CN103691438B - A kind of controllable method for preparing of Ag-manganese monoxide nanometer rods - Google Patents
A kind of controllable method for preparing of Ag-manganese monoxide nanometer rods Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 29
- VASIZKWUTCETSD-UHFFFAOYSA-N manganese(II) oxide Inorganic materials [Mn]=O VASIZKWUTCETSD-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 15
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 15
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 229940071125 manganese acetate Drugs 0.000 claims description 11
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical group [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 11
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims description 9
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical class [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 7
- 238000001556 precipitation Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000001307 helium Substances 0.000 claims description 6
- 229910052734 helium Inorganic materials 0.000 claims description 6
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 6
- 239000013049 sediment Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 239000004094 surface-active agent Substances 0.000 claims description 6
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 5
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 5
- 229940071536 silver acetate Drugs 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims 1
- 229940069328 povidone Drugs 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 13
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 6
- 238000011065 in-situ storage Methods 0.000 abstract description 5
- 239000011572 manganese Substances 0.000 abstract description 5
- 238000006479 redox reaction Methods 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 229910052748 manganese Inorganic materials 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 239000000243 solution Substances 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 241000208340 Araliaceae Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 150000002696 manganese Chemical class 0.000 description 1
- 150000002697 manganese compounds Chemical class 0.000 description 1
- XYXLRVFDLJOZJC-CVBJKYQLSA-L manganese(2+);(z)-octadec-9-enoate Chemical compound [Mn+2].CCCCCCCC\C=C/CCCCCCCC([O-])=O.CCCCCCCC\C=C/CCCCCCCC([O-])=O XYXLRVFDLJOZJC-CVBJKYQLSA-L 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- -1 nanometer rods Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to a kind of controllable method for preparing of Ag-manganese monoxide nanometer rods, be specifically related to a kind of method by in-situ oxidation method of reducing controlled synthesis Ag-manganese monoxide nanometer rods.The object of the invention is to solve prior art at preparation pure phase one dimension manganese monoxide, the difficulty of monodimension nanometer material existence is particularly prepared by simple, gentle method, comprise and use manganese organic double compound, pyroreaction, the problem that in reaction, multivalent state coexists, provides a kind of preparation method being prepared Ag-manganese monoxide nanometer rods by in-situ oxidation reduction reaction.
Description
Technical field
The invention belongs to 1-dimention nano catalysis material preparation field, be specifically related to a kind of method by in-situ oxidation method of reducing controlled synthesis Ag-manganese monoxide nanometer rods.
Background technology
One dimension (1-D) nano material (as, nano wire, nanobelt, nanometer rods, nanotube etc.) in fields such as catalysis, electronics and solar energy, there is peculiar property and application potential, its preparation method is paid close attention to widely [Adv.Mater., 2003,15:353-389].Up to now, the emphasis of most of research work is the pure phase system of synthesizing one-dimensional nano material, comprises metal/non-metal (e.g., Au and Ag) and metal oxide (e.g., TiO
2) [Adv.Mater., 2012,24:4801-4841; Angew.Chem.Int.Ed., 2009,48 (1): 60-103; Inorg.Chem., 2006,45:6944-6949].Compared with the 1-D nano material of pure phase, by building different system
p-nknot; or by the coupling between metal/oxide; the secondary obtained, three level composite materials not only have the character of each material itself; simultaneously due to the synergy between different material; also produce new, special character; application have fabulous prospect [Inorg.Chem., 2006,45:6944-6949 in electro-catalysis, optics, bactericidal lamp etc.; Langmiur, 2006,22:1307-1312; J.Am.Chem.Soc., 2005,127:270-278; ChemPhysChem., 2010,11:2506-2509; Small, 2007,3:1356-1361; Angew.Chem., 2012,124:4274-4279; NanoLett., 2002,2 (10): 1109-1112].
