CN106829882B - PbSe nanocrystals and preparation method thereof - Google Patents
PbSe nanocrystals and preparation method thereof Download PDFInfo
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- CN106829882B CN106829882B CN201611152827.XA CN201611152827A CN106829882B CN 106829882 B CN106829882 B CN 106829882B CN 201611152827 A CN201611152827 A CN 201611152827A CN 106829882 B CN106829882 B CN 106829882B
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- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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- 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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Abstract
The invention discloses a kind of PbSe nanocrystals and preparation method thereof.The nanocrystalline cross section by its orthogonal feeler is that six feeler PbSe nanocrystals of quadrangular shape form, 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 oleic acid lead solution to be added in inert atmosphere in two Bian amine under stirring, obtain mixed solution, the two Bian amine aqueous solutions containing selenium are added dropwise in inert atmosphere in mixed solution again, obtain reaction solution, later, first reaction solution is stirred in inert atmosphere and is cooled to room temperature, obtain reaction paste, purpose product is made in the processing for being separated by solid-liquid separation and being washed to reaction paste again.It can be used as the base unit of infrared detector of new generation, be widely used for the infrared device of commercialization manufacture hypersensitivity and detectivity.
Description
Technical field
The present invention relates to a kind of nanocrystalline and preparation method, the especially a kind of nanocrystalline and its preparation sides of lead selenide (PbSe)
Method.
Background technology
Lead base chalcogenide is the very extensive inorganic material of a kind of purposes because it is with good optically and electrically performance
Material, they are applied to the fields such as photodetector, field-effect transistor, solar cell in large quantities.Wherein, cubic phase selenizing
The band gap small (about 0.28eV) of lead, bohr exciton radii are big (about 46nm), are conducive to detect 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, has very
Hypersensitivity and detectivity can be made using it as the base unit of infrared detector of new generation in high specific surface area
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 (" liquid phase controllable preparation, growth mechanism and the surface characteristic of PbSe nanostructures ",《Langmuir》2014 volume 30 the 10th
2863-2872 pages of phase) article.The ingredient of the product referred in this article is that PbSe is nanocrystalline, pattern is orthogonal hexagonal
Star, size are 100~200nm；Preparation method uses solvent method, and detailed process is forerunner with triphenylphosphine selenium and tetraphernl-lead
Body, the solvent burden ratio by adjusting two Bian amine, oleic acid and oleyl amine are 13:1:When 1, the PbSe for obtaining hexagram is nanocrystalline.This
Though kind of product can be used as the base unit of the infrared detector of a new generation, all there is shortcomings with preparation method, first
First, product is taper in three dimensions, easily makes mutual cross stacking and reunites, greatly reduces specific surface
Product；Secondly, in preparation process because use the tetraphernl-lead of price higher than lead acetate more than 30 times for presoma due to greatly improve
The cost of making makes it be difficult to scale industrial production and the commercial applications of product.
Invention content
The technical problem to be solved in the present invention is to overcome shortcoming in the prior art, provide it is a kind of reasonable for structure, no
The PbSe nanocrystals of easy cross stacking.
The invention solves another technical problem be that a kind of preparation method of above-mentioned PbSe nanocrystals is provided.
To solve the technical problem of the present invention, used technical solution is：PbSe nanocrystals are by orthogonal six
Feeler PbSe nanocrystals form, in particular,
The cross section of the six feelers PbSe nanocrystals feeler is quadrangular shape；
The cross section is that the length of quadrangular shape feeler is 90~110nm；
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。
To solve another technical problem of the present invention, another used technical solution is：Above-mentioned lead selenide nanometer
Brilliant preparation method includes that organic solwution method, especially key step are as follows：
Step 1, elder generation is 1 according to the oleic acid lead solution of 35~45mmol/L and the volume ratio of two Bian amine：8~12 ratio,
80~120 DEG C of oleic acid lead solution is added in inert atmosphere in 140~160 DEG C of two Bian amine under stirring, waits for its temperature
10~20min is kept the temperature after stabilizing to 140~160 DEG C, obtains mixed solution, then containing 80~120 DEG C of 35~45mmol/L
Two Bian amine aqueous solutions of selenium are added dropwise in inert atmosphere in mixed solution, and temperature is risen to 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, it obtains anti-
Answer solution；
Step 2, first reaction solution is stirred in inert atmosphere and is cooled to room temperature, obtain reaction paste, then to reaction slurry
Expect the processing for being separated by solid-liquid separation and being washed, PbSe nanocrystals are made.
