CN106129142B - A kind of preparation method of vulcanized lead quantum dot - Google Patents
A kind of preparation method of vulcanized lead quantum dot Download PDFInfo
- Publication number
- CN106129142B CN106129142B CN201610465936.0A CN201610465936A CN106129142B CN 106129142 B CN106129142 B CN 106129142B CN 201610465936 A CN201610465936 A CN 201610465936A CN 106129142 B CN106129142 B CN 106129142B
- Authority
- CN
- China
- Prior art keywords
- solution
- quantum dot
- preparation
- vulcanized lead
- amount
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000002096 quantum dot Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims description 47
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 28
- 239000001509 sodium citrate Substances 0.000 claims description 22
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 22
- 239000011259 mixed solution Substances 0.000 claims description 15
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 13
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 12
- PNZVFASWDSMJER-UHFFFAOYSA-N acetic acid;lead Chemical compound [Pb].CC(O)=O PNZVFASWDSMJER-UHFFFAOYSA-N 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 241000238370 Sepia Species 0.000 claims description 6
- 239000012752 auxiliary agent Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 239000003643 water by type Substances 0.000 claims description 5
- 229940046892 lead acetate Drugs 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 239000005864 Sulphur Substances 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000001228 spectrum Methods 0.000 abstract description 3
- 230000009466 transformation Effects 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 5
- IZFHEQBZOYJLPK-SSDOTTSWSA-N (R)-dihydrolipoic acid Chemical compound OC(=O)CCCC[C@@H](S)CCS IZFHEQBZOYJLPK-SSDOTTSWSA-N 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerol Natural products OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
- -1 monothio glycerine Chemical compound 0.000 description 4
- 235000005979 Citrus limon Nutrition 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 235000011187 glycerol Nutrition 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 244000248349 Citrus limon Species 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 230000003749 cleanliness Effects 0.000 description 2
- 238000009775 high-speed stirring Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000090 biomarker Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- PJUIMOJAAPLTRJ-UHFFFAOYSA-N monothioglycerol Chemical compound OCC(O)CS PJUIMOJAAPLTRJ-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004153 renaturation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0352—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their shape or by the shapes, relative sizes or disposition of the semiconductor regions
- H01L31/035209—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their shape or by the shapes, relative sizes or disposition of the semiconductor regions comprising a quantum structures
- H01L31/035218—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their shape or by the shapes, relative sizes or disposition of the semiconductor regions comprising a quantum structures the quantum structure being quantum dots
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
- H01L31/0324—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312 comprising only AIVBVI or AIIBIVCVI chalcogenide compounds, e.g. Pb Sn Te
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- 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
-
- C—CHEMISTRY; METALLURGY
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Electromagnetism (AREA)
- Inorganic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a kind of preparation method of vulcanized lead quantum dot.Prepared using water bath heating with good monodispersity, the vulcanized lead quantum dot that size is about 3 ~ 5 nm.Vulcanized lead quanta point material can reduce the energy loss of transmitted light and long wavelength's incident light, improve utilization ratio of the solar cell in the range of whole solar spectrum, further improve the photoelectric transformation efficiency of solar cell.The method is simple, it is easy to operate, and cost is low, can large-area manufacturing production.
Description
Technical field
The present invention relates to technical field of solar batteries, more particularly to a kind of preparation method of vulcanized lead quantum dot.
Background technology
At present, reduce increasingly in fossil fuel, greenhouse effects are constantly in the case of aggravation, solar energy makes as the mankind
With the important component of the energy.Solar energy is due to cleanliness without any pollution, rich reserves.Solar energy is the renewable of cleanliness without any pollution
The energy, and rich reserves and without geographical restrictions, be used to substituting will be exhausted fossil energy, and China facing can be solved
Low-carbon economy impact.In all kinds of new solar cells, quantum dot is combined in solar-electricity with up-conversion luminescent material
Pond field is with simple, the of a relatively high photoelectric transformation efficiency of low cost, manufacture craft as study hotspot.
