CN106129142A - 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
- CN106129142A CN106129142A CN201610465936.0A CN201610465936A CN106129142A CN 106129142 A CN106129142 A CN 106129142A CN 201610465936 A CN201610465936 A CN 201610465936A CN 106129142 A CN106129142 A CN 106129142A
- 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.)
- Granted
Links
- 239000002096 quantum dot Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims description 45
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 26
- 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
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 17
- 239000011259 mixed solution Substances 0.000 claims description 15
- 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
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 12
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 12
- 229940046892 lead acetate Drugs 0.000 claims description 12
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 12
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 8
- 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
- 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 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000003643 water by type Substances 0.000 claims description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 239000011593 sulfur Substances 0.000 claims description 3
- 229910052717 sulfur Inorganic materials 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims 2
- 239000007788 liquid Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 5
- 238000001228 spectrum Methods 0.000 abstract description 3
- 230000009466 transformation Effects 0.000 abstract description 3
- 230000005540 biological transmission Effects 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000005286 illumination Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 235000005979 Citrus limon Nutrition 0.000 description 6
- 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
- 244000248349 Citrus limon Species 0.000 description 4
- PJUIMOJAAPLTRJ-UHFFFAOYSA-N monothioglycerol Chemical compound OCC(O)CS PJUIMOJAAPLTRJ-UHFFFAOYSA-N 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 230000033228 biological regulation Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002866 fluorescence resonance energy transfer Methods 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 244000131522 Citrus pyriformis Species 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 230000003749 cleanliness Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000000090 biomarker Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- WQABCVAJNWAXTE-UHFFFAOYSA-N dimercaprol Chemical compound OCC(S)CS WQABCVAJNWAXTE-UHFFFAOYSA-N 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 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
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 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
- 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)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Electromagnetism (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Composite Materials (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses the preparation method of a kind of vulcanized lead quantum dot.Using water bath heating to prepare and have good monodispersity, size is about the vulcanized lead quantum dot of 3 ~ 5 nm.Vulcanized lead quanta point material can reduce transmission light and the energy loss of long wavelength's incident illumination, improves solar cell utilization ratio in the range of whole solar spectrum, improves the photoelectric transformation efficiency of solaode further.The method is simple, it is easy to operation, low cost, can large-area manufacturing produce.
Description
Technical field
The present invention relates to technical field of solar batteries, particularly relate to the preparation method of a kind of vulcanized lead quantum dot.
Background technology
At present, increasingly reducing at Fossil fuel, in the case of greenhouse effect constantly aggravates, solar energy has become the mankind to be made
By the important component part 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 for substituting will be exhausted fossil energy, and China facing can be solved
The impact of low-carbon economy.In all kinds of novel solar cells, quantum dot combines in solar-electricity with up-conversion luminescent material
Field, pond becomes study hotspot with simple, the of a relatively high photoelectric transformation efficiency of low cost, processing technology.
Quantum dot (QDs), can be described as again nanocrystalline, typically by the nanometer that II VI race or group IV-VI are elementary composition
Grain, particle diameter is typically in the range of between 1 ~ 10 nm.When being smaller in size than its effective Bohr radius of quantum dot, quantum limitation effect
(quantum confinement effect) is fairly obvious, shows the thing of this change along with size own of uniqueness
Physicochemical performance, photoelectric properties and magnetic performance.The main application fields of quanta point material be solaode, biomarker and
Biosensor etc..Such as efficiency in the range of application sizes quanta point material can improve whole solar spectrum, decreases
Through and short wavelength range in energy loss, it means that the photoelectric transformation efficiency of solaode can obtain significantly
Improve.Additionally, quantum dot as FRET (fluorescence resonance energy transfer) (Fluorescence resonant energy transfer,
FRET) donor or donor, combine with up-conversion luminescent material and have at aspects such as biomedicine, sensor, solaodes
The biggest application potential.
