CN106391054B - A kind of carbon nanotube/indium sulfide heterojunction nano-wire and preparation method thereof - Google Patents
A kind of carbon nanotube/indium sulfide heterojunction nano-wire and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of carbon nanotube/indium sulfide heterojunction nano-wires and preparation method thereof, the carbon nanotube/indium sulfide heterojunction nano-wire is made by the following method: (1) indium trichloride and thioacetamide are sequentially added into ethylene glycol, it is uniformly dispersed, indium trichloride/thioacetamide mixed solution is made；(2) ethylene glycol solution of carboxylic carbon nano-tube is added in indium trichloride/thioacetamide mixed solution made from step (1) again, obtains reaction precursor liquid；(3) reaction precursor liquid made from step (2) is placed in ultrasonic tank, ultrasonic reaction, products therefrom centrifugation, is dried to get carbon nanotube/indium sulfide heterojunction nano-wire is arrived washing.Compared with prior art, heterojunction nano-wire of the invention has excellent homogeneity, and preparation method is simple, securely and reliably, at low cost etc..
Description
Technical field
The present invention relates to the preparation technical fields of photochemical catalyst, more particularly, to a kind of carbon nanotube/indium sulfide hetero-junctions
Nano wire and preparation method thereof.
Background technique
Nowadays in the research field of new material, nano material be it is most dynamic, human social development is possessed very
The research object of great influence.The semiconductor materials such as nano-oxide and sulfide, due to its large specific surface area, unique structure,
Specific energy than it is big the advantages that, be suitable for applying electrode material in terms of.Recent domestic scholar research
And develop it is a series of have photoactive semiconductor material, and be applied to solar energy catalytic field research.
Indium trisulfide is very important one kind in metal sulfide material, have photoelectricity in visible-range,
The performances such as luminescence generated by light.Since visible light contains the nearly half of sunlight contained energy, so being studied compared to titanium dioxide etc.
Earlier to the catalyst of ultraviolet-sensitive, indium trisulfide significantly improves the utilization rate of sunlight.
And carbon nanotube belongs to the hot topic of recent researches, due to carbon atom p electronics constitute delocalized pi-bond and its solely
Special dimensional properties, so that it has good conductive property, it, will along with its outstanding mechanical property and chemical stability
Carbon nanotube and indium trisulfide are compounded to form hetero-junctions and are beneficial to the photoelectronic export of indium trisulfide and its stability
It is promoted.
Publication No. is that the Chinese patent application of CN103962156A discloses a kind of hydro-thermal reaction method preparation nanometer indium sulfide
Method.The preparation method is simple, easy to operate, has very high photocatalytic activity, can be effectively by CO2Reduction, acquisition
Product is relatively uniform.But the larger therefore opposite specific surface area of the Product size that this method obtains is smaller.Publication No. is
The Chinese patent application of CN102923761A discloses a kind of wet chemistry method synthesis silver/indium sulfide heterojunction structure nano material side
Method.Obtained silver is high with indium sulfide heterojunction nano-wire product purity, and structure novel has excellent electric conductivity and mechanical endurance.
Li et al. people discloses a kind of method (J.Mater.Chem., 2011,21,18398) that hydro-thermal method is prepared with the indium sulfide of carbon coating.
