Oxide nanocrystalline synthesis method

A synthesis method and oxide technology, applied in chemical instruments and methods, single crystal growth, crystal growth, etc., can solve the problems of harsh test conditions, poor monodispersity and weak stability of nanocrystals, and achieve good monodispersity , strong stability and low cost

Inactive Publication Date: 2011-04-27
南京紫同纳米科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The object of the present invention is to provide a kind of synthesis method of oxide nanocrystal, especially the synthesis method of manganese tetraoxide, manganese oxide, ferric oxide, cobaltous oxide nanocrystal, to overcome the nanocrystal monodisperse of making Poor performance, weak stability, high cost, harsh test conditions, etc.

Method used

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  • Oxide nanocrystalline synthesis method
  • Oxide nanocrystalline synthesis method
  • Oxide nanocrystalline synthesis method

Examples

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Embodiment 1

[0066] Manganous acetonide (0.506g, 2.0mmol), liquid paraffin (10mL), oleic acid (0.285g, 1.0mmol), oleylamine (0.803g, 3.0mmol), dodecanol (0.559g, 3.0mmol) Mix in a 50mL three-necked bottle; under nitrogen protection, the mixed solution was heated to 220°C for 2-3 minutes; then liquid paraffin (5mL) was quickly injected into the above solution and the reaction temperature dropped rapidly by 20-40°C; Set at 190°C for 60 minutes. Finally a black clear solution was formed which was slowly cooled to room temperature. Pour the above black solution into a separatory funnel containing a mixed solution of n-hexane (10 mL) and methanol (100 mL). Mix evenly and slightly heat (60-80°C) to precipitate out precipitates. The above purification is carried out 5 times, and finally a Mn of about 5nm can be obtained. 3 o 4 Nanocrystalline. The above-mentioned nanocrystalline precipitates can be easily dissolved in organic solvents such as n-hexane, octane, and toluene. Its X-ray diffrac...

Embodiment 2

[0068] Manganous acetonide (0.506g, 2.0mmol), liquid paraffin (10mL), oleic acid (0.285g, 1.0mmol), oleylamine (0.803g, 3.0mmol), dodecanol (0.559g, 3.0mmol) Mixed in a 50mL three-necked bottle; under the protection of nitrogen, the mixed solution was heated to 280°C for 2-3 minutes; then 5mL of liquid paraffin was quickly injected into the above solution, and the reaction temperature dropped rapidly; at the same time, the temperature was set at 250°C and kept for 60 Minutes, finally forming a black clear solution slowly cooled to room temperature. Purification method is with embodiment 1. Finally, MnO nanocrystals of about 15nm can be produced. By adjusting the injection temperature (240-330°C), we can obtain nanocrystals of different sizes. The corresponding X-ray diffraction pattern and transmission electron microscope pattern are shown in figure 1 , figure 2 .

Embodiment 3

[0070] Acetaldehyde acetonate iron (0.353g, 1.0mmol), liquid paraffin (10mL), oleic acid (0.285g, 1.0mmol), oleylamine (0.803g, 3.0mmol), dodecanol (0.559g, 3.0mmol) mixed In a 50mL three-neck flask. Under nitrogen protection, the mixed solution was heated to 270°C for 2-3 minutes; then 5mL of liquid paraffin was quickly injected into the above solution, and the reaction temperature dropped rapidly; at the same time, the temperature was set at 240°C for 60 minutes , and finally formed a black clear solution which was slowly cooled to room temperature. The purification method is the same as that in Example 1, and finally Fe of about 4nm can be obtained. 3 o 4 Nanocrystalline. By adjusting the injection temperature (270-330°C), we can obtain nanocrystals of different sizes. Its X-ray diffraction pattern and transmission electron microscope pattern are shown in image 3 , Figure 4 .

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Abstract

The invention relates to a method for synthesizing nano-crystalline of trimanganese tetroxide, manganous oxide, ferroferric oxide and cobaltous oxide. The method comprises the following steps: oxide precursor, non-coordinating solvent and activating agent are mixed, the mixed solution is heated to 210 to 330 DEG C in inert atmosphere and kept for 2 to 5min, then the temperature is reduced by 20 to 40 DEG C correspondingly and kept for 50 to 80min, and the oxide nano-crystalline can be obtained after the reaction solution is separated and purified. The method has the advantages of simple steps, strong operability, good repeatability, low cost and high production, nano-crystalline of different grain diameters can be synthesized, and simultaneously the synthesized nano-crystalline has good monodispersity and strong stability; particles of different sizes can be manufactured by simply changing the experimental conditions, therefore, the method has great application value not only in lab synthesis but also in industrial production.

Description

(1) Technical field [0001] The invention relates to a synthesis of oxide nanocrystals, in particular to a synthesis method of trimanganese tetraoxide, manganous oxide, ferric oxide and cobaltous oxide nanocrystals. (2) Background technology [0002] Oxide nanocrystals such as trimanganese tetroxide, manganous oxide, ferroferric oxide, and cobaltous oxide have shown great potential application value in many fields, such as catalysis, high-density magnetic storage, solar cells, varistors, magnetic fluids, magnetic Separation, magnetic imaging and other fields are research hotspots in today's science and technology and industry. [0003] Based on the above development prospects, the synthesis of monodisperse manganese tetraoxide, manganous oxide, ferric oxide, and cobalt oxide nanocrystals is a research hotspot in the academic and industrial circles. Previously reported methods mainly include: (1) Synthesis of manganese acetate, iron acetate or cobalt acetate with tri-n-octyla...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B7/14C01G1/02C30B29/16
Inventor 李林松司红磊
Owner 南京紫同纳米科技有限公司
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