CN106829882A - PbSe nanocrystals and preparation method thereof - Google Patents
PbSe nanocrystals and preparation method thereof Download PDFInfo
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- CN106829882A CN106829882A CN201611152827.XA CN201611152827A CN106829882A CN 106829882 A CN106829882 A CN 106829882A CN 201611152827 A CN201611152827 A CN 201611152827A CN 106829882 A CN106829882 A CN 106829882A
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
- C09K11/881—Chalcogenides
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- 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
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The invention discloses a kind of PbSe nanocrystals and preparation method thereof.The nanocrystalline cross section by orthogonal its feeler constitutes for six feeler PbSe nanocrystals of quadrangular shape, wherein, the length of feeler is 90~110nm, a length of 55~65nm of seamed edge of the root of feeler, a length of 35~45nm of seamed edge of end；Method is first during oleic acid lead solution to add in inert atmosphere two Bian amine under stirring, obtain mixed solution, the two Bian amine aqueous solutions containing selenium are added dropwise in mixed solution in inert atmosphere again, obtain reaction solution, afterwards, first reaction solution is stirred in inert atmosphere and is cooled to room temperature, obtain reaction paste, the treatment of separation of solid and liquid and washing is carried out to reaction paste again, purpose product is obtained.It can be widely used for the infrared device of commercialization manufacture hypersensitivity and detectivity as the base unit of Infrared Detectors of new generation.
Description
Technical field
The present invention relates to a kind of nanocrystalline and preparation method, the especially a kind of nanocrystalline and its preparation side of lead selenide (PbSe)
Method.
Background technology
Lead base chalcogenide has good optically and electrically performance because of it, is a class purposes inorganic material widely
Material, they are applied to the fields such as photodetector, field-effect transistor, solar cell in large quantities.Wherein, Emission in Cubic selenizing
The band gap small (about 0.28eV) of lead, bohr exciton radii are big (about 46nm), are conducive to detecting near-infrared and short-wave infrared,
It is a kind of very important infrared detecting materials.PbSe is nanocrystalline due to being in nanoscale in three dimensions, with very
Specific surface area high, using it as the base unit of Infrared Detectors of new generation, can be obtained hypersensitivity and detectivity
Infrared device.In the recent period, people are nanocrystalline in order to obtain PbSe, are made that unremitting effort, such as entitled " Organometallic-
Route Synthesis,Controllable Growth,Mechanism Investigation,and Surface
Feature of PbSe Nanostructures with Tunable Shapes ", Langmuir, 2014,30,2863-
2872 (" the liquid phase controllable preparation of PbSe nanostructureds, growth mechanism and surface characteristic ",《Langmuir》2014 volume 30 the 10th
2863-2872 pages of phase) article.The composition of the product referred in this article is for PbSe is nanocrystalline, pattern is orthogonal hexagonal
Star, size are 100~200nm；Preparation method uses solvent method, and detailed process is with triphenylphosphine selenium and tetraphernl-lead as forerunner
Body, is 13 by the solvent burden ratio for adjusting two Bian amine, oleic acid and oleyl amine:1:When 1, the PbSe for obtaining hexagram is nanocrystalline.This
Though kind of product can be used as the base unit of the Infrared Detectors of a new generation, weak point is all there is with its preparation method, it is first
First, product is taper, easily makes mutual cross stacking and reunite in three dimensions, greatly reduces specific surface
Product；Secondly, because the tetraphernl-lead using price higher than lead acetate more than 30 again is drastically increased for presoma in preparation process
The cost of making, the commercial applications for making it be difficult to scale industrial production and product.
The content of the invention
The technical problem to be solved in the present invention is to overcome weak point of the prior art, there is provided a kind of rational in infrastructure, no
The PbSe nanocrystals of easy cross stacking.
The invention solves the problems that another technical problem be that a kind of preparation method of above-mentioned PbSe nanocrystals is provided.
