CN104261478A - Preparation method of Mn3O4 nanowire or nanorod - Google Patents
Preparation method of Mn3O4 nanowire or nanorod Download PDFInfo
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- CN104261478A CN104261478A CN201410480565.4A CN201410480565A CN104261478A CN 104261478 A CN104261478 A CN 104261478A CN 201410480565 A CN201410480565 A CN 201410480565A CN 104261478 A CN104261478 A CN 104261478A
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- 239000002070 nanowire Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 title abstract description 12
- 239000002073 nanorod Substances 0.000 title abstract description 11
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 25
- 239000001632 sodium acetate Substances 0.000 claims abstract description 25
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 15
- 239000011572 manganese Substances 0.000 claims description 57
- 229960004249 sodium acetate Drugs 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 238000005119 centrifugation Methods 0.000 claims description 14
- 150000003839 salts Chemical class 0.000 claims description 8
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N nitrate group Chemical group [N+](=O)([O-])[O-] NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 150000002696 manganese Chemical class 0.000 abstract description 11
- 238000009826 distribution Methods 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract 2
- 238000004729 solvothermal method Methods 0.000 abstract 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 230000005389 magnetism Effects 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- BXRRQHBNBXJZBQ-UHFFFAOYSA-L dichloromanganese;hydrate Chemical compound O.Cl[Mn]Cl BXRRQHBNBXJZBQ-UHFFFAOYSA-L 0.000 description 7
- BZDIAFGKSAYYFC-UHFFFAOYSA-N manganese;hydrate Chemical compound O.[Mn] BZDIAFGKSAYYFC-UHFFFAOYSA-N 0.000 description 5
- 239000002086 nanomaterial Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- VASIZKWUTCETSD-UHFFFAOYSA-N manganese(II) oxide Inorganic materials [Mn]=O VASIZKWUTCETSD-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000007669 thermal treatment Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical compound [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000035484 reaction time Effects 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
- 229910003174 MnOOH Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method of a Mn3O4 nanowire or nanorod. The preparation method comprises the following steps: adding a divalent manganese salt and sodium acetate into low alcohol, and stirring to obtain a transparent liquid; preparing a Mn3O4 nanowire or nanorod from the liquid by adopting a solvothermal method; centrifugally separating and washing after the reaction to obtain the Mn3O4 nanowire or nanorod. According to the preparation method of the Mn3O4 nanowire or nanorod, the Mn3O4 nanowire or nanorod is synthesized by one step by utilizing the solvothermal method; and the Mn3O4 nanowire or nanorod with a needed slenderness ratio can be obtained in a controllable manner by changing the reaction conditions. The preparation method is simple in preparation process, efficient and low in raw material cost, and has significance in large-scale industrial production and practical application of the Mn3O4 nanowire or nanorod. The obtained Mn3O4 nanowire or nanorod is high in yield, high in purity, uniform in morphology and narrow in dimension distribution, has relatively good magnetism and is widely applied in catalysis, solar cells, heavy metal ion adsorption and the like.
Description
Technical field
The present invention relates to a kind of Mn
3o
4the preparation method of nano wire or nanometer rod, is specifically related to the Mn that a kind of length-to-diameter ratio is adjustable
3o
4the preparation method of nano wire or nanometer rod.
Background technology
Mn
3o
4nano material from the brown effect having reversible color to yellow, can be applied in the electrochromic material in anode material due to it, also can as catalyst application in oxidation or reduction reaction.One dimension Mn
3o
4nano material, due to the physicochemical property of its uniqueness, has good optics, electricity and mechanical characteristic usually, catalysis, solar cell, heavy metal ion adsorbed etc. in have a wide range of applications.
Domestic and international report prepares one dimension Mn
3o
4nano material is not a lot.CN 200810103467.3 discloses one and utilizes chemical Vapor deposition process to prepare Mn
3o
4the method of nano wire, is placed on Mn powder in aluminium sesquioxide crucible, directly over place plated film silicon chip, pass into the Mn that argon thermal treatment obtains tetragonal
3o
4nano wire.Document " Odair P. Ferreira; Larissa Otubo; Ricardo Romano; and Oswaldo L. Alves. Crystal Growth & Design; 2006; 6 (2), 601-606 " reports and the MnOOH nanometer rod thermal treatment of preparation is obtained MnO
2, Mn
2o
3, Mn
3o
4nanometer rod.Document " Wenzhong Wang and Ling Ao. Crystal Growth & Design, 2008,8 (1), 358-362 " reports and presoma is obtained Mn by thermal treatment in the environment of sodium-chlor
3o
4nano wire.
