CN113880142B - MnMoO 4 Micro-nano material and preparation method thereof - Google Patents
MnMoO 4 Micro-nano material and preparation method thereof Download PDFInfo
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 20
- 239000011259 mixed solution Substances 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 10
- KHSTZMGCKHBFJX-UHFFFAOYSA-N 3-(dibutylamino)phenol Chemical compound CCCCN(CCCC)C1=CC=CC(O)=C1 KHSTZMGCKHBFJX-UHFFFAOYSA-N 0.000 claims description 7
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 7
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 7
- 229940082328 manganese acetate tetrahydrate Drugs 0.000 claims description 6
- CESXSDZNZGSWSP-UHFFFAOYSA-L manganese(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Mn+2].CC([O-])=O.CC([O-])=O CESXSDZNZGSWSP-UHFFFAOYSA-L 0.000 claims description 6
- 235000015393 sodium molybdate Nutrition 0.000 claims description 6
- 239000011684 sodium molybdate Substances 0.000 claims description 6
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 6
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052748 manganese Inorganic materials 0.000 abstract description 10
- 239000011572 manganese Substances 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 3
- 239000011733 molybdenum Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 229910016895 MnMoO4 Inorganic materials 0.000 abstract 1
- 238000010923 batch production Methods 0.000 abstract 1
- 238000006555 catalytic reaction Methods 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 7
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000002071 nanotube Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001523 electrospinning Methods 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- -1 humidity detectors Substances 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention provides MnMoO 4 A micro-nano material and a preparation method thereof belong to the field of micro-nano material synthesis. The MnMoO is prepared by taking a manganese source and a molybdenum source which are low in price as reaction raw materials and adopting a simple ultrasonic method in combination with calcination 4 And (3) micro-nano materials. The invention has the advantages of easily obtained raw materials, simple and convenient process, lower cost, suitability for batch production and wide application prospect. The prepared MnMoO4 micro-nano material has distinct morphology and characteristic, has a unique multi-stage structure, and has wide application prospects in the fields of catalysis, sensing, new energy and the like.
Description
Technical Field
The invention belongs to the field of micro-nano materials, and particularly relates to MnMoO 4 Micro-nano material and a preparation method thereof.
Background
Manganese molybdate (MnMoO) 4 ) The material is an important inorganic functional material, has excellent magnetic property, catalytic property and electrochemical property due to the special crystal structure and the changeable combination state of molybdenum and manganese elements, is often used for preparing catalysts, luminescent materials, humidity detectors, electrode materials and the like, and is widely applied to the fields of chemical industry, national defense, electronic industry and the like.
MnMoO 4 The preparation and application of micro-nano materials and composite materials thereof are also reported. For example, chinese patent No. cn201710130453.x prepares a manganese molybdate porous nanotube by using an electrostatic spinning method, and a cross-linked network structure is formed between the porous nanotubes, so that the transfer of ions/electrons and the permeation of an electrolyte can be effectively promoted, the diffusion path of electrolyte ions in a material is shortened, and the manganese molybdate porous nanotube has a higher specific capacity, an excellent rate capability and a better cycling stability as an electrode material. The Chinese patent CN202011505651.8 combines a coprecipitation method with high-temperature calcination to prepare the carbon-coated manganese molybdate single-crystal micron rod, and the carbon-coated manganese molybdate single-crystal micron rod as a cathode material of a sodium ion battery shows better electrochemical performance compared with the manganese molybdate micron rod without carbon coating. Chinese patent CN201110347430.7 takes ammonium molybdate and manganese nitrate as reaction raw materials, cetyl Trimethyl Ammonium Bromide (CTAB) as a surfactant, distilled water as a solvent, and a microwave radiation method is utilized to prepare a manganese molybdate material assembled into a micron rod structure by nanosheets. MnMoO disclosed above 4 Related reports prove that the MnMoO with different micro-nano structures 4 Has wide application in various aspects. However, the above MnMoO 4 The preparation of nanomaterials usually requires relatively complex and expensive equipment, such as microwave radiation, electrospinning, etc. Therefore, the MnMoO having a novel structure is prepared using a relatively simple method 4 The micro-nano material is worth further exploration.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide MnMoO 4 Micro-nano material and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
MnMoO 4 The preparation method of the micro-nano material comprises the following steps:
1) Dissolving 1 part of sodium molybdate, 0.5-1 part of polyvinylpyrrolidone and 1-4 parts of manganese acetate tetrahydrate in 50 parts of deionized water according to parts by mass to obtain a mixed solution A;
2) Reacting the mixed solution A under an ultrasonic condition for 1-3 h, and filtering, washing and drying the obtained product after the reaction is finished to obtain a product B;
3) Dissolving 1 part of the product B and 0.5-1 part of 3- (dibutylamino) phenol in 50 parts of deionized water by mass, stirring at room temperature for 1-3 hours, and then filtering, washing and drying to obtain a product C;
4) Calcining the product C at 600-800 ℃ for 1h to obtain MnMoO 4 And (3) micro-nano materials.