Be to solve technical problem of the invention, the technical scheme for being used for：PbSe nanocrystals are by orthogonal six
Feeler PbSe nanocrystals are constituted, particularly,
The cross section of the six feelers PbSe nanocrystals feeler is quadrangular shape；
The cross section is 90~110nm for the length of quadrangular shape feeler；
The cross section is a length of 55~65nm of seamed edge of root of quadrangular shape feeler, the seamed edge a length of 35 of end~
45nm。
Be to solve another technical problem of the invention, another technical scheme for being used for：Above-mentioned lead selenide nanometer
Brilliant preparation method includes that organic solwution method, particularly key step are as follows：
Step 1, is first 1 according to the oleic acid lead solution of 35~45mmol/L and the volume ratio of two Bian amine：8~12 ratio,
During 80~120 DEG C of oleic acid lead solution added into 140~160 DEG C of two Bian amine under stirring in inert atmosphere, its temperature is treated
10~20min is incubated after stabilizing to 140~160 DEG C, mixed solution, then containing 80~120 DEG C of 35~45mmol/L is obtained
Two Bian amine aqueous solutions of selenium are added dropwise in mixed solution in inert atmosphere, temperature is risen into 190~210 DEG C after completion of dropwise addition and is protected
20~30min of temperature, wherein, the volume ratio of two Bian amine in two Bian amine aqueous solutions and mixed solution containing selenium is 1：8~12, obtain anti-
Answer solution；
Step 2, reaction solution is first stirred be cooled to room temperature in inert atmosphere, obtains reaction paste, then to reaction slurry
Material carries out the treatment of separation of solid and liquid and washing, and PbSe nanocrystals are obtained.
As the further improvement of the preparation method of PbSe nanocrystals：
Preferably, inert atmosphere is nitrogen atmosphere, or argon gas atmosphere, or helium atmosphere.
Preferably, the process for preparation of oleic acid lead solution is, by three acetate hydrate lead (Pb (CH3COO)2·3H2O oil) is added
After in acid, it is placed in inert atmosphere in stirring at least 4h at 80~120 DEG C.
Preferably, the process for preparation of the two Bian amine aqueous solutions containing selenium is, according to the weight ratio of selenium powder, triphenyl phosphorus and two Bian amine
It is 1：3~4：30~35 ratio, after in selenium powder and triphenyl phosphorus two Bian amine of addition, is placed in inert atmosphere in 80~120
At least 6h is stirred at DEG C.
Preferably, separation of solid and liquid is processed as centrifugation, its rotating speed be 6000~10000r/min, the time be 10~
15min。
Preferably, carrying out washing treatment is that the alternating that 3~5 times are carried out to isolated solid using second alcohol and water is cleaned,
It is centrifugation that solid is separated during cleaning.
Preferably, be placed in after obtained PbSe nanocrystals are disperseed in ethanol≤10 DEG C at preserve.
Beneficial effect relative to prior art is：
First, obtained purpose product is characterized using X-ray diffractometer and ESEM respectively, can by its result
Know, the composition of purpose product is PbSe nanocrystals, pattern is orthogonal six feeler；Wherein, six feeler lead selenides nanometer
The cross section of brilliant feeler is quadrangular shape, and the length of quadrangular shape feeler is 90~110nm, the seamed edge a length of 55 of the root of feeler
~65nm, a length of 35~45nm of seamed edge of end.This purpose that orthogonal six feeler is assembled into by PbSe nanocrystals
Product, both due to the speciality of lead selenide itself, and because it is nano-scale dimension, due also to the end of orthogonal six feeler is
Quadrangular, and make it that not only there is good optically and electrically performance, it may have high specific surface area, it is also less prone to because of accumulation
Generation agglomeration.
Second, preparation method is simple, science, efficiently.Not only be obtained it is rational in infrastructure, be difficult cross stacking purpose produce
Thing --- PbSe nanocrystals；Also there is low production cost, it is easy to the characteristics of industrial-scale production；So that purpose product is easy
In the base unit as Infrared Detectors of new generation, it is widely used for the infrared of commercialization manufacture hypersensitivity and detectivity
Device.
Brief description of the drawings
Fig. 1 is one of result for being characterized using X-ray diffraction (XRD) instrument to purpose product obtained in preparation method.
Wherein, XRD standard spectral line, spectral line that upper curve be purpose product of the bottom curve of XRD spectra for lead selenide；The XRD is composed
The bright purpose product of chart is the perfect monocrystalline lead selenide of crystallization.
Fig. 2 is one of result for being characterized using ESEM (SEM) to obtained purpose product.SEM image shows
The pattern for going out purpose product is that the cross section of orthogonal its feeler is six feelers of quadrangular shape.
Specific embodiment
Preferred embodiment of the invention is described in further detail below in conjunction with the accompanying drawings.
Bought from market first or be voluntarily obtained：
Oleic acid lead solution；
Two Bian amine；
The two Bian amine aqueous solutions containing selenium；
As the nitrogen of inert atmosphere, argon gas and helium；Wherein,
The process for preparation of oleic acid lead solution is after in three acetate hydrate lead addition oleic acid, to be placed in inert atmosphere in 80
At least 4h is stirred at~120 DEG C.