At present, synthesizing one-dimensional Mn
3o
4the preparation process major part of nano material all needs thermal treatment and higher temperature, and some method also needs protection or the secondary treatment of rare gas element.Operating process relative complex, cost is higher, is unfavorable for accurate control and suitability for industrialized production.
Summary of the invention
The present invention is directed to the deficiency that existing method exists, provide a kind of Mn
3o
4the preparation method of nanometer rod or nano wire.This preparation method is simple to operate, one-step synthesis, and without the need to protection of inert gas, the prices of raw and semifnished materials are cheap, and product length-to-diameter ratio is adjustable, and controllability is strong.
The present invention is manganese source with manganous salt, mixes be made into clear solution with sodium-acetate, then adopts solvent-thermal method to obtain Mn
3o
4nano wire or nanometer rod.The method can be comparatively simple, controlled the Mn obtaining required length-to-diameter ratio
3o
4nano wire or nanometer rod, have good industrial applications prospect.
Concrete technical scheme is as follows:
A kind of Mn
3o
4the preparation method of nano wire or nanometer rod, comprises the following steps:
(1) manganous salt and sodium-acetate are joined in lower alcohol, stir and obtain clear solution;
(2) solvent-thermal method is adopted to prepare Mn above-mentioned clear solution
3o
4nano wire or nanometer rod;
(3) centrifugation after reaction, washing, obtain Mn
3o
4nano wire or nanometer rod.
In aforesaid method, the nanometer rod of indication, be diameter at 500nm or following, length-to-diameter ratio exists
20following material; The nano wire of indication, refers to that diameter is at 500nm or following, the material of length-to-diameter ratio more than 30.
By method of the present invention, Mn can be obtained easily
3o
4nano wire or nanometer rod, gained Mn
3o
4the diameter of nano wire is 70-500 nm, and length-to-diameter ratio is 30-240; Mn
3o
4the diameter of nanometer rod is 70-500 nm, and length-to-diameter ratio is
7-20.
In above-mentioned steps (1), the mol ratio of divalence water-soluble manganese salt and sodium-acetate is 1:4-20.The mol ratio of manganese salt and sodium-acetate is control Mn
3o
4one of important factor of pattern.When other experiment conditions remain unchanged, the mol ratio of manganese salt and sodium-acetate is lower, when being in 1:4-9 scope, can obtain Mn
3o
4nanometer rod; When the mol ratio of manganese salt and sodium-acetate is higher, when being in 1:10-20 scope, Mn can be obtained
3o
4nano wire.The relative content of sodium-acetate is higher, Mn
3o
4the length of nanostructure is longer.
In above-mentioned steps (1), described lower alcohol is methyl alcohol, ethanol, propyl alcohol, butanols or Virahol.
In above-mentioned steps (1), described divalence water-soluble manganese salt is nitrate or the halogenide of manganese.
In above-mentioned steps (1), the concentration of divalence water-soluble manganese salt in clear solution is 0.06-0.15 mol/L.
In above-mentioned steps (2), the temperature of solvent-thermal method is 160-190 DEG C.
In above-mentioned steps (2), the reaction times of solvent-thermal method is 8-30 h, preferred 14-30 h.
In aforesaid method of the present invention, by changing reaction conditions, the Mn of different length-to-diameter ratio can be obtained
3o
4nano wire or nanometer rod, controllability is strong.The mol ratio of manganese salt and sodium-acetate, and react solvent system (alcohol system) used to Mn
3o
4pattern be formed with vital role, by their cooperation, nano wire or the nanorod structure of required pattern can be obtained.In addition, the Mn of different length-to-diameter ratio can be obtained by the concentration of adjustment manganese salt, the temperature and time of solvent-thermal method
3o
4nano wire or nanometer rod, the selection of these conditions also can make that the pattern of product is more regular, distribution of sizes is narrower.
