CN102956359A - Manganese dioxide/ferric oxide nanometer composite material as well as preparation method and application thereof - Google Patents
Manganese dioxide/ferric oxide nanometer composite material as well as preparation method and application thereof Download PDFInfo
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- CN102956359A CN102956359A CN2012104020734A CN201210402073A CN102956359A CN 102956359 A CN102956359 A CN 102956359A CN 2012104020734 A CN2012104020734 A CN 2012104020734A CN 201210402073 A CN201210402073 A CN 201210402073A CN 102956359 A CN102956359 A CN 102956359A
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Abstract
The invention relates to a manganese dioxide/ferric oxide nanometer composite material as well as a preparation method and application thereof, and belongs to a preparation technology and application field of inorganic matter composite materials. The structure of the composite material is characterized by utilizing a manganese dioxide nanometer bar as main body and covering nanometer ferric oxide granules on the surface of the manganese dioxide nanometer bar, wherein the composite material is prepared by utilizing potassium ferrocyanide and potassium permanganate as raw materials, and performing hydro-thermal synthesis, solid-liquid separation and drying steps on the raw materials, and the prepared inorganic nanometer composite material has excellent supercapacitor property. The preparation method of manganese dioxide/ferric oxide nanometer composite material provided by the invention is simple in structure and low in cost, and no dispersing agent or template is added; furthermore, the obtained manganese dioxide/ferric oxide nanometer composite material has the advantages of strong controllability, excellent supercapacitor property, and the like, so that the manganese dioxide/ferric oxide nanometer composite material has brilliant industrial application prospect.
Description
Technical field
[0001] the invention belongs to inorganic matter Nano-composite materials technical field, be specifically related to a kind of manganese dioxide/ferric oxide nano composite material, its preparation method, and by the composite electrode of described manganese dioxide/ferric oxide nano composite material preparation.
Background technology
[0002] present, super capacitor material mainly comprises porous carbon material, transition metal oxide, conducting polymer and compound or composite material etc.The chemical property of transition metal oxide is good, the electric double layer capacitance that not only has separation of charge on the electrode/electrolyte to produce, also have by fast, faraday's electric capacity of producing of highly reversible chemisorbed/desorption and oxidation/reduction reaction.The reserves of manganese dioxide are abundant, cheap and environmentally friendly, receive much concern in the research of electrode material for super capacitor in recent years.But the manganese dioxide conductivity is low to have limited its practical application as electrode material to a great extent, therefore by coming its conductivity with other transition metal oxides are compound, improves the capacitance of electrode material.
[0003] preparation method of manganese dioxide and compound or composite material has liquid-phase precipitation method, sol-gel process, electrochemical deposition method, low-temperature solid-phase method, template and hydro thermal method etc.Wherein liquid-phase precipitation method [J Power Sources, 2009,187 (1): 284-289] synthesis temperature is had relatively high expectations and the particle for preparing is easy to reunite; Sol-gel process [Mater. Lett., 2010,64 (24): 2670-2 672] is washed with the impact of drying condition larger, and product yield is low, and manufacturing cycle is longer; The high easily brine electrolysis of electrochemical deposition method [J Power Sources, 2010,195 (7): 2 110-2 117] sedimentation potential, energy consumption is large; The contact of low-temperature solid-phase method [J Alloys. Compd., 2010,507 (2): 526-530] powder is inhomogeneous and reaction is insufficient; It is complicated that template [J Power Sources, 2007,164 (2): 953-958] is removed template procedure; Hydro thermal method [J Cryst Growth, 2008,310 (3): 716-722] can be prepared the manganese bioxide material of various crystal structures and pattern, becomes study hotspot in recent years.Need not to add template Hydrothermal Synthesis manganese dioxide/ferric oxide nano composite material by potassium ferrocyanide and potassium permanganate at present and not yet see report.
Summary of the invention
[0004] the invention discloses a kind of manganese dioxide/ferric oxide nano composite manufacture method, purpose is to limit the problem that use on border in fact for single manganese dioxide conductivity is low, proposes a kind of manganese dioxide that improves manganese dioxide conductivity and super capacitor performance thereof/ferric oxide nano composite manufacture method.
