CN107265504A - One-dimensional MnO2Nanotube and its preparation method and application - Google Patents
One-dimensional MnO2Nanotube and its preparation method and application Download PDFInfo
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- CN107265504A CN107265504A CN201710387978.1A CN201710387978A CN107265504A CN 107265504 A CN107265504 A CN 107265504A CN 201710387978 A CN201710387978 A CN 201710387978A CN 107265504 A CN107265504 A CN 107265504A
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- C—CHEMISTRY; METALLURGY
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- C01G45/00—Compounds of manganese
- C01G45/02—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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
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- C01P2004/00—Particle morphology
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- C01P2004/13—Nanotubes
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a kind of one-dimensional MnO2Nanotube and its preparation method and application, the preparation method includes high manganese ion and Te nano wires redox reaction occurring in the solution, to prepare one-dimensional MnO2The step of nanotube.One-dimensional MnO is prepared with existing2The method of nanotube is compared, and preparation method controllable, yield easy to operate proposed by the present invention is high.Resulting materials have fake capacitance property, with preferable discharge and recharge coulomb effect and larger specific capacitance during for electrode material for super capacitor.
Description
Technical field
One-dimensional tubular nanometer material is prepared the present invention relates to template, in particular it relates to a kind of one-dimensional MnO2Nanotube and
Its preparation method and application.
Background technology
One-dimensional nano structure material, particularly nanotube-shaped material has some peculiar properties such as specific surface area height, density
Low, osmosis is good, electrochemical performance, therefore rationally designs and synthesizes 1-dimention nano tubular material to realizing modern society
The efficient storage of the energy and conversion have important theoretical significance and practical value.
Template can design aperture and the controllable template model of pore size, Neng Gou in certain media environment
Wherein it is effectively embedding various nano-particles, and controllable its shape, size, moreover it is possible to prevent the generation reunited, in recent years
Made great progress in terms of the nano material of variously-shaped and size is prepared.
Template also has a wide range of applications in the synthesis of monodimension nanometer material.In general nano-confined mould can be divided into
Plate and orientation template.Wherein nano-confined template mainly includes mesoporous template, anodised aluminium etc., and orientation template mainly includes carbon
Nano material, inorganic, metal oxide nano material and metal nano material etc..Wherein such as Te nanometers of wire rod of metal nano material
Expect electrical conductivity height, morphology controllable, support frame effect can not only be played during the course of the reaction as template, while can be dissolved,
Therefore template need not be eliminated, course of reaction is more simple, controllable.
The content of the invention
It is an object of the invention to provide a kind of one-dimensional MnO2Nanotube and preparation method thereof, one-dimensional MnO2Nanotube and application,
One-dimensional template is used as by one-dimensional Te nano wires, MnO4 is occurred redox reaction with Te, so as to obtain having preferably
The tubulose of chemical property is layered one-dimensional MnO2Nano-tube material.The preparation method controllable, yield easy to operate is high.
To achieve these goals, the present invention provides a kind of one-dimensional MnO2The preparation method of nanotube, the preparation method
Including high manganese ion and Te nano wires in the solution into redox reaction occur, to prepare one-dimensional MnO2The step of nanotube
Suddenly.
The present invention also provides a kind of one-dimensional MnO2Nanotube, according to previously described one-dimensional MnO2The preparation method of nanotube
Prepare.
Moreover, the present invention also provides one kind according to previously described one-dimensional MnO2Nanotube is in as electrode material
Application.
By above-mentioned technical proposal, the present invention is anti-in simple liquid phase by the use of one-dimensional Te nano wires as template and reducing agent
Answering makes MnO4 occur redox reaction with Te nano wires in system, so as to obtain the one-dimensional MnO of tubulose layering2Nanotube
Material.One-dimensional MnO is prepared with existing2The method of nanotube is compared, and the present invention proposes preparation method controllable, yield easy to operate
It is high.Resulting materials have fake capacitance property, have during for electrode material for super capacitor preferable discharge and recharge coulomb effect and
Larger specific capacitance.
Other features and advantages of the present invention will be described in detail in subsequent embodiment part.