As the important compound in group IV-VI quasiconductor, vulcanized lead due to less band gap (0.41 eV, 300
And bigger exciton radii (18 nm) K), the PbS of nanoscale can band from near-infrared blue shift to visible region, present solely
Special optical property and electrical properties.Using organometallic route method synthesis PbS nano material traditionally, the method has often used
Toxic starting materials, and need the reaction condition such as high temperature and high boiling point.At present, some researchers have reported that employing wet chemical method synthesis
The PbS nano material of different-shape, such as nanometer rods, nanometer sheet, tree etc., but use wet chemical method synthesis PbS amount
Son point but rarely has report.Bakueva research group reported first employing surfactant monothio glycerol (TGL) and two sulfur
Prepare size uniform in aqueous for the mixture of glycerol (DTG), diameter is about the PbS quantum of 4 nm ± 1 nm
Point.Deng etc. use surfactant dihydrolipoic acid (DHLA) success synthesizing water-solubility under room temperature and aqueous conditions
PbS quantum.Although by using surfactant monothio glycerol (TGL) and dithio glycerol or dihydrolipoic acid
(DHLA) PbS quantum can be prepared under aqueous conditions, but this type of stabilizer is expensive, and toxic, uncomfortable
Close large-scale production.Therefore, in the urgent need to finding the preparation method of a kind of cheap preparation PbS quantum.
Summary of the invention
Present invention aims to the deficiency in prior art, it is provided that the preparation method of a kind of vulcanized lead quantum dot.
The preparation method of a kind of vulcanized lead quantum dot, comprises the steps:
A. auxiliary agent is prepared according to the amount of material: cetyl trimethylammonium bromide 20 ~ 30 parts, sodium lauryl sulphate 20 ~
30 parts, sodium citrate 40 ~ 60 parts；
B. above-mentioned mixed aid being added bath temperature is in 50 DEG C ~ 70 DEG C deionized waters, continues high-speed stirred 3 ~ 5 min and makes
Be completely dissolved, be configured to mixed solution；
C. add few drops dilute nitric acid solution in above-mentioned mixed solution, pH value is adjusted to 3 ~ 5, in this solution, then add lemon
Lemon acid sodium, the amount of sodium citrate material is 2 ~ 4 times of lead acetate, and solution continues high-speed stirred 1 ~ 2 min, until becoming light yellow
Solution；
D. continuing to be slowly added to sodium citrate, the amount of sodium citrate material is 2 ~ 4 times of thiourea, and solution continues high-speed stirred 3 ~ 5
Min, solution colour is slowly become sepia from orange-yellow；
E. by above-mentioned gained mixed solution, after room temperature cooling, through centrifugal treating, use deionized water, dehydrated alcohol each clearly successively
Wash three times, the vulcanized lead obtained is stored in dehydrated alcohol.
The amount of the material of described sodium citrate is cetyl trimethylammonium bromide, both sodium lauryl sulphates material
Amount sum.
Described lead acetate 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: cetyl trimethylammonium bromide 25 parts, sodium lauryl sulphate 25 parts, lemon
50 parts of lemon acid sodium；
Described lead acetate solution and the amount of thiourea solution contained substance are all the amount 2.5 times of sodium citrate material.
Described preparation process adds time that time from thiourea solution and counts, and after reactant has added, the time controls
3 ~ 5 minutes.Response time strictly to control, overlong time, then can not prepare quantum dot.
In described step b, above-mentioned mixed aid being added bath temperature is in 60 DEG C of deionized waters.
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, experimental repeatability
Good；Gained vulcanized lead quantum dot has good monodispersity.
Accompanying drawing explanation
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 figure spectrum.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, right
The present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, not
For limiting the present invention.