[0005] purpose of the present invention can be implemented by the following technical programs:
[0006] the invention discloses a kind of manganese dioxide/ferric oxide nano composite manufacture method, it is characterized in that may further comprise the steps:
[0007] (1) joins potassium ferrocyanide in the liquor potassic permanganate, and the mol ratio that makes iron and manganese is the transparent mixed solution of 2～4:1;
[0008] (2) import the mixed solution that step (1) makes in the hydrothermal reaction kettle, carry out hydro-thermal reaction 10～72 hours under 120 ℃～160 ℃ temperature, make suspension;
[0009] (3) suspension filtered that step (2) is made, the filter cake that obtains washs with distilled water, and then oven dry namely makes manganese dioxide/ferric oxide nano composite material.
[0010] among the above-mentioned preparation method, can not use any dispersant and/or template.
[0011] among the above-mentioned preparation method, the concentration of liquor potassic permanganate is preferably 0.001～0.1mol/L.
[0012] among the above-mentioned preparation method, the oven dry in the step (3) is preferably carried out under 40-90 ℃.
[0013] the present invention also provides a kind of manganese dioxide/ferric oxide nano composite material, and the structure of described manganese dioxide/ferric oxide nano composite material is take manganese dioxide nano-rod as main body, and the nano-sized iron oxide particle in the surface coverage of manganese dioxide nano-rod.
[0014] the present invention also provides a kind of composite electrode, it is characterized in that, the manganese dioxide that described composite electrode is made by the method for the invention/ferric oxide nano composite material and conductive carbon and adhesive mixed pressuring plate make, manganese dioxide/ferric oxide nano composite material wherein: conductive carbon: the mass ratio of adhesive is 70～80:20～15:10～5, is preferably 75:20:5.
[0015] the present invention can with adhesive be selected from Kynoar, polytetrafluoroethylene and/or butadiene-styrene rubber.
[0016] the ratio electric capacity by the composite electrode that described manganese dioxide/the ferric oxide nano composite material makes is larger, be 350-700F/g, and the good cycling stability of described composite electrode, after discharging and recharging for 2000 times specific capacity still remain on original 86% or more than.
[0017] advantage of the present invention and good effect are:
[0018] (1) manganese dioxide/ferric oxide nano composite material has remedied the defective of single manganese dioxide poorly conductive.
[0019] (2) manganese dioxide/ferric oxide nano composite manufacture method simple, easily row, cost is low, pattern is controlled, and is pollution-free.
[0020] good physical performance of (3) manganese dioxide/ferric oxide nano composite material has that specific area is large, granularity is little and good dispersion.
[0021] (4) manganese dioxide/ferric oxide nano composite material has good super capacitor performance: the large and good cycling stability than electric capacity.
Description of drawings
[0022] Fig. 1 is the SEM figure of the manganese dioxide/ferric oxide nano composite material of the method for the invention preparation.
[0023] Fig. 2 is the XRD figure of the manganese dioxide/ferric oxide nano composite material of the method for the invention preparation.
Embodiment
[0024] the present invention makes further detailed description to the specific embodiment of the present invention by the following specific embodiments.
Embodiment 1
[0025] (1) joins potassium ferrocyanide in the 0.002 mol/L liquor potassic permanganate, makes iron: the transparent mixed solution of mol ratio 3 ︰ 1 of manganese.
[0026] (2) import the mixed solution that step (1) makes in the hydrothermal reaction kettle, carry out hydro-thermal reaction 24 hours under 120 ℃, make suspension.
[0027] (3) suspension filtered that step (2) is made, filter cake washs with distilled water, then dries under 60 ℃ of temperature, namely makes manganese dioxide/ferric oxide nano composite material.
[0028] (4) will make composite material that step (3) makes and conductive carbon, polytetrafluoroethylene in mass ratio the 75:20:5 mixed pressuring plate make composite electrode.In three-electrode system, the ratio electric capacity of the composite electrode for preparing in the metabisulfite solution of 1 mol/L reaches 530 F/g, discharges and recharges rear specific capacity for 2000 times and remains on original 92%.
