CN105965027A - Solution phase synthetic method for indium antimonide nanowire - Google Patents
Solution phase synthetic method for indium antimonide nanowire Download PDFInfo
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- CN105965027A CN105965027A CN201610291285.8A CN201610291285A CN105965027A CN 105965027 A CN105965027 A CN 105965027A CN 201610291285 A CN201610291285 A CN 201610291285A CN 105965027 A CN105965027 A CN 105965027A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a solution phase synthetic method for an indium antimonide nanowire. The solution phase synthetic method for the indium antimonide nanowire is characterized by (1) using indium source and antimony source as reaction material, then heating to 100-120 DEG C in reaction medium consisting of octadecene and organic amine, and obtaining mixed liquor; (2) heating the mixed liquor to 160-220 DEG C, then adding borane-tert-butylamine complex which is dissolved in oleylamine and organic phosphine, and reacting; (3) washing the product with methylbenzene and absolute ethyl alcohol after the reaction, and then conducting centrifugal separation to obtain the indium antimonide nanowire which is good in crystallinity and uniform in morphology. The solution phase synthetic method is simple in technology, mild in reaction condition and suited for large scale production.
Description
Technical field
The invention belongs to inorganic compound technical field of nano material, be specifically related to a kind of solution and be combined to the side of indium antimonide nano wire
Method.
Background technology
Indium antimonide (InSb) is a kind of important Group III-V compound semiconductor, and indium antimonide block materials has the least band gap length
Degree (0.17eV), the highest electron mobility (78000cm2/ V s) and the biggest bohr exciton radii (60nm), these
Character makes it have a wide range of applications in fields such as high-speed field effect transistors, Magnetic Sensor, Infrared Detectorss.Additionally,
Compared with indium antimonide block materials, indium antimonide nano wire is owing to having the quantum limitation effect, anisotropic being associated with size
Geometry, good electron transport property and bigger specific surface area, consequently, it is possible to show than indium antimonide block materials more
Superior character.In order to meet these application as far as possible, the synthetic method developing a kind of simple effective indium antimonide nano wire is compeled
At the eyebrows and eyelashes.
In prior art, the method preparing indium antimonide nano wire is mainly chemical gas phase synthetic method (CVD) (Nano letters
2012,12,1794；Nanotechnology 2009,20,495606；Nature materials 2004,3,769).Use CVD
Although the indium antimonide nano wire pattern of preparation is more uniform, but its diameter is thick, be frequently more than its bohr exciton radii, and whole synthesis
During generally require higher temperature and vacuum equipment costly, its energy consumption is relatively big, and product cost is higher.
Summary of the invention
The present invention be directed to the problem in the presence of chemical gaseous phase synthetic method, it is provided that the solution of a kind of indium antimonide nano wire is combined to
New method, its synthesis temperature is low, and technique is simple, and aggregate velocity is fast.
The present invention solves technical problem, adopts the following technical scheme that
The Solution phase synthetic methods of indium antimonide nano wire of the present invention, its feature is:
With indium source and antimony source as reaction raw materials, the reaction medium being made up of octadecylene and organic amine is heated to 100～120 DEG C,
Obtain mixed liquor；Described mixed liquor is warming up to 160～220 DEG C, adds the monoborane-tertiary fourth being dissolved in oleyl amine and tri octyl phosphine
Amine complex also reacts；After reaction terminates, with toluene and absolute ethanol washing product, centrifugation, obtain good crystallinity, shape
Looks uniform indium antimonide nano wire；It is distributed to products therefrom in dehydrated alcohol preserve.
Wherein: the mol ratio in described indium source and antimony source is 1～1.5:1；Described monoborane-tert-butylamine complex and the mol ratio in antimony source
It is 10～15:1.
The Solution phase synthetic methods of indium antimonide nano wire of the present invention, is carried out the most as follows:
Step 1: by proportioning, indium source and antimony source are dissolved in benzyl ether solvent, it is thus achieved that mixed liquor A；
Step 2: by octadecylene and organic amine mix homogeneously, constitutes reaction medium；Mixed liquor A step 1 obtained joins
In reaction medium, under inert gas shielding, it is heated to 100～120 DEG C, removes moisture and low boiling impurity, it is thus achieved that mixed liquid B；
Step 3: monoborane-tert-butylamine complex is dissolved in oleyl amine and tri octyl phosphine, it is thus achieved that mixed liquor C；
Step 4: mixed liquid B step 2 obtained is heated to 160～220 DEG C, the mixed liquor C then step 3 obtained is fast
Speed is injected in mixed liquid B, reacts 5～60min, naturally cools to room temperature；
Step 5: with toluene and absolute ethanol washing product, centrifugation, i.e. obtain indium antimonide nano wire.
