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CN103691438A - Controllable preparation method of Ag-manganese monoxide nanorods - Google Patents

Controllable preparation method of Ag-manganese monoxide nanorods Download PDF

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CN103691438A
CN103691438A CN201310593517.1A CN201310593517A CN103691438A CN 103691438 A CN103691438 A CN 103691438A CN 201310593517 A CN201310593517 A CN 201310593517A CN 103691438 A CN103691438 A CN 103691438A
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manganese
nanorods
controllable preparation
preparation
manganese monoxide
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CN103691438B (en
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吕晓萌
魏晓骏
刘军
吴子伟
谢吉民
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Jiangsu University
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Abstract

本发明涉及一种Ag-一氧化锰纳米棒的可控制备方法，具体涉及一种通过原位氧化还原方法可控制备Ag-一氧化锰纳米棒的方法。本发明的目的在于解决现有技术在制备纯相一维一氧化锰，特别是通过简单、温和方法来制备一维纳米材料存在的困难，包括使用锰有机复合物，高温反应，反应中多价态共存的问题，提供一种通过原位氧化还原反应来制备Ag-一氧化锰纳米棒的制备方法。

Figure 201310593517

The invention relates to a controllable preparation method of Ag-manganese monoxide nanorods, in particular to a method for controllable preparation of Ag-manganese monoxide nanorods by an in-situ redox method. The purpose of the present invention is to solve the difficulties in the preparation of pure phase one-dimensional manganese monoxide in the prior art, especially the preparation of one-dimensional nanomaterials by a simple and mild method, including the use of manganese organic compounds, high temperature reaction, and multivalent To address the problem of state coexistence, a preparation method for preparing Ag-manganese monoxide nanorods by in situ redox reaction is provided.

