CN107265504B - 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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- CN107265504B CN107265504B CN201710387978.1A CN201710387978A CN107265504B CN 107265504 B CN107265504 B CN 107265504B CN 201710387978 A CN201710387978 A CN 201710387978A CN 107265504 B CN107265504 B CN 107265504B
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- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a kind of one-dimensional MnO2Nanotube and its preparation method and application, which includes that redox reaction is occurred in the solution for high manganese ion and Te nano wire, to prepare one-dimensional MnO2The step of nanotube.One-dimensional MnO is prepared with existing2The method of nanotube is compared, and preparation method proposed by the present invention is easy to operate and control, yield is high.Resulting materials have fake capacitance property, are used to have preferable charge and discharge coulomb effect and biggish specific capacitance when electrode material for super capacitor.
Description
Technical field
The present invention relates to templates to prepare one-dimensional tubular nanometer material, and in particular, to a kind of one-dimensional MnO2Nanotube and
Preparation method and application.
Background technique
One-dimensional nano structure material, especially nanotube-shaped material have some peculiar properties such as specific surface area height, density
It is low, osmosis is good, electrochemical performance, therefore rationally design and the nanotube-shaped material of synthesizing one-dimensional to realize 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
Various nanoparticles are wherein effectively embedding, and can control its shape, size, moreover it is possible to prevent the generation reunited, in recent years
It is made great progress in terms of the nano material of preparation various shape and size.
Template also has a wide range of applications in the synthesis of monodimension nanometer material.In general it can be divided into nano-confined mould
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 conductivity height, morphology controllable, braced frame can not only be played the role of during the reaction as template, while can be dissolved,
Therefore template need not be eliminated, reaction process is more simple, controllable.
Summary of the invention
The object of the present invention is to provide a kind of one-dimensional MnO2Nanotube and preparation method thereof, one-dimensional MnO2Nanotube and application,
By one-dimensional Te nano wire as one-dimensional template, make MnO4 and Te that redox reaction occur, to obtain having preferable
The tubulose of chemical property is layered one-dimensional MnO2Nano-tube material.The preparation method is easy to operate and control, yield is high.
To achieve the goals above, the present invention provides a kind of one-dimensional MnO2The preparation method of nanotube, the preparation method
Including redox reaction is occurred in the solution for high manganese ion and Te nano wire, 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
It is prepared.
Moreover, the present invention also provides a kind of according to previously described one-dimensional MnO2Nanotube is in as electrode material
Application.
Through the above technical solutions, the present invention is using one-dimensional Te nano wire as template and reducing agent, it is anti-in simple liquid phase
Answering makes MnO4 and Te nano wire that redox reaction occur in system, 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 that preparation method is easy to operate and control, yield
It is high.Resulting materials have fake capacitance property, be used for electrode material for super capacitor when have preferable charge and discharge coulomb effect and
Biggish specific capacitance.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Detailed description of the invention
The drawings are intended to provide a further understanding of the invention, and constitutes part of 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 wire；
Fig. 1 (b) is the X-ray powder diffraction figure of Te nano wire；
Fig. 2 (a) is the low power scanning electron microscope (SEM) photograph of 1 products therefrom of embodiment；
Fig. 2 (b) is the high power scanning electron microscope (SEM) photograph of 1 products therefrom of embodiment；
Fig. 2 (c) is the transmission electron microscope picture of 1 products therefrom of embodiment；
Fig. 3 is the X-ray powder diffraction figure of 1 products therefrom of embodiment；
Fig. 4 is one-dimensional MnO prepared by embodiment 12Cyclic voltammetry curve of the nanotube as electrode material for super capacitor
(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 2 products therefrom of embodiment；
Fig. 7 is the low power scanning electron microscope (SEM) photograph of 3 products therefrom of embodiment；
Fig. 8 is the low power scanning electron microscope (SEM) photograph of 4 products therefrom of embodiment；
Fig. 9 is the low power scanning electron microscope (SEM) photograph of 5 products therefrom of embodiment；
Figure 10 is the low power scanning electron microscope (SEM) photograph of 6 products therefrom of embodiment；
Figure 11 is the low power scanning electron microscope (SEM) photograph of 7 products therefrom of embodiment.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical 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 include by high manganese ion
Redox reaction occurs in the solution with Te nano wire, to prepare one-dimensional MnO2The step of nanotube.