Quantum dot (QDs), can be described as nanocrystalline, to be typically made up of II-VI races or group IV-VI element nanometer again
Grain, particle diameter is typically in the range of between 1 ~ 10 nm.When the size of quantum dot is less than its effective Bohr radius, quantum limitation effect
(quantum confinement effect) is fairly obvious, shows the thing of the change with size itself of uniqueness
Physicochemical performance, photoelectric properties and magnetic performance.The main application fields of quanta point material be solar cell, biomarker and
Biology sensor etc..The efficiency in the range of whole solar spectrum for example can be improved using sizes quanta point material, is reduced
Through and short wavelength range in energy loss, it means that the photoelectric transformation efficiency of solar cell can be obtained significantly
Improve.In addition, quantum dot as FRET (Fluorescence resonant energy transfer,
FRET donor) or donor, be combined with up-conversion luminescent material has in terms of biomedicine, sensor, solar cell
Very big application potential.
As the important compound in group IV-VI semiconductor, vulcanized lead is due to less band gap (0.41 eV, 300
K) and larger exciton radii (18 nm), the PbS of nanoscale can band from near-infrared blue shift to visible region, show solely
Special optical property and electrical properties.Traditionally using organometallic route method synthesis PbS nano materials, the method, which is often used, to be had
Toxic starting materials, and need the reaction conditions such as high temperature and higher boiling.At present, some researchers have reported that being synthesized using wet chemical method
The PbS nano materials of different-shape, PbS amounts are synthesized such as nanometer rods, nanometer sheet, tree, but using wet chemical method
Son point is but rarely reported.Bakueva research groups report using surfactant monothio glycerine (TGL) and two sulphur first
The PbS quantum that size uniform, diameter are about the nm of 4 nm ± 1 are prepared in aqueous for the mixture of glycerine (DTG)
Point.The success synthesizing water-solubility under room temperature and aqueous conditions using surfactant dihydrolipoic acid (DHLA) such as Deng
PbS quantum.Although by using surfactant monothio glycerine (TGL) and two thio glycerine or dihydrolipoic acid
(DHLA) PbS quantum can be prepared under aqueous conditions, but such stabilizer is expensive, and also it is toxic, it is uncomfortable
Close large-scale production.Therefore, in the urgent need to finding a kind of cheap preparation method for preparing PbS quantum.
The content of the invention
It is an object of the invention to for the deficiency in prior art, there is provided a kind of preparation method of vulcanized lead quantum dot.
A kind of preparation method of vulcanized lead quantum dot, comprises the following steps：
A. auxiliary agent is prepared according to the amount of material：20 ~ 30 parts of cetyl trimethylammonium bromide, lauryl sodium sulfate
20 ~ 30 parts, 40 ~ 60 parts of sodium citrate；
B. above-mentioned mixed aid is added bath temperature in 50 DEG C ~ 70 DEG C deionized waters, to continue high-speed stirred 3 ~ 5
Min is allowed to be completely dissolved, and is configured to mixed solution；
C. addend drips dilute nitric acid solution in above-mentioned mixed solution, and then pH value regulation to 3 ~ 5 adds into the solution
Enter sodium citrate, the amount of sodium citrate material is 2 ~ 4 times of lead acetate, and solution continues the min of high-speed stirred 1 ~ 2, until being changed into shallow
Yellow solution；
D. continue to be slowly added to sodium citrate, the amount of sodium citrate material is 2 ~ 4 times of thiocarbamide, and solution continues high-speed stirring
3 ~ 5 min are mixed, solution colour is slowly changed into sepia from orange-yellow；
E. by above-mentioned gained mixed solution, after room temperature cooling, by centrifugal treating, successively with deionized water, absolute ethyl alcohol
It is each to clean three times, obtained vulcanized lead is stored in absolute ethyl alcohol.
The amount of the material of described sodium citrate is cetyl trimethylammonium bromide, both lauryl sodium sulfate material
Amount sum.
Described acetic acid lead solution and the amount of thiourea solution contained substance are equal.
The diameter dimension of the described vulcanized lead quantum dot prepared is 3 ~ 5 nm.
Described auxiliary agent is with the gauge of material：25 parts of cetyl trimethylammonium bromide, 25 parts of lauryl sodium sulfate, lemon
Lemon 50 parts of sodium of acid；
Described acetic acid lead solution and the amount of thiourea solution contained substance are all 2.5 times of the amount of sodium citrate material.
Described preparation process adds time that time from thiourea solution and counted, and time control exists after reactant has been added
3 ~ 5 minutes.Reaction time will strictly control, and overlong time can not prepare quantum dot then.
Above-mentioned mixed aid is added into bath temperature in 60 DEG C of deionized waters in the step b.
Beneficial effects of the present invention：
Reaction temperature is relatively low, and reaction condition is gentle；Without using high boiling solvent；Preparation method safety non-toxic, experiment weight
Renaturation is good；Gained vulcanized lead quantum dot has good monodispersity.