Preparation method as PbSe nanocrystals is further improved：
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 at 80~120 DEG C and stirs at least 4h.
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 is placed in inert atmosphere after selenium powder and triphenyl phosphorus are added in two Bian amine in 80~120
At least 6h is stirred at DEG C.
Preferably, solid-liquid separation treatment is to centrifuge, rotating speed is 6000~10000r/min, the time be 10~
15min。
Preferably, carrying out washing treatment is the alternating cleaning for carrying out 3~5 times to isolated solid using second alcohol and water,
It is to centrifuge that solid is detached when cleaning.
Preferably, PbSe nanocrystals obtained are disperseed to be placed at≤10 DEG C in ethyl alcohol and is preserved.
Advantageous effect compared with the existing technology is：
First, purpose product obtained is characterized using X-ray diffractometer and scanning electron microscope respectively, it can by its result
Know, the ingredient of purpose product is PbSe nanocrystals, pattern is orthogonal six feeler；Wherein, six feeler lead selenide 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, end a length of 35~45nm of seamed edge.This purpose that orthogonal six feeler is assembled by PbSe nanocrystals
Product, not only due to the speciality of lead selenide itself, but also because it is nano-scale dimension, due also to the end of orthogonal six feeler is
Quadrangular, and making it not only has good optically and electrically performance, it may have high specific surface area is also less prone to due to accumulation
Agglomeration occurs.
Second, preparation method is simple, science, efficiently.It has not only been made reasonable for structure, has been not easy the purpose production of cross stacking
Object --- PbSe nanocrystals；The characteristics of also having production cost low, being easy to industrial-scale production；To keep purpose product easy
In the base unit as infrared detector of new generation, it is widely used for the infrared of commercialization manufacture hypersensitivity and detectivity
Device.
Description of the drawings
Fig. 1 is to use one of the result that X-ray diffraction (XRD) instrument is characterized to purpose product made from preparation method.
Wherein, the bottom curve of XRD spectra is the XRD standards spectral line of lead selenide, the spectral line that upper curve is purpose product；The XRD is composed
The bright purpose product of chart is to crystallize perfect monocrystalline lead selenide.
Fig. 2 is to use one of the result that scanning electron microscope (SEM) is characterized to purpose product obtained.SEM image is shown
The pattern for going out purpose product is that the cross section of its orthogonal feeler is six feelers of quadrangular shape.
Specific implementation mode
The preferred embodiment of the present invention is described in further detail below in conjunction with the accompanying drawings.
It buys from market or is voluntarily made first：
Oleic acid lead solution；
Two Bian amine；
The two Bian amine aqueous solutions containing selenium；
Nitrogen, argon gas and helium as inert atmosphere；Wherein,
The process for preparation of oleic acid lead solution is after three acetate hydrate lead are added in 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 that the weight ratio according to selenium powder, triphenyl phosphorus and two Bian amine is 1：3~
4：30~35 ratio is placed in inert atmosphere at 80~120 DEG C and stirs after selenium powder and triphenyl phosphorus are added in two Bian amine
At least 6h.
Then,
Embodiment 1
Prepare the specific steps are：
Step 1, elder generation is 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 inert atmosphere in 160 DEG C of two Bian amine under stirring, is kept the temperature after its temperature stabilizes to 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 inert atmosphere in mixed solution, and temperature is risen to 190 DEG C after completion of dropwise addition and keeps the temperature 30min；Wherein, contain selenium
Two Bian amine aqueous solutions and mixed solution in two Bian amine volume ratio be 1：12, inert atmosphere is nitrogen atmosphere, obtains reacting molten
Liquid.