Through the above technical solutions, the present invention utilizes one-dimensional Te nano wire and reducing agent, in simple liquid-phase reaction system
Make MnO4 and Te nano wire that redox reaction occur, to obtain the one-dimensional MnO of tubulose layering2Nano-tube material.Hair
Bright people speculates that Te nano-material plays a part of template in above-mentioned reaction process, can not only play the role of braced frame, together
When can be dissolved, therefore Te nano wire need not be eliminated, reaction process is more simple, controllable.One-dimensional MnO is prepared with existing2It receives
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
There is preferable charge and discharge coulomb effect and biggish specific capacitance when grade capacitor electrode material.
In the above-mentioned technical solutions, there are many selections for the dosage molar ratio of Te nano wire and MnO4, in order to make to prepare
One-dimensional MnO2Naraotube yield height and morphology controllable, it is preferable that in solution, relative to the Te nano wire of 8-12.8mg, Gao Meng
The amount of the substance of acid group are as follows: 0.0024-0.0036mol.
In the above-mentioned technical solutions, selection there are many redox reaction conditions of Te nano wire and MnO4, in order to
Make the one-dimensional MnO of preparation2Naraotube yield is high and morphology controllable, redox reaction carry out under conditions of adding the concentrated sulfuric acid.
In the above-mentioned technical solutions, the concentrated sulfuric acid is the aqueous solution of bright sulfur acid of the mass fraction 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, there are many redox reaction conditions and reaction process of Te nano wire and MnO4
Selection, in order to make the one-dimensional MnO of preparation2Naraotube yield height and morphology controllable, it is preferable that the preparation method includes following step
It is rapid: a, the nanowire suspended liquid of Te being added in the solution containing high manganese ion, the concentrated sulfuric acid is added under stiring, continues to stir
Certain time t1 obtains mixed liquor M1；B, M1 is heated and stirs certain time t2 and obtain product M2；C, by products therefrom M2 from
The heart washs, and drying obtains one-dimensional MnO2Nano-tube material.
In the above-mentioned technical solutions, the nanowire suspended liquid of Te is added there are many modes in solution, is such as rapidly injected, drips
Add, dropwise be added dropwise etc. modes, be able to achieve the present invention, be illustrated in a manner of being added dropwise in embodiment later.
In this specific embodiment, in order to make preparation one-dimensional MnO2Naraotube yield height and morphology controllable, it is preferable that
In terms of parts by volume, the solution containing high manganese ion for being 0.08-0.12mol/L relative to 30mL concentration, the Te of 1.6mg/mL
The dosage of nanowire suspended liquid is 5-8mL, and the dosage for the concentrated sulfuric acid that mass fraction is 98% is 10~550 μ L.
In this specific embodiment, in order to make preparation one-dimensional MnO2Naraotube yield height and morphology controllable, it is preferable that
Preparation method at least meets: t1 8-12min；And/or t2 1-2h；And/or heating temperature is 80 DEG C~100 in step b
℃。
In the above-mentioned technical solutions, the source of high manganese ion can there are many selections, as long as aqueous solution can be dissolved in
In, the present invention can be realized by generating high manganese ion.In order to make the one-dimensional MnO of preparation2Naraotube 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 of barium, zinc permanganate, magnesium permanganate, permanganic acid mercury, cadmium permanganate and permanganic acid rubidium are a variety of.
Te nano wire, which has, is horizontally limited in 100 nanometers of one-dimentional structures below, aspect ratio 1000 with
On, therefore commonly known as one-dimensional material.
In the above-mentioned technical solutions, Te nano wire can be obtained by a variety of preparation methods, such as by TeO2, polyethylene pyrrole
Pyrrolidone and NaOH are dissolved in ethylene glycol, and Te nano wire can be obtained in reaction certain time.
Further, Te nano wire is prepared by the following technical programs: relative to 0.25mmol TeO2, will
0.25mmol TeO2Powder, 0.2g polyvinylpyrrolidone (PVP) and 10mmol NaOH are dissolved in 16mL ethylene glycol, pass through
Heating for dissolving forms clear solution, is then transferred in 20mL polytetrafluoroethyllining lining autoclave, and Te is obtained after 180 DEG C of reaction 4h
Nano wire.
After above-mentioned 16mgTe nano wire acetone and deionization are washed 2-6 times, it is dispersed in 10mL deionized water
Obtain the nanowire suspended liquid of Te of 1.6mg/mL.
The present invention also provides a kind of one-dimensional MnO2Nanotube, according to previously described one-dimensional MnO2The preparation method of nanotube
It is prepared.Resulting one-dimensional MnO2Nanotube has fake capacitance property, is used to have when electrode material for super capacitor preferable
Charge and discharge coulomb effect and biggish specific capacitance.