Brief description of the drawings
Below in conjunction with drawings and Examples, the invention will be further described, in accompanying drawing：
Fig. 1 is prepared PbS quantum transmission electron microscope picture；
Fig. 2 is prepared PbS quantum XRD spectrums.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only to explain the present invention, not
For limiting the present invention.
A kind of preparation method of vulcanized lead quantum dot, comprises the following steps：
A. auxiliary agent is prepared according to the amount of material：20 ~ 30 parts of cetyl trimethylammonium bromide, lauryl sodium sulfate 20
~ 30 parts, 40 ~ 60 parts of sodium citrate；
B. it is 50 DEG C ~ 70 DEG C water above-mentioned mixed aid to be added into temperature, continues the min of high-speed stirred 3 ~ 5 and is allowed to completely molten
Solution, is configured to mixed solution；
C. addend drips dilute nitric acid solution in above-mentioned mixed solution, and then pH value regulation to 3 ~ 5 adds into the solution
Enter sodium citrate, the amount of sodium citrate material is 2 ~ 4 times of lead acetate, and solution continues the min of high-speed stirred 1 ~ 2, until being changed into shallow
Yellow solution；
D. continue to be slowly added to sodium citrate, the amount of sodium citrate material is 2 ~ 4 times of thiocarbamide, and solution continues high-speed stirring
3 ~ 5 min are mixed, solution colour is slowly changed into sepia from orange-yellow；
E. by above-mentioned gained mixed solution, after room temperature cooling, by centrifugal treating, successively with deionized water, absolute ethyl alcohol
It is each to clean three times, obtained vulcanized lead is stored in absolute ethyl alcohol.
The amount of the material of described sodium citrate is cetyl trimethylammonium bromide, both lauryl sodium sulfate material
Amount sum.
The amount of the acetic acid lead solution and thiourea solution contained substance is equal.
The diameter dimension for the vulcanized lead quantum dot prepared is 3 ~ 5 nm.
The auxiliary agent is with the gauge of material：25 parts of cetyl trimethylammonium bromide, 25 parts of lauryl sodium sulfate, lemon
Sour 50 parts of sodium；
The amount of the acetic acid lead solution and thiourea solution contained substance is all 2.5 times of the amount of sodium citrate material.
Described preparation process adds time that time from thiourea solution and counted, and time control exists after reactant has been added
3 ~ 5 minutes.Reaction time will strictly control, and overlong time can not prepare quantum dot then.
Above-mentioned mixed aid is added into bath temperature in 60 DEG C of deionized waters in the step b.
Embodiment 1
1）The mg of cetyl trimethylammonium bromide 18.2 (0.05 mmol), lauryl sodium sulfate 14.4 are weighed respectively
Mg (0.05 mmol), the mg of sodium citrate 29.4 (0.1 mmol), are added in the beaker that 50 mL water temperatures are 60 DEG C, continue
The min of high-speed stirred 3 ~ 5 is allowed to be completely dissolved；
2）Addend drips dilute nitric acid solution in above-mentioned mixed solution, and adjusts pH value to 4 with pH meter, then adds 5 mL
0.05 mol/L acetic acid lead solution simultaneously continues high-speed stirred 2min, and now solution is changed into light yellow；
3）10 mL concentration are slowly added to for 0.025 mol/L thiourea solution and continue the min of high-speed stirred 4, solution face
Color is slowly changed into sepia from orange-yellow.
4）By above-mentioned gained mixed solution, after room temperature cooling, by centrifugal treating, successively with deionized water, absolute ethyl alcohol
It is each to clean three times, obtained vulcanized lead is stored in absolute ethyl alcohol.
Embodiment 2
1）Cetyl trimethylammonium bromide 36.4mg (0.1 mmol), lauryl sodium sulfate 28.8mg are weighed respectively
(0.1 mmol), the mg of sodium citrate 58.8 (0.2 mmol), is added in the beaker that 100 mL water temperatures are 70 DEG C, continues at a high speed
3 ~ 5 min of stirring are allowed to be completely dissolved；
2）Addend drips dilute nitric acid solution in above-mentioned mixed solution, and adjusts pH value to 5 with pH meter, then adds 40ml
0.05 mol/L thiourea solutions simultaneously continue the min of high-speed stirred 2；
3）80 mL concentration are slowly added to for 0.025 mol/L acetic acid lead solution and continue high-speed stirred 3min, solution
Color is slowly changed into sepia from light yellow, orange-yellow, it means that the generation of PbS quantum；
4）By above-mentioned gained mixed solution, after room temperature cooling, by centrifugal treating, successively with deionized water, absolute ethyl alcohol
It is each to clean three times, obtained vulcanized lead is stored in absolute ethyl alcohol.