Figure 201310593517

Description

A kind of controllable method for preparing of Ag-manganese monoxide nanometer rods
Technical field
The invention belongs to 1-dimention nano catalysis material preparation field, be specifically related to a kind of by the method for the controlled Ag-of the preparation manganese monoxide of in-situ oxidation method of reducing 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 [Adv. Mater., 2003,15:353-389] widely.Up to now, the emphasis of most of research work is pure phase systems of synthesizing one-dimensional nano material, comprise metal/non-metal (as, Au and Ag) and metal oxide (as, TiO 2) [Adv. Mater., 2012,24:4801-4841; Angew. Chem. Int. Ed., 2009,48 (1): 60-103; Inorg. Chem., 2006,45:6944-6949].Compare with the 1-D nano material of pure phase, by building different systems p-nknot; or by the coupling between metal/oxide; the secondary obtaining, 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; in the application such as aspect electro-catalysis, optics, bactericidal lamp, there is fabulous prospect [Inorg. Chem., 2006,45:6944-6949; 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; Nano Lett., 2002,2 (10): 1109-1112].
Preparation pure phase manganese oxide (as: MnO, MnO 2and Mn 3o 4) one dimension pattern, the general organic compound using containing manganese, if manganese oleate is as intermediate reaction thing, under hot conditions by adding assistant 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. Interface Anal., 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 being reduced completely, the catalyst yield therefore obtaining is also low.
It is raw material that this method be take silver salt and manganese salt (II), prepares the compound system of Nano silver grain and manganese compound by normal temperature and at original position redox reaction, by high-temperature roasting, has prepared the Ag-manganese monoxide nanometer rods with certain electro catalytic activity.
Summary of the invention
The object of the invention is to solve prior art at preparation pure phase one dimension Mn oxide, particularly by simple, gentle method, prepare the difficulty that monodimension nanometer material exists, comprise and use manganese organic double compound, pyroreaction, the problem that in reaction, multivalence state coexists, provides a kind of preparation method who prepares Ag-manganese monoxide nanometer rods by in-situ oxidation reduction reaction.Concrete steps are as follows:
(1) take silver salt and manganese (II) salt is 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): 110 mol/mol/mg/ml.(2) after reactant is mixed with certain proportion, standing over night, after repeatedly centrifugal, washing, collecting precipitation thing.(3) last, sediment, 80 ℃ of oven dry, is ground, the powder obtaining is placed in tube furnace, under high-temperature roasting, obtains.
The controllable method for preparing of above-mentioned Ag-manganese monoxide nanometer rods, the dropping in step (1) process, sequentially for silver salt and the PVP aqueous solution are added drop-wise in manganese (II) saline solution, obtains product a, and contrary dropping sequentially can not get product a.
The controllable method for preparing of above-mentioned Ag-manganese monoxide nanometer rods, in step (1) process, silver salt used is silver nitrate, a kind of in silver acetate; Wherein manganese (II) salt is manganese acetate, a kind of in manganese nitrate.
The controllable method for preparing of above-mentioned Ag-manganese monoxide nanometer rods, the described high-temperature roasting temperature of step (3) is 600-900 ℃, and programming rate is 1 ~ 20 ℃/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, acetone, and a kind of or mixture carrying out washing treatment in water, the processing time is 6-48h, collecting precipitation then, the dry sample a that obtains.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, and original position generates product a, and this reaction condition is gentle, does not need to add other catalyst or the condition such as external heat source in course of reaction.Reacted product a can a step generate pure phase manganese monoxide nanometer rods through calcination process, does not have the material of other multivalence states synchronously to generate as product.The product A g-MnO obtaining has higher ORR(oxygen reduction reaction) catalytic activity, approach the quadrielectron and shift.Be expected to replace expensive Pt catalyst and realize quadrielectron 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, will the accompanying drawing of required use in embodiment or description of the Prior Art be briefly described below.
Fig. 1 is the XRD spectra of sample after the product a of embodiment 1 preparation and 600 ℃ of roastings.
Fig. 2 is the TEM spectrogram of the sample of embodiment 2 preparations.
Fig. 3. be the TEM spectrogram of the sample of embodiment 3 preparation.
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.
the specific embodiment:
Below the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Embodiment based in the present invention, those of ordinary skills, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
(1) take silver nitrate and manganese acetate (II) is raw material, take deionized water as solvent, configures respectively 10mM liquor argenti nitratis ophthalmicus 10mL, 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 finish after, standing over night, after repeatedly centrifugal, washing, collecting precipitation thing.(3) last, sediment, 80 ℃ of oven dry, is ground, the powder obtaining is placed in tube furnace, and under the condition that has helium protection (temperature rate-of-rise is 20 ℃/min, is raised to 600 ℃ from room temperature), roasting 5h obtains.Fig. 1 is a sample of preparation and the XRD spectra of the product after 600 ℃ of roastings.
Embodiment 2
(1) take silver acetate and manganese nitrate (II) is raw material, take deionized water as solvent, configures respectively 50mM silver acetate solution 10mL, 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 finish after, standing over night, after repeatedly centrifugal, washing, collecting precipitation thing.(3) last, sediment, 80 ℃ of oven dry, is ground, the powder obtaining is placed in tube furnace, under the condition that has helium protection (temperature rate-of-rise is 1 ℃/min,, from room temperature, be raised to 900 ℃), roasting 1h obtains.Fig. 2 is the TEM spectrogram of the sample of preparation.
Embodiment 3
(1) take silver nitrate and manganese acetate (II) is raw material, take deionized water as solvent, configures respectively 10mM liquor argenti nitratis ophthalmicus 10mL, 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 finishes, standing over night, after repeatedly centrifugal, acetone/water washing, collecting precipitation thing.(3) last, sediment, 80 ℃ of oven dry, is ground, the powder obtaining is placed in tube furnace, and under the condition that has helium protection (temperature rate-of-rise is 5 ℃/min, is raised to 800 ℃ from room temperature), roasting 4h obtains.Fig. 3 is the TEM spectrogram of the sample of preparation.
Embodiment 4
(1) take silver nitrate and manganese acetate (II) is raw material, take deionized water as solvent, configures respectively 10mM liquor argenti nitratis ophthalmicus 10mL, 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 finishes, standing over night, after repeatedly centrifugal, ethanol/water washing, collecting precipitation thing.(3) last, sediment, 80 ℃ of oven dry, is ground, the powder obtaining is placed in tube furnace, and under the condition that has helium protection (temperature rate-of-rise is 20 ℃/min, is raised to 800 ℃ from room temperature), roasting 4h obtains product.The product obtaining is comprising glass carbon rotating disk electrode (r.d.e) (RDE), platinum electrode, and test its chemical property in the three-electrode battery of Hg/HgO ginseng electrode, and the KOH of concentration 0.1M of take is electrolyte.Before carrying out electrochemical measurement, with the alumina slurry polishing RDE(0.196 cm of 1 micron 2, MT134, Pine Instrument Co.), then with distilled water and ethanol washing several.The catalyst of 5 mg is dispersed in 5 ml ethanol, and the brown solution of sonic oscillation to form.The sample of drawing 20 these mixtures of μ L moves on to RDE, and then sample surfaces applies the Nafion/ethanol mixed liquor of 0.1 wt% of 5 μ L, protects sample in order to avoid sample departs from measuring process.Cyclic voltammetry curve (CV) is collected at the saturated oxygen of used for electrolyte and nitrogen scanning.The ORR activity of Ag-MnO nanometer rods catalyst is used spinning disk at the scan rate measurement of 5 m/s at the saturated electrolyte of oxygen, in measuring process, keeps continuing logical oxygen, guarantees that oxygen in electrolyte solution is all the time in saturation state.Fig. 4 be sample at the ORR polarization curve of different disk electrode electrode rotating speeds, illustration is Koutecky-Levich curve.

