CN108059191A - A kind of alkali formula manganese oxide of nano wire pattern and preparation method thereof - Google Patents
A kind of alkali formula manganese oxide of nano wire pattern and preparation method thereof Download PDFInfo
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- CN108059191A CN108059191A CN201810066957.4A CN201810066957A CN108059191A CN 108059191 A CN108059191 A CN 108059191A CN 201810066957 A CN201810066957 A CN 201810066957A CN 108059191 A CN108059191 A CN 108059191A
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- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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Abstract
Alkali formula manganese oxide the invention discloses a kind of nano wire pattern and preparation method thereof, be by manganese acetate, sodium acid carbonate, potassium permanganate be raw material, using deionized water as solvent, be made using simple hydro-thermal method.The method of the present invention adopts water as solvent for the first time, the MnOOH for the superfine nanowire pattern that diameter is about 7 12nm has been prepared in the case of no any adjuvant, and the nano wire has very excellent performance in terms of applied to supercapacitive.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, and in particular to a kind of system of the alkali formula manganese oxide of nano wire pattern
Preparation Method.
Background technology
In recent years, Lee seminars find cobaltosic oxide (Co3O4) etc. as transition metal oxide have higher ratio
One of thermal capacitance and cyclical stability, the electrode material available for ultracapacitor, so far after, transition metal oxide and its spread out
Biology becomes capacitor material most with prospects.Among them, manganese has changeable oxidation number and crystal structure in itself
The defects of type, electronics is caused easily to shift, so as to good chemical property.Therefore, alkali formula manganese oxide obtains
Extensive concern, manganese are+trivalent, itself can aoxidize to obtain trivalent manganese compound, can be used as and prepare that manganese oxide is simple and convenient, ring
The predecessor of border friendly is also commonly used for battery and electrochromic field.It is right with the development of current nano material science and technology
The pattern control of MnOOH nano materials has become one of research hotspot.
At present, the method for preparing MnOOH nano materials is mainly electrochemical deposition method, reverse micelle method, but both sides
Method operation is relatively difficult, generally requires special experimental instrument and equipment and higher cost, is unfavorable for mass producing.Therefore
It is badly in need of providing a kind of easy to operate and is easy to industrialized method.In recent years, not similar shape was prepared by some solution chemical processes
The MnOOH nano materials of looks are also developed rapidly：Tan project team systems it is standby go out tubular morphology MnOOH；The success of Cao seminars
Prepare rodlike MnOOH；Hu and K.A.M.Ahmed project team systems it is standby go out wire MnOOH.CN102502848A discloses a kind of solvent
The method that hot method prepares alkali formula manganese oxide nano wire, but on the one hand this method uses organic solvent n-butanol as solvent, not environmentally,
On the other hand, the diameter of prepared nano wire is up to 50nm, and performance can't be fully met when preparing ultracapacitor
It is required that.Therefore, a kind of more environmentally-friendly, more excellent performance of nanometer wire MnOOH of exploitation seems very necessary.
The content of the invention
For overcome the deficiencies in the prior art, it is an object of the invention to provide a kind of alkali formula manganese oxide of nano wire pattern
And preparation method thereof, the technical problem to be solved is that solvent is adopted water as, it is prepared into the case of no any adjuvant
To the MnOOH of superfine nanowire pattern.
To realize goal of the invention, the present invention adopts the following technical scheme that：
A kind of preparation method of nano wire pattern alkali formula manganese oxide of the present invention, includes the following steps：
(1) manganese acetate and sodium acid carbonate are taken, is added in deionized water, 1-3h is stirred on magnetic stirring apparatus, is obtained molten
Liquid A；Potassium permanganate is dissolved in deionized water, 1-3h is stirred, obtains solution B；
(2) solution A in step (1) and solution B are transferred to polytetrafluoroethylsubstrate substrate stainless steel reaction after mixing
In kettle, then at a temperature of 120 DEG C -180 DEG C, 12-24h is reacted；After reaction, product is centrifuged, gained precipitation
It is washed successively with deionized water and ethyl alcohol, then is placed in vacuum drying oven and is dried, it is last ground, that is, obtain nano wire pattern alkali
Formula manganese oxide powder.
