CN107416907B - A kind of preparation method of manganese oxide nanosphere - Google Patents
A kind of preparation method of manganese oxide nanosphere Download PDFInfo
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- CN107416907B CN107416907B CN201710861801.0A CN201710861801A CN107416907B CN 107416907 B CN107416907 B CN 107416907B CN 201710861801 A CN201710861801 A CN 201710861801A CN 107416907 B CN107416907 B CN 107416907B
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Abstract
The invention belongs to nano material synthesis and preparation fields, and in particular to a kind of preparation method of manganese oxide nanosphere.It is mixed in a certain ratio CaSi2Powder, Mg powder, Al powder, MnO2Powder, Mn powder and MgO powder, and the powder mixed is put into crucible and is lighted in calm place with Laser Igniter.In crucible after powder combustion reaction, windless condition is still maintained, target product (dust-like) is made to descend slowly and lightly, settle naturally and is adsorbed in the nickel panel surface of crucible surrounding.It is finished to the sedimentation of target complete product, manganese oxide nanosphere attached to it can be collected from nickel panel surface.Manganese oxide nanosphere is prepared using the method for the present invention, equipment investment is small, high production efficiency, easy to operate, technology reproducibility is good, single batch output of production is high, process is environment friendly and pollution-free, gained manganese oxide nanosphere purity is high, best in quality, great commercial introduction value.
Description
Technical field
The invention belongs to nano material synthesis and preparation fields, and in particular to a kind of preparation method of manganese oxide nanosphere.
Background technique
Mn oxide is many kinds of, and the performance and purposes of various Mn oxides depend not only on the valence state of Mn also by its structure
It influences.Commonly referred manganese oxide refers to that chemical formula is MnO morexThe Mn oxide of (x is between 1 and 2) has tunnel structure, main
To be used as the base of catalyst, adsorbent, sensor, wave absorbing agent, manganese oxide lithium primary cell, lithium ion cell positive, ion sieve etc.
Plinth raw material.The manganese oxide nanosphere of Nano grade is even more because of small-size effect, quantum size effect, skin effect and maroscopic quantity
Sub- tunnel-effect and show many properties, such as more excellent electrochemical properties, catalytic capability, microwave absorbing property and absorption
Ability and good surface modification, modification power.
Currently, the synthesis of manganese oxide nanosphere and preparation method specifically include that chemical vapour deposition technique, hydro-thermal method, micro emulsion
Liquid method, sol-gal process, chemical deposition, electrochemical process, ball-milling method, microwave-assisted emulsion method, template method, solution combustion method,
Sonochemical method etc..Manganese oxide nanosphere purity is high, good dispersion, even particle distribution made from these methods, and have excellent
Good chemical property, but preparation process it is complicated, to equipment or operating experience require high, single batch output of production is low, synthesis with
Long preparation period, and generally require to clean final product or intermediate product, a large amount of pollution waste liquids are discharged, rest on more
Laboratory research and development or small-scale low yield scale up test stage.Exactly early investment brought by these deficiencies is excessively high, produces effect
The problems such as rate is too low, technology reproducibility is poor, production cost is excessively high, waste gas and waste liquid is not easy to handle, causes the prior art and is difficult to
Obtain industrial applications.As it can be seen that being needed to meet inexpensive, efficient, environmentally protective modern industrialization large-scale production requirement
It is proposed a kind of new manganese oxide nanosphere preparation method.
Summary of the invention
Technical problem to be solved by the present invention lies in the deficiencies for being directed to existing manganese oxide nanosphere technology of preparing, provide
It is a kind of be simple and efficient, environmentally protective and high product purity manganese oxide nanosphere preparation method.