What this method obtained has the indium sulfide material of carbon coating to have because of the direct contact of indium sulfide and electrolyte that carbon coating prevents
Higher stability, while the conductivity of electrode is increased, reduce the risk for generating side reaction.And pass through mesoporous and carbon coating
Combination, buffer volumes change and improve electrode reaction invertibity on have advantageous performance.But this method passes through two step water
Thermal method, reaction temperature is higher, and preparation process is complicated.It is heterogeneous that Yang et al. discloses a kind of hydro-thermal method preparation carbon nanotube/indium sulfide
The method (J.Mater.Chem.A, 2014,2,1710) of junction nanowire.This method prepares carbon by the method that is heated at reflux compared with low temperature
Nanotube/indium sulfide heterojunction nano-wire improves the separation of photo-generated carrier, material light catalysis due to the addition of carbon nanotube
Performance significantly increases.But its process is relatively complicated, and prepare carbon nanotube/indium sulfide heterojunction nanometer material homogeneity compared with
Difference.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of carbon nanotube/vulcanizations
Indium heterojunction nano-wire and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of carbon nanotube/indium sulfide heterojunction nano-wire, the heterojunction nano-wire carbon nano-tube bundle, and cladding
The indium sulfide nanometer sheet of nanotube bundle.
Carbon nanotube/indium sulfide heterojunction nano-wire preparation method, comprising the following steps:
(1) indium trichloride and thioacetamide are sequentially added into ethylene glycol, are uniformly dispersed, obtained indium trichloride/thio
Acetamide mixed solution；
(2) carboxylic carbon nano-tube is added in indium trichloride/thioacetamide mixed solution made from step (1) again
Ethylene glycol solution obtains reaction precursor liquid；
(3) reaction precursor liquid made from step (2) is placed in ultrasonic tank, ultrasonic reaction, products therefrom centrifugation, washing,
It dries to get carbon nanotube/indium sulfide heterojunction nano-wire is arrived.
Preferably, the additional amount of indium trichloride is 0.01-1mol/L ethylene glycol, the addition of thioacetamide in step (1)
Amount is 0.02-2mol/L ethylene glycol.
Preferably, the ethylene glycol solution and indium trichloride/thioacetamide of carboxylic carbon nano-tube described in step (2)
The ratio between additional amount of mixed solution is 0.1-10mL/10mL.
Preferably, the concentration of the ethylene glycol solution of carboxylic carbon nano-tube described in step (2) is 0.05-0.15g/L.
Preferably, the temperature of ultrasonic reaction is 20~90 DEG C in step (3), and the time is 5min~for 24 hours.
Preferably, the power of ultrasonic reaction is 50-200W in step (3).
Basic principle of the invention is to mix carboxylic carbon nano-tube with the reaction reagent of indium sulfide, at ultrasound
Reason, obtains uniform carbon nanotube/indium sulfide heterojunction nanometer material by ultrasonic reaction method.Two be ultrasonically treated in this method
Big effect are as follows: 1, promote carboxylated in the solution evenly dispersed；2, thermally decompose thioacetamide, the sulphion and indium of generation
Ions binding forms indium sulfide.
Fundamental reaction principle of the invention is under the acoustic cavitation effect of ultrasound, and ethylene glycol generates hydroperoxyl radical, and thio
Acetamide reacts to obtain hydrogen sulfide, reacts to obtain indium sulfide afterwards with indium ion, attached using the carbon nano-tube bundle dispersed in solution as core
Formation heterojunction nano-wire.It is summarized as following reaction equation.
(CH2OH)2→2H·+(CH2O·)2
RS+2H·→R·+H2S (R=CH3CSNH2)
2In3++3H2S→In2S3+6H+
When thioacetamide and inidum chloride relative concentration are higher in the present invention, indium sulfide product is more, is coated on carbon completely
On nanotube bundle, gained nanowire size is larger, and is easy to reunite so more difficult observe heterojunction structure.Carbon nanotube is opposite
When concentration is higher, obtained nanometer vulcanization indium sheet is relatively fewer, is in that small group is attached to and receives because of the homogenization of ultrasound condition
On mitron beam.When shorter between when reacted, react insufficient, gained indium sulfide amount is insufficient, thus is attached to nanotube in small group
Shu Shang, when reacted between it is sufficient when, obtain ideal heterojunction nano-wire.When reaction temperature is lower, have in product with In3+For
It is main.When the more high or ultra acoustical power of temperature is larger, reaction speed is relatively fast.