One or more in Indium sesquioxide., Indium Tris acetylacetonate, Indium-111 chloride, indium nitrate or indium acetate of described indium source.Described
One or more in stibium oxide, antimony triphenyl, Butter of antimony. or antimony acetate of antimony source.Described organic amine selected from oleyl amine, ten
One or more in eight amine or cetylamine.
Described organic amine is 5～20:1 with the mol ratio in described indium source；Described organic amine is 1～10 with the mol ratio of described octadecylene:
1；Described tri octyl phosphine is 1～4:1 with the volume ratio of described oleyl amine.
The InSb nano wire that the present invention prepares is zincblende lattce structure InSb, and average diameter is 50nm, a length of 5～10 μm.
Can be seen that the inventive method gained InSb receives from the transmission electron microscope picture of product, high-resolution-ration transmission electric-lens figure, SEAD figure
Rice noodle is the nano wire with twin structure along the growth of [111] direction, and product good crystallinity, pattern are more uniform.
The present invention has reproducibility due to monoborane-tert-butylamine complex, under certain condition can be Sb3+It is reduced into Sb3-, Sb3-
With In3+Effect growth InSb nano wire then.
Compared with prior art, beneficial effects of the present invention is embodied in:
1, the present invention uses common presoma to be raw material, by solution be combined to have prepared good crystallinity, pattern more uniform,
The indium antimonide nano wire that diameter is little, it is not necessary to intermediate steps synthesizes, easy to operate.
2, it is different from traditional chemical gaseous phase synthetic method, the inventive method reaction condition is gentle, equipment is simple, growth cycle is short,
Crystal yield is high, can be used for large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is the XRD figure of embodiment 1 gained InSb nano wire, and as can be seen from the figure product is zincblende lattce structure InSb.
Fig. 2 is the transmission electron microscope photo of embodiment 1 gained InSb nano wire.
Fig. 3 is the high-resolution-ration transmission electric-lens photo of embodiment 1 gained InSb nano wire, and as can be seen from the figure gained InSb receives
Rice noodle has twin structure and crystallinity is good.
Fig. 4 is the SEAD figure of embodiment 1 gained InSb nano wire, as can be seen from the figure gained InSb nano wire
Grow along [111] direction.
Fig. 5 is the transmission electron microscope photo of embodiment 2 gained InSb nano wire.
Fig. 6 is the transmission electron microscope photo of embodiment 3 gained InSb nano wire.
Fig. 7 is the transmission electron microscope photo of embodiment 4 gained InSb nano wire.
Detailed description of the invention
By embodiment, the present invention is made the most concrete detailed description below in conjunction with the accompanying drawings, here it will be understood that these examples are only
For the present invention is described, it is not limiting as the present invention.
Embodiment 1:
The present embodiment synthesizes indium antimonide nano wire as follows:
Weigh 0.0206g Indium Tris acetylacetonate, 0.0176g antimony triphenyl joins in 1mL benzyl ether, ultrasonic makes it be completely dissolved,
Obtain mixed liquor A；0.121g cetylamine and 10mL octadecylene, ultrasonication under room temperature is added in 50mL three-neck flask
Make cetylamine be dissolved completely in octadecylene, obtain reaction medium；Mixed liquor A is carefully transferred to fill the 50mL of reaction medium
In three-neck flask, then pass to argon, under agitation reactant be heated to 120 DEG C, keep 45min go moisture removal and
Other lower boiling impurity, obtains mixed liquid B；During this period, by 0.5mL oleyl amine, 1.5mL tri octyl phosphine and 0.109g
Monoborane-tert-butylamine complex mixing, it is thus achieved that mixed liquor C；When three-neck flask is heated to 180 DEG C, mixed liquor C is quickly noted
Enter in three-neck flask, and keep 180 DEG C of reaction 60min.After reaction terminates, naturally cool to room temperature, the product that will obtain
With toluene and absolute ethanol washing repeatedly, i.e. obtain InSb nano wire, product is distributed in dehydrated alcohol standby.
Fig. 1 is the XRD figure of InSb nano wire obtained by the present embodiment, and as can be seen from the figure product is zincblende lattce structure InSb.
Fig. 2 is the transmission electron microscope photo of InSb nano wire obtained by the present embodiment, and as can be seen from the figure product is nano wire, shape
Looks are uniform.
Fig. 3 is the high-resolution-ration transmission electric-lens photo of InSb nano wire, as can be seen from the figure gained InSb obtained by the present embodiment
Nano wire has twin structure and crystallinity is good.
Fig. 4 is the SEAD figure of InSb nano wire, as can be seen from the figure gained InSb nanometer obtained by the present embodiment
Line grows along [111] direction.