Embodiment 2
[0029] (1) joins potassium ferrocyanide and makes iron in the 0.002 mol/L liquor potassic permanganate: the transparent mixed solution of mol ratio 3 ︰ 1 of manganese.
[0030] (2) import the mixed solution that step (1) makes in the hydrothermal reaction kettle, carry out hydro-thermal reaction 48 hours under 120 ℃, make suspension.
[0031] (3) suspension filtered that step (2) is made, filter cake washs with distilled water, then dries under 60 ℃ of temperature, namely makes manganese dioxide/ferric oxide nano composite material.
[0032] (4) composite material that step (3) is made and conductive carbon, Kynoar in mass ratio the 75:20:5 mixed pressuring plate make composite electrode.In three-electrode system, the ratio electric capacity of composite electrode in the metabisulfite solution of 1 mol/L for preparing is reached 462 F/g, discharge and recharge rear specific capacity for 2000 times and remain on original 87%.
Embodiment 3
[0033] (1) joins potassium ferrocyanide and makes iron in the 0.01 mol/L liquor potassic permanganate: the transparent mixed solution of mol ratio 3 ︰ 1 of manganese.
[0034] (2) import the mixed solution that step (1) makes in the hydrothermal reaction kettle, carry out hydro-thermal reaction 48 hours under 150 ℃, make suspension.
[0035] (3) suspension filtered that step (2) is made, filter cake washs with distilled water, then dries under 60 ℃ of temperature, namely makes manganese dioxide/ferric oxide nano composite material.
[0036] (4) composite material that step (3) is made and conductive carbon, butadiene-styrene rubber in mass ratio the 75:20:5 mixed pressuring plate make composite electrode.In three-electrode system, the ratio electric capacity of composite electrode in the metabisulfite solution of 1 mol/L for preparing is reached 380 F/g, discharge and recharge rear specific capacity for 2000 times and remain on original 86%.
Embodiment 4
[0037] (1) joins potassium ferrocyanide and makes iron in the 0.005 mol/L liquor potassic permanganate: the transparent mixed solution of mol ratio 2 ︰ 1 of manganese.
[0038] (2) import the mixed solution that step (1) makes in the hydrothermal reaction kettle, carry out hydro-thermal reaction 24 hours under 150 ℃, make suspension.
[0039] (3) suspension filtered that step (2) is made, filter cake washs with distilled water, then dries under 90 ℃ of temperature, namely makes manganese dioxide/ferric oxide nano composite material.
[0040] (4) composite material that step (3) is made and conductive carbon, butadiene-styrene rubber in mass ratio the 80:15:5 mixed pressuring plate make composite electrode.In three-electrode system, the ratio electric capacity of composite electrode in the metabisulfite solution of 1 mol/L for preparing is reached 653 F/g, discharge and recharge rear specific capacity for 2000 times and remain on original 90%.
Embodiment 5
[0041] (1) joins potassium ferrocyanide and makes iron in the 0.006 mol/L liquor potassic permanganate: the transparent mixed solution of mol ratio 4 ︰ 1 of manganese.
[0042] (2) import the mixed solution that step (1) makes in the hydrothermal reaction kettle, carry out hydro-thermal reaction 24 hours under 130 ℃, make suspension.
[0043] (3) suspension filtered that step (2) is made, filter cake washs with distilled water, then dries under 90 ℃ of temperature, namely makes manganese dioxide/ferric oxide nano composite material.
[0044] (4) composite material that step (3) is made and conductive carbon, Kynoar in mass ratio the 70:20:10 mixed pressuring plate make composite electrode.In three-electrode system, the ratio electric capacity of composite electrode in the metabisulfite solution of 1 mol/L for preparing is reached 542 F/g, discharge and recharge rear specific capacity for 2000 times and remain on original 88%.
Embodiment 6
[0045] (1) joins potassium ferrocyanide and makes iron in the 0.01 mol/L liquor potassic permanganate: the transparent mixed solution of mol ratio 3.5 ︰ 1 of manganese.
