CN106753357A - A kind of preparation method of PbS quantum - Google Patents
A kind of preparation method of PbS quantum Download PDFInfo
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- CN106753357A CN106753357A CN201611050553.3A CN201611050553A CN106753357A CN 106753357 A CN106753357 A CN 106753357A CN 201611050553 A CN201611050553 A CN 201611050553A CN 106753357 A CN106753357 A CN 106753357A
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Abstract
The invention discloses a kind of preparation method of PbS quantum, comprise the following steps：(1) halogen compound of lead and oleyl amine are mixed to form mixture；Then, under an inert atmosphere, the mixture is heated to 80 DEG C~150 DEG C, and is incubated the oleyl amine solution of the halide for obtaining lead；(2) by ZnS nanometer rods solution well prepared in advance in the oleyl amine solution for being injected into the halide of lead, reacted at a temperature of 80 DEG C~190 DEG C, that is, obtained including the product including PbS quantum.The present invention is improved by reaction condition to crucial preparation method principle and each step reaction etc., PbS quantum preparation method complexity, the problem of high cost are can effectively solve the problem that compared with prior art, and the features such as nano particle that the present invention is prepared has highly crystalline, dimensional homogeneity, stability, good optical characteristics, is especially advantageous for playing the various characteristics of PbS quantum.
Description
Technical field
The invention belongs to compound semiconductor technical field of nanometer material preparation, more particularly, to a kind of PbS quantum
Preparation method, i.e. the preparation method of vulcanized lead quantum dot.
Background technology
Semiconductor-quantum-point is a kind of nano material of quasi-zero dimension, when particle size enters nanometer scale, size confinement
Dimensional effect, quantum confined effect, macro quanta tunnel effect and skin effect will be caused, it is different so as to derive nanometer system
In meta system and the low-dimensional physical property of microsystem, many physicochemical properties different from macroscopic body material are shown.
PbS quantum, as IV-VI race's semi-conducting material, is also important pi-pi bond semi-conducting material.It has narrower
Direct band gap.Compared with other semiconductor-quantum-points, its exciton radii is 18nm, it is readily available very strong quantum confinement
Effect.Because the fluorescence that quantum dot is produced can cover whole transmission window, therefore it has widely in terms of optics
Application prospect.Such as Infrared Detectors, solar collector, optical switch etc..Importantly, multiple exciton effect exists
Observed on quantum dot, this discovery causes that quantum dot is expected to turn into efficient photoelectric conversion device.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, it is an object of the invention to a kind of preparation of PbS quantum
Method, wherein be improved by reaction condition to crucial preparation method principle and each step reaction etc., with prior art
Compared to can effectively solve the problem that PbS quantum preparation method is complicated, high cost problem, and the nanometer that the present invention is prepared
The features such as grain has highly crystalline, dimensional homogeneity, stability, good optical characteristics, is especially advantageous for playing PbS quantum
Various characteristics.
To achieve the above object, according to the invention provides a kind of preparation method of PbS quantum, it is characterised in that bag
Include following steps：
(1) halogen compound of lead and oleyl amine are mixed to form mixture, the halogen compound of the lead is in the mixture
In concentration be 0.1mol/L~0.4mol/L；Then, under an inert atmosphere, the mixture is heated to 80 DEG C~150 DEG C, and
Insulation, obtains the oleyl amine solution of the halide of lead；
(2) ZnS nanometer rods solution well prepared in advance is being injected into the halide of the lead that the step (1) is obtained
Oleyl amine solution in, reacted at a temperature of 80 DEG C~190 DEG C, the reaction time control in 10s~25min, that is, wrapped
PbS quantum is included in interior product.
Used as present invention further optimization, the preparation method of the PbS quantum also includes step：
(3) product that the step (2) obtains is cooled down；70 DEG C are down at a temperature of the product
When, to injecting n-hexane in the product；When being down to 40 DEG C at a temperature of the product, to the product
Middle injection oleic acid；
(4) to cooling after the product carry out centrifugation, then, to added in the precipitation for obtaining just oneself
Alkane simultaneously carries out centrifugal filtration and obtains supernatant, is then to obtain PbS quantum to ethanol is added in the supernatant.