Embodiment 2:
The present embodiment synthesizes indium antimonide nano wire as follows:
Weigh 0.0206g Indium Tris acetylacetonate, 0.0176g antimony triphenyl joins in 1mL benzyl ether, ultrasonic makes it be completely dissolved
Obtain mixed liquor A；0.0605g cetylamine and 10mL octadecylene, ultrasonication under room temperature is added in 50mL three-neck flask
Make cetylamine be dissolved completely in octadecylene, obtain reaction medium；Mixed liquor A is carefully transferred to fill the 50mL of reaction medium
In three-neck flask, then pass to argon, under agitation reactant be heated to 120 DEG C, keep 45min go moisture removal and
Other lower boiling impurity, obtains mixed liquid B；During this period, by 0.5mL oleyl amine, 1.5mL tri octyl phosphine and 0.109g
Monoborane-tert-butylamine complex mixing, it is thus achieved that mixed liquor C；When three-neck flask is heated to 180 DEG C, mixed liquor C is quickly noted
Enter in three-neck flask, and keep 180 DEG C of reaction 60min.After reaction terminates, naturally cool to room temperature, the product that will obtain
With toluene and absolute ethanol washing repeatedly, i.e. obtain InSb nano wire, product is distributed in dehydrated alcohol standby.
Fig. 5 is the transmission electron microscope photo of InSb nano wire obtained by the present embodiment, and as can be seen from the figure product is nano wire, shape
Looks are uniform.
Embodiment 3:
The present embodiment synthesizes indium antimonide nano wire as follows:
Weigh 0.0206g Indium Tris acetylacetonate, 0.0176g antimony triphenyl joins in 1mL benzyl ether, ultrasonic makes it be completely dissolved,
Obtain mixed liquor A；0.242g cetylamine and 10mL octadecylene, ultrasonication under room temperature is added in 50mL three-neck flask
Make cetylamine be dissolved completely in octadecylene, obtain reaction medium；And carefully transfer to fill the 50 of reaction medium by mixed liquor A
In mL three-neck flask, then pass to argon, under agitation reactant is heated to 120 DEG C, keep 45min to remove water
Divide and other lower boiling impurity, obtain mixed liquid B；During this period, by 0.5mL oleyl amine, 1.5mL tri octyl phosphine and 0.109
G monoborane-tert-butylamine complex mixing, it is thus achieved that mixed liquor C；When three-neck flask is heated to 180 DEG C, by quick for mixed liquor C
It is injected in three-neck flask, and keeps 180 DEG C of reaction 60min.After reaction terminates, naturally cool to room temperature, the product that will obtain
Thing toluene and absolute ethanol washing repeatedly, i.e. obtain InSb nano wire, are distributed to by product in dehydrated alcohol standby.
Fig. 6 is the transmission electron microscope photo of InSb nano wire obtained by the present embodiment, and as can be seen from the figure product is nano wire, shape
Looks are uniform.
Embodiment 4:
The present embodiment synthesizes indium antimonide nano wire as follows:
Weigh 0.0206g Indium Tris acetylacetonate, 0.0221g antimony triphenyl joins in 1mL benzyl ether, ultrasonic makes it be completely dissolved,
Obtain mixed liquor A；0.121g cetylamine and 10mL octadecylene, ultrasonication under room temperature is added in 50mL three-neck flask
Make cetylamine be dissolved completely in octadecylene, obtain reaction medium；Mixed liquor A is carefully transferred to fill the 50mL of reaction medium
In three-neck flask, then pass to argon, under agitation reactant be heated to 120 DEG C, keep 45min go moisture removal and
Other lower boiling impurity, obtains mixed liquid B；During this period, by 0.5mL oleyl amine, 1.5mL tri octyl phosphine and 0.109g
Monoborane-tert-butylamine complex mixing, it is thus achieved that mixed liquor C；When three-neck flask is heated to 180 DEG C, mixed liquor C is quickly noted
Enter in three-neck flask, and keep 180 DEG C of reaction 60min.After reaction terminates, naturally cool to room temperature, the product that will obtain
With toluene and absolute ethanol washing repeatedly, i.e. obtain InSb nano wire, product is distributed in dehydrated alcohol standby.
Fig. 7 is the transmission electron microscope photo of InSb nano wire obtained by the present embodiment, and as can be seen from the figure product is nano wire, shape
Looks are uniform.