Obtained in the present invention using carbon nano-tube bundle as core, indium sulfide nanometer sheet be shell heterojunction structure photocatalysis lead
The advantages of domain, is that indium sulfide possesses the performances such as photoelectricity, luminescence generated by light in visible-range.Since visible light contains the sun
The nearly half of light contained energy, so compared to researchs such as titanium dioxide earlier to the catalyst of ultraviolet-sensitive, it is trisulfides
Two indiums significantly improve the utilization rate of sunlight.And carbon nanotube possesses good electric conductivity, is formed with indium sulfide nanometer sheet
The photoelectronic export for being conducive to indium sulfide generation after heterojunction structure, to improve its photo-catalysis capability.
Compared with prior art, the invention has the following advantages that
1), carbon nanotube/indium sulfide heterojunction nano-wire that present invention production obtains is the vulcanization using carbon nano-tube bundle as core
Indium nanometer sheet is the heterojunction structure of shell, and has excellent homogeneity；Preparation process is simple, yield is higher and cost is relatively low,
It is able to satisfy the demand of large-scale production.
2) after, the present invention is mixed by organic solvent, product can be obtained by ultrasonic treatment, raw material is simple, and product is pure
It spends higher.
Detailed description of the invention
Fig. 1 is carbon nanotube/indium sulfide heterojunction nanometer material relatively low magnification TEM figure in the present invention；
Fig. 2 is carbon nanotube/indium sulfide heterojunction nanometer material higher magnification TEM figure in the present invention；
Fig. 3 is carbon nanotube/indium sulfide heterojunction nanometer material XRD diagram in the present invention.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
A kind of supersonically preparation method of carbon nanotube/indium sulfide heterojunction nano-wire, comprises the following steps:
(1) 1L ethylene glycol is dispersed for 0.1g carboxylic carbon nano-tube by ultrasonic treatment and obtains carbon nanotube suspension；
(2) 2.212g indium trichloride is dissolved in 10mL ethylene glycol simultaneously ultrasonic dissolution, then adds the thio second of 1.526g
Amide is simultaneously uniformly dispersed；
(3) carbon nanotube suspension that 0.1mL disperses in advance is added dropwise and obtains reaction precursor liquid in mixed liquor；
(4) reaction vessel equipped with precursor liquid is placed in ultrasonic tank at 20 DEG C and 2h is ultrasonically treated with 50W power, will produced
Drying powder obtained is pure uniform carbon nanotube/indium sulfide hetero-junctions nanometer after object is cleaned through centrifugation and repeatedly
Line.
The carbon nanotube that the present embodiment obtains/indium sulfide heterojunction nano-wire, due to the more and carbon nanometer of sulphur source indium source amount
Pipe content is less, and obtained carbon nanotube/indium sulfide heterojunction nano-wire is that indium sulfide is coated on carbon nano-tube bundle completely, compared with
Difficulty observes heterojunction structure.
Embodiment 2
A kind of supersonically preparation method of carbon nanotube/indium sulfide heterojunction nano-wire, comprises the following steps:
(1) 1L ethylene glycol is dispersed for 0.1g carboxylic carbon nano-tube by ultrasonic treatment and obtains carbon nanotube suspension；
(2) 0.022g indium trichloride is dissolved in 10mL carbon nanotube suspension, it is thio to add 0.015g for ultrasonic dissolution
Acetamide dissolution, obtains mixed solution；
(3) carbon nanotube suspension that 10mL disperses in advance is added dropwise and obtains reaction precursor liquid in mixed solution；
(4) reaction vessel equipped with precursor liquid is placed in ultrasonic tank at 90 DEG C and 4h is ultrasonically treated with 200W power, it will
Drying powder obtained is pure uniform carbon nanotube/indium sulfide hetero-junctions nanometer after product is cleaned through centrifugation and repeatedly
Line.