Used as present invention further optimization, in the step (1), the halogen compound of the lead is lead chloride, bromination
Any one in lead, lead iodide；Preferably, the soaking time of the insulation is 15min~60min.
As present invention further optimization, in the step (2), the material of S elements in the ZnS nanometer rods solution
The amount ratio between two for measuring the material of the halogen compound of lead described in the oleyl amine solution with the halide of the lead is at most 1：2；
The ZnS nanometer rods solution is injected into injection length used in the oleyl amine solution of the halide of the lead and is no more than 10s.
By the contemplated above technical scheme of the present invention, compared with prior art, using the method system of cation exchange
Standby vulcanized lead quantum dot, with ZnS nanometer rods as sulphur source, with halogen compound (e.g., the PbCl of lead2、PbBr2、PbI2Deng) and oleyl amine
Mixture be Pb sources, ZnS nanometer rods are converted to PbS quantum, preparation method low cost, it is simple to operate, will to environment
Ask not strict, the PbS quantum for preparing is single dispersing state and even size distribution, stabilization, the PbS quantum for preparing
Point is spherical, and diameter is about 4.3nm to 9nm.
The present invention by simple and economic mode can synthesis PbS quantum, it is various anti-in preparation method by controlling
Answer the concentration (e.g., concentration of halogen compound of lead etc. in the oleyl amine solution of the halide of lead) of raw material and the temperature of reaction
It is controlled with time, and PbS quantum its separation to preparing, the entirety using each step in preparation method is matched somebody with somebody
Close, it can be ensured that the PbS quantum that the present invention is prepared is stablized and good in having highly crystalline, dimensional homogeneity, air
The features such as optical characteristics got well.In the present invention, the concentration and scale topography of reaction raw materials ZnS nanometer rods are to preparing
PbS quantum influence is little, if in ZnS nanometer rods the amount of the material of S elements and both Pb elements in the halide of lead thing
The amount ratio between two of matter is at most 1：(that is, the ratio of both lead element and element sulphur is greater than equal to 2 by 2:1)；The present invention
It is middle that the injection length that ZnS nanometer rods solution is injected into the oleyl amine solution of the halide of lead is preferably controlled within 10s, injection
The PbS quantum size of time shorter generation is better；The temperature that both ZnS nanometer rods solution and halide of lead are reacted is
80 DEG C~190 DEG C, the reaction time be 10s~25min, reaction time of 10s~25min had both included the time of positive exchange reaction,
Also including the growth time of PbS quantum after the completion of cation exchange；80 DEG C~190 DEG C of reaction temperature is to preparing
PbS quantum has crucial effect, and reaction temperature can influence the speed of cation exchange, and can influence the growth of PbS quantum；
The present invention is controlled at 80 DEG C~190 DEG C by by reaction temperature, can effectively ensure that the PbS quantum that the present invention is prepared has
Highly crystalline, dimensional homogeneity.
Specifically, the preparation method of PbS quantum has following technique effect in the present invention：
(1) operating process is simple, and preparation process is not high to environmental requirement, and required equipment and the cost of raw material are low.
(2) various sizes of quantum dot can be prepared, the shapes and sizes of quantum dot can be well controlled.
(3) suitable for largely preparing quantum dot.
(4) the gained aerial stability of quantum dot is very good.
Brief description of the drawings
Fig. 1 is PbCl2As the absorption spectra of the PbS quantum in Pb sources.
Fig. 2 is PbCl2As the X-ray diffractogram of the PbS quantum in Pb sources.
Fig. 3 is PbCl2TEM as the PbS quantum in Pb sources schemes.
Fig. 4 is the stability collection of illustrative plates of PbS quantum.
Fig. 5 is PbBr2As the absorption spectra of the PbS quantum in Pb sources.
Fig. 6 is PbI2As the absorption spectra of the PbS quantum in Pb sources.