The present invention utilizes solvent-thermal method one-step synthesis Mn
3o
4nano wire or nanometer rod, by changing manganese salt and the mol ratio of sodium-acetate, the condition such as concentration, temperature of reaction, reaction times of manganese salt, the Mn obtaining required length-to-diameter ratio that can be controlled
3o
4nano wire or nanometer rod.Preparation technology of the present invention is simple, efficient, low raw-material cost, production cost are low, can regulate and control to obtain the Mn of different length-to-diameter ratio by controlling reaction conditions
3o
4nano wire or nanometer rod, to Mn
3o
4mass industrialized production and the practical application thereof of nano wire or nanometer rod are significant.Products therefrom output is high, purity is high, pattern is homogeneous, narrow size distribution, has good magnetic, catalysis, solar cell, heavy metal ion adsorbed etc. in have a wide range of applications.
Accompanying drawing explanation
Fig. 1 is scanning electron microscope (SEM) picture of the manganic manganous oxide nanometer wire that the embodiment of the present invention 1 is synthesized.
Fig. 2 is X-ray diffraction (XRD) collection of illustrative plates of the manganic manganous oxide nanometer wire that the embodiment of the present invention 1 is synthesized.
Fig. 3 is magnetic hysteresis loop (VSM) collection of illustrative plates of the manganic manganous oxide nanometer wire that the embodiment of the present invention 1 is synthesized.
Fig. 4 is scanning electron microscope (SEM) picture of the trimanganese tetroxide nano rod that the embodiment of the present invention 3 is synthesized.
Fig. 5 is scanning electron microscope (SEM) picture of the trimanganese tetroxide structure of comparative example 1 of the present invention synthesis.
Embodiment
Below by embodiment, the present invention will be further elaborated, and following explanation has been only explanation the present invention, do not limit its content.
embodiment 1
The four chloride hydrate manganese of 0.495 g, the sodium-acetate of 2.914 g join in 25 mL ethanol and stir to clarify by 1.1;
Above-mentioned solution is transferred in reactor by 1.2, reacts 16 h at 180 DEG C;
After 1.3 reactions terminate, through centrifugation and washing, obtaining diameter is 80-130 nm, and length-to-diameter ratio is the Mn of 65-85
3o
4nano wire.As shown in Figure 1, as can be seen from the figure, products obtained therefrom pattern is regular, single, smooth surface for the SEM figure of product.As shown in Figure 2, XRD result and standard x RD card (24-0734) are consistent the XRD figure of product, prove that the crystalline phase of products therefrom is Mn
3o
4phase.As shown in Figure 3, can find out that the magnetic performance of product is good, its magnetic saturation intensity is 0.0236 emu/g to the magnetic hysteresis loop of product, and coercive force is 98.7 Oe.
embodiment 2
The four nitric hydrate manganese of 0.628 g, the sodium-acetate of 4.100 g join in 40 mL methyl alcohol and stir to clarify by 2.1;
Above-mentioned solution is transferred in reactor by 2.2, reacts 25 h at 190 DEG C;
After 2.3 reactions terminate, through centrifugation and washing, obtaining diameter is 380-430 nm, and length-to-diameter ratio is the Mn of 92-110
3o
4nano wire.
embodiment 3
The four chloride hydrate manganese of 0.495 g, the sodium-acetate of 1.457 g join in 25 mL ethanol and stir to clarify by 3.1;
Above-mentioned solution is transferred in reactor by 3.2, reacts 16 h at 180 DEG C;
After 3.3 reactions terminate, through centrifugation and washing, obtaining diameter is 130-160 nm, and length-to-diameter ratio is the Mn of 15-18
3o
4nanometer rod, as shown in Figure 4, as can be seen from the figure, products obtained therefrom is club shaped structure to the SEM figure of product, smooth surface.
embodiment 4
The four nitric hydrate manganese of 0.628 g, the sodium-acetate of 3.076 g join in 17 mL propyl alcohol and stir to clarify by 4.1;
Above-mentioned solution is transferred in reactor by 4.2, reacts 9 h at 160 DEG C;
After 4.3 reactions terminate, through centrifugation and washing, obtaining diameter is 75-110 nm, and length-to-diameter ratio is the Mn of 80-102
3o
4nano wire.
embodiment 5
The four chloride hydrate manganese of 0.495 g, the sodium-acetate of 2.060 g join in 20 mL butanols and stir to clarify by 5.1;
Above-mentioned solution is transferred in reactor by 5.2, reacts 29 h at 170 DEG C;
After 5.3 reactions terminate, through centrifugation and washing, obtaining diameter is 175-210 nm, and length-to-diameter ratio is the Mn of 52-74
3o
4nano wire.