The carbon nanotube that the present embodiment obtains/indium sulfide heterojunction nano-wire is obtained since content of carbon nanotubes is more
Nanometer vulcanization indium sheet is attached on nanotube bundle in small group.
Embodiment 3
A kind of supersonically preparation method of carbon nanotube/indium sulfide heterojunction nano-wire, comprises the following steps:
(1) 1L ethylene glycol is dispersed for 0.1g carboxylic carbon nano-tube by ultrasonic treatment and obtains carbon nanotube suspension；
(2) 1.106g indium trichloride is dissolved in 8mL ethylene glycol simultaneously ultrasonic dissolution, then adds 0.752g thioacetyl
Amine is simultaneously uniformly dispersed；
(3) carbon nanotube suspension that 2mL disperses in advance is added dropwise and obtains reaction precursor liquid in mixed liquor；
(4) reaction vessel equipped with precursor liquid is placed in ultrasonic tank at 40 DEG C and 8h is ultrasonically treated with 100W, by product
Through centrifugation and repeatedly after cleaning, dry powder obtained is pure uniform carbon nanotube/indium sulfide heterojunction nano-wire.
The carbon nanotube that the present embodiment obtains/indium sulfide heterojunction nano-wire is more uniform, and Fig. 1~2 give according to reality
Apply carbon nanotube/indium sulfide heterojunction nano-wire TEM figure that example 3 obtains.As shown in Figure 1, this embodiment products therefrom pattern,
Waiting for size is more uniform, and core-shell structure is complete.Product housing diameter is in 200nm or so (Fig. 2), In2S3Agglomerate is adhered in the form of sheets
In on carbon nano-tube bundle, opposite specific surface area is larger., Fig. 3 is that carbon nanotube/indium sulfide hetero-junctions made from the present embodiment is received
The XRD diagram of rice noodles, it can be seen that existing three diffraction peaks respectively correspond In2S3(113) (116) (300) three crystal faces.
Embodiment 4
A kind of supersonically preparation method of carbon nanotube/indium sulfide heterojunction nano-wire, comprises the following steps:
(1) 1L ethylene glycol is dispersed for 0.1g carboxylic carbon nano-tube by ultrasonic treatment and obtains carbon nanotube suspension；
(2) 1.106g indium trichloride is dissolved in 8mL ethylene glycol simultaneously ultrasonic dissolution, then adds 0.751g thioacetyl
Amine dissolution；
(3) carbon nanotube suspension that 2mL disperses in advance is added dropwise and obtains reaction precursor liquid in mixed liquor；
(4) reaction vessel equipped with precursor liquid is placed in ultrasonic tank at 40 DEG C and 5min is ultrasonically treated with 100W power,
Dry powder obtained is that pure uniform carbon nanotube/indium sulfide hetero-junctions is received after product is cleaned through centrifugation and repeatedly
Rice noodles.
Since the reaction time is shorter, reaction does not carry out the present embodiment completely, and obtained product is the lesser nano-sulfur of size
Change the heterojunction nano-wire of indium sheet and carbon nano-tube bundle composition.
Embodiment 5
A kind of supersonically preparation method of carbon nanotube/indium sulfide heterojunction nano-wire, comprises the following steps:
(1) 1L ethylene glycol is dispersed for 0.1g carboxylic carbon nano-tube by ultrasonic treatment and obtains carbon nanotube suspension；
(2) 1.106g indium trichloride is dissolved in 9mL ethylene glycol simultaneously ultrasonic dissolution, then adds 0.752g thioacetyl
Amine dissolution；
(4) carbon nanotube suspension that 1mL disperses in advance is added dropwise and obtains reaction precursor liquid in mixed liquor；
(5) reaction vessel equipped with precursor liquid is placed in ultrasonic tank at 40 DEG C with 100W power ultrasonic treatment for 24 hours, it will
Drying powder obtained is pure uniform carbon nanotube/indium sulfide hetero-junctions nanometer after product is cleaned through centrifugation and repeatedly
Line.