Preferably：In the solution A, the dosage of manganese acetate, sodium acid carbonate and deionized water be respectively 3-10g, 2-9g,
20-100mL；In the solution B, the dosage of potassium permanganate and deionized water is respectively 2-10g, 40-200mL.It can equal proportion
Amplification.
More preferably：In the solution A, the dosage of manganese acetate, sodium acid carbonate and deionized water be respectively 3.42g,
2.35g、30mL；In the solution B, the dosage of potassium permanganate and deionized water is respectively 2.18g, 50mL.Can equal proportion put
Greatly.
Preferably, temperature dry in step (2) is 70 DEG C, the time is for 24 hours.
The invention also discloses the alkali formula manganese oxide of the preparation-obtained nano wire pattern of the above method, the alkali formula oxidation
Nano wire pattern is presented in manganese, and diameter is in 7-12nm, specific surface area 300-450m2/g。
The alkali formula manganese oxide of gained nano wire pattern of the invention is used as the electrode material of ultracapacitor.
Compared with prior art, technique effect of the invention is：
(1) present invention is only by four kinds of manganese acetate, sodium acid carbonate, potassium permanganate and deionized water inorganic raw materials, using letter
Single hydro-thermal method is to produce the alkali formula manganese oxide of nanowire pattern, and any organic solvent and adjuvant is not used, in ability
Domain belongs to pioneering, has no any report before this and obtains the alkali formula manganese oxide of nanometer wire using water for direct solvent, real
Complete free of contamination process for cleanly preparing is showed；
(2) the alkali formula manganese oxide of the nano wire pattern prepared by the present invention possesses very excellent property, and on the one hand it is in
Existing superfine wire, diameter is only 7-12nm, specific surface area 300-450m2/ g had not had been reported that also accomplished so at this stage
Size, and the alkali formula manganese oxide of above-mentioned nano wire pattern shows fabulous capacitive properties, and under operating current 1A, capacitance C is
480.57F/g has very excellent property in terms of applied to supercapacitive.
Description of the drawings
Fig. 1 is the XRD diagram of the alkali formula oxidation manganese material prepared by the embodiment of the present invention 1；
Fig. 2 is the SEM figures of the alkali formula oxidation manganese material prepared by the embodiment of the present invention 1；
Fig. 3 is the TEM figures of the alkali formula oxidation manganese material prepared by the embodiment of the present invention 1
Fig. 4 aoxidizes the capacitive properties comparison diagram of manganese material for the alkali formula prepared by the embodiment of the present invention 1 and comparative example 1.
Specific embodiment
Technical scheme is further elaborated with reference to embodiment：
Embodiment 1
A kind of preparation method of the alkali formula manganese oxide of nano wire pattern, includes the following steps：
(1) manganese acetate of 3.42g and 2.35g sodium acid carbonates are taken, is added in the deionized water of 30mL, in magnetic stirring apparatus
Upper stirring 2h, obtains solution A；The potassium permanganate of 2.18g is dissolved in 50mL deionized waters, 2h is stirred, obtains solution B；
(2) solution A in step (1) and solution B are transferred to polytetrafluoroethylsubstrate substrate stainless steel reaction after mixing
In kettle, then at a temperature of 180 DEG C, 12h is reacted；After reaction, product is centrifuged, gained precipitation deionized water
Washed successively with ethyl alcohol it is each then be placed in vacuum drying oven that 70 DEG C of drying are for 24 hours, finally ground three times, obtain the alkali formula of sepia
Manganese oxide powder.