embodiment 6
The four chloride hydrate manganese of 0.495 g, the sodium-acetate of 1.840 g join in 30 mL Virahols and stir to clarify by 6.1;
Above-mentioned solution is transferred in reactor by 6.2, reacts 8 h at 170 DEG C;
After 6.3 reactions terminate, through centrifugation and washing, obtaining diameter is 95-120 nm, and length-to-diameter ratio is the Mn of 12-16
3o
4nanometer rod.
embodiment 7
The four nitric hydrate manganese of 0.628 g, the sodium-acetate of 1.330 g join in 17 mL methyl alcohol and stir to clarify by 7.1;
Above-mentioned solution is transferred in reactor by 7.2, reacts 24 h at 170 DEG C;
After 7.3 reactions terminate, through centrifugation and washing, obtaining diameter is 180-195 nm, and length-to-diameter ratio is the Mn of 14-17
3o
4nanometer rod.
embodiment 8
The four chloride hydrate manganese of 0.495 g, the sodium-acetate of 0.83 g join in 40 mL butanols and stir to clarify by 8.1;
Above-mentioned solution is transferred in reactor by 8.2, reacts 10 h at 180 DEG C;
After 8.3 reactions terminate, through centrifugation and washing, obtaining diameter is 165-178 nm, and length-to-diameter ratio is the Mn of 10-13
3o
4nanometer rod.
embodiment 9
The four nitric hydrate manganese of 0.628 g, the sodium-acetate of 1.025 g join in 22 mL Virahols and stir to clarify by 9.1;
Above-mentioned solution is transferred in reactor by 9.2, reacts 28 h at 190 DEG C;
After 9.3 reactions terminate, through centrifugation and washing, obtaining diameter is 220-245 nm, and length-to-diameter ratio is the Mn of 9-13
3o
4nanometer rod.
comparative example 1
The four chloride hydrate manganese of 0.495 g, the sodium-acetate of 0.728 g join in 25 mL ethanol and stir to clarify by 1.1;
Above-mentioned solution is transferred in reactor by 1.2, reacts 16 h at 180 DEG C;
After 1.3 reactions terminate, through centrifugation and washing, obtain the Mn that pattern mixes
3o
4structure, as shown in Figure 5, product Mn
3o
4microscopic appearance be that particle and one-dimentional structure coexist.
comparative example 2
The four nitric hydrate manganese of 0.628 g, the sodium hydroxide of 0.725 g join in 30 mL methyl alcohol and stir to clarify by 2.1;
Above-mentioned solution is transferred in reactor by 2.2, reacts 16 h at 170 DEG C;
After 2.3 reactions terminate, through centrifugation and washing, the product obtained is irregular particle, distribution of sizes heterogeneity.
comparative example 3
The four chloride hydrate manganese of 0.495 g, the sodium-acetate of 1.640 g join in 25 mL water and stir to clarify by 3.1;
Above-mentioned solution is transferred in reactor by 3.2, reacts 20 h at 170 DEG C;
After 3.3 reactions terminate, through centrifugation and washing, the product obtained is octahedral structure, pattern rule, smooth surface.
Claims (9)
1. a Mn
3o
4the preparation method of nano wire or nanometer rod, is characterized in that comprising the following steps:
(1) manganous salt and sodium-acetate are joined in lower alcohol, stir and obtain clear solution;
(2) solvent-thermal method is adopted to prepare Mn above-mentioned clear solution
3o
4nano wire or nanometer rod;
(3) centrifugation after reaction, washing, obtain Mn
3o
4nano wire or nanometer rod.
2. preparation method according to claim 1, is characterized in that: in step (1), and the mol ratio of manganous salt and sodium-acetate is 1:4-20.
3. preparation method according to claim 1 and 2, is characterized in that: in step (1), when the mol ratio of manganous salt and sodium-acetate is 1:4-9, and gained Mn
3o
4structure is Mn
3o
4nanometer rod; When the mol ratio of manganous salt and sodium-acetate is 1:10-20, gained Mn
3o
4structure is Mn
3o
4nano wire.
4. the preparation method according to any one of claim 1-3, is characterized in that: in step (1), and described lower alcohol is methyl alcohol, ethanol, propyl alcohol, butanols or Virahol.
