2mL of deionized water by using an injector, and reacting at normal temperature until the black tellurium powder completely disappears to obtain a colorless transparent solution.
0.044mg of cadmium acetate is weighed into a three-neck flask, 200mL of deionized water is injected, trimercaptopropionic acid (MPA) is added according to the proportion of Te to MPA being 1:2.4, and Te to BF4 -Adding ammonium tetrafluoroborate according to the ratio of 1:5, adjusting the pH value to be about 9 by NaOH, then filling nitrogen for 30min, injecting the prepared NaHTe into a three-mouth bottle, and refluxing at 100 ℃ for 55min to obtain a clear and transparent solution. Adding 20mL of isopropanol into the obtained clear transparent solution to remove redundant MPA and salt, then centrifuging the CdTe nanocrystal solution for 5min at 8000r/min, removing supernatant, taking precipitate, then washing with ethanol, centrifuging for three times, and then performing vacuum drying to obtain CdTe nanocrystals.
FIG. 5 is a TEM photograph of the CdTe nanocrystal prepared in example 2. As can be seen from the figure, the size of the CdTe nanocrystal particles produced is about 4.5 nanometers.
Example 3
Weighing 0.026mg of tellurium powder, 0.009mg of sodium borohydride in a bottle with a branch mouth, and filling 10min of nitrogen to remove air in the bottle with the branch mouth. Injecting 1.2mL of deionized water by using an injector, and reacting at normal temperature until the black tellurium powder completely disappears to obtain a colorless transparent solution.
0.044mg of cadmium acetate is weighed into a three-neck flask, 200mL of deionized water is injected, trimercaptopropionic acid (MPA) is added according to the proportion of Te to MPA to 1:2.4, and Te to PF6 -Ammonium hexafluorophosphate is added according to the ratio of 1:7.5, the pH value is adjusted to about 9 by NaOH, then nitrogen is filled for 30min, the prepared NaHTe is injected into a three-mouth bottle, and the mixture is refluxed for 55min at the temperature of 100 ℃ to obtain clear and transparent solution. Adding 20mL of isopropanol into the obtained clear transparent solution to remove redundant MPA and salt, then centrifuging the CdTe nanocrystal solution for 5min at 8000r/min, removing supernatant, taking precipitate, then washing with ethanol, centrifuging for three times, and then performing vacuum drying to obtain CdTe nanocrystals.
FIG. 6 is a TEM photograph of the CdTe nanocrystal prepared in example 3. As can be seen from the figure, the size of the CdTe nanocrystal particles produced is about 4.8 nanometers.
The embodiments of the present invention have been described in detail, but the description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. Any modification, equivalent replacement, and improvement made within the scope of the application of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of CdTe nanocrystal based on halogen-like in-situ passivation method is characterized by comprising the following steps:
1) under nitrogen atmosphere, 0.2X 10-3mixing mmol tellurium powder with excessive sodium borohydride, injecting 1.2-1.5mL of deionized water, and reacting at normal temperature until black tellurium powder completely disappears to obtain NaHTe;
2) taking the molar quantity of Te in the NaHTe as a scalar; adding cadmium acetate into a three-neck flask according to the molar weight of Cd being 1:1.2, injecting 200-250mL of deionized water, adding trimercaptopropionic acid into the flask according to the molar weight of trimercaptopropionic acid being 1:2.4, and adding SCN according to the scalar weight-Adding ammonium thiocyanate according to the molar weight of 1: 2.5-7.5, adjusting the pH to 9-10, turning to a nitrogen atmosphere, adding the NaHTe, and refluxing for 50-60 minutes at 100 ℃; adding 10-20mL of isopropanol, then carrying out solid-liquid separation to obtain a solid phase, washing with ethanol, and drying to obtain the CdTe nanocrystal.
2. The preparation method of CdTe nanocrystal based on halogen-like in-situ passivation method as claimed in claim 1, wherein SCN is added according to scalar ratio-Adding ammonium thiocyanate into the mixture according to the molar weight of 1: 2.5-7.5, and replacing the ammonium thiocyanate with the mixture: according to scalar BF4Adding ammonium tetrafluoroborate into the mixture according to the molar weight ratio of 1: 2.5-7.5.
3. The preparation method of CdTe nanocrystal based on halogen-like in-situ passivation method as claimed in claim 1, wherein SCN is added according to scalar ratio-Adding ammonium thiocyanate into the mixture according to the molar weight of 1: 2.5-7.5, and replacing the ammonium thiocyanate with the mixture: according to scalar quantity of PF6Ammonium hexafluorophosphate is added in a molar ratio of 1: 2.5-7.5.
4. The method according to any one of claims 1 to 3, wherein in step 1), the mixing place is a branched bottle; the nitrogen atmosphere is constructed by the following method: and filling nitrogen into the branch mouth bottle for 8-10min, and removing the air in the branch mouth bottle.
5. The method according to any one of claims 1 to 3, wherein the step 1) of injecting 1.2 to 1.5mL of deionized water is performed by using a syringe.
6. The method according to any one of claims 1 to 3, wherein the pH adjustment in step 2) is carried out using NaOH or KOH.
7. The method according to any one of claims 1 to 3, wherein the step 2) of converting the nitrogen atmosphere comprises the steps of: and filling nitrogen into the three-neck flask for 30-40 minutes.
8. The method according to any one of claims 1 to 3, wherein in the step 2), the solid-liquid separation is performed to take out a solid phase, and the solid phase is centrifuged at 8000r/min for 5min to take out a precipitate.
9. The method according to any one of claims 1 to 3, wherein the ethanol washing in step 2) is performed by washing with ethanol, centrifuging, and repeating three times.
10. The method according to any one of claims 1 to 3, wherein in the step 2), the drying method is vacuum drying.
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Citations (5)
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Application publication date: 20201110 |