Step 2, first reaction solution is stirred in inert atmosphere and is cooled to room temperature, obtain reaction paste；Wherein, indifferent gas
Atmosphere is nitrogen atmosphere.The processing that reaction paste is separated by solid-liquid separation and is washed again；Wherein, solid-liquid separation treatment is centrifugation point
From rotating speed 6000r/min, time 15min, carrying out washing treatment are to be carried out to isolated solid using second alcohol and water
3 alternating cleanings, separation solid is to centrifuge when cleaning.It is made as shown by the curve in figure 1, and is similar to Fig. 2
Shown in PbSe nanocrystals.
Embodiment 2
Prepare the specific steps are：
Step 1, elder generation is 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 inert atmosphere in 155 DEG C of two Bian amine under stirring, is kept the temperature after its temperature stabilizes to 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 inert atmosphere in mixed solution, and temperature is risen to 195 DEG C after completion of dropwise addition and keeps the temperature 28min；Wherein, contain selenium
Two Bian amine aqueous solutions and mixed solution in two Bian amine volume ratio be 1：11, inert atmosphere is nitrogen atmosphere, obtains reacting molten
Liquid.
Step 2, first reaction solution is stirred in inert atmosphere and is cooled to room temperature, obtain reaction paste；Wherein, indifferent gas
Atmosphere is nitrogen atmosphere.The processing that reaction paste is separated by solid-liquid separation and is washed again；Wherein, solid-liquid separation treatment is centrifugation point
From rotating speed 7000r/min, time 13min, carrying out washing treatment are to be carried out to isolated solid using second alcohol and water
3 alternating cleanings, separation solid is to centrifuge when cleaning.It is made as shown by the curve in figure 1, and is similar to Fig. 2
Shown in PbSe nanocrystals.
Embodiment 3
Prepare the specific steps are：
Step 1, elder generation is 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 be added in inert atmosphere stirring under 150 DEG C of two Bian amine in, kept the temperature after its temperature stabilizes to 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 inert atmosphere in mixed solution, and temperature is risen to 200 DEG C after completion of dropwise addition and keeps the temperature 25min；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, first reaction solution is stirred in inert atmosphere and is cooled to room temperature, obtain reaction paste；Wherein, indifferent gas
Atmosphere is nitrogen atmosphere.The processing that reaction paste is separated by solid-liquid separation and is washed again；Wherein, solid-liquid separation treatment is centrifugation point
From rotating speed 8000r/min, time 12min, carrying out washing treatment are to be carried out to isolated solid using second alcohol and water
4 alternating cleanings, separation solid is to centrifuge when cleaning.It is made as shown by the curve in figure 1, and as shown in Figure 2
PbSe nanocrystals.
Embodiment 4
Prepare the specific steps are：
Step 1, elder generation is 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 inert atmosphere in 145 DEG C of two Bian amine under stirring, is kept the temperature after its temperature stabilizes to 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 inert atmosphere in mixed solution, and temperature is risen to 205 DEG C after completion of dropwise addition and keeps the temperature 23min；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 reacting molten
Liquid.
Step 2, first reaction solution is stirred in inert atmosphere and is cooled to room temperature, obtain reaction paste；Wherein, indifferent gas
Atmosphere is nitrogen atmosphere.The processing that reaction paste is separated by solid-liquid separation and is washed again；Wherein, solid-liquid separation treatment is centrifugation point
From rotating speed 9000r/min, time 11min, carrying out washing treatment are to be carried out to isolated solid using second alcohol and water
4 alternating cleanings, separation solid is to centrifuge when cleaning.It is made as shown by the curve in figure 1, and is similar to Fig. 2
Shown in PbSe nanocrystals.
Embodiment 5
Prepare the specific steps are：
Step 1, elder generation is 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 inert atmosphere in 140 DEG C of two Bian amine under stirring, is kept the temperature after its temperature stabilizes to 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 inert atmosphere in mixed solution, and temperature is risen to 210 DEG C after completion of dropwise addition and keeps the temperature 20min；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 reacting molten
Liquid.
Step 2, first reaction solution is stirred in inert atmosphere and is cooled to room temperature, obtain reaction paste；Wherein, indifferent gas
Atmosphere is nitrogen atmosphere.The processing that reaction paste is separated by solid-liquid separation and is washed again；Wherein, solid-liquid separation treatment is centrifugation point
From, rotating speed 10000r/min, time 10min, carrying out washing treatment be using second alcohol and water to isolated solid into
The cleaning of alternating that row is 5 times, separation solid is to centrifuge when cleaning.It is made as shown by the curve in figure 1, and is similar to figure
PbSe nanocrystals shown in 2.
