CN109761280A - A kind of molybdenum trioxide superfine nanowire of size adjustable and preparation method thereof - Google Patents
A kind of molybdenum trioxide superfine nanowire of size adjustable and preparation method thereof Download PDFInfo
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- CN109761280A CN109761280A CN201910243921.3A CN201910243921A CN109761280A CN 109761280 A CN109761280 A CN 109761280A CN 201910243921 A CN201910243921 A CN 201910243921A CN 109761280 A CN109761280 A CN 109761280A
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Abstract
The application belongs to the technical field of optical electro-chemistry more particularly to a kind of molybdenum trioxide superfine nanowire of size adjustable and preparation method thereof.The invention discloses a kind of preparation methods of the molybdenum trioxide superfine nanowire of size adjustable, comprising the following steps: step 1 closes molybdate solution and acid-mixed, and precipitate molybdic acid is then obtained by filtration；Step 2 mixes the precipitate molybdic acid, strong acid and surfactant, carries out solvent thermal reaction, obtains the molybdenum trioxide superfine nanowire of size adjustable.The molybdenum trioxide superfine nanowire of size adjustable provided by the present application, can solve traditional MoO3It the size dimension of nanometer rods and is unevenly distributed, the technological deficiency low as the conversion ratio and selectivity of photochemical catalyst.Disclosed herein as well is a kind of molybdenum trioxide superfine nanowires of size adjustable, can fill up the vacancy of the preparation method of current molybdenum trioxide nano-wire.
Description
Technical field
The application belongs to the technical field of optical electro-chemistry more particularly to a kind of molybdenum trioxide superfine nanowire of size adjustable
And preparation method thereof.
Background technique
Due to becoming increasingly conspicuous for fossil energy shortage and CO2 emission problem, finding clean renewable energy becomes
Whole world problem in the urgent need to address.Photocatalitic Technique of Semiconductor be nowadays society solve energy crisis it is important have before
One of the approach on way.Due to its unique structure and excellent optical property, molybdenum trioxide has wide in industrial application
Application prospect, as gas sensor, photochromic and electrochromic device, display material, energy storage material and as sewage at
The catalyst etc. of reason and air cleaning.Molybdenum trioxide (MoO3) it is the solar battery anode layer material highly studied, because
It is it with the transparency high in good hole mobility, good environmental stability and visible-range.Currently, three oxidations
Prepared by the mode that molybdenum anode buffer layer generallys use vacuum evaporation, the efficiency of polymer solar cell device and steady can be improved
It is qualitative, but be not suitable for large area production.
But molybdenum trioxide nano material only has molybdenum trioxide nanorod, traditional MoO at present3Although nanometer rods can be with
Improve the thermocatalytic effect of light, but low output, nanometer rods size dimension and distribution and uneven, and as photochemical catalyst
Conversion ratio and selectivity be not high.In conclusion developing, a kind of preparation method is simple, the molybdenum trioxide that yield is high, at low cost
The preparation method of nano wire is those skilled in the art's technical problem urgently to be resolved.
Related ultra-fine MoO3The synthesis report of nano wire is less, and experimentation of the present invention is simple, easily operated, synthesized
Ultra-fine MoO3Nano wire good dispersion, the uniformity is high, has potential application prospect in optical electro-chemistry field.
Apply for content
In view of this, there is provided a kind of molybdenum trioxide superfine nanowire of size adjustable, energy for first purpose of the application
Solve traditional MoO3It the size dimension of nanometer rods and is unevenly distributed, and MoO3The uncontrollable technology of the size of nanometer rods lacks
It falls into.
Second purpose of the application is to disclose a kind of preparation method of the molybdenum trioxide superfine nanowire of size adjustable, energy
Fill up the vacancy of the preparation method of the molybdenum trioxide nano-wire of current size adjustable.
The invention discloses a kind of preparation methods of the molybdenum trioxide superfine nanowire of size adjustable, comprising the following steps:
Step 1 closes 100~1500mg molybdate solution and acid-mixed, and precipitate molybdic acid is then obtained by filtration；
Step 2 mixes the precipitate molybdic acid, 0.5~10mL strong acid and surfactant, carries out solvent thermal reaction, obtains
To the molybdenum trioxide superfine nanowire of size adjustable.
Preferably, the molybdate solution is made in step 1 for ultrasonic disperse after molybdate and water mixing.
Specifically, the molybdate solution is that molybdate ultrasonic disperse soluble in water obtains.
More preferably, the water is deionized water.
More preferably, the molybdate solution is made in step 1 for ultrasonic disperse 30min after molybdate and water mixing.
Preferably, in step 1, the acid selected from sulfuric acid, hydrochloric acid, nitric acid, perchloric acid, formic acid, acetic acid, propionic acid, butyric acid,
One of valeric acid, caproic acid, enanthic acid and octanoic acid are a variety of.
Preferably, the molar ratio of the molybdate of the molybdate solution and the acid is (2.5-6): 1 in step 1.
Preferably, the strong acid is selected from sulfuric acid, hydrochloric acid, nitric acid, perchloric acid, formic acid, acetic acid, propionic acid, fourth in step 2
One of acid, valeric acid, caproic acid, enanthic acid and octanoic acid are a variety of.
Preferably, the polymeric surfactant is selected from polyvinylpyrrolidone, cetyl front three in step 3
One of base ammonium bromide, polypropylene ammonia, polyacrylic acid, oleic acid and dibutyl sebacate are a variety of.
More preferably, including: in step 2
Step 1: the precipitate molybdic acid is mixed with strong acid, molybdic acid mixture is obtained；
Step 2: the molybdic acid mixture is mixed with polymeric surfactant, solvent thermal reaction is then carried out, is obtained
The molybdenum trioxide superfine nanowire of size adjustable.
Wherein, in step 1, the precipitate molybdic acid mixes the specially precipitate molybdic acid and strong acid ultrasonic disperse with strong acid
1h mixing；The molybdic acid mixture mixes specially ultrasonic disperse 1h mixing with polymeric surfactant.
Preferably, the molar ratio of the strong acid and the molybdate is (2.5-6): 1 in step 2；In step 3, institute
The molar ratio for stating polymeric surfactant and the molybdate is (2-10): 1.
Preferably, the range of reaction temperature of the solvent thermal reaction is 120 DEG C~200 DEG C in step 4；The solvent
The reaction time of thermal response be 16~for 24 hours.
Specifically, it is that the mixture is placed in polytetrafluoroethylene (PTFE) high pressure that the mixture, which carries out solvent thermal reaction, in step 4
In reaction kettle, it is then placed into baking oven and carries out solvent thermal reaction.
The present invention also provides a kind of molybdenum trioxide superfine nanowires of size adjustable, are made including the preparation method
Size adjustable molybdenum trioxide superfine nanowire.
Preferably, the cross-sectional diameter range of the molybdenum trioxide superfine nanowire of the size adjustable is 0.1~3nm.
More preferably, the preparation method of the molybdenum trioxide superfine nanowire of size adjustable of the invention further include: step 5,
After the molybdenum trioxide superfine nanowire for the size adjustable that step 2 obtains is cooled to room temperature, using alcoholic solution by size adjustable
The washing of molybdenum trioxide superfine nanowire.
More preferably, the alcoholic solution is selected from acetone or/and ethyl alcohol.
Specifically, the molybdenum trioxide superfine nanowire of size adjustable of the invention is placed in ethyl alcohol and saves.
It is a discovery of the invention that its conversion ratio and selectivity as photochemical catalyst, three oxygen can be improved in molybdenum trioxide nano-wire
Change molybdenum nano wire is a kind of one-dimentional structure for having and being horizontally limited in 100 nanometers or less (longitudinal there is no limit).Three oxygen
Changing molybdenum nano wire can gather naturally sunlight in a very small region in crystal, and light gathering is common intensity of illumination
15 times.Since the diameter of molybdenum trioxide nano-wire crystal is less than the wavelength of incident sunlight, molybdenum trioxide nano can be caused
The resonance of line crystals and surrounding light intensity.In photocatalysis cyclohexane oxidation, molybdenum trioxide nano-wire is than common nanometer rods
With higher conversion ratio and selectivity, to improve photo-thermal catalytic efficiency.Therefore, the invention provides a kind of ruler
Very little adjustable molybdenum trioxide superfine nanowire, the diameter range of the cross section of nano wire of the invention reach Nano grade.Meanwhile
The preparation method very simple of the molybdenum trioxide superfine nanowire of size adjustable provided by the invention, passes through one-step synthesis method first
Then precipitate molybdic acid prepares size adjustable by the solvent thermal reaction of precipitate molybdic acid and strong acid and polymeric surfactant
Molybdenum trioxide superfine nanowire, wherein the synthesis of precipitate molybdic acid and inventive point of the invention, precipitate molybdic acid and size adjustable
The preparation method of molybdenum trioxide superfine nanowire is simple, high without using expensive instrument yield, at low cost.Three be prepared
The dispersibility of molybdenum oxide nanowires is high, and the diameter of the cross section of molybdenum trioxide nano-wire is nanoscale.
Detailed description of the invention
In order to illustrate the technical solutions in the embodiments of the present application or in the prior art more clearly, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described.
Fig. 1 shows the TEM figure for the molybdenum trioxide nano-wire that embodiment 1 provided by the present application is prepared；
Fig. 2 shows the TEM figure for the molybdenum trioxide nano-wire that embodiment 2 provided by the present application is prepared；
Fig. 3 shows the TEM figure for the molybdenum trioxide nano-wire that embodiment 3 provided by the present application is prepared；
Fig. 4 shows the TEM figure for the molybdenum trioxide nano-wire that embodiment 4 provided by the present application is prepared.
Specific embodiment
This application provides molybdenum trioxide superfine nanowires of a kind of size adjustable and preparation method thereof, on the one hand for solving
Certainly traditional MoO3It the size dimension of nanometer rods and is unevenly distributed, and MoO3The uncontrollable technology of the size of nanometer rods lacks
It falls into, another party can fill up the vacancy of the preparation method of the molybdenum trioxide nano-wire of current size adjustable.
Below by the technical scheme in the embodiment of the application is clearly and completely described, it is clear that described implementation
Example is merely a part but not all of the embodiments of the present application.Based on the embodiment in the application, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model of the application protection
It encloses.
Wherein, it is commercially available or self-control that following embodiment is raw materials used.
Embodiment 1
Present embodiments provide the specific embodiment of the first molybdenum trioxide nano-wire preparation method:
1, the molybdate for weighing 100mg is dissolved in 15mL deionized water and disperses 30min with ultrasonic wave, and it is molten to obtain molybdate
Liquid；By molybdate solution and 3mL mixed in hydrochloric acid, mixture 1 is obtained；
2, mixture 1 is filtered, obtains wet precipitate molybdic acid；
3,0.5mL formic acid is added in the precipitate molybdic acid of step 2, ultrasonic wave disperses 1h, obtains molybdic acid mixture；
4, into scattered molybdic acid mixture, the polyvinylpyrrolidone of 1g is added, continues ultrasonic wave and disperses 1h, obtain
Mixture 2；
5, mixture 2 is transferred in the polytetrafluoroethylene (PTFE) autoclave of 50mL, is placed in baking oven, with 180 DEG C
Temperature solvents thermal response for 24 hours, obtains molybdenum trioxide nano-wire；
6, it after the reaction was completed, molybdenum trioxide nano-wire cooled to room temperature and is transferred in centrifuge tube, with acetone and second
Alcohol repeatedly washs.
7,20mL ethyl alcohol is added to save.
8, TEM detection and diameter measurement are carried out to the molybdenum trioxide nano-wire that the present embodiment is prepared, as a result such as Fig. 1
Shown, the diameter of the cross section of the molybdenum trioxide nano-wire of the present embodiment is 0.2nm.
Embodiment 2
Present embodiments provide the specific embodiment of second of molybdenum trioxide nano-wire preparation method:
1, the molybdate for weighing 500mg is dissolved in 20mL deionized water and disperses 30min with ultrasonic wave, and it is molten to obtain molybdate
Liquid；By molybdate solution and 3mL mixed in hydrochloric acid, mixture 1 is obtained；
2, mixture 1 is filtered, obtains wet precipitate molybdic acid；
3,3mL octanoic acid is added in the precipitate molybdic acid of step 2, ultrasonic wave disperses 1h, obtains molybdic acid mixture；
4, into scattered molybdic acid mixture, the cetyl trimethylammonium bromide of 2g is added, continues ultrasonic wave dispersion
1h obtains mixture 2；
5, mixture 2 is transferred in the polytetrafluoroethylene (PTFE) autoclave of 50mL, is placed in baking oven, with 180 DEG C
Temperature solvents thermal response for 24 hours, obtains molybdenum trioxide nano-wire；
6, it after the reaction was completed, molybdenum trioxide nano-wire cooled to room temperature and is transferred in centrifuge tube, with acetone and second
Alcohol repeatedly washs.
7,20mL ethyl alcohol is added to save.
8, TEM detection and diameter measurement are carried out to the molybdenum trioxide nano-wire that the present embodiment is prepared, as a result such as Fig. 2
Shown, Fig. 2 shows the good dispersion of the molybdenum trioxide nano-wire of the present embodiment, and the uniformity is high, molybdenum trioxide nano-wire it is transversal
The diameter in face is 0.8nm.
Embodiment 3
Present embodiments provide the specific embodiment of the third molybdenum trioxide nano-wire preparation method:
1, the molybdate for weighing 800mg is dissolved in 25mL deionized water and disperses 30min with ultrasonic wave, and it is molten to obtain molybdate
Liquid；By molybdate solution and 3mL mixed in hydrochloric acid, mixture 1 is obtained；
2, mixture 1 is filtered, obtains wet precipitate molybdic acid；
3,4mL hydrochloric acid is added in the precipitate molybdic acid of step 2, ultrasonic wave disperses 1h, obtains molybdic acid mixture；
4, into scattered molybdic acid mixture, the polypropylene ammonia of 0.5g is added, continues ultrasonic wave and disperses 1h, mixed
Object 2；
5, mixture 2 is transferred in the polytetrafluoroethylene (PTFE) autoclave of 50mL, is placed in baking oven, with 180 DEG C
Temperature solvents thermal response for 24 hours, obtains molybdenum trioxide nano-wire；
6, it after the reaction was completed, molybdenum trioxide nano-wire cooled to room temperature and is transferred in centrifuge tube, with acetone and second
Alcohol repeatedly washs.
7,20mL ethyl alcohol is added to save.
8, TEM detection and diameter measurement are carried out to the molybdenum trioxide nano-wire that the present embodiment is prepared, as a result such as Fig. 3
Shown, Fig. 3 shows the good dispersion of the molybdenum trioxide nano-wire of the present embodiment, and the uniformity is high, molybdenum trioxide nano-wire it is transversal
The diameter in face is 2nm.
Embodiment 4
Present embodiments provide the specific embodiment of the 4th kind of molybdenum trioxide nano-wire preparation method:
1, the molybdate for weighing 1500mg is dissolved in 30mL deionized water and disperses 30min with ultrasonic wave, and it is molten to obtain molybdate
Liquid；By molybdate solution and 3mL mixed in hydrochloric acid, mixture 1 is obtained；
2, mixture 1 is filtered, obtains wet precipitate molybdic acid；
3,10mL sulfuric acid is added in the precipitate molybdic acid of step 2, ultrasonic wave disperses 1h, obtains molybdic acid mixture；
4, into scattered molybdic acid mixture, the polyacrylic acid of 2g is added, continues ultrasonic wave and disperses 1h, obtain mixture
2；
5, mixture 2 is transferred in the polytetrafluoroethylene (PTFE) autoclave of 50mL, is placed in baking oven, with 180 DEG C
Temperature solvents thermal response for 24 hours, obtains molybdenum trioxide nano-wire；
6, it after the reaction was completed, molybdenum trioxide nano-wire cooled to room temperature and is transferred in centrifuge tube, with acetone and second
Alcohol repeatedly washs.
7,20mL ethyl alcohol is added to save.
8, TEM detection and diameter measurement are carried out to the molybdenum trioxide nano-wire that the present embodiment is prepared, as a result such as Fig. 4
Shown, Fig. 4 shows the good dispersion of the molybdenum trioxide nano-wire of the present embodiment, and the uniformity is high, molybdenum trioxide nano-wire it is transversal
The diameter in face is 3nm.
The above is only the preferred embodiment of the application, it is noted that for the ordinary skill people of the art
For member, under the premise of not departing from the application principle, several improvements and modifications can also be made, these improvements and modifications are also answered
It is considered as the protection scope of the application.
Claims (10)
1. a kind of preparation method of the molybdenum trioxide superfine nanowire of size adjustable, which comprises the following steps:
Step 1 closes 100~1500mg molybdate solution and acid-mixed, and precipitate molybdic acid is then obtained by filtration；
Step 2 mixes the precipitate molybdic acid, 0.5~10mL strong acid and polymeric surfactant, carries out solvent thermal reaction,
Obtain the molybdenum trioxide superfine nanowire of size adjustable.
2. preparation method according to claim 1, which is characterized in that in step 1, the molybdate solution be molybdate and
Ultrasonic disperse is made after water mixing.
3. preparation method according to claim 1, which is characterized in that in step 1, the acid is selected from sulfuric acid, hydrochloric acid, nitre
One of acid, perchloric acid, formic acid, acetic acid, propionic acid, butyric acid, valeric acid, caproic acid, enanthic acid and octanoic acid are a variety of.
4. preparation method according to claim 1, which is characterized in that in step 1, the molybdate of the molybdate solution with
The molar ratio of the acid is (2.5-6): 1.
5. preparation method according to claim 1, which is characterized in that in step 2, the strong acid is selected from sulfuric acid, hydrochloric acid, nitre
One of acid, perchloric acid, formic acid, acetic acid, propionic acid, butyric acid, valeric acid, caproic acid, enanthic acid and octanoic acid are a variety of.
6. preparation method according to claim 1, which is characterized in that in step 3, the polymeric surfactant is selected from
In polyvinylpyrrolidone, cetyl trimethylammonium bromide, polypropylene ammonia, polyacrylic acid, oleic acid and dibutyl sebacate
It is one or more.
7. preparation method according to claim 1, which is characterized in that in step 2, the strong acid and the molybdate
Molar ratio is (2.5-6): 1；In step 3, the molar ratio of the polymeric surfactant and the molybdate is (2-10): 1.
8. preparation method according to claim 1, which is characterized in that in step 4, the reaction temperature of the solvent thermal reaction
Range is 120 DEG C~200 DEG C；The reaction time of the solvent thermal reaction be 16~for 24 hours.
9. a kind of molybdenum trioxide superfine nanowire of size adjustable, which is characterized in that including such as claim 1-8 any one institute
The molybdenum trioxide superfine nanowire of size adjustable made from the preparation method stated.
10. the molybdenum trioxide superfine nanowire of size adjustable according to claim 9, the molybdenum trioxide of the size adjustable
The cross-sectional diameter range of superfine nanowire is 0.1~3nm.
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| CN112978798A (en) * | 2021-02-02 | 2021-06-18 | 昆明理工大学 | Method and device for preparing molybdenum oxide nano material with adjustable phase, shape and size |
| CN114702072A (en) * | 2021-12-08 | 2022-07-05 | 昆明理工大学 | Method for preparing molybdenum trioxide nanowire by sol-gel method |
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| CN114702072A (en) * | 2021-12-08 | 2022-07-05 | 昆明理工大学 | Method for preparing molybdenum trioxide nanowire by sol-gel method |
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