Preparation pure phase manganese oxide (as: MnO, MnO
2and Mn
3o
4) one dimension pattern, the general organic compound used containing manganese, if manganese oleate is as intermediate reaction thing, under the high temperature conditions by adding adjuvant preparation [J.Phys.Chem.C, 2008,112:6981-6987; Langmuir, 2011,27 (3): 1152-1157; J.Phys, Chem, C, 2010,114 (32): 13608-13613; J.Phys, Chem, C, 2012,116:851-860; J.Am.Chem.Soc., 2009,131:6648-6655; J.Nanopart.Res., 2011,13 (10): 3139-3184; J.Phys.Chem.B, 2004,108:13594-13598; J.Phys.Chem.B, 2006,110:2-4; Chem.Mater., 2006,18:1821-1829; Chem.Mater., 2012,24:525-535; Adv.Funct.Mater.2012,22:4584-4591; Chem.Mater., 2007,19 (17): 4292-4299; J.Phys.Chem.C, 2008,112:5307-5315; Chem.Mater., 1995,7 (1): 148-153; Surf.InterfaceAnal., 2002,33 (3): 274-282; Phys.Rev.B, 2002,65:113102 (1-4); J.Electrochem.Soc., 2000,147 (6): 2246-2251].This kind of method step is numerous and diverse, and simultaneously owing to metal precursor can not be reduced completely, the catalyst yield therefore obtained is also low.
This method for raw material with silver salt and manganese salt (II), is prepared the compound system of Nano silver grain and manganese compound, by high-temperature roasting, has been prepared the Ag-manganese monoxide nanometer rods with certain electro catalytic activity by normal temperature and at original position redox reaction.
Summary of the invention
The object of the invention is to solve prior art at preparation pure phase one dimension Mn oxide, the difficulty of monodimension nanometer material existence is particularly prepared by simple, gentle method, comprise and use manganese organic double compound, pyroreaction, the problem that in reaction, multivalent state coexists, provides a kind of preparation method being prepared Ag-manganese monoxide nanometer rods by in-situ oxidation reduction reaction.Concrete steps are as follows:
(1) with silver salt and manganese (II) salt for raw material, polyvinylpyrrolidone (PVP) is surfactant, deionized water is solvent, and wherein the addition ratio of silver salt, manganese (II) salt, polyvinylpyrrolidone and deionized water is: (0.0001 ~ 0.0005): (0.002 ~ 0.02): (10 ~ 100): 110mol/mol/mg/ml.(2) by reactant with certain proportion mixing after, hold over night, after repeatedly centrifugal, washing, collecting precipitation thing.(3) last, by sediment 80 DEG C of oven dry, grinding, the powder obtained is placed in tube furnace, obtains under high-temperature roasting.
The controllable method for preparing of above-mentioned Ag-manganese monoxide nanometer rods, the dropping order in step (1) process is added drop-wise in manganese (II) saline solution for silver salt and the PVP aqueous solution, obtains product a, and contrary dropping order can not get product a.
The controllable method for preparing of above-mentioned Ag-manganese monoxide nanometer rods, silver salt used in step (1) process is silver nitrate, the one in silver acetate; Wherein manganese (II) salt is manganese acetate, the one in manganese nitrate.
The controllable method for preparing of above-mentioned Ag-manganese monoxide nanometer rods, the high-temperature roasting temperature described in step (3) is 600-900 DEG C, and programming rate is 1 ~ 20 DEG C/min, and heat treatment time is 1-5h.
The controllable method for preparing of above-mentioned Ag-manganese monoxide nanometer rods, the protective gas used in high-temperature calcination process of the sample described in step (3) is the one or more kinds of mixtures in nitrogen, argon gas, helium.Product in step (2) is through ethanol, and acetone, the one in water or mixture carrying out washing treatment, the processing time is 6-48h, then collecting precipitation, and drying obtains sample a.The method thinking is for utilizing Ag
+/ Ag and MnO
2/ Mn
2+the right electrode potential of electricity is different, carries out redox reaction, in-situ preparation product a, and this reaction condition is gentle, does not need to add the conditions such as other catalyst or external heat source in course of reaction.Reacted product a a step can generate pure phase manganese monoxide nanometer rods through calcination process, does not have the material of other multivalent state synchronously to generate as product.The product A g-MnO obtained has higher ORR(oxygen reduction reaction) catalytic activity, close to four electro transfer.Be expected to replace expensive Pt catalyst and realize four electro transfer.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below.