Claims (6)

1.一种Ag-一氧化锰纳米棒的可控制备方法，按照下述步骤进行：（1）以银盐和锰（II）盐为原料，聚乙烯吡咯烷酮为表面活性剂，去离子水为溶剂，其中银盐、锰（II）盐、聚乙烯吡咯烷酮和去离子水的加入量比例为：（0.0001~0.0005）：（0.002~0.02）：（10~100）:110 mol/mol/mg/ml；（2）将反应物以一定比例混合后，静置过夜，后多次离心、洗涤，收集沉淀物；（3）最后，将沉淀物在80℃烘干，研磨，得到的粉末置于管式炉中，高温焙烧下得到。 1. A controllable preparation method of Ag-manganese monoxide nanorods is carried out according to the following steps: (1) taking silver salt and manganese (II) salt as raw material, polyvinylpyrrolidone as surfactant, and deionized water as Solvent, 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): 110 mol/mol/mg/ ml; (2) After mixing the reactants in a certain proportion, let them stand overnight, and then centrifuge and wash several times to collect the precipitate; (3) Finally, dry the precipitate at 80°C, grind it, and place the obtained powder in In a tube furnace, it is obtained under high temperature roasting. 2.根据权利要求1所述的一种Ag-一氧化锰纳米棒的可控制备方法，其特征在于：步骤（1）过程中的滴加顺序为银盐与聚乙烯吡咯烷酮水溶液滴加到锰（II）盐水溶液中。 2. The controllable preparation method of a kind of Ag-manganese monoxide nanorods according to claim 1, characterized in that: the dripping sequence in the process of step (1) is that silver salt and polyvinylpyrrolidone aqueous solution are added dropwise to manganese (II) In saline solution. 3.根据权利要求1所述的一种Ag-一氧化锰纳米棒的可控制备方法，其特征在于：步骤（1）过程中所用的银盐为硝酸银，醋酸银中的一种；其中锰（II）盐为醋酸锰，硝酸锰中的一种。 3. the controllable preparation method of a kind of Ag-manganese monoxide nanorod according to claim 1, is characterized in that: the silver salt used in the process of step (1) is silver nitrate, a kind of in silver acetate; Wherein The manganese (II) salt is manganese acetate, one of manganese nitrates. 4.根据权利要求2所述的一种Ag-一氧化锰纳米棒的可控制备方法，其特征在于：步骤（2）中的生成物经乙醇，丙酮，水中的一种或者混合物洗涤处理，处理时间为6-48h，然后收集沉淀，干燥，得到产物a。 4. A controllable preparation method of Ag-manganese monoxide nanorods according to claim 2, characterized in that: the product in step (2) is washed with ethanol, acetone, or a mixture of water, The treatment time is 6-48h, and then the precipitate is collected and dried to obtain the product a. 5.根据权利要求1所述的一种Ag-一氧化锰纳米棒的可控制备方法，其特征在于：步骤（3）所述的高温焙烧温度为600-900℃，升温速度为1~20℃/min，热处理时间为1-5h。 5. A controllable preparation method of Ag-manganese monoxide nanorods according to claim 1, characterized in that: the high-temperature calcination temperature in step (3) is 600-900°C, and the heating rate is 1-20 ℃/min, heat treatment time is 1-5h. 6.根据权利要求1所述的一种Ag-一氧化锰纳米棒的可控制备方法，其特征在于：步骤（3）中所述的样品在高温焙烧过程中所用的保护气体为氮气、氩气、氦气中的一种或者两种以上的混合物。 6. A controllable preparation method of Ag-manganese monoxide nanorods according to claim 1, characterized in that: the protective gas used in the high-temperature roasting process of the sample described in step (3) is nitrogen, argon One or more mixtures of gas and helium.
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CN105514449A (en) * 2015-11-11 2016-04-20 中国科学院宁波材料技术与工程研究所 Metal-air battery cathode catalyst and preparation method thereof
CN105632791A (en) * 2016-03-25 2016-06-01 上海工程技术大学 A kind of Ag-doped MnO2 nano-array supercapacitor material and preparation method thereof
CN106424753A (en) * 2016-10-14 2017-02-22 泉州师范学院 Preparation and application of a kind of MnO2‑Ag nanocomposite material
CN107441512A (en) * 2017-09-22 2017-12-08 合肥工业大学 A kind of preparation method and applications of paramagnetism manganese monoxide nano particle
CN111482617A (en) * 2020-01-30 2020-08-04 浙江大学 Preparation method of in-situ growth of metal oxide nucleation point composites on silver nanowire surfaces

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CN105514449A (en) * 2015-11-11 2016-04-20 中国科学院宁波材料技术与工程研究所 Metal-air battery cathode catalyst and preparation method thereof
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CN111482617A (en) * 2020-01-30 2020-08-04 浙江大学 Preparation method of in-situ growth of metal oxide nucleation point composites on silver nanowire surfaces

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