Embodiment 3
1）The mg of cetyl trimethylammonium bromide 29.12 (0.08 mmol), lauryl sodium sulfate are weighed respectively
34.56 mg (0.12 mmol), the mg of sodium citrate 58.8 (0.2 mmol), are added to the beaker that 300mL water temperatures are 70 DEG C
In, continue the min of high-speed stirred 3 ~ 5 and be allowed to be completely dissolved；
2）Addend drips dilute nitric acid solution in above-mentioned mixed solution, and adjusts pH value to 5 with pH meter, then adds 80 ml
0.05 mol/L thiourea solutions simultaneously continue the min of high-speed stirred 2；
3）160 mL concentration are slowly added to for 0.025 mol/L acetic acid lead solution and continue high-speed stirred 3min, solution
Color is slowly changed into sepia from light yellow, orange-yellow, it means that the generation of PbS quantum；
4）By above-mentioned gained mixed solution, after room temperature cooling, by centrifugal treating, successively with deionized water, absolute ethyl alcohol
It is each to clean three times, obtained vulcanized lead is stored in absolute ethyl alcohol.
It should be appreciated that for those of ordinary skills, can according to the above description be improved or converted,
And all these modifications and variations should all belong to the protection domain of appended claims of the present invention.
Claims (7)
1. a kind of preparation method of vulcanized lead quantum dot, it is characterised in that comprise the following steps：
A, the amount preparation auxiliary agent according to material：20~30 parts of cetyl trimethylammonium bromide, lauryl sodium sulfate 20~30
Part, 40~60 parts of sodium citrate；
B, above-mentioned mixed aid added during bath temperature is 50 DEG C~70 DEG C deionized waters, continuing 3~5min of high-speed stirred makes
Be completely dissolved, be configured to mixed solution；
C, addend drip dilute nitric acid solution in above-mentioned mixed solution, by pH value regulation to 3~5, then add second into the solution
Lead plumbate solution, the amount of sodium citrate material is 2~4 times of lead acetate, and solution continues 1~2min of high-speed stirred, until being changed into shallow
Yellow solution；
D, continue to be slowly added to thiourea solution, the amount of sodium citrate material is 2~4 times of thiocarbamide, solution continue high-speed stirred 3~
5min, solution colour is slowly changed into sepia from orange-yellow；
E, by above-mentioned gained mixed solution, it is each clear with deionized water, absolute ethyl alcohol successively by centrifugal treating after room temperature cooling
Wash three times, obtained vulcanized lead is stored in absolute ethyl alcohol.
2. the preparation method of vulcanized lead quantum dot according to claim 1, it is characterised in that the material of the sodium citrate
Amount be cetyl trimethylammonium bromide, the amount sum of both lauryl sodium sulfate material.
3. the preparation method of vulcanized lead quantum dot according to claim 1, it is characterised in that the acetic acid lead solution and sulphur
The amount of urea solution contained substance is equal.
4. the preparation method of vulcanized lead quantum dot according to claim 1, it is characterised in that the vulcanized lead quantum prepared
The diameter dimension of point is 3~5nm.
5. the preparation method of vulcanized lead quantum dot according to claim 1, it is characterised in that the auxiliary agent is with the amount of material
Meter：25 parts of cetyl trimethylammonium bromide, 25 parts of lauryl sodium sulfate, 50 parts of sodium citrate.
6. the preparation method of vulcanized lead quantum dot according to claim 1, it is characterised in that add that from thiourea solution
Time at quarter is counted, and time control was at 3~5 minutes after reactant has been added.