Brief description of the drawings
Accompanying drawing is, for providing a further understanding of the present invention, and to constitute a part for specification, with following tool
Body embodiment is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings：
Fig. 1 (a) is the low power scanning electron microscope (SEM) photograph of Te nano wires；
Fig. 1 (b) is the X-ray powder diffraction figure of Te nano wires；
Fig. 2 (a) is the low power scanning electron microscope (SEM) photograph of the products therefrom of embodiment 1；
Fig. 2 (b) is the high power scanning electron microscope (SEM) photograph of the products therefrom of embodiment 1；
Fig. 2 (c) is the transmission electron microscope picture of the products therefrom of embodiment 1；
Fig. 3 is the X-ray powder diffraction figure of the products therefrom of embodiment 1；
Fig. 4 is one-dimensional MnO prepared by embodiment 12Nanotube as electrode material for super capacitor cyclic voltammetry curve
(CV) figure；
Fig. 5 is one-dimensional MnO prepared by embodiment 12Nanotube is as electrode material for super capacitor in different current densities
Under charging and discharging curve (CP) figure；
Fig. 6 is the low power scanning electron microscope (SEM) photograph of the products therefrom of embodiment 2；
Fig. 7 is the low power scanning electron microscope (SEM) photograph of the products therefrom of embodiment 3；
Fig. 8 is the low power scanning electron microscope (SEM) photograph of the products therefrom of embodiment 4；
Fig. 9 is the low power scanning electron microscope (SEM) photograph of the products therefrom of embodiment 5；
Figure 10 is the low power scanning electron microscope (SEM) photograph of the products therefrom of embodiment 6；
Figure 11 is the low power scanning electron microscope (SEM) photograph of the products therefrom of embodiment 7.
Embodiment
The embodiment to the present invention is described in detail below.It should be appreciated that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to limit the invention.
The end points and any value of disclosed scope are not limited to the accurate scope or value herein, these scopes or
Value should be understood to comprising the value close to these scopes or value.For number range, between the endpoint value of each scope, respectively
It can be combined with each other between the endpoint value of individual scope and single point value, and individually between point value and obtain one or more
New number range, these number ranges should be considered as specific open herein.
The present invention provides a kind of one-dimensional MnO2The preparation method of nanotube, the preparation method is included high manganese ion
Redox reaction occurs in the solution with Te nano wires, to prepare one-dimensional MnO2The step of nanotube.
By above-mentioned technical proposal, the present invention utilizes one-dimensional Te nano wires and reducing agent, in simple liquid-phase reaction system
MnO4 is set to occur redox reaction with Te nano wires, so as to obtain the one-dimensional MnO of tubulose layering2Nano-tube material.Hair
A person of good sense speculates that Te nano-materials play a part of template in above-mentioned course of reaction, can not only play support frame effect, together
When can be dissolved, therefore Te nano wires need not be eliminated, course of reaction is more simple, controllable.One-dimensional MnO is prepared with existing2Receive
The method of mitron is compared, and the present invention proposes that preparation method is easy to operate, controllable.Resulting materials have fake capacitance property, for surpassing
With preferable discharge and recharge coulomb effect and larger specific capacitance during level capacitor electrode material.
In the above-mentioned technical solutions, the consumption mol ratio of Te nano wires and MnO4 has multiple choices, in order that preparing
One-dimensional MnO2Naraotube yield height and morphology controllable, it is preferable that in solution, the Te nano wires relative to 8-12.8mg, Gao Meng
The amount of the material of acid group is：0.0024-0.0036mol.
In the above-mentioned technical solutions, the redox reaction condition of Te nano wires and MnO4 has multiple choices, in order to
Make the one-dimensional MnO of preparation2Naraotube yield height and morphology controllable, redox reaction are carried out under conditions of the addition concentrated sulfuric acid.
In the above-mentioned technical solutions, the concentrated sulfuric acid is the aqueous solution for the bright sulfur acid that mass fraction is more than or equal to 70%, it is preferable that
The concentrated sulfuric acid is the concentrated sulfuric acid of mass fraction 98%.
In the above-mentioned technical solutions, the redox reaction condition and course of reaction of Te nano wires and MnO4 have a variety of
Selection, in order that the one-dimensional MnO prepared2Naraotube yield height and morphology controllable, it is preferable that the preparation method includes following step
Suddenly：A, the nanowire suspended liquid of Te added in the solution containing high manganese ion, the concentrated sulfuric acid is added under agitation, continues to stir
Certain time t1, obtains mixed liquor M1；B, M1 is heated and stirred certain time t2 obtain product M2；C, by products therefrom M2 from
The heart, is washed, and drying obtains one-dimensional MnO2Nano-tube material.