The one-dimensional MnO that the present invention synthesizes2There are many selections for tube diameters, it is preferable that the one-dimensional MnO2Nanotube
Diameter is 140-160nm.
The one-dimensional MnO that the present invention synthesizes2There are many selections for the structure of nanotube, it is preferable that the one-dimensional MnO2Nanotube
For tubulose layered structure.Tubulose layered structure, which refers to, has low dimensional structures unit (such as zero-dimension nano particle, one in nanotube surface
Wiener rice noodles/stick, two-dimensional nano piece etc.) composition micro/nano structure, the one-dimensional MnO that the present invention synthesizes2Nanotube is by MnO2
The tubulose layered structure of nanometer sheet composition.
The present invention also provides a kind of according to previously described one-dimensional MnO2Nanotube is as the application in electrode material.It should
One-dimensional MnO2Nanotube has fake capacitance property, is used to have preferable charge and discharge coulomb effect when electrode material for super capacitor
With biggish specific capacitance.
Below 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, is purchased from Shanghai Aladdin biochemical technology limited liability company,
Other are conventional commercial products.
Preparation example 1
(1) 0.25mmol TeO is taken2Powder, 0.2g polyvinylpyrrolidone (PVP) and 10mmol NaOH are dissolved in
In 16mL ethylene glycol, clear solution is formed by dissolving by heating, is then transferred in 20mL polytetrafluoroethyllining lining autoclave,
Te nano wire is obtained after 180 DEG C of reaction 4h；
(2) after 16mg Te nano wire being washed 6 times with acetone and deionized water respectively, it is dispersed in 10mL deionized water
In, obtain the nanowire suspended liquid of Te of 1.6mg/mL.
The low power scanning electron microscope (SEM) photograph of Te nano wire is shown in Fig. 1 (a)；The X-ray powder diffraction figure of Te nano wire is shown in Fig. 1 (b).
Fig. 1 (a) be Te nano wire low power scanning electron microscope (SEM) photograph, it can be seen from Fig. 1 (a) Te nanowire surface it is smooth and
Long, Fig. 1 (b) is the X-ray powder diffraction figure of Te nano wire, is consistent with Te (JCPDS No.04-0555).
Embodiment 1
A, the nanowire suspended liquid of the Te of 8mL 1.6mg/mL is added dropwise to the KMnO of 30mL 0.1mol/L4In solution,
The dense H that 450 μ L mass fractions are 98% is added under stiring2SO4, stir 10min；
B, solution in step (a) is transferred in 50mL round-bottomed flask, in oil bath 80 DEG C of stirring 1.5h；
C, products therefrom is centrifuged, is washed 6 times with deionized water and dehydrated alcohol, 80 DEG C of drying；Obtain one-dimensional MnO2It receives
Nanotube material.
Fig. 2 (a) is the low power scanning electron microscope (SEM) photograph of 1 products therefrom of embodiment, and Fig. 2 (b) is the height of 1 products therefrom of embodiment
Times scanning electron microscope (SEM) photograph, as can be seen from Figure, product are tubulose layered structure, diameter 140-160nm.Fig. 2 (c) is embodiment 1
The transmission electron microscope picture of products therefrom, as seen from the figure apparent tubulose layered structure.
Fig. 3 is the X-ray powder diffraction figure of 1 products therefrom of embodiment, 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 respectively corresponds
(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 of preparation2Nano-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 right
The curve table prescribed electrode of title charge and discharge coulomb effect with higher and preferable capacitor.
Embodiment 2
A, the nanowire suspended liquid of the Te of 8mL 1.6mg/mL is added dropwise to the KMnO of 30mL 0.1mol/L4In solution,
The dense H that 300 μ L mass fractions are 98% is added under stiring2SO4, stir 10min；
B, solution in step (a) is transferred in 50mL round-bottomed flask, in oil bath 80 DEG C of stirring 1.5h；
C, products therefrom is centrifuged, is washed 6 times with deionized water and dehydrated alcohol, 80 DEG C of drying；Obtain one-dimensional MnO2It receives
Nanotube material, morphology characterization respectively correspond Fig. 6.
As seen from Figure 6, product is tubulose layered structure, diameter 140-160nm.
Embodiment 3
A, the nanowire suspended liquid of the Te of 5mL 1.6mg/mL is added dropwise to the KMnO of 30mL 0.08mol/L4In solution,
The dense H that 10 μ L mass fractions are 98% is added under stiring2SO4, stir 8min；
B, solution in step (a) is transferred in 50mL round-bottomed flask, in oil bath 80 DEG C of stirring 1h；
C, products therefrom is centrifuged, is washed 6 times with deionized water and dehydrated alcohol, 80 DEG C of drying；Obtain one-dimensional MnO2It receives
Nanotube material, morphology characterization respectively correspond Fig. 7.