Further, in step 2), the ultrasonic condition is provided by an ultrasonic generator.
Further, the ultrasonic power of the ultrasonic generator is 60-100W.
Further, in the step 2), washing with water is performed 3 to 6 times.
Further, in the step 2), the drying temperature is 50-70 ℃, and the drying time is 6-10 hours.
Further, in step 3), washing with water is performed 3 to 6 times.
Furthermore, the drying temperature is 50-70 ℃, and the drying time is 6-10 hours.
The MnMoO prepared by the preparation method of the invention 4 And (3) micro-nano materials.
Furthermore, the structure is in a cauliflower-shaped multilevel structure.
Compared with the prior art, the invention has the following beneficial effects:
MnMoO of the invention 4 The preparation method of the micro-nano material uses a molybdenum source and a manganese source which are cheap as raw materials, and MnMoO is prepared by adjusting technological parameters such as ultrasound, calcination and the like 4 The nanoparticles self-assemble into unique micron-scale multilevel structures. The invention adjusts the ultrasonic condition to form regular MnMoO at room temperature 4 And (3) precursor. And the addition of polyvinylpyrrolidone and 3- (dibutylamino) phenol solution to MnMoO 4 The formation of the cauliflower-shaped special appearance has certain auxiliary effect. After the product is properly calcined, the purity and crystallinity of the product are further improved. The preparation method is simple and easy to operate, has strong repeatability, low cost and no pollution to the environment, and is suitable for industrial mass production.
MnMoO of the invention 4 The micro-nano material has the characteristics of distinct morphological characteristics, high purity, high crystallinity, large specific surface and the like, and has wide application prospects in the fields of photocatalysis materials, luminescent materials, sensing, new energy and the like.
Drawings
FIG. 1 is an XRD pattern of the product prepared in example 1;
FIG. 2 is a scanning electron micrograph of the product prepared in example 1.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
example 1
According to the mass parts, 1 part of sodium molybdate, 0.5 part of polyvinylpyrrolidone and 1 part of manganese acetate tetrahydrate are dissolvedTo 50 parts of deionized water, a mixed solution a was obtained. And (3) uniformly stirring the mixed solution A, transferring the mixed solution A into an ultrasonic generator, reacting for 1h under the ultrasonic power of 100W, filtering, washing with water, and drying to obtain a product B. And (3) dissolving 1 part of the product B and 0.5 part of 3- (dibutylamino) phenol in 50 parts of deionized water according to parts by mass, stirring for 3 hours at room temperature, filtering, washing with water, and drying to obtain a product C. Calcining the product C in a muffle furnace at 600 ℃ for 1h to obtain MnMoO 4 And (3) micro-nano materials.
Referring to fig. 1, fig. 1 shows MnMoO prepared according to the present invention 4 The XRD pattern of the micro-nano material can determine MnMoO from figure 1 4 The micro-nano material has high phase composition and high purity.
Referring to fig. 2, fig. 2 shows MnMoO prepared according to the present invention 4 The obtained MnMoO can be seen in the scanning electron microscope picture of the micro-nano material 4 The micro-nano material has distinct morphology and features and is in a cauliflower-shaped multi-level structure.
Example 2
According to the mass parts, 1 part of sodium molybdate, 0.8 part of polyvinylpyrrolidone and 50 parts of deionized water of 2 parts of manganese acetate tetrahydrate are added to obtain a mixed solution A. And (3) uniformly stirring the mixed solution A, transferring the mixed solution A into an ultrasonic generator, reacting for 3 hours under the ultrasonic power of 60W, filtering, washing with water, and drying to obtain a product B. Dissolving 1 part of the product B and 1 part of 3- (dibutylamino) phenol in 50 parts of deionized water by mass, stirring for 1 hour at room temperature, filtering, washing with water, and drying to obtain a product C. Calcining the product C at 800 ℃ for 1h to obtain MnMoO 4 And (3) micro-nano materials.
Example 3
According to the mass parts, 1 part of sodium molybdate, 1 part of polyvinylpyrrolidone and 4 parts of manganese acetate tetrahydrate are dissolved in 50 parts of deionized water to obtain a mixed solution A. And (3) uniformly stirring the mixed solution A, transferring the mixed solution A into an ultrasonic generator, reacting for 2 hours under the ultrasonic power of 80W, filtering, washing with water, and drying to obtain a product B. Dissolving 1 part of product B and 0.5 part of 3- (dibutylamino) phenol in 50 parts of deionized water according to parts by mass, stirring for 2 hours at room temperature, filtering, washing and drying to obtain the productAnd (C) a compound. Calcining the product C at 700 ℃ for 1h to obtain MnMoO 4 And (3) micro-nano materials.
