CN101525155B - Method for preparing manganese sesquioxide one dimension nano material - Google Patents
Method for preparing manganese sesquioxide one dimension nano material Download PDFInfo
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- CN101525155B CN101525155B CN2009100683708A CN200910068370A CN101525155B CN 101525155 B CN101525155 B CN 101525155B CN 2009100683708 A CN2009100683708 A CN 2009100683708A CN 200910068370 A CN200910068370 A CN 200910068370A CN 101525155 B CN101525155 B CN 101525155B
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Abstract
The invention relates to a method for preparing manganese sesquioxide one dimension nano material, comprising the process: organic complex aqueous solution with the mass concentration of 1-6% is prepared; metal salt containing manganese element and the organic complex aqueous solution are evenly mixed with each other according to the mass ratio of 1:5-5:1; a base plate is dipped into the mixed solution and tiled at the bottom of the solution; the mixed solution with the base plate is put into a baking oven and heated up to 120-150 DEG C at the speed of 5-20 DEG C/min and then the temperature is maintained for 0.5-3h; the manufactured sample is transferred into a box-type resistance furnace and heated up to 290-310 DEG C at the speed of 5-20 DEG C/min, then the temperature is maintained for 0.5-1h; the temperature is risen to 530-560 DEG C at the speed of 5-20 DEG C/min, and temperature is maintained for 0.5-3h; finally, the manganese sesquioxide one dimension nano material is formed on the base plate. The technique provided by the invention can be used for preparing the nano material with smaller and more uniform size; the method is also further simplified, and the optional scope of the raw materials is wider, thus further reducing the manufacturing cost.
Description
Technical field
The invention belongs to the monodimension nanometer material technical field, relate to a kind of method for preparing manganese sesquioxide one dimension nano material, belong to the technology that sintering prepares manganese sesquioxide one dimension nano material.
Background technology
Nano manganese oxide is little owing to its size, specific surface area is big, thereby has the peculiar property different with the oxide compound of common manganese, and the application in fields such as electrode materials, catalytic material, stupaliths has caused scientific worker's great attention.For example replace Manganse Dioxide with manganese oxide, the positive and negative electrode that has solved the MH-MnO2 battery discharges and recharges mismatch problem.And trimanganese tetroxide has solved the specific discharge capacity attenuation problem of battery preferably as the raw material of preparation spinel Li2Mn2O4.Up to now, the method for preparing nano manganese oxide mainly contains sol method, sol-gel method, micro emulsion method, phase oxidative reduction synthesis process and laser and steams the method for coagulating etc.The method for preparing manganese sesquioxide one dimension nano material in the bibliographical information so far mainly concentrates on hydrothermal method, but this type of reaction needed is carried out under the autoclave environment, the equipment complexity, and the very long reaction times of needs more than 24 hours, the popularization that these have all limited this technology is difficult to realize extensive growth.
The patent No. is 200510122214 patent of invention " method for preparing zinc oxide nanowire or zinc oxide nano-belt ", and a kind of method for preparing zinc oxide nanowire or zinc oxide nano-belt is provided.The contriver finds in follow-up technical study, when the nano wire of the prepared that adopts this patent to provide such as ZnO and so on or nano belt, can be because the increase of holding stage, and make the oversize of nano material, and this technology more complicated, cost of manufacture is also than higher.Aspect material choice,, then can limit to the design of technology simultaneously if be restricted to metal acetate salt and polyvinyl alcohol.
Summary of the invention
Purpose of the present invention provides a kind of method for preparing manganese sesquioxide one dimension nano material, and this procedure is simple, and expense is lower, can with unicircuit, semiconductor technology compatibility.