Fig. 7 is the schematic flow sheet of preparation method of the present invention.
Specific 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 the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as additionally, technical characteristic involved in invention described below each implementation method
Not constituting conflict each other can just be mutually combined.
The present invention is by the use of previously prepared ZnS nanometer rods as sulphur source, with lead halide (e.g., lead chloride etc.) and oleyl amine
Mixture prepares vulcanized lead quantum dot (as shown in Figure 7) using the method for cation exchange as lead source, specifically may include with
Lower step：
(1) halogen compound of lead is mixed with oleyl amine, the halogen compound of lead concentration in the mixture for 0.1~
0.4mol/L, under an inert atmosphere, heats the mixture to 80 DEG C~150 DEG C, keeps 15min~60min, obtains the halogenation of lead
The oleyl amine solution of thing；
(2) the ZnS nanometer rods solution that will have been prepared injects the oleyl amine solution of the halide of lead in 10s, 80 DEG C~
10s~25min (being preferably 15s~20min), ZnS nanometers are maintained at a temperature of 190 DEG C (being preferably 80 DEG C~150 DEG C)
The amount of the ZnS in rod solution causes that S and the halogen compound of lead meet stoichiometric proportion；
(3) n-hexane is injected when product temperature being down into 70 DEG C after the completion of reacting, oleic acid is injected when being down to 40 DEG C；
(4) centrifugation is carried out, precipitation is dissolved in n-hexane centrifugal filtration, add the solid that ethanol centrifugation obtains black
Powder is PbS quantum.
It is below specific embodiment：
Embodiment 1
The present embodiment is comprised the following steps：
(1) 0.417g lead chlorides are weighed in two mouthfuls of reaction bulbs, 5ml OLA are measured, mixture is vacuumized.
(2) 140 DEG C of maintenance 30min are heated the mixture to, mixture is then dropped to 120 DEG C, be rapidly injected 2ml ZnS
Nanometer rods solution, keeps 3min.
(3) reaction drops to room temperature after terminating, add ethanol centrifugation, is subsequently adding n-hexane centrifugation, filtering, adds ethanol
Centrifugation obtains PbS quantum.
The performance characterization of gained PbS quantum is：
PbS quantum solution is taken, its optical absorption is determined in XRF, its absorption spectra is as shown in Fig. 1-a.
PbS quantum diffracting spectrum is determined on X-ray diffractometer, as shown in Figure 2.
Embodiment 2
The present embodiment is comprised the following steps：
(1) 0.417g lead chlorides are weighed in two mouthfuls of reaction bulbs, 5ml OLA are measured, mixture is vacuumized.
(2) 140 DEG C of maintenance 30min are heated the mixture to, mixture is then raised to 190 DEG C, be rapidly injected 2ml ZnS
Nanometer rods solution, keeps 20s.
(3) reaction drops to room temperature after terminating, add ethanol centrifugation, is subsequently adding n-hexane centrifugation, filtering, adds ethanol
Centrifugation obtains PbS quantum.
The performance characterization of gained PbS quantum is：
PbS quantum solution is taken, its optical absorption is determined in XRF, its absorption spectra is as shown in Fig. 1-b.
PbS quantum diffracting spectrum is determined on X-ray diffractometer, it is similar to Fig. 2.
Embodiment 3
The present embodiment is comprised the following steps：
(1) 0.417g lead chlorides are weighed in two mouthfuls of reaction bulbs, 5ml OLA are measured, mixture is vacuumized.
(2) 140 DEG C of maintenance 30min are heated the mixture to, mixture is then raised to 190 DEG C, be rapidly injected 2ml ZnS
Nanometer rods solution, keeps 5min.
(3) reaction drops to room temperature after terminating, add ethanol centrifugation, is subsequently adding n-hexane centrifugation, filtering, adds ethanol
Centrifugation obtains PbS quantum.
The performance characterization of gained PbS quantum is：
PbS quantum solution is taken, its optical absorption is determined in XRF, its absorption spectra is as shown in fig 1-c.