Fig. 1 is the XRD spectra of sample after product a and the 600 DEG C roasting of embodiment 1 preparation.
Fig. 2 is the TEM spectrogram of sample prepared by embodiment 2.
Fig. 3. be the TEM spectrogram of sample prepared by embodiment 3.
Fig. 4. be the ORR polarization curve of the different disk electrode rotating speeds of the sample of embodiment 4 preparation, illustration is Koutecky-Levich curve.
detailed description of the invention:
Be clearly and completely described the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
(1) with silver nitrate and manganese acetate (II) for raw material, take deionized water as solvent, configure 10mM liquor argenti nitratis ophthalmicus 10mL respectively, 20mM manganese acetate solution 100mL.10mg polyvinylpyrrolidone (PVP, K=30000) is surfactant.(2) liquor argenti nitratis ophthalmicus is added drop-wise in the manganese acetate aqueous solution, reaction terminate after, hold over night, after repeatedly centrifugal, washing, collecting precipitation thing.(3) last, by sediment 80 DEG C of oven dry, grinding, the powder obtained is placed in tube furnace, and under the condition protected there being helium (temperature rate-of-rise is 20 DEG C/min, is raised to 600 DEG C from room temperature), roasting 5h obtains.Fig. 1 is the XRD spectra of the product after a sample and 600 DEG C of roastings prepared.
Embodiment 2
(1) with silver acetate and manganese nitrate (II) for raw material, take deionized water as solvent, configure 50mM silver acetate solution 10mL respectively, 200mM manganese nitrate solution 100mL.100mg polyvinylpyrrolidone (PVP, K=30000) is surfactant.(2) silver acetate solution is added drop-wise in manganese nitrate aqueous solution, reaction terminate after, hold over night, after repeatedly centrifugal, washing, collecting precipitation thing.(3) last, by sediment 80 DEG C of oven dry, grinding, the powder obtained is placed in tube furnace, under the condition protected there being helium (temperature rate-of-rise is 1 DEG C/min, be raised to 900 DEG C from room temperature), roasting 1h obtains.Fig. 2 is the TEM spectrogram of the sample of preparation.
Embodiment 3
(1) with silver nitrate and manganese acetate (II) for raw material, take deionized water as solvent, configure 10mM liquor argenti nitratis ophthalmicus 10mL respectively, 200mM manganese acetate solution 100mL.56mg polyvinylpyrrolidone (PVP, K=30000) is surfactant.(2) liquor argenti nitratis ophthalmicus is added drop-wise in the manganese acetate aqueous solution, after reaction terminates, hold over night, after repeatedly centrifugal, acetone/water washing, collecting precipitation thing.(3) last, by sediment 80 DEG C of oven dry, grinding, the powder obtained is placed in tube furnace, and under the condition protected there being helium (temperature rate-of-rise is 5 DEG C/min, is raised to 800 DEG C from room temperature), roasting 4h obtains.Fig. 3 is the TEM spectrogram of the sample of preparation.
Embodiment 4
(1) with silver nitrate and manganese acetate (II) for raw material, take deionized water as solvent, configure 10mM liquor argenti nitratis ophthalmicus 10mL respectively, 200mM manganese acetate solution 100mL.56mg polyvinylpyrrolidone (PVP, K=30000) is surfactant.(2) liquor argenti nitratis ophthalmicus is added drop-wise in the manganese acetate aqueous solution, after reaction terminates, hold over night, after repeatedly centrifugal, ethanol/water washing, collecting precipitation thing.(3) last, by sediment 80 DEG C of oven dry, grinding, the powder obtained is placed in tube furnace, and under the condition protected there being helium (temperature rate-of-rise is 20 DEG C/min, is raised to 800 DEG C from room temperature), roasting 4h obtains product.The product obtained is comprising glass carbon rotating disk electrode (r.d.e) (RDE), platinum electrode, and tests its chemical property, with the KOH of concentration 0.1M for electrolyte in the three-electrode battery of Hg/HgO ginseng electrode.Before carrying out electrochemical measurement, with the alumina slurry polishing RDE(0.196cm of 1 micron
2, MT134, PineInstrumentCo.), then wash with distilled water and ethanol for several times.The catalyst of 5mg is dispersed in 5ml ethanol, and sonic oscillation is with the brown solution formed.The sample drawing 20 these mixtures of μ L moves on to RDE, and then sample surfaces applies the Nafion/ethanol mixed liquor of the 0.1wt% of 5 μ L, and protection sample is in order to avoid sample departs from measuring process.Cyclic voltammetry curve (CV) is collected at saturated oxygen used for electrolyte and nitrogen scanning.The ORR of Ag-MnO Nanorods Catalyst is active uses spinning disk at the scan rate measurement of 5m/s at the saturated electrolyte of oxygen, in measuring process, keeps continuing logical oxygen, guarantees that the oxygen in electrolyte solution is in saturation state all the time.Fig. 4 is the ORR polarization curve of sample at different disk electrode electrode rotating speed, and illustration is Koutecky-Levich curve.