The preparation method of a kind of vulcanized lead quantum dot, comprises the steps:
A. according to the amount preparation auxiliary agent of material: cetyl trimethylammonium bromide 20 ~ 30 parts, sodium lauryl sulphate 20 ~ 30
Part, sodium citrate 40 ~ 60 parts；
B. above-mentioned mixed aid being added temperature is 50 DEG C ~ 70 DEG C water, continues high-speed stirred 3 ~ 5 min and is allowed to be completely dissolved, joins
It is set to mixed solution；
C. add few drops dilute nitric acid solution in above-mentioned mixed solution, pH value is adjusted to 3 ~ 5, in this solution, then add lemon
Lemon acid sodium, the amount of sodium citrate material is 2 ~ 4 times of lead acetate, and solution continues high-speed stirred 1 ~ 2 min, until becoming light yellow
Solution；
D. continuing to be slowly added to sodium citrate, the amount of sodium citrate material is 2 ~ 4 times of thiourea, and solution continues high-speed stirred 3 ~ 5
Min, solution colour is slowly become sepia from orange-yellow；
E. by above-mentioned gained mixed solution, after room temperature cooling, through centrifugal treating, use deionized water, dehydrated alcohol each clearly successively
Wash three times, the vulcanized lead obtained is stored in dehydrated alcohol.
The amount of the material of described sodium citrate is cetyl trimethylammonium bromide, both sodium lauryl sulphates material
Amount sum.
The amount of described lead acetate solution and thiourea solution contained substance is equal.
The diameter dimension of the vulcanized lead quantum dot prepared is 3 ~ 5 nm.
Described auxiliary agent is with the gauge of material: cetyl trimethylammonium bromide 25 parts, sodium lauryl sulphate 25 parts, Fructus Citri Limoniae
50 parts of sodium of acid；
The amount of described lead acetate solution and thiourea solution contained substance is all the amount 2.5 times of sodium citrate material.
Described preparation process adds time that time from thiourea solution and counts, and after reactant has added, the time controls
3 ~ 5 minutes.Response time strictly to control, overlong time, then can not prepare quantum dot.
In described step b, above-mentioned mixed aid being added bath temperature is in 60 DEG C of deionized waters.
Embodiment 1
1) cetyl trimethylammonium bromide 18.2 mg (0.05 mmol), sodium lauryl sulphate 14.4 mg are weighed respectively
(0.05 mmol), sodium citrate 29.4 mg (0.1 mmol), join in the beaker that 50 mL water temperatures are 60 DEG C, continues height
Speed stirring 3 ~ 5 min are allowed to be completely dissolved；
2) add few drops dilute nitric acid solution in above-mentioned mixed solution, and with pH meter regulation pH value to 4, be subsequently adding 5 mL 0.05
Mol/L lead acetate solution persistently high-speed stirred 2min, now solution becomes light yellow；
3) be slowly added to thiourea solution that 10 mL concentration are 0.025 mol/L lasting high-speed stirred 4 min, solution colour by
Orange-yellow slowly become sepia.
4) by above-mentioned gained mixed solution, after room temperature cooling, through centrifugal treating, successively with deionized water, dehydrated alcohol
Each cleaning three times, is stored in dehydrated alcohol by the vulcanized lead obtained.
Embodiment 2
1) cetyl trimethylammonium bromide 36.4mg (0.1 mmol), sodium lauryl sulphate 28.8mg are weighed respectively
(0.1 mmol), sodium citrate 58.8 mg (0.2 mmol), join in the beaker that 100 mL water temperatures are 70 DEG C, continues at a high speed
Stirring 3 ~ 5 min are allowed to be completely dissolved；
2) add few drops dilute nitric acid solution in above-mentioned mixed solution, and with pH meter regulation pH value to 5, be subsequently adding 40ml 0.05
Mol/L thiourea solution persistently high-speed stirred 2 min；
3) lead acetate solution that 80 mL concentration are 0.025 mol/L persistently high-speed stirred 3min, solution colour it are slowly added to
Sepia is slowly become, it means that the generation of PbS quantum from light yellow, orange-yellow；
4) by above-mentioned gained mixed solution, after room temperature cooling, through centrifugal treating, use deionized water, dehydrated alcohol each clearly successively
Wash three times, the vulcanized lead obtained is stored in dehydrated alcohol.