The present invention is realized by the following technical programs: a kind of method for preparing manganese sesquioxide one dimension nano material, it is characterized in that, and comprise following process:
1) with the organic substance that contains in hydroxyl, carboxyl or the amino three kinds of functional groups one or more as organic complexing agent, under 75～95 ℃ of water-baths or heating condition, described organic complexing agent is dissolved in the deionized water, be mixed with mass concentration and be 1～6% organic complex solution;
2) will contain the water-soluble metal salt of manganese element and the described organic complex aqueous solution 1: 5～5: 1 uniform mixing of mass ratio by metal-salt and organic complexing agent;
3) substrate is immersed mixing solutions, be tiled in the solution bottom;
4) mixing solutions that is equipped with substrate of step 3) is placed baking oven and be warming up to 120～150 ℃, insulation 0.5～3h with the speed of 5～20 ℃/min;
5) sample transfer that step 4) is made is in chamber type electric resistance furnace, is warming up to 290～310 ℃, insulation 0.5～1h with the speed of 5～20 ℃/min; Speed with 5～20 ℃/min is warming up to 530～560 ℃, and insulation 0.5～3h forms manganese sesquioxide one dimension nano material on substrate.
The above-mentioned method for preparing manganese sesquioxide one dimension nano material, described organic complexing agent is to contain in hydroxyl, carboxyl or the amino three kinds of functional groups one or more organic substance as organic complexing agent, as gelatin, chitosan, cyclodextrin, Xylo-Mucine, POTASSIUM BOROHYDRIDE, polyvinyl alcohol, have more than and be limited to this example; The described water-soluble metal salt that contains manganese element is Manganous chloride tetrahydrate or manganous acetate; Described substrate is silicon, quartz or glass material.
Beneficial effect of the present invention is: (all water-soluble inorganic salts of manganese are as Manganous chloride tetrahydrate etc. to adopt the metal-salt contain manganese element; The water-soluble organic salt of all of manganese, as manganous acetate etc.) and organic complexing agent (gelatin, chitosan, cyclodextrin, Xylo-Mucine, POTASSIUM BOROHYDRIDE, polyvinyl alcohol etc., be not only limited to these materials, can be used as the material of organic complexing agent, comprise that all contain in hydroxyl, carboxyl, the amino three kinds of functional groups one or more organic substance) the preparation manganese sesquioxide one dimension nano material, have advantages such as controllability is strong, simple to operate, expense is lower, manganese sesquioxide one dimension nano material, length can reach more than the 10 μ m.Because organic complexing agent has functional group abundant, that be evenly distributed (as hydroxyl, carboxyl, amino etc.), functional group on manganese positively charged ion and the organic complexing agent interacts, make manganese salt in the space frame of organic complexing agent, locate, arrange, through the program control type thermal treatment that is rapidly heated, reactions such as metal-salt and the organic complexing agent that contains manganese element decomposes stage by stage, cracking, oxidation are by the proportioning realization manganese sesquioxide one dimension nano material controlledly synthesis of sequence of control intensification parameter and different concns.Because thermal treatment temp is low, can with existing integrated circuits, semiconductor technology compatibility.Operational path compared to the preparation zinc oxide nanowire of the application of contriver before, technology provided by the invention, owing to reduced holding stage, can make the littler nano material of size, the size of while nano material is homogeneous more, and the trend that presents array arrangement, and also further simplification of technology, thereby further reduced cost of manufacture.Simultaneously aspect material choice, more wide in range, it is bigger to make the design of synthesis technique and conditional parameter choose the space.