Understand that alkali formula manganese oxide manufactured in the present embodiment is presented refering to the SEM figures, TEM figures, XRD diagram of Fig. 1, Fig. 2 and Fig. 3
Elongated nano wire pattern, diameter are about 7-8nm nanometers, and are monoclinic system, do not find dephasign peak, show the purity of product
Compare high；After tested, the specific surface area of the present embodiment products therefrom is 450m2/g。
Embodiment 2
A kind of preparation method of nano wire pattern alkali formula manganese oxide, includes the following steps：
(1) manganese acetate of 3.42g and 2.35g sodium acid carbonates are taken, is added in the deionized water of 30mL, in magnetic stirring apparatus
Upper stirring 2h, obtains solution A；The potassium permanganate of 2.18g is dissolved in 50mL deionized waters again, 2h is stirred, obtains solution B；
(2) solution A in step (1) and solution B are transferred to polytetrafluoroethylsubstrate substrate stainless steel reaction after mixing
In kettle, then at a temperature of 120 DEG C, 12h is reacted；After reaction, product is centrifuged, gained precipitation deionized water
Washed successively with ethyl alcohol it is each then be placed in vacuum drying oven that 70 DEG C of drying are for 24 hours, finally ground three times, obtain the alkali formula of sepia
Manganese oxide powder.
Through characterization, elongated nano wire pattern is presented in the alkali formula manganese oxide prepared by the present embodiment, and diameter is about that 12nm receives
Rice, specific surface area 300m2/ g, and be monoclinic system, it does not find dephasign peak, shows that the purity of product is higher.
Embodiment 3
A kind of preparation method of nano wire pattern alkali formula manganese oxide, includes the following steps：
(1) manganese acetate of 3g and 2g sodium acid carbonates are taken, is added in the deionized water of 25mL, is stirred on magnetic stirring apparatus
2h obtains solution A；The potassium permanganate of 2g is dissolved in 40mL deionized waters again, 2h is stirred, obtains solution B；
(2) solution A in step (1) and solution B are transferred to polytetrafluoroethylsubstrate substrate stainless steel reaction after mixing
In kettle, then at a temperature of 150 DEG C, 12h is reacted；After reaction, product is centrifuged, gained precipitation deionized water
Washed successively with ethyl alcohol it is each then be placed in vacuum drying oven that 70 DEG C of drying are for 24 hours, finally ground three times, obtain the alkali formula of sepia
Manganese oxide powder.
Through characterization, elongated nano wire pattern is presented in the alkali formula manganese oxide prepared by the present embodiment, and diameter is about that 10nm receives
Rice, specific surface area 375.11m2/ g, and be monoclinic system, it does not find dephasign peak, shows that the purity of product is higher.
Embodiment 4
A kind of preparation method of nano wire pattern alkali formula manganese oxide, includes the following steps：
(1) manganese acetate of 6.8g and 4.6g sodium acid carbonates are taken, is added in the deionized water of 60mL, on magnetic stirring apparatus
3h is stirred, obtains solution A；The potassium permanganate of 4.3g is dissolved in 100mL deionized waters again, 2h is stirred, obtains solution B；
(2) solution A in step (1) and solution B are transferred to polytetrafluoroethylsubstrate substrate stainless steel reaction after mixing
In kettle, then at a temperature of 180 DEG C, 16h is reacted；After reaction, product is centrifuged, gained precipitation deionized water
Washed successively with ethyl alcohol it is each then be placed in vacuum drying oven that 70 DEG C of drying are for 24 hours, finally ground three times, obtain the alkali formula of sepia
Manganese oxide powder.
Through characterization, elongated nano wire pattern is presented in the alkali formula manganese oxide prepared by the present embodiment, and diameter is about 9-10nm
Nanometer, specific surface area 413.28m2/ g, and be monoclinic system, it does not find dephasign peak, shows that the purity of product is higher.
Embodiment 5
A kind of preparation method of nano wire pattern alkali formula manganese oxide, includes the following steps：
(1) manganese acetate of 10g and 9g sodium acid carbonates are taken, is added in the deionized water of 100mL, is stirred on magnetic stirring apparatus
3h is mixed, obtains solution A；The potassium permanganate of 9g is dissolved in 200mL deionized waters again, 3h is stirred, obtains solution B；
(2) solution A in step (1) and solution B are transferred to polytetrafluoroethylsubstrate substrate stainless steel reaction after mixing
In kettle, then at a temperature of 150 DEG C, 16h is reacted；After reaction, product is centrifuged, gained precipitation deionized water
Washed successively with ethyl alcohol it is each then be placed in vacuum drying oven that 70 DEG C of drying are for 24 hours, finally ground three times, obtain the alkali formula of sepia
Manganese oxide powder.