Manganese oxide nanosphere preparation method provided by the invention, is achieved by the steps of:
Step (1), is respectively CaSi according to mass fraction210.4-16.9 parts of powder, 4.2-12.5 parts of Mg powder, Al powder 9.5-
15.9 parts, MnO246.3-58.7 parts of powder, 6.1-9.0 parts of Mn powder, the ratio that 4.6-5.9 parts of MgO powder weighs CaSi2Powder, Mg powder, Al
Powder, MnO2Powder, Mn powder and MgO powder, and it is uniformly mixed, it is put into crucible；
Crucible equipped with mixed-powder is placed in a nickel disk upper surface the center point by step (2)；
Step (3) lights powder with Laser Igniter in calm place, is allowed to burn and react；
Step (4) maintains windless condition, target product (dust-like) is made to descend slowly and lightly, settle naturally and adsorb after reaction
In nickel panel surface；
Step (5) finishes to the sedimentation of target complete product, manganese oxide attached to it can be collected from nickel panel surface and is received
Rice ball.
Preferably, the CaSi2Powder, Mg powder, Al powder, MnO2The partial size of powder, Mn powder and MgO powder is 500-1000 mesh.
Preferably, the nickel disk diameter is 2.5-5 times of crucible outer diameter.
Preferably, the crucible material is high purity graphite.
Preferably, obtained manganese oxide nanometer bulb diameter is distributed between about 40nm-719nm.
Preferably, the chemical formula of obtained manganese oxide nanosphere is MnOx(x=1.32-1.78).
A kind of manganese oxide nanosphere, is prepared using above-mentioned preparation method.
The chemical formula of gained manganese oxide nanosphere is MnOx(x=1.32-1.78), diameter is between about 40nm-719nm.
In the reaction process, CaSi2Powder, Mg powder, Al powder and MnO2It is had occurred between powder acutely and complicated solid-state burning
It reacts and discharges amount of heat.Reaction product CaO, SiO2, MgO and Al2O3It is heated that partial melting occurs, and under the effect of gravity
Floating is gathered in reaction system surface, and the cellular for forming (discontinuous) off and on is crushed skull.Reaction product Mn is together with original
Mn powder melted by heat in feed powder end, a part of Mn escape up reactant in the explosive vaporization of high-temperature fusant in gaseous form
System；And another part Mn then moment be full of in crucible high temperature and pressure effect under, be extruded in liquid form it is spouting,
And when passing through inflated slag shell moment be atomized, reaction system is finally left in the form of microlayer model.Mn steam and the micro- liquid of Mn
Drop continues up rear natural subsidence after leaving reaction system in air, therebetween rapid cooling and fully oxidized, most end form
The nickel panel surface being attached at manganese oxide nanosphere around high purity graphite crucible.Related related chemistry reaction are as follows:
2CaSi2+6Mg+4Al+11MnO2=2Al2O3+6MgO+4SiO2+2CaO+11Mn。
Select MnO2As unique reducing agent, other metal simple-substances avoided in addition to Mn are generated, and improve target product
Purity.
Product Al2O3, MgO, SiO2, CaO form unique solid-liquid two-phase skull according to a certain percentage, the outlet of closing crucible,
When so that product Mn not leaving crucible, in confined space, and there is biggish pressure；When product Mn leaves crucible, skull
On liquid phase region broken through by Mn, formed micropore, become the channel that product Mn leaves crucible.
Nickel has good high-temperature stability, carries out target product (manganese oxide nanosphere) using nickel disk and collects, Neng Gouyou
Effect avoids collection device to the element pollution of target product；Collection device is located at crucible bottom, directly receives not above crucible
Collect target product, but allow target product natural subsidence on collection device under no-wind environment, this makes target product exist
Residence time in air greatly prolongs, and degree of oxidation is higher.
The major advantage and beneficial effect of method involved by the present invention are: equipment investment is small, high production efficiency, operates letter
List, technology reproducibility are good, single batch output of production is high, process is environment friendly and pollution-free.Manganese oxide nanosphere purity obtained
Height has good electrochemical properties, adsorptivity, catalytic and wave absorbtion.