Example 4
According to the mass parts, 1 part of sodium molybdate, 0.5 part of polyvinylpyrrolidone and 1-4 parts of manganese acetate tetrahydrate are dissolved in 50 parts of deionized water to obtain a mixed solution A. And (3) uniformly stirring the mixed solution A, transferring the mixed solution A into an ultrasonic generator, reacting for 1h under the ultrasonic power of 100W, filtering, washing with water, and drying to obtain a product B. And (3) dissolving 1 part of the product B and 1 part of 3- (dibutylamino) phenol in 50 parts of deionized water according to parts by mass, stirring for 1 hour at room temperature, filtering, washing with water, and drying to obtain a product C. Calcining the product C at 800 ℃ for 1h to obtain MnMoO 4 And (3) micro-nano materials.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (9)
1. MnMoO 4 The preparation method of the micro-nano material is characterized by comprising the following steps:
1) Dissolving 1 part of sodium molybdate, 0.5-1 part of polyvinylpyrrolidone and 1-4 parts of manganese acetate tetrahydrate in 50 parts of deionized water according to parts by mass to obtain a mixed solution A;
2) Reacting the mixed solution A under an ultrasonic condition for 1-3 h, and filtering, washing and drying the obtained product after the reaction is finished to obtain a product B;
3) Dissolving 1 part of the product B and 0.5-1 part of 3- (dibutylamino) phenol in 50 parts of deionized water by mass, stirring at room temperature for 1-3 hours, and then filtering, washing and drying to obtain a product C;
4) Calcining the product C at 600-800 ℃ for 1h to obtain MnMoO 4 And (3) micro-nano materials.
2. The MnMoO of claim 1 4 Of micro-nano materialsThe preparation method is characterized in that in the step 2), ultrasonic conditions are provided by an ultrasonic generator.
3. The MnMoO of claim 2 4 The preparation method of the micro-nano material is characterized in that the ultrasonic power of the ultrasonic generator is 60-100W.
4. The MnMoO of claim 1 4 The preparation method of the micro-nano material is characterized in that in the step 2), the micro-nano material is washed for 3 to 6 times.
5. The MnMoO of claim 1 4 The preparation method of the micro-nano material is characterized in that in the step 2), the drying temperature is 50-70 ℃, and the drying time is 6-10 hours.
6. The MnMoO of claim 1 4 The preparation method of the micro-nano material is characterized in that in the step 3), washing is carried out for 3-6 times.
7. The MnMoO of claim 1 4 The preparation method of the micro-nano material is characterized in that in the step 3), the drying temperature is 50-70 ℃, and the drying time is 6-10 hours.
8. MnMoO produced by the method according to any one of claims 1 to 7 4 And (3) micro-nano materials.
9. The MnMoO of claim 8 4 The micro-nano material is characterized by being in a cauliflower-shaped multi-level structure.
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Citations (3)
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| CN107459063A (en) * | 2017-07-25 | 2017-12-12 | 陕西科技大学 | A kind of manganese molybdate micro Nano material and its preparation method and application |
| CN110342579A (en) * | 2019-08-16 | 2019-10-18 | 陕西科技大学 | A kind of manganese molybdate carbon composite nano ball and preparation method thereof |
| CN110386625A (en) * | 2019-08-16 | 2019-10-29 | 陕西科技大学 | A kind of manganese oxide carbon composite and preparation method thereof that molybdenum adulterates in situ |
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2021
- 2021-11-01 CN CN202111285263.8A patent/CN113880142B/en active Active
Patent Citations (3)
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| CN107459063A (en) * | 2017-07-25 | 2017-12-12 | 陕西科技大学 | A kind of manganese molybdate micro Nano material and its preparation method and application |
| CN110342579A (en) * | 2019-08-16 | 2019-10-18 | 陕西科技大学 | A kind of manganese molybdate carbon composite nano ball and preparation method thereof |
| CN110386625A (en) * | 2019-08-16 | 2019-10-29 | 陕西科技大学 | A kind of manganese oxide carbon composite and preparation method thereof that molybdenum adulterates in situ |
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| Title |
|---|
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| Engineering pseudocapacitive MnMoO4@C microrods for high energy sodium ion hybrid capacitors;Lin Gao等;《Electrochimica Acta》;138185 * |
| Facile room temperature synthesis and application of MnMoO4·0.9H2O as supercapacitor electrode material;Frederick Nti等;《Materials Letters》;146-150 * |
| Sonochemical synthesis, characterization, and electrochemical properties of MnMoO4 nanorods for supercapacitor applications;Ganesh Kumar Veerasubramani等;《Materials Chemistry and Physics》;836-842 * |
| Top-down tailoring of nanostructured manganese molybdate enhances its lithium storage properties;Lifeng Zhang等;《CrystEngComm》;5374-5381 * |
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