In the above-mentioned technical solutions, the mode that the nanowire suspended liquid of Te is added in solution has a variety of, is such as rapidly injected, drips
Plus, the mode such as be added dropwise dropwise, can realize and illustrated in the present invention, embodiment later in the way of being added dropwise.
In this specific embodiment, in order that the one-dimensional MnO prepared2Naraotube yield height and morphology controllable, it is preferable that
In terms of parts by volume, relative to the solution containing high manganese ion that 30mL concentration is 0.08-0.12mol/L, 1.6mg/mL Te
The consumption of nanowire suspended liquid is 5-8mL, and the consumption for the concentrated sulfuric acid that mass fraction is 98% is 10~550 μ L.
In this specific embodiment, in order that the one-dimensional MnO prepared2Naraotube yield height and morphology controllable, it is preferable that
Preparation method is at least met：T1 is 8-12min；And/or, t2 is 1-2h；And/or heating-up temperature is 80 DEG C~100 in step b
℃。
In the above-mentioned technical solutions, the source of high manganese ion can have multiple choices, as long as the aqueous solution can be dissolved in
In, it is that can realize the present invention to produce high manganese ion.In order that the one-dimensional MnO prepared2Naraotube yield is high and pattern can
Control, it is preferable that high manganese ion source is high manganese lithium, sodium permanganate, potassium permanganate, ammonium permanganate, acerdol, permanganic acid
One or more in barium, zinc permanganate, magnesium permanganate, permanganic acid mercury, cadmium permanganate and permanganic acid rubidium.
Te nano wires have is limited in less than 100 nanometers of one-dimentional structure in the horizontal, its aspect ratio more than 1000,
Therefore commonly known as one-dimensional material.
In the above-mentioned technical solutions, Te nano wires can be obtained by a variety of preparation methods, such as by TeO2, polyethylene pyrrole
Pyrrolidone and NaOH are dissolved in ethylene glycol, and reaction certain time is that can obtain Te nano wires.
Further, Te nano wires are prepared by the following technical programs：Relative to 0.25mmol TeO2, will
0.25mmol TeO2Powder, 0.2g polyvinylpyrrolidones (PVP) and 10mmol NaOH are dissolved in 16mL ethylene glycol, are passed through
Heating for dissolving forms clear solution, is then transferred in 20mL polytetrafluoroethyllining lining autoclaves, and Te is obtained after reacting 4h at 180 DEG C
Nano wire.
After above-mentioned 16mgTe nano wires acetone and deionization are washed 2-6 times, it is dispersed in 10mL deionized waters, you can
Obtain the 1.6mg/mL nanowire suspended liquid of Te.
The present invention also provides a kind of one-dimensional MnO2Nanotube, according to previously described one-dimensional MnO2The preparation method of nanotube
Prepare.The one-dimensional MnO of gained2Nanotube has fake capacitance property, has during for electrode material for super capacitor preferable
Discharge and recharge coulomb effect and larger specific capacitance.
The one-dimensional MnO that the present invention is synthesized2Tube diameters have multiple choices, it is preferable that the one-dimensional MnO2Nanotube it is straight
Footpath is 140-160nm.
The one-dimensional MnO that the present invention is synthesized2The structure of nanotube has multiple choices, it is preferable that the one-dimensional MnO2Nanotube is
Tubulose hierarchy.Tubulose hierarchy refers to there is low dimensional structures unit (such as zero-dimension nano particle, one-dimensional in nanotube surface
Nano wire/rod, two-dimensional nano piece etc.) composition micro/nano structure, the one-dimensional MnO that synthesizes of the present invention2Nanotube is by MnO2Receive
The tubulose hierarchy of rice piece composition.
The present invention also provides one kind according to previously described one-dimensional MnO2Application of the nanotube in as electrode material.Should
One-dimensional MnO2Nanotube has fake capacitance property, has preferable discharge and recharge coulomb effect during for electrode material for super capacitor
With larger specific capacitance.
With reference to embodiment, the present invention is described in detail, but protection scope of the present invention is not only restricted to these implementations
Example.
The number-average molecular weight of polyvinylpyrrolidone is 58000, purchased from Shanghai Aladdin biochemical technology limited company,
Other are conventional commercial product.
Preparation example 1
(1) 0.25mmol TeO are taken2Powder, 0.2g polyvinylpyrrolidones (PVP) and 10mmol NaOH are dissolved in 16mL
In ethylene glycol, clear solution is formed by dissolving by heating, is then transferred in 20mL polytetrafluoroethyllining lining autoclaves, 180
DEG C reaction 4h after Te nano wires；
(2) 16mg Te nano wires are washed after 6 times with acetone and deionized water respectively, are dispersed in 10mL deionized waters,
Obtain the 1.6mg/mL nanowire suspended liquid of Te.
