CN105152225A - Preparation method of nanometer transition metal oxide and metal elementary substance material - Google Patents
Preparation method of nanometer transition metal oxide and metal elementary substance material Download PDFInfo
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- CN105152225A CN105152225A CN201510404102.4A CN201510404102A CN105152225A CN 105152225 A CN105152225 A CN 105152225A CN 201510404102 A CN201510404102 A CN 201510404102A CN 105152225 A CN105152225 A CN 105152225A
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Abstract
A preparation method of a nanometer transition metal oxide and metal elementary substance material is characterized in that the material comprises Cr2O3, TiO2, MnO, Fe3O4, CoO, NiO, ZnO, Cu, Au and Ag nanoparticles; and the method comprises the following steps: 1, mixing a metal salt with a long-chain amino organic matter solution, carrying out a reflux condensation reaction in nitrogen or argon atmosphere, and cooling to room temperature to obtain a reaction solution; and 2, adding a low boiling point solvent A to the reaction solution, uniformly stirring, standing for settlement, centrifuging, dispersing the above obtained particle product in n-hexane, and preserving the dispersed product in a ventilating dry place. The product particle prepared in the invention has the advantages of small particle size, narrow particle size distribution, good dispersion, easy control, high catalytic activity, and good electrochemical performances and cycle performances; and the preparation method has the advantages of simple process, low cost, easy operation, low energy consumption, environmental protection, and suitableness for large scale production.
Description
Technical field
The present invention relates to the preparation method of metal oxide nanoparticles, particularly a kind of transition metal oxide of nanometer and the preparation method of metal simple-substance material.
Background technology
Metal oxide is the important multifunctional material of a class, and the application in energy field receives much concern.Wherein, the cheap transition metal oxide of the nanometer of little, the high dispersive of particle diameter has high reactivity, advantages of simple structure and simple and being widely studied and applied because of it.But in current synthetic method, the temperature of reaction that the particle size prepared because of it such as hydrothermal method, sol-gel method is large and higher and limit practical application.Therefore, exploitation is a kind of simple to operate, with low cost, and the transition metal oxide material that eco-friendly method carrys out synthesis of nano has great importance.
Summary of the invention
The object of the invention is for above-mentioned existing problems, a kind of technique is simple, temperature of reaction is low, with low cost and energy consumption the is low transition metal oxide of nanometer and the preparation method of metal simple-substance material are provided.
Technical scheme of the present invention:
The transition metal oxide of nanometer and a preparation method for metal simple-substance material, transition metal oxide and the metal simple-substance material of described nanometer comprise Cr
2o
3, TiO
2, MnO, Fe
3o
4, CoO, NiO, ZnO, Cu, Au and Ag nano particle, step is as follows:
1) by metal-salt and long chain amino organic solution mixing and vigorous stirring after, under nitrogen or argon gas atmosphere, carry out condensing reflux, reflux temperature is 100-200 DEG C, and return time 1-12 hour obtains reaction solution after being cooled to room temperature;
2) low boiling point solvent A is added stir in above-mentioned reaction solution after standing sedimentation, the centrifugal granular product normal hexane obtained is disperseed and is kept at air seasoning place.
Described metal-salt is the muriate of transition metal, nitrate, carbonate or vitriol, and wherein transition metal is titanium, chromium, manganese, iron, cobalt, nickel, copper, zinc, silver or golden; Long chain amino organic solution is oleic acid solutions, amino dodecane solution, cetylamine solution or octadecenyl amine solution; The mol ratio of metal-salt and long chain amino organic solution is 1:40.
Described solvent orange 2 A is ethanol, acetone or methylene dichloride, and the volume ratio of low boiling point solvent A and reaction solution is 3:1.
Advantage of the present invention and beneficial effect are:
This preparation method's technique is simple, with low cost, easy handling and energy consumption is low; The product grain particle diameter of preparation is little, size distribution is narrower, good dispersion degree and be easy to control, and the transition metal oxide of nanometer shows higher catalytic activity, better chemical property and cycle performance; Can not environmental pollution be caused in preparation process, environmental protection, be applicable to scale operation.