5. the preparation method according to any one of claim 1-4, is characterized in that: in step (1), and the concentration of manganous salt in clear solution is 0.06-0.15 mol/L.
6. the preparation method according to any one of claim 1-5, is characterized in that: in step (2), and the temperature of solvent-thermal method is 160-190 DEG C.
7. the preparation method according to any one of claim 1-6, is characterized in that: in step (2), and the time of solvent-thermal method is 8-30 h.
8. the preparation method according to any one of claim 1-7, is characterized in that: in step (1), and described manganous salt is nitrate or the halogenide of manganese.
9. the preparation method according to any one of claim 1-8, is characterized in that: Mn
3o
4the diameter of nano wire is 70-500 nm, and length-to-diameter ratio is 30-240; Mn
3o
4the diameter of nanometer rod is 70-500 nm, and length-to-diameter ratio is 7-20.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105797698A (en) * | 2016-04-13 | 2016-07-27 | 同济大学 | Preparation method and application of petal-shaped MoS2-Mn3O4 nanowire magnetic composite material |
| CN107555480A (en) * | 2017-09-19 | 2018-01-09 | 济南大学 | A kind of wax crayon shape Mn3O4The preparation method and products obtained therefrom of microstructure |
| CN108273518A (en) * | 2018-01-17 | 2018-07-13 | 济南大学 | A kind of SnS2/Mn3O4The synthetic method and products obtained therefrom of flower-shaped composite construction |
| CN110040783A (en) * | 2019-05-20 | 2019-07-23 | 新乡医学院 | Manganic manganous oxide nano-material, preparation method and application |
| CN111087030A (en) * | 2019-12-20 | 2020-05-01 | 佛山科学技术学院 | LiNi0.5Mn1.5O4Method for producing materials and use thereof |
| CN115028202A (en) * | 2022-01-13 | 2022-09-09 | 渤海大学 | Preparation of high saturation magnetization Mn 3 O 4 Method for magnetic nano rod |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102745749A (en) * | 2012-07-05 | 2012-10-24 | 兰州理工大学 | Preparation method for nanometer Mn3O4 particles |
| CN103193273A (en) * | 2013-05-03 | 2013-07-10 | 广东工业大学 | Preparation method of extra-long manganese dioxide nanowires |
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2014
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| CN102745749A (en) * | 2012-07-05 | 2012-10-24 | 兰州理工大学 | Preparation method for nanometer Mn3O4 particles |
| CN103193273A (en) * | 2013-05-03 | 2013-07-10 | 广东工业大学 | Preparation method of extra-long manganese dioxide nanowires |
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| CN105797698A (en) * | 2016-04-13 | 2016-07-27 | 同济大学 | Preparation method and application of petal-shaped MoS2-Mn3O4 nanowire magnetic composite material |
| CN107555480A (en) * | 2017-09-19 | 2018-01-09 | 济南大学 | A kind of wax crayon shape Mn3O4The preparation method and products obtained therefrom of microstructure |
| CN107555480B (en) * | 2017-09-19 | 2019-04-05 | 济南大学 | A kind of wax crayon shape Mn3O4The preparation method and products obtained therefrom of microstructure |
| CN108273518A (en) * | 2018-01-17 | 2018-07-13 | 济南大学 | A kind of SnS2/Mn3O4The synthetic method and products obtained therefrom of flower-shaped composite construction |
| CN108273518B (en) * | 2018-01-17 | 2021-03-02 | 济南大学 | Flower-shaped composite structure SnS2/Mn3O4Synthetic method of (2) and the resulting product |
| CN110040783A (en) * | 2019-05-20 | 2019-07-23 | 新乡医学院 | Manganic manganous oxide nano-material, preparation method and application |
| CN110040783B (en) * | 2019-05-20 | 2021-09-10 | 新乡医学院 | Manganous-manganic oxide nano material, preparation method and application thereof |
| CN111087030A (en) * | 2019-12-20 | 2020-05-01 | 佛山科学技术学院 | LiNi0.5Mn1.5O4Method for producing materials and use thereof |
| CN115028202A (en) * | 2022-01-13 | 2022-09-09 | 渤海大学 | Preparation of high saturation magnetization Mn 3 O 4 Method for magnetic nano rod |
| CN115028202B (en) * | 2022-01-13 | 2022-12-27 | 渤海大学 | Preparation of high saturation magnetization Mn 3 O 4 Method for magnetic nano rod |
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