The process for preparation of the two Bian amine aqueous solutions containing selenium is, is 1 according to the weight ratio of selenium powder, triphenyl phosphorus and two Bian amine：3~
4：30~35 ratio, after in selenium powder and triphenyl phosphorus two Bian amine of addition, is placed in inert atmosphere in stirring at 80~120 DEG C
At least 6h.
Then,
Embodiment 1
What is prepared concretely comprises the following steps：
Step 1, is first 1 according to the oleic acid lead solution of 35mmol/L and the volume ratio of two Bian amine：12 ratio, by 80 DEG C
Oleic acid lead solution is added in two Bian amine of 160 DEG C under stirring in inert atmosphere, is incubated after its temperature stabilization is 160 DEG C
10min；Wherein, inert atmosphere is nitrogen atmosphere, obtains mixed solution.It is again that the two Bian amine containing selenium of 80 DEG C of 35mmol/L are molten
Liquid is added dropwise in mixed solution in inert atmosphere, and temperature is risen into 190 DEG C after completion of dropwise addition and 30min is incubated；Wherein, containing selenium
Two Bian amine aqueous solutions and mixed solution in two Bian amine volume ratio be 1：12, inert atmosphere is nitrogen atmosphere, obtains reaction molten
Liquid.
Step 2, reaction solution is first stirred be cooled to room temperature in inert atmosphere, obtains reaction paste；Wherein, indifferent gas
Atmosphere is nitrogen atmosphere.The treatment of separation of solid and liquid and washing is carried out to reaction paste again；Wherein, separation of solid and liquid is processed as centrifugation point
From its rotating speed is 6000r/min, the time is 15min, and carrying out washing treatment is that isolated solid is carried out using second alcohol and water
The alternating cleaning of 3 times, it is centrifugation that solid is separated during cleaning.It is obtained as shown by the curve in figure 1, and is similar to Fig. 2
Shown PbSe nanocrystals.
Embodiment 2
What is prepared concretely comprises the following steps：
Step 1, is first 1 according to the oleic acid lead solution of 38mmol/L and the volume ratio of two Bian amine：11 ratio, by 90 DEG C
Oleic acid lead solution is added in two Bian amine of 155 DEG C under stirring in inert atmosphere, is incubated after its temperature stabilization is 155 DEG C
13min；Wherein, inert atmosphere is nitrogen atmosphere, obtains mixed solution.It is again that the two Bian amine containing selenium of 90 DEG C of 38mmol/L are molten
Liquid is added dropwise in mixed solution in inert atmosphere, and temperature is risen into 195 DEG C after completion of dropwise addition and 28min is incubated；Wherein, containing selenium
Two Bian amine aqueous solutions and mixed solution in two Bian amine volume ratio be 1：11, inert atmosphere is nitrogen atmosphere, obtains reaction molten
Liquid.
Step 2, reaction solution is first stirred be cooled to room temperature in inert atmosphere, obtains reaction paste；Wherein, indifferent gas
Atmosphere is nitrogen atmosphere.The treatment of separation of solid and liquid and washing is carried out to reaction paste again；Wherein, separation of solid and liquid is processed as centrifugation point
From its rotating speed is 7000r/min, the time is 13min, and carrying out washing treatment is that isolated solid is carried out using second alcohol and water
The alternating cleaning of 3 times, it is centrifugation that solid is separated during cleaning.It is obtained as shown by the curve in figure 1, and is similar to Fig. 2
Shown PbSe nanocrystals.
Embodiment 3
What is prepared concretely comprises the following steps：
Step 1, is first 1 according to the oleic acid lead solution of 40mmol/L and the volume ratio of two Bian amine：10 ratio, by 100 DEG C
Oleic acid lead solution add two Bian amine of lower 150 DEG C of stirring in inert atmosphere, the insulation after its temperature stabilization is 150 DEG C
15min；Wherein, inert atmosphere is nitrogen atmosphere, obtains mixed solution.Again by the two Bian amine containing selenium of 100 DEG C of 40mmol/L
Solution is added dropwise in mixed solution in inert atmosphere, and temperature is risen into 200 DEG C after completion of dropwise addition and 25min is incubated；Wherein, contain
The volume ratio of two Bian amine in the two Bian amine aqueous solutions and mixed solution of selenium is 1：10, inert atmosphere is nitrogen atmosphere, is reacted
Solution.