Accompanying drawing explanation
Fig. 1 is Fe
3o
4the XRD figure of nano particle.
Fig. 2 is Fe
3o
4the TEM figure of nano particle.
Fig. 3 is the XRD figure of CoO nano particle.
Fig. 4 is the TEM figure of CoO nano particle.
Fig. 5 is the XRD figure of NiO nano particle.
Fig. 6 is the TEM figure of NiO nano particle.
Fig. 7 is the XRD figure of ZnO nano particle.
Fig. 8 is the TEM figure of ZnO nano particle.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1:
A kind of transition metal oxide Fe
3o
4the preparation method of nano particle, step is as follows:
1) by 0.2gFe (NO
3)
39H
2o and 10mL oleic acid solutions adds in there-necked flask after vigorous stirring respectively, carries out condensing reflux under an argon atmosphere, and reflux temperature is 200 DEG C, and return time 4 hours, obtains reaction solution after being cooled to room temperature;
2) 30mL ethanol is added stir in above-mentioned reaction solution after standing sedimentation, the centrifugal granular product normal hexane obtained is disperseed, is kept at air seasoning place.
Fig. 1 is obtained Fe
3o
4the XRD figure of nano particle, shows in figure: all diffraction peaks of product all can be attributed to the Fe of Emission in Cubic
3o
4.
Fig. 2 is obtained Fe
3o
4the TEM figure of nano particle, shows in figure: Fe
3o
4the pattern of nano particle is quantum dot, and particle diameter is 3-7nm.
Embodiment 2:
A preparation method for transition metal oxide CoO nano particle, step is as follows:
1) by 0.2gCoCO
3, 10mL oleic acid solutions adds in there-necked flask after vigorous stirring respectively, carry out condensing reflux under an argon atmosphere, reflux temperature is 180 DEG C, and return time 8 hours, obtains reaction solution after being cooled to room temperature;
2) 30mL acetone is added stir in above-mentioned reaction solution after standing sedimentation, the centrifugal granular product normal hexane obtained is disperseed, is kept at air seasoning place.
Fig. 3 is the XRD figure of obtained CoO nano particle, shows in figure: all diffraction peaks of product all can be attributed to the CoO of Emission in Cubic.
Fig. 4 is the TEM figure of obtained CoO nano particle, shows: the pattern of CoO nano particle is nano cubic, and particle diameter is 20-25nm in figure.
Embodiment 3:
A preparation method for transition metal oxide NiO nano particle, step is as follows:
1) by 0.5gNiSO
46H
2o, 8mL amino dodecane solution adds in there-necked flask after vigorous stirring respectively, carries out condensing reflux under an argon atmosphere, and reflux temperature is 100 DEG C, and return time 12 hours, obtains reaction solution after being cooled to room temperature;
2) 30mL acetone is added stir in above-mentioned reaction solution after standing sedimentation, the centrifugal granular product normal hexane obtained is disperseed, is kept at air seasoning place.
Fig. 5 is the XRD figure of obtained NiO nano particle, shows in figure: all diffraction peaks of product all can be attributed to the NiO of Emission in Cubic.
Fig. 6 is the TEM figure of obtained NiO nano particle, shows: the pattern of NiO nano particle is nano flower, and particle diameter is 30-40nm in figure.
Embodiment 4:
A preparation method for transition metal oxide ZnO nano particle, step is as follows:
1) by 0.3gZnCl
26H
2o, 10mL octadecenyl amine solution adds in there-necked flask after vigorous stirring respectively, carries out condensing reflux in a nitrogen atmosphere, and reflux temperature is 200 DEG C, and return time 8 hours, obtains reaction solution after being cooled to room temperature;
2) 20mL methylene dichloride is added stir in above-mentioned reaction solution after standing sedimentation, the centrifugal granular product hexanaphthene obtained is disperseed, is kept at air seasoning place.