Detailed description of the invention
Fig. 1 is the side view of device figure used by preparation method of the present invention；
Fig. 2 is the top view of device figure used by preparation method of the present invention；
Fig. 3 is the electron scanning micrograph of 2 gained manganese oxide nanosphere of the embodiment of the present invention.
Appended drawing reference:
1, nickel disk；2, raw material powder；3, graphite crucible.
Specific embodiment
It will be helpful to understand the present invention by the following description of the embodiments, but be not intended to limit the contents of the present invention.
Embodiment 1
Firstly, weighing mass fraction is respectively 10.4%, 12.5%, 15.9%, 46.3%, 9.0% and 5.9% 500
The CaSi of mesh size2Powder, Mg powder, Al powder, MnO2Powder, Mn powder and MgO powder, and it is uniformly mixed, gained raw material powder 2 is put
Enter in high purity graphite crucible 3.Then, high purity graphite crucible 3 is placed in 1 the center point of nickel disk that diameter is 5 times of crucible outer diameters, such as schemed
Shown in 1,2.Finally, lighting raw material powder 2 with Laser Igniter, being allowed to burn and reacting, and whole holding ambient enviroment
In windless condition.After reaction, windless condition is maintained, target product (dust-like) is made to descend slowly and lightly, settle naturally and be adsorbed in
1 surface of nickel disk.It is finished to the sedimentation of target complete product, manganese oxide nanosphere that can be attached to it from 1 surface collection of nickel disk.
TEM, SEM observation and XRD, EDS analysis are carried out to gained nanosphere, the results showed that gained manganese oxide nanosphere contains only Mn and O two
Kind element, purity is higher, chemical formula MnOx(x=1.32-1.69)；Nanometer bulb diameter is distributed between about 51nm-714nm.
Embodiment 2
Firstly, weighing 700 mesh that mass fraction is respectively 13.7%, 8.4%, 12.7%, 52.5%, 7.5% and 5.2%
The CaSi of size2Powder, Mg powder, Al powder, MnO2Powder, Mn powder and MgO powder, and it is uniformly mixed, gained raw material powder 2 is put into
In high purity graphite crucible 3.Then, high purity graphite crucible 3 is placed in 1 the center point of nickel disk that diameter is 3.5 times of crucible outer diameters, such as schemed
Shown in 1,2.Finally, lighting raw material powder 2 with Laser Igniter, being allowed to burn and reacting, and whole holding ambient enviroment
In windless condition.After reaction, windless condition is maintained, target product (dust-like) is made to descend slowly and lightly, settle naturally and be adsorbed in
1 surface of nickel disk.It is finished to the sedimentation of target complete product, manganese oxide nanosphere that can be attached to it from 1 surface collection of nickel disk.
TEM, SEM observation and XRD, EDS analysis are carried out to gained nanosphere, the results showed that gained manganese oxide nanosphere contains only Mn and O two
Kind element, purity is higher, chemical formula MnOx(x=1.39-1.78)；Nanometer bulb diameter is distributed between about 45nm-706nm,
As shown in Figure 3.
Embodiment 3
Firstly, weighing 1000 mesh that mass fraction is respectively 16.9%, 4.2%, 9.5%, 58.7%, 6.1% and 4.6%
The CaSi of size2Powder, Mg powder, Al powder, MnO2Powder, Mn powder and MgO powder, and it is uniformly mixed, gained raw material powder 2 is put into
In high purity graphite crucible 3.Then, high purity graphite crucible 3 is placed in 1 the center point of nickel disk that diameter is 2.5 times of crucible outer diameters, such as schemed
Shown in 1,2.Finally, lighting raw material powder 2 with Laser Igniter, being allowed to burn and reacting, and whole holding ambient enviroment
In windless condition.After reaction, windless condition is maintained, target product (dust-like) is made to descend slowly and lightly, settle naturally and be adsorbed in
1 surface of nickel disk.It is finished to the sedimentation of target complete product, manganese oxide nanosphere that can be attached to it from 1 surface collection of nickel disk.