Embodiment 3
1) cetyl trimethylammonium bromide 29.12 mg (0.08 mmol), sodium lauryl sulphate 34.56 are weighed respectively
Mg (0.12 mmol), sodium citrate 58.8 mg (0.2 mmol), join in the beaker that 300mL water temperature is 70 DEG C, continues
High-speed stirred 3 ~ 5 min is allowed to be completely dissolved；
2) add few drops dilute nitric acid solution in above-mentioned mixed solution, and with pH meter regulation pH value to 5, be subsequently adding 80 ml 0.05
Mol/L thiourea solution persistently high-speed stirred 2 min；
3) lead acetate solution that 160 mL concentration are 0.025 mol/L persistently high-speed stirred 3min, solution colour it are slowly added to
Sepia is slowly become, it means that the generation of PbS quantum from light yellow, orange-yellow；
4) by above-mentioned gained mixed solution, after room temperature cooling, through centrifugal treating, use deionized water, dehydrated alcohol each clearly successively
Wash three times, the vulcanized lead obtained is stored in dehydrated alcohol.
It should be appreciated that for those of ordinary skills, can be improved according to the above description or be converted,
And all these modifications and variations all should belong to the protection domain of claims of the present invention.
Claims (8)
1. the preparation method of a vulcanized lead quantum dot, it is characterised in that comprise the steps:
A, according to material amount prepare auxiliary agent: cetyl trimethylammonium bromide 20 ~ 30 parts, sodium lauryl sulphate 20 ~ 30
Part, sodium citrate 40 ~ 60 parts；
B, by above-mentioned mixed aid addition bath temperature be in 50 DEG C ~ 70 DEG C deionized waters, continue high-speed stirred 3 ~ 5 min be allowed to
It is completely dissolved, is configured to mixed solution；
C, add few drops dilute nitric acid solution in above-mentioned mixed solution, pH value is adjusted to 3 ~ 5, in this solution, then adds Fructus Citri Limoniae
Acid sodium, the amount of sodium citrate material is 2 ~ 4 times of lead acetate, and solution continues high-speed stirred 1 ~ 2 min, until becoming light yellow molten
Liquid；
D, continuing to be slowly added to sodium citrate, the amount of sodium citrate material is 2 ~ 4 times of thiourea, and solution continues high-speed stirred 3 ~ 5
Min, solution colour is slowly become sepia from orange-yellow；
E, by above-mentioned gained mixed solution, after room temperature cooling, through centrifugal treating, each clearly with deionized water, dehydrated alcohol successively
Wash three times, the vulcanized lead obtained is stored in dehydrated alcohol.
The preparation method of vulcanized lead quantum dot the most according to claim 1, it is characterised in that the material of described sodium citrate
The amount sum that amount is cetyl trimethylammonium bromide, both sodium lauryl sulphates material.
The preparation method of vulcanized lead quantum dot the most according to claim 1, it is characterised in that described lead acetate solution and sulfur
The amount of urea solution contained substance is equal.
The preparation method of vulcanized lead quantum dot the most according to claim 1, it is characterised in that the vulcanized lead quantum prepared
The diameter dimension of point is 3 ~ 5 nm.
The preparation method of vulcanized lead quantum dot the most according to claim 1, it is characterised in that described auxiliary agent is with the amount of material
Meter: cetyl trimethylammonium bromide 25 parts, sodium lauryl sulphate 25 parts, sodium citrate 50 parts.
The preparation method of vulcanized lead quantum dot the most according to claim 1, it is characterised in that described lead acetate solution and sulfur
The amount of urea solution contained substance is all the amount 2.5 times of sodium citrate material.
The preparation method of vulcanized lead quantum dot the most according to claim 1, it is characterised in that add that from thiourea solution
Time at quarter is counted, and after reactant has added, the time controlled at 3 ~ 5 minutes.
The preparation method of vulcanized lead quantum dot the most according to claim 1, it is characterised in that by above-mentioned in described step b
It is in 60 DEG C of deionized waters that mixed aid adds bath temperature.