It selects the argon gas atmosphere or helium atmosphere as inert atmosphere respectively again, repeats above-described embodiment 1~5, it is same to make
Obtained as shown by the curve in figure 1, and as or be similar to PbSe nanocrystals shown in Fig. 2.
If for the benefit of long-term preservation of purpose product, PbSe nanocrystals obtained can be disperseed in ethyl alcohol to be placed on≤
It is preserved at 10 DEG C.
Obviously, those skilled in the art can carry out various change to PbSe nanocrystals of the present invention and preparation method thereof
Dynamic and modification is without departing from the spirit and scope of the present invention.If in this way, belonging to this hair to these modifications and changes of the present invention
Within the scope of bright claim and its equivalent technologies, then the present invention is also intended to include these modifications and variations.
Claims (7)
1. a kind of preparation method of PbSe nanocrystals, including organic solwution method, it is characterised in that key step is as follows：
Step 1, elder generation is 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 inert atmosphere in 140~160 DEG C of two Bian amine under stirring, waits for that its temperature is stablized
10~20min is kept the temperature after being 140~160 DEG C, obtain mixed solution, then by 80~120 DEG C of 35~45mmol/L containing selenium
Two Bian amine aqueous solutions are added dropwise in inert atmosphere in mixed solution, and temperature is risen to 190~210 DEG C after completion of dropwise addition and keeps the temperature 20
~30min, wherein the volume ratio of two Bian amine in two Bian amine aqueous solutions and mixed solution containing selenium is 1：8~12, it obtains reacting molten
Liquid；
Step 2, first reaction solution is stirred in inert atmosphere and is cooled to room temperature, obtain reaction paste, then to reaction paste into
Row is separated by solid-liquid separation and the processing of washing, and PbSe nanocrystals are made；
The PbSe nanocrystals are made of orthogonal six feelers PbSe nanocrystals, wherein six feeler lead selenide nanometers
The cross section of brilliant feeler is quadrangular shape, and cross section is that the length of quadrangular shape feeler is 90~110nm, and cross section is quadrangular
A length of 55~the 65nm of seamed edge of the root of shape feeler, a length of 35~45nm of seamed edge of end.
2. the preparation method of PbSe nanocrystals according to claim 1, it is characterized in that inert atmosphere is nitrogen atmosphere, or
Argon gas atmosphere or helium atmosphere.
3. the preparation method of PbSe nanocrystals according to claim 1, 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 at 80~120 DEG C and stirring at least 4h.
4. the preparation method of PbSe nanocrystals according to claim 1, it is characterized in that the two Bian amine aqueous solutions containing selenium are matched
Process processed is that the weight ratio according to selenium powder, triphenyl phosphorus and two Bian amine is 1：3~4：30~35 ratio, by selenium powder and triphen
After base phosphorus is added in two Bian amine, it is placed in inert atmosphere at 80~120 DEG C and stirs at least 6h.
5. the preparation method of PbSe nanocrystals according to claim 1, it is characterized in that solid-liquid separation treatment is centrifugation point
From rotating speed is 6000~10000r/min, the time is 10~15min.
6. the preparation method of PbSe nanocrystals according to claim 1, it is characterized in that carrying out washing treatment be using ethyl alcohol and
The alternating that water carries out isolated solid 3~5 times is cleaned, and separation solid is to centrifuge when cleaning.
7. the preparation method of PbSe nanocrystals according to claim 1, it is characterized in that by PbSe nanocrystals obtained
Dispersion, which is placed at≤10 DEG C, in ethyl alcohol preserves.
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Citations (2)
| 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 |
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| WO2012174533A2 (en) * | 2011-06-17 | 2012-12-20 | University Of Florida Research Foundation, Inc. | Laterally aligned colloidal nanorods assemblies |
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Patent Citations (2)
| 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 |
| 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 |
|---|
| 金属硫族半导体纳米材料的液相控制合成及机理研究;曹红亮;《中国博士学位论文全文数据库 工程科技I辑》;20080615(第6期);第B020-20页 * |
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