As seen from Figure 7, product is tubulose layered structure, diameter 140-160nm.
Embodiment 4
A, the nanowire suspended liquid of the Te of 8mL 1.6mg/mL is added dropwise to the KMnO of 30mL 0.12mol/L4In solution,
The dense H that 550 μ L mass fractions are 98% is added under stiring2SO4, stir 12 min；
B, solution in step (a) is transferred in 50mL round-bottomed flask, in oil bath 100 DEG C of stirring 2h；
C, products therefrom is centrifuged, is washed 6 times with deionized water and dehydrated alcohol, 100 DEG C of drying；Obtain one-dimensional MnO2It receives
Nanotube material, morphology characterization corresponding diagram 8.
As seen from Figure 8, product is tubulose layered structure, diameter 140-160nm.
Embodiment 5
A, the nanowire suspended liquid of the Te of 5mL 1.6mg/mL is added dropwise to the KMnO of 30mL 0.12mol/L4In solution,
The dense H that 100 μ L mass fractions are 98% is added under stiring2SO4, stir 12 min；
B, solution in step (a) is transferred in 50mL round-bottomed flask, in oil bath 100 DEG C of stirring 2h；
C, products therefrom is centrifuged, is washed 6 times with deionized water and dehydrated alcohol, 100 DEG C of drying；Obtain one-dimensional MnO2It receives
Nanotube material, morphology characterization corresponding diagram 8.
As seen from Figure 9, product is tubulose layered structure, diameter 140-160nm.
Embodiment 6
One-dimensional MnO is prepared according to the method for embodiment 12Nano-tube material, unlike, wherein not adding the concentrated sulfuric acid, obtain
To one-dimensional MnO2Nano-tube material, morphology characterization corresponding diagram 9.
As seen from Figure 10, a large amount of graininess accumulations of product, tubular structure product is less, and layered structure is unobvious.
Embodiment 7
One-dimensional MnO is prepared according to the method for embodiment 12Nano-tube material, unlike, wherein oil bath temperature in step (b)
Degree is 110 DEG C, obtains one-dimensional MnO2Nano-tube material, morphology characterization corresponding diagram 10.
As seen from Figure 11, a large amount of graininess accumulations of product, tubular structure product is less, and layered structure is unobvious.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
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 also be regarded as the disclosure of the present invention.
Claims (9)
1. a kind of one-dimensional MnO2The preparation method of nanotube, which is characterized in that the preparation method include by high manganese ion with
Redox reaction occurs in the solution for Te nano wire, to prepare one-dimensional MnO2The step of nanotube；
Wherein, redox reaction carries out under conditions of adding the concentrated sulfuric acid.
2. preparation method according to claim 1, wherein in solution, relative to the Te nano wire of 8-12.8mg, permanganic acid
The amount of the substance of root are as follows: 0.0024-0.0036mol.
3. preparation method according to claim 1, wherein the preparation method comprises the following steps:
A, the nanowire suspended liquid of Te is added in the solution containing high manganese ion, the concentrated sulfuric acid is added under stiring, continues to stir
Certain time t1 is mixed, mixed liquor M1 is obtained；
B, M1 is heated and stirs certain time t2 and obtain product M2；
C, products therefrom M2 is centrifuged, is washed, drying obtains one-dimensional MnO2Nano-tube material.
4. preparation method according to claim 3, wherein be 0.08- relative to 30mL concentration in terms of parts by volume
The solution containing high manganese ion of 0.12mol/L, the dosage of the nanowire suspended liquid of the Te of 1.6mg/mL are 5-8mL, quality point
Number is 10~550 μ L for the dosage of 98% concentrated sulfuric acid.
5. preparation method according to claim 3, wherein at least meet: t1 be 8-12min and/or, t2 1-2h；With/
Or, heating temperature is 80 DEG C~100 DEG C in step b.
6. 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
One of or it is a variety of.
7. a kind of one-dimensional MnO2Nanotube, which is characterized in that one-dimensional MnO according to claim 1 to 62Nanometer
The preparation method of pipe is prepared.
8. one-dimensional MnO according to claim 72Nanotube, wherein the one-dimensional MnO2Nanotube is tubulose layered structure,
Diameter is 140-160nm.
9. a kind of one-dimensional MnO according to claim 7 or 82Nanotube is as the application in electrode material.
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