For the present embodiment due to reaction time abundance, obtained carbon nanotube/indium sulfide heterojunction nano-wire is more uniform.
Embodiment 6
A kind of supersonically preparation method of carbon nanotube/indium sulfide heterojunction nano-wire, comprises the following steps:
(1) 1L ethylene glycol is dispersed for 0.15g carboxylic carbon nano-tube by ultrasonic treatment and obtains carbon nanotube suspension；
(2) 1.106g indium trichloride is dissolved in 8mL ethylene glycol simultaneously ultrasonic dissolution, then adds 0.752g thioacetyl
Amine is simultaneously uniformly dispersed；
(3) carbon nanotube suspension that 2mL disperses in advance is added dropwise and obtains reaction precursor liquid in mixed liquor；
(4) reaction vessel equipped with precursor liquid is placed in ultrasonic tank at 40 DEG C and 8h is ultrasonically treated with 100W, by product
Through centrifugation and repeatedly after cleaning, dry powder obtained is pure uniform carbon nanotube/indium sulfide heterojunction nano-wire.
Embodiment 7
A kind of supersonically preparation method of carbon nanotube/indium sulfide heterojunction nano-wire, comprises the following steps:
(1) 1L ethylene glycol is dispersed for 0.05g carboxylic carbon nano-tube by ultrasonic treatment and obtains carbon nanotube suspension；
(2) 1.106g indium trichloride is dissolved in 8mL ethylene glycol simultaneously ultrasonic dissolution, then adds 0.752g thioacetyl
Amine is simultaneously uniformly dispersed；
(3) carbon nanotube suspension that 2mL disperses in advance is added dropwise and obtains reaction precursor liquid in mixed liquor；
(4) reaction vessel equipped with precursor liquid is placed in ultrasonic tank at 40 DEG C and 8h is ultrasonically treated with 100W, by product
Through centrifugation and repeatedly after cleaning, dry powder obtained is pure uniform carbon nanotube/indium sulfide heterojunction nano-wire.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention
Within protection scope.
Claims (2)
1. a kind of carbon nanotube/indium sulfide heterojunction nano-wire preparation method, which is characterized in that the heterojunction nano-wire
Carbon nano-tube bundle, and the indium sulfide nanometer sheet of cladding nanotube bundle；
The preparation method comprises the following steps:
(1) indium trichloride and thioacetamide are sequentially added into ethylene glycol, is uniformly dispersed, and indium trichloride/thioacetyl is made
Amine mixed solution；
(2) second two of carboxylic carbon nano-tube is added in indium trichloride/thioacetamide mixed solution made from step (1) again
Alcoholic solution obtains reaction precursor liquid；
(3) reaction precursor liquid made from step (2) is placed in ultrasonic tank, ultrasonic reaction, products therefrom centrifugation, washing, drying,
Obtain carbon nanotube/indium sulfide heterojunction nano-wire；
The additional amount of indium trichloride is 0.01-1mol/L ethylene glycol in step (1), and the additional amount of thioacetamide is 0.02-
2mol/L ethylene glycol；
Ethylene glycol solution and indium trichloride/thioacetamide mixed solution of carboxylic carbon nano-tube described in step (2)
The ratio between additional amount is 0.1-10mL/10mL；
The concentration of the ethylene glycol solution of carboxylic carbon nano-tube described in step (2) is 0.05-0.15g/L；
The temperature of ultrasonic reaction is 20~90 DEG C in step (3), and the time is 5min~for 24 hours.
2. a kind of preparation method of carbon nanotube/indium sulfide heterojunction nano-wire according to claim 1, feature exist
In the power of ultrasonic reaction is 50-200W in step (3).
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| CN101293645A (en) * | 2008-06-06 | 2008-10-29 | 东华大学 | A kind of preparation method of indium tin oxide assembled carbon nanotube composite material |
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