Specific implementation method
Generally, preparation method of the present invention is as follows:
1) under 75～95 ℃ of water-baths or heating condition, with organic complexing agent (gelatin, chitosan, cyclodextrin, Xylo-Mucine, POTASSIUM BOROHYDRIDE, polyvinyl alcohol etc., be not only limited to these materials, can be used as the material of organic complexing agent, comprise that all contain hydroxyl, carboxyl, amino organic substance) dissolve in the deionized water, be mixed with mass concentration and be 1～6% organic complex solution;
2) (all water-soluble inorganic salts of manganese are as Manganous chloride tetrahydrate etc. will to contain the metal-salt of manganese element; The water-soluble organic salt of all of manganese is as manganous acetate etc.) and the organic complex aqueous solution press 1: 5～5: 1 uniform mixing of mass ratio of metal-salt and organic complexing agent;
3) substrate (as silicon, quartz or glass) is immersed mixing solutions, be tiled in the solution bottom;
4) mixing solutions that is equipped with substrate of step 3) is placed baking oven and be warming up to 120～150 ℃, insulation 0.5～3h with the speed of 5～20 ℃/min;
5) sample transfer that step 4) is made is in chamber type electric resistance furnace, is warming up to 290～310 ℃, insulation 0.5～1h with the speed of 5～20 ℃/min; Speed with 5～20 ℃/min is warming up to 530～560 ℃, and insulation 0.5～3h forms manganese sesquioxide one dimension nano material on substrate.
Manganese sesquioxide one dimension nano material with Manganous chloride tetrahydrate, manganous nitrate, manganous acetate and gelatin, polyvinyl alcohol preparation is that example illustrates how to implement the present invention below, the invention is not restricted to these embodiment.
Embodiment 1
In quartz beaker, under 75～95 ℃ of water-baths or heating condition, the 4g polyvinyl alcohol is dissolved in the 100ml deionized water; Add the 2g Manganous chloride tetrahydrate, adopt magnetic agitation 0.5h, rotating speed 800 commentaries on classics/min are with the ultrasonic dispersing 0.5h of 40KHz, 150W.Quartz glass substrate is tiled in the quartz beaker bottom.Then quartz beaker is placed baking oven and be warming up to 120 ℃ with the speed of 5 ℃/min, insulation 0.5h is until oven dry.Sample transfer in chamber type electric resistance furnace, is warming up to 300 ℃ of following thermal treatment 0.5h with the speed of 5 ℃/min; Speed with 5 ℃/min is warming up to 550 ℃, insulation 1h.SEM observes discovery, and formation diameter 30～50nm, length surpass the nano wire of 15 μ m on substrate.
Embodiment 2
Present embodiment to implement 1 similarly, difference is that the consumption of manganous acetate and gelatin is 4g in the step 2, is warming up to 130 ℃ with the speed of 10 ℃/min, insulation 0.5h is until oven dry.Sample transfer in chamber type electric resistance furnace, is warming up to 310 ℃ of following thermal treatment 0.5h with the speed of 10 ℃/min; Speed with 10 ℃/min is warming up to 560 ℃, insulation 1h.SEM observes discovery, and product is the nanometer rod of the about 50～80nm of diameter, length 10 μ m.
Embodiment 3
Present embodiment is similar to example 1, and difference is that the consumption of manganous nitrate and gelatin is 4g and 2g in the step 2, is warming up to 150 ℃ with the speed of 15 ℃/min, and insulation 1h is until oven dry.With sample transfer in chamber type electric resistance furnace, with 310 ℃ of the speed of 15 ℃/min, insulation 1h; Speed with 15 ℃/min is warming up to 560 ℃, insulation 3h.SEM observes discovery, and product is the nanometer rod of the about 80～100nm of diameter, length 10 μ m.
Embodiment 4
Present embodiment is similar to example 1, and difference is that the consumption of Manganous chloride tetrahydrate and gelatin is 4g and 2g in the step 2, is warming up to 140 ℃ with the speed of 20 ℃/min, and insulation 1h is until oven dry.With sample transfer in chamber type electric resistance furnace, with 315 ℃ of the speed of 20 ℃/min, insulation 1h; Speed with 20 ℃/min is warming up to 550 ℃, insulation 2h.SEM observes discovery, and product is the nanometer rod of the about 100～150nm of diameter, length 10 μ m.