Step 2, reaction solution is first stirred be cooled to room temperature in inert atmosphere, obtains reaction paste；Wherein, indifferent gas
Atmosphere is nitrogen atmosphere.The treatment of separation of solid and liquid and washing is carried out to reaction paste again；Wherein, separation of solid and liquid is processed as centrifugation point
From its rotating speed is 8000r/min, the time is 12min, and carrying out washing treatment is that isolated solid is carried out using second alcohol and water
The alternating cleaning of 4 times, it is centrifugation that solid is separated during cleaning.It is obtained as shown by the curve in figure 1, and as shown in Figure 2
PbSe nanocrystals.
Embodiment 4
What is prepared concretely comprises the following steps：
Step 1, is first 1 according to the oleic acid lead solution of 43mmol/L and the volume ratio of two Bian amine：9 ratio, by 110 DEG C
Oleic acid lead solution is added in two Bian amine of 145 DEG C under stirring in inert atmosphere, is incubated after its temperature stabilization is 145 DEG C
18min；Wherein, inert atmosphere is nitrogen atmosphere, obtains mixed solution.Again by the two Bian amine containing selenium of 110 DEG C of 43mmol/L
Solution is added dropwise in mixed solution in inert atmosphere, and temperature is risen into 205 DEG C after completion of dropwise addition and 23min is incubated；Wherein, contain
The volume ratio of two Bian amine in the two Bian amine aqueous solutions and mixed solution of selenium is 1：9, inert atmosphere is nitrogen atmosphere, obtains reaction molten
Liquid.
Step 2, reaction solution is first stirred be cooled to room temperature in inert atmosphere, obtains reaction paste；Wherein, indifferent gas
Atmosphere is nitrogen atmosphere.The treatment of separation of solid and liquid and washing is carried out to reaction paste again；Wherein, separation of solid and liquid is processed as centrifugation point
From its rotating speed is 9000r/min, the time is 11min, and carrying out washing treatment is that isolated solid is carried out using second alcohol and water
The alternating cleaning of 4 times, it is centrifugation that solid is separated during cleaning.It is obtained as shown by the curve in figure 1, and is similar to Fig. 2
Shown PbSe nanocrystals.
Embodiment 5
What is prepared concretely comprises the following steps：
Step 1, is first 1 according to the oleic acid lead solution of 45mmol/L and the volume ratio of two Bian amine：8 ratio, by 120 DEG C
Oleic acid lead solution is added in two Bian amine of 140 DEG C under stirring in inert atmosphere, is incubated after its temperature stabilization is 140 DEG C
20min；Wherein, inert atmosphere is nitrogen atmosphere, obtains mixed solution.Again by the two Bian amine containing selenium of 120 DEG C of 45mmol/L
Solution is added dropwise in mixed solution in inert atmosphere, and temperature is risen into 210 DEG C after completion of dropwise addition and 20min is incubated；Wherein, contain
The volume ratio of two Bian amine in the two Bian amine aqueous solutions and mixed solution of selenium is 1：8, inert atmosphere is nitrogen atmosphere, obtains reaction molten
Liquid.
Step 2, reaction solution is first stirred be cooled to room temperature in inert atmosphere, obtains reaction paste；Wherein, indifferent gas
Atmosphere is nitrogen atmosphere.The treatment of separation of solid and liquid and washing is carried out to reaction paste again；Wherein, separation of solid and liquid is processed as centrifugation point
From its rotating speed is 10000r/min, the time is 10min, and carrying out washing treatment is that isolated solid is entered using second alcohol and water
The alternating cleaning that row is 5 times, it is centrifugation that solid is separated during cleaning.It is obtained as shown by the curve in figure 1, and is similar to figure
PbSe nanocrystals shown in 2.
Again respectively from the argon gas atmosphere or helium atmosphere as inert atmosphere, above-described embodiment 1~5, same system are repeated
Obtained as shown by the curve in figure 1, and as or the PbSe nanocrystals that are similar to shown in Fig. 2.
If for the benefit of long-term preservation of purpose product, be placed in after can obtained PbSe nanocrystals be disperseed in ethanol≤
Preserved at 10 DEG C.
Obviously, those skilled in the art can carry out various changing to PbSe nanocrystals of the invention and preparation method thereof
Dynamic and modification is without departing from the spirit and scope of the present invention.So, if belonging to this hair to these modifications of the invention and modification
Within the scope of bright claim and its equivalent technologies, then the present invention is also intended to comprising these changes and modification.