Through characterization, elongated nano wire pattern is presented in the alkali formula manganese oxide prepared by the present embodiment, and diameter is about that 10nm receives
Rice, specific surface area 378.96m2/ g, and be monoclinic system, it does not find dephasign peak, shows that the purity of product is higher.
Comparative example 1
A kind of preparation method of alkali formula manganese oxide, includes the following steps：
(1) manganese acetate of 3.42g and 2.35g sodium acid carbonates are taken, is added in the n-butanol of 30mL, on magnetic stirring apparatus
2h is stirred, obtains solution A；The potassium permanganate of 2.18g is dissolved in 50mL n-butanols again, 2h is stirred, obtains solution B；
(2) solution A in step (1) and solution B are transferred to polytetrafluoroethylsubstrate substrate stainless steel reaction after mixing
In kettle, then at a temperature of 180 DEG C, 12h is reacted；After reaction, product is centrifuged, gained precipitation deionized water
Washed successively with ethyl alcohol it is each then be placed in vacuum drying oven that 70 DEG C of drying are for 24 hours, finally ground three times, obtain the alkali formula of sepia
Manganese oxide powder.
Through measuring point, the graininess for the material presentation size unevenness that the present embodiment is prepared, granular size 50-100nm,
Specific surface area is 80-120m2/g。
The capacitive properties of 1 products therefrom of embodiment 1 and comparative example is measured below, method is as follows：
(1) by prepared alkali formula manganese oxide powder, acetylene black, ptfe micropowder according to 8:1:1 mass ratio is total to
It weighs 6mg to be placed in mortar, adds in 4 drop N-Methyl pyrrolidones, be fully ground uniformly；
(2) prepare the nickel foam of 1cm × 3cm standard, handled three times, dried successively with deionized water and ethyl alcohol, claimed
Weight；
(3) after the sample of step 1 is uniformly applied in nickel foam, the dry 12h at 60 DEG C；
(4) by dried nickel foam sample under 10MPa pressure, tabletting is carried out, is weighed；
(5) under 6mol/LKOH electrolyte, by electrochemical workstation to the capacitive character of nano wire pattern alkali formula manganese oxide
Matter is tested, and wherein operating current is respectively 10A, 8A, 5A, 3A, 1A.
Fig. 4 aoxidizes capacitive properties pair of the manganese material under 1A operating currents for the alkali formula prepared by embodiment 1 and comparative example 1
Than figure, it can be seen that for the alkali formula manganese oxide of 1 gained nano wire pattern of embodiment under operating current 1A, capacitance C is 480.57F/g；
And the granular alkali formula manganese oxide of the gained of comparative example 1 is under operating current 1A, capacitance C is 272.73F/g.
In addition, the alkali formula manganese oxide of 1 gained nano wire pattern of embodiment is under operating current 10A, 8A, 5A, 3A, capacitance C
Respectively 369.21,388.52,425 and 465.52F/g；And the 1 granular alkali formula manganese oxide of gained of comparative example is in operating current
Under 10A, 8A, 5A, 3A, capacitance C is respectively 193.17,196.22,203.98 and 244F/g.
It these are only exemplary embodiment of the present invention, be not intended to limit the invention, all spirit in the present invention
With all any modification, equivalent and improvement made within principle etc., should all be included in the protection scope of the present invention.