[0046] (2) import the mixed solution that step (1) makes in the hydrothermal reaction kettle, carry out hydro-thermal reaction 12 hours under 140 ℃, make suspension.
[0047] (3) suspension filtered that step (2) is made, filter cake washs with distilled water, then dries under 80 ℃ of temperature, namely makes manganese dioxide/ferric oxide nano composite material.
[0048] (4) composite material that step (3) is made and conductive carbon, polytetrafluoroethylene in mass ratio the 78:14:8 mixed pressuring plate make composite electrode.In three-electrode system, the ratio electric capacity of composite electrode in the metabisulfite solution of 1 mol/L for preparing is reached 412 F/g, discharge and recharge rear specific capacity for 2000 times and remain on original 86%.
Embodiment 7
[0049] (1) joins potassium ferrocyanide and makes iron in the 0.009 mol/L liquor potassic permanganate: the transparent mixed solution of mol ratio 2.5 ︰ 1 of manganese.
[0050] (2) import the mixed solution that step (1) makes in the hydrothermal reaction kettle, carry out hydro-thermal reaction 36 hours under 160 ℃, make suspension.
[0051] (3) suspension filtered that step (2) is made, filter cake washs with distilled water, then dries under 80 ℃ of temperature, namely makes manganese dioxide/ferric oxide nano composite material.
[0052] (4) composite material that step (3) is made and conductive carbon, Kynoar in mass ratio the 80:15:5 mixed pressuring plate make composite electrode.In three-electrode system, the ratio electric capacity of composite electrode in the metabisulfite solution of 1 mol/L for preparing is reached 398 F/g, discharge and recharge rear specific capacity for 2000 times and remain on original 88%.
Claims (10)
1. manganese dioxide/ferric oxide nano composite manufacture method is characterized in that may further comprise the steps:
(1) potassium ferrocyanide is joined in the liquor potassic permanganate, the mol ratio that makes iron and manganese is the transparent mixed solution of 2～4:1;
(2) mixed solution that step (1) is made imports in the hydrothermal reaction kettle, carries out hydro-thermal reaction 10～72 hours under 120 ℃～160 ℃ temperature, makes suspension;
(3) suspension filtered that step (2) is made, the filter cake that obtains washs with distilled water, and then oven dry namely makes manganese dioxide/ferric oxide nano composite material.
2. manganese dioxide as claimed in claim 1/ferric oxide nano composite manufacture method is characterized in that, does not use any dispersant and/or template among the described preparation method.
3. manganese dioxide as claimed in claim 1 or 2/ferric oxide nano composite manufacture method is characterized in that, the concentration of liquor potassic permanganate is 0.001～0.1mol/L.
4. a kind of manganese dioxide as claimed in claim 1 or 2/ferric oxide nano composite manufacture method is characterized in that, the oven dry in the described step (3) is carried out under 40-90 ℃.
5. the manganese dioxide of method preparation/ferric oxide nano composite material as described in arbitrary such as claim 1-4, the structure of described manganese dioxide/ferric oxide nano composite material is take manganese dioxide nano-rod as main body, and the nano-sized iron oxide particle in the surface coverage of manganese dioxide nano-rod.
6. composite electrode, it is characterized in that, the manganese dioxide that described composite electrode is made by the arbitrary described method of claim 1-4/ferric oxide nano composite material and conductive carbon and adhesive mixed pressuring plate make, wherein manganese dioxide/ferric oxide nano composite material: conductive carbon: the mass ratio of adhesive is 70～80:20～15:10～5.
7. composite electrode as claimed in claim 6 is characterized in that, described adhesive is selected from Kynoar, polytetrafluoroethylene and/or butadiene-styrene rubber.
8. such as claim 6 or 7 described composite electrodes, it is characterized in that described manganese dioxide/ferric oxide nano composite material: conductive carbon: the mass ratio of adhesive is 75:20:5.
9. such as claim 6 or 7 described composite electrodes, it is characterized in that, the ratio electric capacity of described composite electrode is 350～700F/g.