Embodiment 5
Present embodiment is similar to example 3, and difference is in the step 2 that present embodiment only adopts mechanical stirring 0.5h, rotating speed 800 commentaries on classics/min.SEM observes discovery, has the nano wire of diameter 100～1000nm, the about 10 μ m of length and surface that incomplete nanometer rod is arranged in the product.
Claims (3)
1. a method for preparing manganese sesquioxide one dimension nano material is characterized in that, comprises following process:
1) with more than one organic substances in gelatin, chitosan, cyclodextrin, Xylo-Mucine, the polyvinyl alcohol as organic complexing agent, under 75～95 ℃ heating condition, described organic complexing agent is dissolved in the deionized water, be mixed with mass concentration and be 1～6% organic complex agent solution;
2) will contain the water-soluble metal salt of manganese element and the described organic complexing agent aqueous solution 1: 5～5: 1 uniform mixing of mass ratio by metal-salt and organic complexing agent;
3) substrate is immersed mixing solutions, be tiled in the solution bottom;
4) mixing solutions that is equipped with substrate of step 3) is placed baking oven and be warming up to 120～150 ℃, insulation 0.5～3h with the speed of 5～20 ℃/min;
5) sample transfer that step 4) is made is in chamber type electric resistance furnace, is warming up to 290～310 ℃, insulation 0.5～1h with the speed of 5～20 ℃/min; Speed with 5～20 ℃/min is warming up to 530～560 ℃, and insulation 0.5～3h forms manganese sesquioxide one dimension nano material on substrate.
2. the method for preparing manganese sesquioxide one dimension nano material according to claim 1 is characterized in that, the described water-soluble metal salt that contains manganese element is Manganous chloride tetrahydrate or manganous acetate.
3. the method for preparing manganese sesquioxide one dimension nano material according to claim 1 is characterized in that, described substrate is silicon, quartz or glass material.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102464355B (en) * | 2010-11-05 | 2013-11-06 | 中国石油化工股份有限公司 | Preparation method of superfine manganese oxide |
| CN102259929B (en) * | 2011-06-27 | 2013-04-10 | 北京工业大学 | Method for preparing porous nano or submicron rod-like manganese oxide |
| CN103420426B (en) * | 2013-08-29 | 2015-01-07 | 重庆工商大学 | Method for pyrogenic decomposing manganous nitrate to generate Mn2O3 |
| CN105858732B (en) * | 2016-06-01 | 2017-06-06 | 中国工程物理研究院化工材料研究所 | The regulation and control method and manganese sesquioxide managnic oxide powder of manganese sesquioxide managnic oxide nanostructured |
| CN106887606B (en) * | 2017-02-23 | 2019-12-13 | 广西大学 | Peach-shaped Mn2O3preparation method of/C particles |
| CN112210371B (en) * | 2020-10-29 | 2022-07-19 | 湖南第一师范学院 | Borate nano material and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1359854A (en) * | 2000-12-19 | 2002-07-24 | 中国科学技术大学 | High-purity tetragonal gamma-MnO3 nano crystal and its preparing process |
| CN1789136A (en) * | 2005-12-07 | 2006-06-21 | 天津大学 | Method for producing nano-wire or nano-belt of zinc oxide |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1359854A (en) * | 2000-12-19 | 2002-07-24 | 中国科学技术大学 | High-purity tetragonal gamma-MnO3 nano crystal and its preparing process |
| CN1789136A (en) * | 2005-12-07 | 2006-06-21 | 天津大学 | Method for producing nano-wire or nano-belt of zinc oxide |
Non-Patent Citations (2)
| Title |
|---|
| Changlu Shao et al..Preparation of Mn2O3 and Mn3O4 nanofibers via an electrospinning technique.Journal of Solid State Chemistry.2004,1772628-2631. * |
| Teressa Nathan et al..Electrode Properties of Mn2O3 Nanospheres Synthesized by Combined Sonochemical/Solvothermal Method for Use in Electrochemical Capacitors.Journal of Nanomaterials.2008,20081-8. * |
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