The low power scanning electron microscope (SEM) photograph of Te nano wires is shown in Fig. 1 (a)；The X-ray powder diffraction figure of Te nano wires is shown in Fig. 1 (b).
Fig. 1 (a) be Te nano wires low power scanning electron microscope (SEM) photograph, it can be seen from Fig. 1 (a) Te nanowire surfaces it is smooth and
Long, Fig. 1 (b) is the X-ray powder diffraction figure of Te nano wires, is consistent with Te (JCPDS No.04-0555).
Embodiment 1
A, the KMnO that the nanowire suspended liquid of 8mL 1.6mg/mL Te is added dropwise to 30mL 0.1mol/L4In solution,
Stirring is lower to add the dense H that 450 μ L mass fractions are 98%2SO4, stir 10min；
B, solution in step (a) is transferred in 50mL round-bottomed flasks, 80 DEG C of stirring 1.5h in oil bath；
C, products therefrom centrifuged, washed with deionized water and absolute ethyl alcohol 6 times, 80 DEG C of drying；Obtain one-dimensional MnO2Receive
Nanotube material.
Fig. 2 (a) is the low power scanning electron microscope (SEM) photograph of the products therefrom of embodiment 1, and Fig. 2 (b) is the high power of the products therefrom of embodiment 1
Scanning electron microscope (SEM) photograph, as can be seen from Figure, product are tubulose hierarchy, diameter 140-160nm.Fig. 2 (c) is the institute of embodiment 1
The transmission electron microscope picture of product is obtained, as seen from the figure obvious tubulose hierarchy.
Fig. 3 is the X-ray powder diffraction figure of the products therefrom of embodiment 1, in spectrogram all diffraction maximums all with birnessite
MnO2(JCPDS No.18-0802) is consistent, and 12.3 °, 18.7 °, 36.8 °, 54.9 ° and 65.7 ° of diffraction maximum is corresponded to respectively
(002), (101), (006), (301) and (119) crystal face.
Fig. 4 is one-dimensional MnO prepared by embodiment 12Nano-tube material is schemed as the CV of electrode material for super capacitor, by scheming
It can be seen that curve is in quasi- rectangle, show the one-dimensional MnO prepared2Nano-tube material has fake capacitance property.
Fig. 5 is one-dimensional MnO prepared by embodiment 12Nanotube is schemed as the CP of electrode material for super capacitor, nearly symmetrically
Curve table prescribed electrode there is higher discharge and recharge coulomb effect and preferable electric capacity.
Embodiment 2
A, the KMnO that the nanowire suspended liquid of 8mL 1.6mg/mL Te is added dropwise to 30mL 0.1mol/L4In solution,
Stirring is lower to add the dense H that 300 μ L mass fractions are 98%2SO4, stir 10min；
B, solution in step (a) is transferred in 50mL round-bottomed flasks, 80 DEG C of stirring 1.5h in oil bath；
C, products therefrom centrifuged, washed with deionized water and absolute ethyl alcohol 6 times, 80 DEG C of drying；Obtain one-dimensional MnO2Receive
Nanotube material, its morphology characterization difference corresponding diagram 6.
As seen from Figure 6, product is tubulose hierarchy, diameter 140-160nm.
Embodiment 3
A, the KMnO that the nanowire suspended liquid of 5mL 1.6mg/mL Te is added dropwise to 30mL 0.08mol/L4In solution,
The dense H that 10 μ L mass fractions are 98% is added under agitation2SO4, stir 8min；
B, solution in step (a) is transferred in 50mL round-bottomed flasks, 80 DEG C of stirring 1h in oil bath；
C, products therefrom centrifuged, washed with deionized water and absolute ethyl alcohol 6 times, 80 DEG C of drying；Obtain one-dimensional MnO2Receive
Nanotube material, its morphology characterization difference corresponding diagram 7.
As seen from Figure 7, product is tubulose hierarchy, diameter 140-160nm.