10. such as claim 6 or 7 described composite electrodes, it is characterized in that, described composite electrode specific capacity after discharging and recharging for 2000 times remain on original 86% or more than.
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| CN103227321A (en) * | 2013-03-27 | 2013-07-31 | 山东大学 | MnOx/Fe2O3 nanocomposite used for negative electrode of lithium ion battery and preparation method and application of MnOx/Fe2O3 nanocomposite |
| CN104992850A (en) * | 2015-07-13 | 2015-10-21 | 同济大学 | Fe3O4/MnO2/RGO material and preparation method and application thereof |
| CN105869915A (en) * | 2016-06-02 | 2016-08-17 | 中南大学 | Manganese dioxide nano-rod composite electrode and preparation method and application thereof |
| CN105895387A (en) * | 2014-10-10 | 2016-08-24 | 南京大学 | Spherical porous Fe3O4/MnO2 supercapacitor material and preparation method thereof |
| CN106099058A (en) * | 2016-06-29 | 2016-11-09 | 渤海大学 | A kind of preparation method of manganese sesquioxide managnic oxide/tin ash composite nano materials |
| WO2016192311A1 (en) * | 2015-06-05 | 2016-12-08 | 中国科学院生态环境研究中心 | Hollow iron-manganese composite material prepared by etching template process and application thereof |
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| CN106571243A (en) * | 2016-10-19 | 2017-04-19 | 上海应用技术大学 | Mesoporous iron oxide/manganese oxide/carbon composite nanomaterial, preparation method and application thereof |
| CN106607045A (en) * | 2015-10-26 | 2017-05-03 | 中国石油化工股份有限公司 | Preparation and application of iron oxide-doped nanometer manganese dioxide catalyst |
| WO2018184182A1 (en) * | 2017-04-07 | 2018-10-11 | 深圳市佩成科技有限责任公司 | Electrode manufacturing method for supercapacitor |
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| US10493425B2 (en) | 2015-06-05 | 2019-12-03 | Research Center For Eco-Environmental Sciences, Chinese Academy Of Sciences | Hollow iron-manganese composite material prepared by etching template process and application thereof |
| CN104992850A (en) * | 2015-07-13 | 2015-10-21 | 同济大学 | Fe3O4/MnO2/RGO material and preparation method and application thereof |
| CN104992850B (en) * | 2015-07-13 | 2017-07-28 | 同济大学 | A kind of Fe3O4/MnO2/ RGO materials and preparation method and application |
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| CN105869915A (en) * | 2016-06-02 | 2016-08-17 | 中南大学 | Manganese dioxide nano-rod composite electrode and preparation method and application thereof |
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| CN106099058B (en) * | 2016-06-29 | 2019-01-04 | 渤海大学 | A kind of preparation method of manganese sesquioxide managnic oxide/stannic oxide composite nano materials |
| CN106229154B (en) * | 2016-08-23 | 2018-08-31 | 宁波中车新能源科技有限公司 | A kind of ultracapacitor aoxidizing combination electrode material based on nanometer ferromanganese |
| CN106229154A (en) * | 2016-08-23 | 2016-12-14 | 宁波中车新能源科技有限公司 | A kind of ultracapacitor based on nanometer ferromanganese oxidation combination electrode material |
| CN106571243A (en) * | 2016-10-19 | 2017-04-19 | 上海应用技术大学 | Mesoporous iron oxide/manganese oxide/carbon composite nanomaterial, preparation method and application thereof |
| CN106571243B (en) * | 2016-10-19 | 2018-03-20 | 上海应用技术大学 | A kind of mesoporous iron oxide/manganese oxide/carbon composite nano-material, preparation method and applications |
| WO2018184182A1 (en) * | 2017-04-07 | 2018-10-11 | 深圳市佩成科技有限责任公司 | Electrode manufacturing method for supercapacitor |
| CN109449005A (en) * | 2018-11-16 | 2019-03-08 | 华中师范大学 | Integrate supercapacitor |
| CN110627126A (en) * | 2019-10-24 | 2019-12-31 | 福州大学 | Preparation and application of self-supporting ultrathin two-dimensional flower-shaped manganese oxide nanosheet |
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