Fig. 7 is the XRD figure of obtained ZnO nano particle, shows in figure: all diffraction peaks of product all can be attributed to the ZnO of six side's phases.
Fig. 8 is the TEM figure of obtained ZnO nano particle, shows: the pattern of ZnO nano particle is nanometer sheet, and particle diameter is 30-40nm in figure.
Claims (3)
1. the transition metal oxide of nanometer and a preparation method for metal simple-substance material, is characterized in that: transition metal oxide and the metal simple-substance material of described nanometer comprise Cr
2o
3, TiO
2, MnO, Fe
3o
4, CoO, NiO, ZnO, Cu, Au and Ag nano particle, step is as follows:
1) by metal-salt and long chain amino organic solution mixing and vigorous stirring after, under nitrogen or argon gas atmosphere, carry out condensing reflux, reflux temperature is 100-200 DEG C, and return time 1-12 hour obtains reaction solution after being cooled to room temperature;
2) low boiling point solvent A is added stir in above-mentioned reaction solution after standing sedimentation, the centrifugal granular product normal hexane obtained is disperseed and is kept at air seasoning place.
2. the transition metal oxide of nanometer and the preparation method of metal simple-substance material according to claim 1, it is characterized in that: described metal-salt is the muriate of transition metal, nitrate, carbonate or vitriol, wherein transition metal is titanium, chromium, manganese, iron, cobalt, nickel, copper, zinc, silver or golden; Long chain amino organic solution is oleic acid solutions, amino dodecane solution, cetylamine solution or octadecenyl amine solution; The mol ratio of metal-salt and long chain amino organic solution is 1:40.
3. the transition metal oxide of nanometer and the preparation method of metal simple-substance material according to claim 1, it is characterized in that: described solvent orange 2 A is ethanol, acetone or methylene dichloride, the volume ratio of low boiling point solvent A and reaction solution is 3:1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105562033A (en) * | 2016-03-09 | 2016-05-11 | 扬州大学 | Preparation method of hydrophilic Fe3O4-Au double-faced particle catalyst |
| CN107399767A (en) * | 2017-08-28 | 2017-11-28 | 四川理工学院 | A kind of Fe doping NiO composites and semiconductor gas sensor |
| CN108080035A (en) * | 2016-11-22 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of method of hydrocarbon catalytic selective oxidation |
| CN109876176A (en) * | 2019-02-22 | 2019-06-14 | 泉州市洛江区汇丰妇幼用品有限公司 | A kind of Traditional Chinese medicine bacteriostatic sanitary napkin |
-
2015
- 2015-07-10 CN CN201510404102.4A patent/CN105152225A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| XUEMIN HE ET AL.: "Phase- and Size-Dependent Optical and Magnetic Properties of CoO Nanoparticles", 《J. PHYS. CHEM. C》 * |
| 窦永华 等: "单分散Fe3O4纳米粒子的合成、表征及其自组装", 《功能材料》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105562033A (en) * | 2016-03-09 | 2016-05-11 | 扬州大学 | Preparation method of hydrophilic Fe3O4-Au double-faced particle catalyst |
| CN108080035A (en) * | 2016-11-22 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of method of hydrocarbon catalytic selective oxidation |
| CN108080035B (en) * | 2016-11-22 | 2021-01-22 | 中国科学院大连化学物理研究所 | Method for catalytic selective oxidation of hydrocarbon |
| CN107399767A (en) * | 2017-08-28 | 2017-11-28 | 四川理工学院 | A kind of Fe doping NiO composites and semiconductor gas sensor |
| CN107399767B (en) * | 2017-08-28 | 2019-05-03 | 四川理工学院 | A kind of Fe doping NiO composite material and semiconductor gas sensor |
| CN109876176A (en) * | 2019-02-22 | 2019-06-14 | 泉州市洛江区汇丰妇幼用品有限公司 | A kind of Traditional Chinese medicine bacteriostatic sanitary napkin |
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