Claims (8)
1. a kind of PbSe nanocrystals, are made up of orthogonal six feelers PbSe nanocrystals, it is characterised in that：
The cross section of the six feelers PbSe nanocrystals feeler is quadrangular shape；
The cross section is 90~110nm for the length of quadrangular shape feeler；
The cross section is a length of 55~65nm of seamed edge, a length of 35~45nm of seamed edge of end of the root of quadrangular shape feeler.
2. a kind of preparation method of PbSe nanocrystals described in claim 1, including organic solwution method, it is characterised in that main step
It is rapid as follows：
Step 1, is first 1 according to the oleic acid lead solution of 35~45mmol/L and the volume ratio of two Bian amine：8~12 ratio, by 80
~120 DEG C of oleic acid lead solution is added in two Bian amine of 140~160 DEG C under stirring in inert atmosphere, treats its temperature stabilization
It is that 10~20min is incubated after 140~160 DEG C, obtains mixed solution, then by 80~120 DEG C of 35~45mmol/L containing selenium
Two Bian amine aqueous solutions are added dropwise in mixed solution in inert atmosphere, and temperature is risen into 190~210 DEG C and insulation 20 after completion of dropwise addition
~30min, wherein, the volume ratio of two Bian amine in two Bian amine aqueous solutions and mixed solution containing selenium is 1：8~12, obtain reaction molten
Liquid；
Step 2, reaction solution is first stirred be cooled to room temperature in inert atmosphere, obtains reaction paste, then reaction paste is entered
Row separation of solid and liquid and the treatment of washing, are obtained PbSe nanocrystals.
3. the preparation method of PbSe nanocrystals according to claim 2, it is characterized in that inert atmosphere is nitrogen atmosphere, or
Argon gas atmosphere, or helium atmosphere.
4. the preparation method of PbSe nanocrystals according to claim 2, it is characterized in that the process for preparation of oleic acid lead solution
After three acetate hydrate lead are added in oleic acid, to be placed in inert atmosphere in stirring at least 4h at 80~120 DEG C.
5. the preparation method of PbSe nanocrystals according to claim 2, it is characterized in that the two Bian amine aqueous solutions containing selenium are matched somebody with somebody
Process processed is, is 1 according to the weight ratio of selenium powder, triphenyl phosphorus and two Bian amine：3~4：30~35 ratio, by selenium powder and triphen
After base phosphorus is added in two Bian amine, it is placed in inert atmosphere in stirring at least 6h at 80~120 DEG C.
6. the preparation method of PbSe nanocrystals according to claim 2, it is characterized in that separation of solid and liquid is processed as centrifugation point
From its rotating speed is 6000~10000r/min, the time is 10~15min.
7. the preparation method of PbSe nanocrystals according to claim 2, it is characterized in that carrying out washing treatment be using ethanol and
Water carries out the alternating cleaning of 3~5 times to isolated solid, and it is centrifugation that solid is separated during cleaning.
8. the preparation method of PbSe nanocrystals according to claim 2, it is characterized in that by obtained PbSe nanocrystals
In ethanol disperse after be placed in≤10 DEG C at preserve.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101600807A (en) * | 2007-01-25 | 2009-12-09 | Iti苏格兰有限公司 | Use optics and electrical measurement method check and analysis thing |
| CN103998656A (en) * | 2011-12-07 | 2014-08-20 | 华东理工大学 | Methods of producing cadmium selenide multi-pod nanocrystals |
| US20140319563A1 (en) * | 2011-06-17 | 2014-10-30 | University Of Florida Research Foundation, Inc. | Laterally aligned colloidal nanorods assemblies |
-
2016
- 2016-12-14 CN CN201611152827.XA patent/CN106829882B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101600807A (en) * | 2007-01-25 | 2009-12-09 | Iti苏格兰有限公司 | Use optics and electrical measurement method check and analysis thing |
| US20140319563A1 (en) * | 2011-06-17 | 2014-10-30 | University Of Florida Research Foundation, Inc. | Laterally aligned colloidal nanorods assemblies |
| CN103998656A (en) * | 2011-12-07 | 2014-08-20 | 华东理工大学 | Methods of producing cadmium selenide multi-pod nanocrystals |
Non-Patent Citations (1)
| Title |
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| 曹红亮: "金属硫族半导体纳米材料的液相控制合成及机理研究", 《中国博士学位论文全文数据库 工程科技I辑》 * |
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