Claims (7)
1. the Solution phase synthetic methods of an indium antimonide nano wire, it is characterised in that:
With indium source and antimony source as reaction raw materials, the reaction medium being made up of octadecylene and organic amine is heated to 100～120 DEG C,
Obtain mixed liquor；Described mixed liquor is warming up to 160～220 DEG C, adds the monoborane-tertiary fourth being dissolved in oleyl amine and tri octyl phosphine
Amine complex also reacts；After reaction terminates, with toluene and absolute ethanol washing product, centrifugation, obtain indium antimonide nano wire；
The mol ratio in described indium source and antimony source is 1～1.5:1；Described monoborane-tert-butylamine complex with the mol ratio in antimony source is
10～15:1.
2. the Solution phase synthetic methods of indium antimonide nano wire as claimed in claim 1, it is characterised in that carry out as follows:
Step 1: by proportioning, indium source and antimony source are dissolved in benzyl ether solvent, it is thus achieved that mixed liquor A；
Step 2: by octadecylene and organic amine mix homogeneously, constitutes reaction medium；Mixed liquor A step 1 obtained joins
In reaction medium, under inert gas shielding, it is heated to 100～120 DEG C, removes moisture and low boiling impurity, it is thus achieved that mixed liquid B；
Step 3: monoborane-tert-butylamine complex is dissolved in oleyl amine and tri octyl phosphine, it is thus achieved that mixed liquor C；
Step 4: mixed liquid B step 2 obtained is heated to 160～220 DEG C, the mixed liquor C then step 3 obtained is fast
Speed is injected in mixed liquid B, reacts 5～60min, naturally cools to room temperature；
Step 5: with toluene and absolute ethanol washing product, centrifugation, i.e. obtain indium antimonide nano wire.
3. the Solution phase synthetic methods of indium antimonide nano wire as claimed in claim 1 or 2, is characterised by: described indium source is selected from
One or more in Indium sesquioxide., Indium Tris acetylacetonate, Indium-111 chloride, indium nitrate or indium acetate.
4. the Solution phase synthetic methods of indium antimonide nano wire as claimed in claim 1 or 2, is characterised by: described antimony source is selected from
One or more in stibium oxide, antimony triphenyl, Butter of antimony. or antimony acetate.
5. the Solution phase synthetic methods of indium antimonide nano wire as claimed in claim 1 or 2, is characterised by: described organic amine selects
One or more in oleyl amine, 18-amine. or cetylamine.
6. the Solution phase synthetic methods of indium antimonide nano wire as claimed in claim 1 or 2, is characterised by: described organic amine with
The mol ratio in described indium source is 5～20:1；Described organic amine is 1～10:1 with the mol ratio of described octadecylene.
7. the Solution phase synthetic methods of indium antimonide nano wire as claimed in claim 1 or 2, is characterised by: described tri octyl phosphine
It is 1～4:1 with the volume ratio of described oleyl amine.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110143620A (en) * | 2019-07-01 | 2019-08-20 | 中国科学技术大学 | A kind of preparation method and nickel cobalt sulphur composite material of nickel cobalt sulphur nano material |
| CN113562763A (en) * | 2021-06-22 | 2021-10-29 | 中国科学技术大学 | Preparation method of InAs nano-particles and preparation method of photoelectric detector |
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| US6576291B2 (en) * | 2000-12-08 | 2003-06-10 | Massachusetts Institute Of Technology | Preparation of nanocrystallites |
| US20090007726A1 (en) * | 2004-11-01 | 2009-01-08 | Seiji Take | InSb NANOPARTICLE |
| CN102154705A (en) * | 2011-03-15 | 2011-08-17 | 上海大学 | Preparation method of indium antimonide nanocrystal |
| US20150147650A1 (en) * | 2013-11-28 | 2015-05-28 | Belenos Clean Power Holding Ag | Antimony based anode material for rechargeable batteries and preparation method |
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2016
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| US6576291B2 (en) * | 2000-12-08 | 2003-06-10 | Massachusetts Institute Of Technology | Preparation of nanocrystallites |
| US20090007726A1 (en) * | 2004-11-01 | 2009-01-08 | Seiji Take | InSb NANOPARTICLE |
| CN102154705A (en) * | 2011-03-15 | 2011-08-17 | 上海大学 | Preparation method of indium antimonide nanocrystal |
| US20150147650A1 (en) * | 2013-11-28 | 2015-05-28 | Belenos Clean Power Holding Ag | Antimony based anode material for rechargeable batteries and preparation method |
Non-Patent Citations (1)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110143620A (en) * | 2019-07-01 | 2019-08-20 | 中国科学技术大学 | A kind of preparation method and nickel cobalt sulphur composite material of nickel cobalt sulphur nano material |
| CN113562763A (en) * | 2021-06-22 | 2021-10-29 | 中国科学技术大学 | Preparation method of InAs nano-particles and preparation method of photoelectric detector |
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