Claims (4)
1. the controllable method for preparing of an Ag-manganese monoxide nanometer rods, carry out according to following step: (1) with silver salt and manganese (II) salt for raw material, polyvinylpyrrolidone is surfactant, deionized water is solvent, and wherein the addition ratio of silver salt, manganese (II) salt, polyvinylpyrrolidone and deionized water is: (0.0001 ~ 0.0005): (0.002 ~ 0.02): (10 ~ 100): 110mol/mol/mg/ml; (2) by reactant with certain proportion mixing after, hold over night, after repeatedly centrifugal, washing, collecting precipitation thing; (3) last, by sediment 80 DEG C of oven dry, grinding, the powder obtained is placed in tube furnace, obtains under high-temperature roasting;
Dropping order in step (1) process is added drop-wise in manganese (II) saline solution for silver salt and aqueous povidone solution.
2. the controllable method for preparing of a kind of Ag-manganese monoxide nanometer rods according to claim 1, is characterized in that: silver salt used in step (1) process is silver nitrate, the one in silver acetate; Wherein manganese (II) salt is manganese acetate, the one in manganese nitrate.
3. the controllable method for preparing of a kind of Ag-manganese monoxide nanometer rods according to claim 1, it is characterized in that: the high-temperature roasting temperature described in step (3) is 600-900 DEG C, programming rate is 1 ~ 20 DEG C/min, and heat treatment time is 1-5h.
4. the controllable method for preparing of a kind of Ag-manganese monoxide nanometer rods according to claim 1, is characterized in that: the protective gas used in high-temperature calcination process of the powder described in step (3) is the one or more kinds of mixtures in nitrogen, argon gas, helium.
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| CN105632791B (en) * | 2016-03-25 | 2018-05-22 | 上海工程技术大学 | A kind of Ag adulterates MnO2Nano-array super capacitor material and preparation method thereof |
| CN106424753B (en) * | 2016-10-14 | 2018-12-07 | 泉州师范学院 | A kind of MnO2The preparation and its application of-Ag nanocomposite |
| CN107441512B (en) * | 2017-09-22 | 2020-05-26 | 合肥工业大学 | Preparation method and application of paramagnetic manganese monoxide nanoparticles |
| CN111482617B (en) * | 2020-01-30 | 2021-09-17 | 浙江大学 | Preparation method of silver nanowire surface in-situ growth metal oxide core point composite material |
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| CN102339996A (en) * | 2011-10-08 | 2012-02-01 | 广州市香港科大霍英东研究院 | Synthesis and performance of spherical mesoporous anode materials MnO/Mn2O3 for lithium ion battery |
| CN102476054A (en) * | 2010-11-29 | 2012-05-30 | 中国科学院大连化学物理研究所 | Ag/MnyOx/C catalyst and preparation and application thereof |
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| CN102157727A (en) * | 2011-03-22 | 2011-08-17 | 北京工业大学 | Preparation method for nano MnO of negative electrode material of lithium ion battery |
| CN102339996A (en) * | 2011-10-08 | 2012-02-01 | 广州市香港科大霍英东研究院 | Synthesis and performance of spherical mesoporous anode materials MnO/Mn2O3 for lithium ion battery |
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