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 true CN106129142A (en) | 2016-11-16 |
| CN106129142B 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) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106882837A (en) * | 2017-03-01 | 2017-06-23 | 华中科技大学 | A kind of method of control PbS or PbSe quantum dot sizes distribution |
Citations (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 |
| CN104297306A (en) * | 2014-09-30 | 2015-01-21 | 江南大学 | Multifunctional photoelectrochemical sensor based on G-tetrahedron/hemin |
| CN105304338A (en) * | 2015-09-21 | 2016-02-03 | 河南师范大学 | Counter electrode for quantum-dot sensitized solar cell and manufacturing method thereof |
-
2016
- 2016-06-24 CN CN201610465936.0A patent/CN106129142B/en not_active Expired - Fee Related
Patent Citations (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 |
| CN104297306A (en) * | 2014-09-30 | 2015-01-21 | 江南大学 | Multifunctional photoelectrochemical sensor based on G-tetrahedron/hemin |
| CN105304338A (en) * | 2015-09-21 | 2016-02-03 | 河南师范大学 | Counter electrode for quantum-dot sensitized solar cell and manufacturing method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106882837A (en) * | 2017-03-01 | 2017-06-23 | 华中科技大学 | A kind of method of control PbS or PbSe quantum dot sizes distribution |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106129142B (en) | 2017-10-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhou et al. | Application of perovskite nanocrystals (NCs)/quantum dots (QDs) in solar cells | |
| Ramasamy et al. | Upconversion nanophosphors for solar cell applications | |
| CN105810442A (en) | Fabrication method of g-C3N4 reinforced solar cell | |
| Zhong et al. | Encapsulation of lead halide perovskite nanocrystals (NCs) at the single-particle level: strategies and properties | |
| Shen et al. | Stability strategies of perovskite quantum dots and their extended applications in extreme environment: A review | |
| CN106430284A (en) | Preparation method of sulfur-doped zinc oxide nano material | |
| CN105670018A (en) | SPEEK/MIL101 loaded phosphotungstic acid hybrid membrane, preparation and application | |
| CN103833080B (en) | A kind of preparation method of molybdic acid cadmium porous ball | |
| CN106807411A (en) | A kind of preparation method of ferrous acid La doped silver bromide compound photocatalyst | |
| Zhang et al. | Deep-red emissive colloidal lead-based triiodide perovskite/telluride nanoscale heterostructures with reduced surface defects and enhanced stability for indoor lighting applications | |
| CN104556232A (en) | Preparation method and application of nano tungsten oxide water solution | |
| CN106848064A (en) | High stability perovskite solar cell and preparation method based on titanium dioxide indium sulphur quantum dot core shell structure | |
| CN105419803B (en) | The preparation method of tellurium mercury cadmium quantum dot and carbon nanotube composite materials | |
| CN106129142B (en) | A kind of preparation method of vulcanized lead quantum dot | |
| Zhao et al. | Three-dimensional ZnO/ZnxCd1− xS/CdS nanostructures modified by microwave hydrothermal reaction-deposited CdSe quantum dots for chemical solar cells | |
| CN105080573B (en) | One kind prepares SnS using microwave-hydrothermal method2/SnO2The method of nano-photo catalytic composite | |
| Wang et al. | Perovskite nanogels: synthesis, properties, and applications | |
| CN108996478B (en) | MN (Mobile node)xSuper crystal and preparation method and application thereof | |
| CN103730536B (en) | The preparation of a kind of rare-earth sulfide quantum dot solar cell and application thereof | |
| CN105536828A (en) | Silver-silver phosphate-zinc oxide ternary heterogeneous composite structure and preparation method thereof | |
| CN106542577B (en) | A kind of nanometer antimony trisulfide particle preparation method under controlled condition | |
| CN106745247B (en) | A kind of vanadic acid silver nanotube assembles ball cluster | |
| CN108793099A (en) | A kind of radial selenium nanotube and preparation method thereof | |
| CN102795658B (en) | Method for regulating zinc oxide crystal microstructure by using hydrogen peroxide | |
| CN104671285B (en) | A kind of preparation method of cadmium molybdate nano rod |
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 |