7. the preparation method of vulcanized lead quantum dot according to claim 1, it is characterised in that will be above-mentioned in the step b
Mixed aid adds bath temperature in 60 DEG C of deionized waters.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610465936.0A CN106129142B (en) | 2016-06-24 | 2016-06-24 | A kind of preparation method of vulcanized lead quantum dot |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610465936.0A CN106129142B (en) | 2016-06-24 | 2016-06-24 | A kind of preparation method of vulcanized lead quantum dot |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106129142A CN106129142A (en) | 2016-11-16 |
| CN106129142B true CN106129142B (en) | 2017-10-24 |
Family
ID=57269062
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610465936.0A Expired - Fee Related CN106129142B (en) | 2016-06-24 | 2016-06-24 | A kind of preparation method of vulcanized lead quantum dot |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106129142B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106882837B (en) * | 2017-03-01 | 2018-09-21 | 华中科技大学 | A method of control PbS or PbSe quantum dot sizes distribution |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070134902A1 (en) * | 2005-12-12 | 2007-06-14 | The Curators Of The University Of Missouri | Patterning of Substrates with Metal-Containing Particles |
| CN101117237A (en) * | 2007-07-17 | 2008-02-06 | 浙江大学 | Method for preparing hexagon star-shaped plumbous sulfide nanocrystalline |
| CN104297306B (en) * | 2014-09-30 | 2016-11-30 | 江南大学 | Optical Electro-Chemistry Multifunction Sensor based on G-tetrahedron/hemin |
| CN105304338B (en) * | 2015-09-21 | 2019-01-08 | 河南师范大学 | It is a kind of for quantum dot sensitized solar battery to electrode and preparation method thereof |
-
2016
- 2016-06-24 CN CN201610465936.0A patent/CN106129142B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN106129142A (en) | 2016-11-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Liang et al. | Recent progress and development in inorganic halide perovskite quantum dots for photoelectrochemical applications | |
| CN107349938B (en) | A kind of nickel sulfide-cadmium sulfide nano wires heterojunction structure and preparation method thereof | |
| US9972731B2 (en) | Precursor for preparing light absorption layer of solar cells and method of preparing the same | |
| CN108690600A (en) | High pressure prepares the method and quantum dot of quantum dot | |
| Sadhu et al. | Recent advances in colloidal quantum dots or perovskite quantum dots as a luminescent downshifting layer embedded on solar cells | |
| Wang et al. | Rapid synthesis of hollow CTS nanoparticles using microwave irradiation | |
| CN105562034A (en) | CdS/BiVO4 compound semiconductor photocatalyst and preparation and application thereof | |
| CN106430284A (en) | Preparation method of sulfur-doped zinc oxide nano material | |
| CN104810159B (en) | Preparation method for tin-doped indium phosphide quantum dot sensitized solar cell | |
| Shen et al. | Stability strategies of perovskite quantum dots and their extended applications in extreme environment: A review | |
| Dai et al. | Tuning solar absorption spectra via carbon quantum dots/VAE composite layer and efficiency enhancement for crystalline Si solar module | |
| CN106129142B (en) | A kind of preparation method of vulcanized lead quantum dot | |
| CN103833080B (en) | A kind of preparation method of molybdic acid cadmium porous ball | |
| CN113643902B (en) | Copper indium selenium tellurium/cadmium sulfide core-shell structure quantum dot and preparation method thereof, and preparation method of photo-anode | |
| CN105419803B (en) | The preparation method of tellurium mercury cadmium quantum dot and carbon nanotube composite materials | |
| CN106848064A (en) | High stability perovskite solar cell and preparation method based on titanium dioxide indium sulphur quantum dot core shell structure | |
| CN103413892B (en) | A kind of alloy quantum dot PbSxse1-xand preparation method thereof and application in solar cells | |
| CN105080573B (en) | One kind prepares SnS using microwave-hydrothermal method2/SnO2The method of nano-photo catalytic composite | |
| CN109935662A (en) | Electron transport material and preparation method thereof, light emitting diode | |
| Zhao et al. | Three-dimensional ZnO/ZnxCd1− xS/CdS nanostructures modified by microwave hydrothermal reaction-deposited CdSe quantum dots for chemical solar cells | |
| CN110311043B (en) | Sb-tin dioxide nano precursor and method for preparing perovskite solar cell by using Sb-tin dioxide nano precursor as electron transport layer | |
| CN102500758A (en) | Core shell nanometer crystal of gold and copper-indium-diselenide and preparation method of core shell nanometer crystal | |
| CN109988370B (en) | Light wave conversion material, preparation method thereof and solar cell | |
| CN114653382B (en) | P-n type stannous sulfide-zinc stannate semiconductor material and preparation method and application thereof | |
| CN106542577B (en) | A kind of nanometer antimony trisulfide particle preparation method under controlled condition |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20171024 Termination date: 20190624 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |