CN106976910A - A kind of porous carbon load molybdenum oxide nanoparticles composite and preparation method thereof - Google Patents
A kind of porous carbon load molybdenum oxide nanoparticles composite and preparation method thereof Download PDFInfo
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- CN106976910A CN106976910A CN201710223243.5A CN201710223243A CN106976910A CN 106976910 A CN106976910 A CN 106976910A CN 201710223243 A CN201710223243 A CN 201710223243A CN 106976910 A CN106976910 A CN 106976910A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a kind of porous carbon load molybdenum oxide nanoparticles composite and preparation method thereof.The preparation method, comprises the following steps：(1) porous carbon adsorption molybdate is utilized, predecessor is obtained；(2) predecessor is heat-treated in hydrogen argon atmospher, you can obtain the porous carbon load molybdenum oxide nanoparticles composite.The present invention is that the space confinement effect based on porous carbon prepares porous carbon load molybdenum oxide nanoparticles composite; relative to other methods; this method cost is low, technique is simple, product is clear and definite and the particle size of gained molybdenum oxide nanoparticles is homogeneous, high degree of dispersion, soilless sticking, suitable for large-scale production；Porous carbon load molybdenum oxide nanoparticles composite of the present invention has huge potential using value in Industrial Catalysis, electrochemistry or other scientific domains.
Description
Technical field
Answered the invention belongs to technical field of nanometer material preparation, more particularly to a kind of porous carbon load molybdenum oxide nanoparticles
Condensation material and preparation method thereof.
Background technology
When the size of material drops to several nanometer scales, it may appear that it is new different from the sound of block materials, light, electricity,
Magnetic, power, hot property, therefore, nano material (particle, line, rod, pipe, piece, flower, ball etc.) is in fundamental research and potential application
Technically play an important roll.Wherein, zero dimension transition metal oxide nano-material is because with special optics, magnetics and electricity
Characteristic becomes current study hotspot.Most stable and most study for molybdenum oxide in molybdenum oxide, they can show excellent
Different optics, catalysis, electric property etc., thus in catalyst, sensor, flat-panel monitor and silicon science and technology and lithium battery
The fields such as pole have broad application prospects.As can be seen that for the preparation method and its performance of zero dimension molybdenum oxide nano material
Research either from it is theoretical or in terms of practical application it is all significant.
Being usually used in preparing the method for molybdenum oxide nanoparticles at present has hydro-thermal method, vapour deposition process, template etc..But these
The shortcomings of molybdenum oxide nanoparticles size that method generally existing yields poorly and prepared is uneven.
The content of the invention
, should it is an object of the invention to provide a kind of porous carbon load molybdenum oxide nanoparticles composite and preparation method thereof
Method prepares molybdenum oxide nanoparticles using the flourishing porous carbon space confinement effect in cheap and space, and what is prepared is compound
In material, molybdenum oxide nanoparticles good dispersion degree, size on porous carbon is small, stability is high, and preparation technology is simple, green ring
Protect, with can industrial prospect.
A kind of porous carbon that the present invention is provided loads the preparation method of molybdenum oxide nanoparticles composite, including following step
Suddenly：
(1) porous carbon adsorption molybdate is utilized, predecessor is obtained；
(2) predecessor is heat-treated in hydrogen argon atmospher, you can obtain the porous carbon load molybdenum oxide and receive
Rice grain composite.
In above-mentioned preparation method, step (1), the mass ratio of the porous carbon and the molybdate can be 12：(1~
30), concretely 12：(5~30), 12：(5~20), 12：(5~10), 12：5、12：10、12：20 or 12：30, preferably 12：
5。
In above-mentioned preparation method, step (1), the porous carbon can for it is any be commercially available from commercial channels or according to
The carbon material with loose structure that conventional method is prepared, in a particular embodiment of the present invention, the porous carbon can be
Ketjen black.The aperture of the porous carbon and specific surface area are unrestricted, in a particular embodiment of the present invention, the porous carbon
Aperture can be 0.5~20 nanometer, and specific surface area can be 1400m2/g。
In above-mentioned preparation method, step (1), the molybdate can be the solubilities such as ammonium molybdate, sodium molybdate and potassium molybdate
One or more in molybdate.
Above-mentioned preparation method, the concrete operations of step (1) are as follows：The porous carbon and the molybdate are dispersed in water
In, centrifuged after standing adsorption, collect solid and be dried in vacuo, obtain the predecessor.
The porous carbon quality and the volume ratio of water can be 30~120 grams：5 liters, concretely 60 grams：5 liters.
The time of the standing adsorption can be 12~36 hours, concretely 12~24 hours, 24~36 hours, it is 12 small
When, 24 hours or 36 hours, preferably 12 hours.
The vacuum drying temperature can be 50~100 DEG C, concretely 60 DEG C；Vacuum drying time can be small for 12~36
When, concretely 24 hours；Vacuum can be -0.05~-0.2 MPa, concretely -0.1 MPa.
In above-mentioned preparation method, step (2), the volumn concentration of hydrogen can be 5~20% in the hydrogen argon atmospher,
It is preferred that 10%.The hydrogen argon atmospher refers to the gaseous mixture of argon gas and hydrogen.
In above-mentioned preparation method, step (2), the temperature of the heat treatment can be 300~700 DEG C, concretely 500~
700 DEG C, 500 DEG C or 700 DEG C；Time can be 0.5~3 hour, and concretely 1~3 hour, 1 hour, 2 hours or 3 hours are excellent
Select 2 hours.
Oxygen is loaded invention further provides the porous carbon that the preparation method described in a kind of any of the above-described is prepared
Change molybdenum nano particle composite material.In the composite, the size of molybdenum oxide nanoparticles can be 0.5~10 nanometer, molybdenum oxide
Load capacity (weight/mass percentage composition) can be 10~50%, preferably 20~30%.
Functional material prepared by the inventive method is a kind of porous carbon load molybdenum oxide nanoparticles composite, is logical
Simple standing adsorption is crossed by molybdate predecessor uniform adsorption on porous carbon, then under reducing atmosphere obtained by annealing.It is porous
The duct space confinement effect of carbon can effectively limit the agglomeration of nano particle, and gained molybdenum oxide nanoparticles are highly dispersed at
On porous carbon, carrying capacity is controllable, and size is less than 10 nanometers, is evenly distributed and controllable.
Preparation method of the present invention is easy, operating process is simple, production cost is low, be easy to mass production；And the preparation
Method universality is strong, can expand and prepare other similar functional materials, with wide prospects for commercial application.
The present invention compared with prior art, has the characteristics that：
1st, the present invention is that the space confinement effect based on porous carbon prepares a kind of porous carbon load molybdenum oxide nanoparticles and answered
Condensation material, relative to other methods, this method cost is low, technique is simple, product is clear and definite and the grain of gained molybdenum oxide nanoparticles
Footpath size is homogeneous, high degree of dispersion, soilless sticking, suitable for large-scale production；Because porous carbon materials have specific surface area big, chemical
Stability is high, conduct electricity very well, good mechanical property and the flourishing characteristic of hole, at the same have wide material sources concurrently, it is with low cost etc.
Feature, has been widely used in the fields such as ultracapacitor, fuel cell, Water warfare absorption, electro-catalysis；Porous carbon of the present invention is born
Carrying molybdenum oxide nano particle composite material has huge potential application valency in Industrial Catalysis, electrochemistry or other scientific domains
Value；
2nd, the predecessor of preparation method of the present invention is ammonium molybdate, sodium molybdate and potassium molybdate etc., and its is cheap, operating process
Simple and safe, inventory is easily controllable；
3rd, the carbon source selected by the present invention is simple and easy to get, with loose structure, there is high specific surface area and more micro- mesoporous,
Excellent absorption property and space confinement effect can be shown.
Brief description of the drawings
The x-ray powder of porous carbon load molybdenum oxide nanoparticles composites of the Fig. 1 to be prepared in embodiment 1 spreads out
Penetrate curve picture.
The transmission electron microscope of porous carbon load molybdenum oxide nanoparticles composites of the Fig. 2 to be prepared in embodiment 1 shines
Piece and grain size distribution, wherein, Fig. 2 (a) is transmission electron microscope photo, and Fig. 2 (b) is high-resolution-ration transmission electric-lens photo, and Fig. 2 (c) is
Grain size distribution.
Fig. 3 is the TGA thermogravimetric analysis of the porous carbon load molybdenum oxide nanoparticles composite prepared in embodiment 1
As a result.
Embodiment
Molybdenum oxide nanoparticles composite and its system are loaded to a kind of porous carbon of the invention below by way of specific embodiment
Preparation Method is described in further detail, but the invention is not limited in following embodiments.
Experimental method used in following embodiments is conventional method unless otherwise specified.
Material, reagent used etc., unless otherwise specified, are commercially obtained in following embodiments.
Embodiment 1, prepare porous carbon load molybdenum oxide nanoparticles composite
Porous carbon load molybdenum oxide nanoparticles composite is prepared in accordance with the following steps：
(1) by purchased from the Ketjen black of Japanese LION companies, (model ECP-600JD, aperture is 0.5~20 nanometer, compares surface
Product is 1400m2/ g) porous carbon and ammonium molybdate be 12 in mass ratio：5 (porous carbon is 60 milligrams, and ammonium molybdate is 25 milligrams) add 5
Ml deionized water, ultrasonic disperse is uniform, and standing adsorption washes centrifugation after 24 hours, and being -0.1 MPa lower 60 DEG C in vacuum does
Dry 24 hours, obtain predecessor；
(2) predecessor is transferred to porcelain boat, inserted in tube furnace quartz ampoule, (hydrogen volume number is hydrogen-argon-mixed
10%) 500 DEG C are warming up under to keep after being heat-treated within 2 hours, room temperature is cooled to, and produce porous carbon load molybdenum oxide nanometer
Granules composite material.
The X-ray powder diffraction curve of porous carbon load molybdenum oxide nanoparticles composite manufactured in the present embodiment is as schemed
Shown in 1.As seen from the figure, molybdenum oxide nanoparticles manufactured in the present embodiment it is smaller so that non-oxidation molybdenum crystal diffraction peak occur,
Only there is the wider amorphous peak of porous carbon.
The electron scanning micrograph of porous carbon manufactured in the present embodiment load molybdenum oxide nanoparticles composite and
Transmission electron microscope photo is as shown in Fig. 2 wherein Fig. 2 (a) is transmission electron microscope photo, and Fig. 2 (b) transmits for high-resolution
Electron micrograph, Fig. 2 (c) is grain size distribution.From Fig. 2 (a), molybdenum oxide nanoparticles manufactured in the present embodiment are high
Degree is dispersed on porous carbon.From Fig. 2 (b) and Fig. 2 (c), molybdenum oxide nanoparticles particle diameter distribution is uniform, and average grain diameter is
1.3 nanometers ± 0.4 nanometer.Lattice fringe image in Fig. 2 (b) proves that the nano particle is molybdenum oxide nanoparticles.
The thermogravimetric curve figure of porous carbon load molybdenum oxide nanoparticles composite manufactured in the present embodiment is as shown in Figure 3.
Analyzed from thermogravimetric curve, in porous carbon load molybdenum oxide nanoparticles composite manufactured in the present embodiment, molybdenum oxide is received
The weight/mass percentage composition of rice grain is 22.81%, and the weight/mass percentage composition of molybdenum is 15.20% after conversion.
From above-mentioned data, the method that the present invention is provided is fully able to preparation and is highly dispersed on porous carbon, and carrying capacity can
Control, size is extra small and the molybdenum oxide nanoparticles that are evenly distributed.
Embodiment 2, prepare porous carbon load molybdenum oxide nanoparticles composite
Porous carbon load molybdenum oxide nanoparticles composite, difference are prepared according to method same as Example 1
For：Carbon source and molybdenum source mass ratio are changed to 12：10 (porous carbon be 60 milligrams, ammonium molybdate be 50 milligrams, deionized water be 5 milli
Rise).In gained composite, the average grain diameter of molybdenum oxide nanoparticles is 1.5 nanometers ± 0.4 nanometer, molybdenum oxide quality percentage
Number is 26.10%.
Embodiment 3, prepare porous carbon load molybdenum oxide nanoparticles composite
Porous carbon load molybdenum oxide nanoparticles composite, difference are prepared according to method same as Example 1
For：Carbon source in step (1) and molybdenum source mass ratio are changed to 12：20 (porous carbon be 60 milligrams, ammonium molybdate be 100 milligrams, deionization
Water is 5 milliliters).In gained composite, the average grain diameter of molybdenum oxide nanoparticles is 1.7 nanometers ± 0.4 nanometer, molybdenum oxide matter
It is 30.20% to measure percentage.
Embodiment 4, prepare porous carbon load molybdenum oxide nanoparticles composite
Porous carbon load molybdenum oxide nanoparticles composite, difference are prepared according to method same as Example 1
For：Carbon source in step (1) and molybdenum source mass ratio are changed to 12：30 (porous carbon be 60 milligrams, ammonium molybdate be 150 milligrams, deionization
Water is 5 milliliters).In gained composite, the average grain diameter of molybdenum oxide nanoparticles is 2.1 nanometers ± 0.4 nanometer, molybdenum oxide matter
It is 33.80% to measure percentage.
Embodiment 5, prepare porous carbon load molybdenum oxide nanoparticles composite
Porous carbon load molybdenum oxide nanoparticles composite is prepared basically according to method same as Example 1, no
It is with part：Heat treatment temperature in step (2) is changed into 700 DEG C, and carbon source in step (1) and molybdenum source quality are changed into 12：
10.In gained composite, the average grain diameter of molybdenum oxide nanoparticles is 2.5 nanometers ± 0.8 nanometer, molybdenum oxide mass percent
For 25.90%.
Embodiment 6, prepare porous carbon load molybdenum oxide nanoparticles composite
Porous carbon load molybdenum oxide nanoparticles composite is prepared basically according to method same as Example 1, no
It is with part：Heat treatment temperature in step (2) is changed into 700 DEG C, and step (1) carbon source and molybdenum source quality are changed into 12：30.
In gained composite, the average grain diameter of molybdenum oxide nanoparticles is 6.8 nanometers ± 1.1 nanometers, and molybdenum oxide mass percent is
34.20%.
Embodiment 7, prepare porous carbon load molybdenum oxide nanoparticles composite
Porous carbon load molybdenum oxide nanoparticles composite is prepared basically according to method same as Example 1, no
It is with part：The 24 hours standing adsorption time in step (1) is changed into 12 hours.In gained composite, molybdenum oxide nanometer
The average grain diameter of grain is 1.25 nanometers ± 0.4 nanometer, and molybdenum oxide mass percent is 21.52%.
Embodiment 8, prepare porous carbon load molybdenum oxide nanoparticles composite
Porous carbon load molybdenum oxide nanoparticles composite is prepared basically according to method same as Example 1, no
It is with part：The 24 hours standing adsorption time in step (1) is changed into 36 hours.In gained composite, molybdenum oxide nanometer
The average grain diameter of grain is 1.35 nanometers ± 0.5 nanometer, and molybdenum oxide mass percent is 22.90%.
Embodiment 9, prepare porous carbon load molybdenum oxide nanoparticles composite
Porous carbon load molybdenum oxide nanoparticles composite is prepared basically according to method same as Example 1, no
It is with part：Heat treatment time in step (2) is changed into 1 hour or 3 hours for 2 hours.In gained composite, extra small molybdenum oxide
Nano particle decentralization, average grain diameter and molybdenum oxide mass percent are similar to Example 1.
Claims (10)
1. a kind of porous carbon loads the preparation method of molybdenum oxide nanoparticles composite, comprise the following steps：
(1) porous carbon adsorption molybdate is utilized, predecessor is obtained；
(2) predecessor is heat-treated in hydrogen argon atmospher, you can obtain the porous carbon load molybdenum oxide nanometer
Granules composite material.
2. preparation method according to claim 1, it is characterised in that：In step (1), the porous carbon and the molybdate
Mass ratio be 12：(1~30).
3. preparation method according to claim 1 or 2, it is characterised in that：In step (1), the molybdate be ammonium molybdate,
One or more in sodium molybdate and potassium molybdate.
4. the preparation method according to any one of claim 1-3, it is characterised in that：The concrete operations of step (1) are as follows：
The porous carbon and the molybdate are dispersed in water, centrifuged after standing adsorption, solid is collected and is dried in vacuo, obtain institute
State predecessor.
5. preparation method according to claim 4, it is characterised in that：The porous carbon quality and the volume ratio of water are (30
~120) gram：5 liters.
6. the preparation method according to claim 4 or 5, it is characterised in that：The time of the standing adsorption is 12~36 small
When.
7. the preparation method according to any one of claim 4-6, it is characterised in that：The vacuum drying temperature be 50~
100 DEG C, the time is 12~36 hours, and vacuum is -0.05~-0.2 MPa.
8. the preparation method according to any one of claim 1-7, it is characterised in that：In step (2), the hydrogen argon atmospher
The volumn concentration of middle hydrogen is 5~20%.
9. the preparation method according to any one of claim 1-8, it is characterised in that：In step (2), the heat treatment
Temperature is 300~700 DEG C, and the time is 0.5~3 hour.
10. the porous carbon load molybdenum oxide nanoparticles that the preparation method any one of claim 1-9 is prepared are answered
Condensation material.
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Application publication date: 20170725 |