TEM, SEM observation and XRD, EDS analysis are carried out to gained nanosphere, the results showed that gained manganese oxide nanosphere contains only Mn and O two
Kind element, purity is higher, chemical formula MnOx(x=1.36-1.71)；Nanometer bulb diameter is distributed between about 40nm-719nm.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (6)
1. a kind of preparation method of manganese oxide nanosphere, it is characterised in that include the following steps:
Step (1), is respectively CaSi according to mass fraction210.4-16.9 parts of powder, 4.2-12.5 parts of Mg powder, Al powder 9.5-15.9
Part, MnO246.3-58.7 parts of powder, 6.1-9.0 parts of Mn powder, the ratio that 4.6-5.9 parts of MgO powder weighs CaSi2Powder, Mg powder, Al powder,
MnO2Powder, Mn powder and MgO powder, and it is uniformly mixed, it is put into crucible；
Crucible equipped with mixed-powder is placed in a nickel disk upper surface the center point by step (2)；
Step (3) lights powder with Laser Igniter in calm place, is allowed to burn and react；
Step (4) maintains windless condition, so that target product descended slowly and lightly, settled naturally and be adsorbed in nickel panel surface after reaction；
Step (5) finishes to the sedimentation of target complete product, manganese oxide nanometer attached to it can be collected from nickel panel surface
Ball.
2. the preparation method of manganese oxide nanosphere according to claim 1, which is characterized in that the CaSi2Powder, Mg powder, Al
Powder, MnO2The partial size of powder, Mn powder and MgO powder is 500-1000 mesh.
3. the preparation method of manganese oxide nanosphere according to claim 1, which is characterized in that the nickel disk diameter is described
2.5-5 times of crucible outer diameter.
4. the preparation method of manganese oxide nanosphere according to claim 1, which is characterized in that the crucible material is high-purity
Graphite.
5. the preparation method of manganese oxide nanosphere according to claim 1, which is characterized in that obtained manganese oxide nanometer
Bulb diameter is distributed between 40nm-719nm.
6. the preparation method of manganese oxide nanosphere according to claim 1, which is characterized in that obtained manganese oxide nanometer
The chemical formula of ball is MnOx, wherein x=1.32-1.78.
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| CN101343081A (en) * | 2008-08-25 | 2009-01-14 | 陕西师范大学 | Method of preparing manganese oxide hollow nano-sphere with large-specific surface area |
| CN102001700A (en) * | 2010-12-07 | 2011-04-06 | 武汉大学 | Method for synthesizing SnO2 nanoribbon by utilizing self-propagating high-temperature reaction |
| CN102874863A (en) * | 2012-10-24 | 2013-01-16 | 武汉大学 | Synthetic method for zinc oxide nano-particles |
| CN103318947A (en) * | 2013-07-08 | 2013-09-25 | 武汉大学 | Combustion synthesis method of zinc oxide nanoparticles |
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Patent Citations (4)
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|---|---|---|---|---|
| CN101343081A (en) * | 2008-08-25 | 2009-01-14 | 陕西师范大学 | Method of preparing manganese oxide hollow nano-sphere with large-specific surface area |
| CN102001700A (en) * | 2010-12-07 | 2011-04-06 | 武汉大学 | Method for synthesizing SnO2 nanoribbon by utilizing self-propagating high-temperature reaction |
| CN102874863A (en) * | 2012-10-24 | 2013-01-16 | 武汉大学 | Synthetic method for zinc oxide nano-particles |
| CN103318947A (en) * | 2013-07-08 | 2013-09-25 | 武汉大学 | Combustion synthesis method of zinc oxide nanoparticles |
Non-Patent Citations (1)
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| Microwave-assisted synthesis of porous Mn2O3 nanoballs as bifunctional electrocatalyst for oxygen reduction and evolution reaction;Srabanti Ghosh等;《Catal. Sci. Technol.》;20151231;第1418页左栏第一段以及图1 |
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