PbS quantum diffracting spectrum is determined on X-ray diffractometer, it is similar to Fig. 2.
Embodiment 4
The present embodiment is comprised the following steps：
(1) 0.417g lead chlorides are weighed in two mouthfuls of reaction bulbs, 5ml OLA are measured, mixture is vacuumized.
(2) 140 DEG C of maintenance 30min are heated the mixture to, mixture is then raised to 190 DEG C, be rapidly injected 2ml ZnS
Nanometer rods solution, keeps 15min.
(3) reaction drops to room temperature after terminating, add ethanol centrifugation, is subsequently adding n-hexane centrifugation, filtering, adds ethanol
Centrifugation obtains PbS quantum.
The performance characterization of gained PbS quantum is：
PbS quantum solution is taken, its optical absorption is determined in XRF, its absorption spectra is as shown in Fig. 1-d.
PbS quantum diffracting spectrum is determined on X-ray diffractometer, it is similar to Fig. 2.
Take PbS quantum solution to drip on copper mesh, spontaneously dry, be imaged under transmission electron microscope (FTEM) on the scene, such as
Shown in Fig. 3.
Will synthesis PbS quantum dry after put in atmosphere after six months, measure its absorption spectrum, as shown in Figure 4.
Embodiment 5
The present embodiment is comprised the following steps：
(1) 0.417g lead bromides are weighed in two mouthfuls of reaction bulbs, 5ml OLA are measured, mixture is vacuumized.
(2) 100 DEG C of maintenance 30min are heated the mixture to, mixture is then raised to 120 DEG C, be rapidly injected 2ml ZnS
Nanometer rods solution, keeps 2min.
(3) reaction drops to room temperature after terminating, add ethanol centrifugation, is subsequently adding n-hexane centrifugation, filtering, adds ethanol
Centrifugation obtains PbS quantum.
The performance characterization of gained PbS quantum is：
PbS quantum solution is taken, its optical absorption is determined in XRF, its absorption spectra is as shown in Figure 5.
Embodiment 6
The present embodiment is comprised the following steps：
(1) 0.417g lead iodides are weighed in two mouthfuls of reaction bulbs, 5ml OLA are measured, mixture is vacuumized.
(2) 100 DEG C of maintenance 30min are heated the mixture to, mixture is then raised to 120 DEG C, be rapidly injected 2ml ZnS
Nanometer rods solution, keeps 2min.
(3) reaction drops to room temperature after terminating, add ethanol centrifugation, is subsequently adding n-hexane centrifugation, filtering, adds ethanol
Centrifugation obtains PbS quantum.
The performance characterization of gained PbS quantum is：
PbS quantum solution is taken, its optical absorption is determined in XRF, its absorption spectra is as shown in Figure 6.
As it will be easily appreciated by one skilled in the art that the foregoing is only presently preferred embodiments of the present invention, it is not used to
The limitation present invention, all any modification, equivalent and improvement made within the spirit and principles in the present invention etc., all should include
Within protection scope of the present invention.
Claims (4)
1. a kind of preparation method of PbS quantum, it is characterised in that comprise the following steps：
(1) halogen compound of lead and oleyl amine are mixed to form mixture, the halogen compound of the lead is in the mixture
Concentration is 0.1mol/L~0.4mol/L；Then, under an inert atmosphere, the mixture is heated to 80 DEG C~150 DEG C, and is protected
Temperature, obtains the oleyl amine solution of the halide of lead；
(2) by ZnS nanometer rods solution well prepared in advance the halide for being injected into the lead that the step (1) is obtained oil
In amine aqueous solution, reacted at a temperature of 80 DEG C~190 DEG C, the reaction time is controlled in 10s~25min, that is, obtain including PbS
Quantum dot is in interior product.