Claims (5)
1. the preparation method of the alkali formula manganese oxide of a kind of nano wire pattern, which is characterized in that include the following steps：
(1) manganese acetate and sodium acid carbonate are taken, is added in deionized water, 1-3h is stirred on magnetic stirring apparatus, obtains solution A；
Potassium permanganate is dissolved in deionized water, 1-3h is stirred, obtains solution B；
(2) solution A in step (1) and solution B are transferred to after mixing in polytetrafluoroethylsubstrate substrate stainless steel cauldron,
Then at a temperature of 120 DEG C -180 DEG C, 12-24h is reacted；After reaction, product is centrifuged, gained precipitation spend from
Sub- water and ethyl alcohol wash successively, then are placed in vacuum drying oven and are dried, last ground, that is, obtain nano wire pattern alkali formula oxygen
Change manganese powder end.
2. preparation method according to claim 1, it is characterised in that：
In the solution A, the dosage of manganese acetate, sodium acid carbonate and deionized water is respectively 3-10g, 2-9g, 20-100mL；
In the solution B, the dosage of potassium permanganate and deionized water is respectively 2-10g, 40-200mL.
3. preparation method according to claim 2, it is characterised in that：
In the solution A, the dosage of manganese acetate, sodium acid carbonate and deionized water is respectively 3.42g, 2.35g, 30mL；
In the solution B, the dosage of potassium permanganate and deionized water is respectively 2.18g, 50mL.
4. preparation method according to claim 1, it is characterised in that：Dry temperature is 70 DEG C in step (2), the time is
24h。
5. a kind of alkali formula manganese oxide of the preparation-obtained nano wire pattern of the method as any one of claim 1-4,
It is characterized in that：Nano wire pattern is presented in the alkali formula manganese oxide, and diameter is in 7-12nm, specific surface area 300-450m2/g。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109455764A (en) * | 2018-11-08 | 2019-03-12 | 广东工业大学 | A kind of preparation method of MnOOH |
| CN109873139A (en) * | 2019-02-03 | 2019-06-11 | 桂林理工大学 | The preparation and application of γ-MnOOH/SFC nanometer combined electrode material |
| CN110767898A (en) * | 2019-09-30 | 2020-02-07 | 合肥国轩高科动力能源有限公司 | Manganese-based nanowire bundle and preparation method and application thereof |
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| CN102502848A (en) * | 2011-10-27 | 2012-06-20 | 湖南科技大学 | Solvothermal preparation method for alkali manganese oxide nanowires |
| CN102531064A (en) * | 2010-12-13 | 2012-07-04 | 西安迈克森新材料有限公司 | Method used for preparing hydroxy manganese oxide superfine single crystal nanometer line |
| CN102765759A (en) * | 2011-05-02 | 2012-11-07 | 三星康宁精密素材株式会社 | Manganese oxide nanowire, rechargeable battery including the same and method of producing manganese oxide |
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| CN102041553A (en) * | 2010-12-21 | 2011-05-04 | 浙江大学 | Preparation method and application of crystalline-state beta-MnOOH nanowire |
| CN102765759A (en) * | 2011-05-02 | 2012-11-07 | 三星康宁精密素材株式会社 | Manganese oxide nanowire, rechargeable battery including the same and method of producing manganese oxide |
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| CN109455764A (en) * | 2018-11-08 | 2019-03-12 | 广东工业大学 | A kind of preparation method of MnOOH |
| CN109455764B (en) * | 2018-11-08 | 2021-07-06 | 广东工业大学 | Preparation method of MnOOH |
| CN109873139A (en) * | 2019-02-03 | 2019-06-11 | 桂林理工大学 | The preparation and application of γ-MnOOH/SFC nanometer combined electrode material |
| CN109873139B (en) * | 2019-02-03 | 2022-03-22 | 桂林理工大学 | Preparation and application of gamma-MnOOH/SFC nano composite electrode material |
| CN110767898A (en) * | 2019-09-30 | 2020-02-07 | 合肥国轩高科动力能源有限公司 | Manganese-based nanowire bundle and preparation method and application thereof |
| CN110767898B (en) * | 2019-09-30 | 2022-06-07 | 合肥国轩高科动力能源有限公司 | Manganese-based nanowire bundle and preparation method and application thereof |
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