Embodiment 4
A, the KMnO that the nanowire suspended liquid of 8mL 1.6mg/mL Te is added dropwise to 30mL 0.12mol/L4In solution,
The dense H that 550 μ L mass fractions are 98% is added under agitation2SO4, stir 12min；
B, solution in step (a) is transferred in 50mL round-bottomed flasks, 100 DEG C of stirring 2h in oil bath；
C, products therefrom centrifuged, washed with deionized water and absolute ethyl alcohol 6 times, 100 DEG C of drying；Obtain one-dimensional MnO2Receive
Nanotube material, its morphology characterization corresponding diagram 8.
As seen from Figure 8, product is tubulose hierarchy, diameter 140-160nm.
Embodiment 5
A, the KMnO that the nanowire suspended liquid of 5mL 1.6mg/mL Te is added dropwise to 30mL 0.12mol/L4In solution,
The dense H that 100 μ L mass fractions are 98% is added under agitation2SO4, stir 12min；
B, solution in step (a) is transferred in 50mL round-bottomed flasks, 100 DEG C of stirring 2h in oil bath；
C, products therefrom centrifuged, washed with deionized water and absolute ethyl alcohol 6 times, 100 DEG C of drying；Obtain one-dimensional MnO2Receive
Nanotube material, its morphology characterization corresponding diagram 8.
As seen from Figure 9, product is tubulose hierarchy, diameter 140-160nm.
Embodiment 6
Method according to embodiment 1 prepares one-dimensional MnO2Nano-tube material, unlike, wherein without the concentrated sulfuric acid, obtaining
To one-dimensional MnO2Nano-tube material, its morphology characterization corresponding diagram 9.
As seen from Figure 10, a large amount of graininess accumulations of product, tubular structure product is less, and hierarchy is not obvious.
Embodiment 7
Method according to embodiment 1 prepares one-dimensional MnO2Nano-tube material, unlike, oil bath temperature wherein in step (b)
Spend for 110 DEG C, obtain one-dimensional MnO2Nano-tube material, its morphology characterization corresponding diagram 10.
As seen from Figure 11, a large amount of graininess accumulations of product, tubular structure product is less, and hierarchy is not obvious.
The preferred embodiment of the present invention described in detail above, still, the present invention are not limited in above-mentioned embodiment
Detail, in the range of the technology design of the present invention, a variety of simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (10)
1. a kind of one-dimensional MnO2The preparation method of nanotube, it is characterised in that the preparation method include by high manganese ion with
Redox reaction occurs in the solution for Te nano wires, to prepare one-dimensional MnO2The step of nanotube.
2. preparation method according to claim 1, wherein, in solution, the Te nano wires relative to 8-12.8mg, permanganic acid
The amount of the material of root is：0.0024-0.0036mol.
3. preparation method according to claim 1 or 2, wherein, redox reaction is entered under conditions of the addition concentrated sulfuric acid
OK.
4. preparation method according to claim 3, wherein, the preparation method comprises the following steps：
A, the nanowire suspended liquid of Te added in the solution containing high manganese ion, the concentrated sulfuric acid is added under agitation, continues to stir
Certain time t1 is mixed, mixed liquor M1 is obtained；
B, M1 is heated and stirred certain time t2 obtain product M2；
C, products therefrom M2 centrifuged, washed, drying obtains one-dimensional MnO2Nano-tube material.
5. preparation method according to claim 4, wherein, it is 0.08- relative to 30mL concentration in terms of parts by volume
The 0.12mol/L solution containing high manganese ion, the consumption of the 1.6mg/mL nanowire suspended liquid of Te is 5-8mL, quality point
The consumption for the concentrated sulfuric acid that number is 98% is 10~550 μ L.
6. preparation method according to claim 4, wherein, at least meet：T1 be 8-12min and/or, t2 is 1-2h；With/
Or, heating-up temperature is 80 DEG C~100 DEG C in step b.
7. preparation method according to claim 1, wherein, high manganese ion source is high manganese lithium, sodium permanganate, Gao Meng
Sour potassium, ammonium permanganate, acerdol, barium permanganate, zinc permanganate, magnesium permanganate, permanganic acid mercury, cadmium permanganate and permanganic acid rubidium
In one or more.
8. a kind of one-dimensional MnO2Nanotube, it is characterised in that the one-dimensional MnO according to any one of claim 1-72Nanometer
The preparation method of pipe is prepared.
9. one-dimensional MnO according to claim 82Nanotube, wherein, the one-dimensional MnO2Nanotube is tubulose hierarchy,
A diameter of 140-160nm.
10. a kind of one-dimensional MnO according to claim 8 or claim 92Application of the nanotube in as electrode material.
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