2. the preparation method of PbS quantum as claimed in claim 1, it is characterised in that also including step：
(3) product that the step (2) obtains is cooled down；When being down to 70 DEG C at a temperature of the product, to
N-hexane is injected in the product；When being down to 40 DEG C at a temperature of the product, noted in the product
Enter oleic acid；
(4) to cooling after the product carry out centrifugation, then, in the precipitation for obtaining add n-hexane simultaneously
Carry out centrifugal filtration and obtain supernatant, be then to obtain PbS quantum to ethanol is added in the supernatant.
3. the preparation method of PbS quantum as claimed in claim 1, it is characterised in that in the step (1), the halogen of the lead
Compounds of group is any one in lead chloride, lead bromide, lead iodide；Preferably, the soaking time of the insulation be 15min~
60min。
4. the preparation method of PbS quantum as claimed in claim 1, it is characterised in that described ZnS nanometers in the step (2)
The material of the halogen compound of lead described in oleyl amine solution of the amount of the material of S elements with the halide of the lead in rod solution
Amount ratio between two is at most 1：2；The ZnS nanometer rods solution is injected into note used in the oleyl amine solution of the halide of the lead
The angle of incidence is no more than 10s.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108163818A (en) * | 2018-01-11 | 2018-06-15 | 武汉华思创新科技有限公司 | A kind of preparation method of PbSe quantum dots |
| CN109850937A (en) * | 2019-01-25 | 2019-06-07 | 深圳扑浪创新科技有限公司 | A kind of preparation method of vulcanized lead quantum dot fluorescence powder |
| CN110697766A (en) * | 2019-09-30 | 2020-01-17 | 武汉理工大学 | Preparation method of zinc-doped lead sulfide quantum dots |
| CN112763419A (en) * | 2021-01-27 | 2021-05-07 | 福州大学 | Hydrogen sulfide photo-thermal detection method of perovskite nano composite material modified based on SBE-beta-CD |
| CN114217012A (en) * | 2021-11-10 | 2022-03-22 | 中国科学院上海技术物理研究所 | Method for in-situ modification of mercury quantum dots in traditional heat injection process |
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| CN102766456A (en) * | 2012-07-04 | 2012-11-07 | 中南大学 | Ultrasonic-assisted method for preparing doped PbS quantum dot at low temperature in liquid phase |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108163818A (en) * | 2018-01-11 | 2018-06-15 | 武汉华思创新科技有限公司 | A kind of preparation method of PbSe quantum dots |
| CN109850937A (en) * | 2019-01-25 | 2019-06-07 | 深圳扑浪创新科技有限公司 | A kind of preparation method of vulcanized lead quantum dot fluorescence powder |
| CN109850937B (en) * | 2019-01-25 | 2022-03-25 | 深圳扑浪创新科技有限公司 | Preparation method of lead sulfide quantum dot fluorescent powder |
| CN110697766A (en) * | 2019-09-30 | 2020-01-17 | 武汉理工大学 | Preparation method of zinc-doped lead sulfide quantum dots |
| CN112763419A (en) * | 2021-01-27 | 2021-05-07 | 福州大学 | Hydrogen sulfide photo-thermal detection method of perovskite nano composite material modified based on SBE-beta-CD |
| CN114217012A (en) * | 2021-11-10 | 2022-03-22 | 中国科学院上海技术物理研究所 | Method for in-situ modification of mercury quantum dots in traditional heat injection process |
| CN114217012B (en) * | 2021-11-10 | 2023-09-12 | 中国科学院上海技术物理研究所 | In-situ modification method in mercury system quantum dot traditional heat injection flow |
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Effective date of registration: 20230920 Address after: Room 1244, 10th Floor, Building B3, Phase I, Longshan Innovation Park, Wuhan Future Science and Technology City, No. 999 Gaoxin Avenue, Donghu New Technology Development Zone, Wuhan City, Hubei Province, 430206 (Wuhan Area of Free Trade Zone) Patentee after: Wuhan Yingrui Technology Co.,Ltd. Address before: 430074 Hubei Province, Wuhan city Hongshan District Luoyu Road No. 1037 Patentee before: HUAZHONG University OF SCIENCE AND TECHNOLOGY |