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Method for preparing nano-composite by controllable deposition of silver atoms on surface of nano-oxide

A nano-oxide and nano-composite technology, applied in the nano field, can solve the problems of large size of silver particles and difficult to effectively control the reduction process, and achieve the effects of high catalytic activity, good application value and mild reaction conditions.

Inactive Publication Date: 2016-01-27
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this method, the photoinduced electronic excitation is generally completed quickly at the beginning of the synthesis process, making it difficult to effectively control the entire reduction process, so the size of the silver particles obtained is often large (≧3nm), and this method is limited to titanium dioxide with optoelectronic properties. materials, other transition metal and rare earth metal oxides with poor photosensitivity cannot be used

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Disperse 50mg of nano-titanium dioxide (5nm) and 20mg of oleylamine into 50mL of cyclohexane solvent, and ultrasonically treat it for 10min to obtain a stable titanium dioxide dispersion A;

[0028] (2) Weigh 0.17g of silver nitrate and 1g of oleylamine into 10ml of cyclohexane, fully stir until completely dissolved, and obtain silver precursor solution B;

[0029] (3) 1ml of silver precursor solution B is added to the above-mentioned titanium dioxide dispersion A, fully stirred and mixed evenly;

[0030] (4) Then add 1 mmol of formaldehyde, and place it in a water bath at 50°C for reaction;

[0031] (5) Take out the sample after 2.5 hours of reaction, add ethanol for sedimentation, centrifuge, wash and repeat three times, and then redisperse in cyclohexane to obtain a silver-titanium dioxide nanocomposite with a silver content of about 15% (mass percentage). According to ultra-high resolution scanning electron microscopy (Ultra-HRSEM) analysis, the average size of...

Embodiment 2

[0033] (1) Disperse 100 mg of nanometer manganese tetraoxide (5 nm) and 10 mg of hexadecylamine into 100 mL of hexane solvent, and ultrasonically treat it for 10 minutes to obtain a stable dispersion A of trimanganese tetraoxide;

[0034] (2) Add 0.62g of silver oxalate and 1mL of ethylenediamine into 10ml of hexane, stir well until completely dissolved, and obtain silver precursor solution B;

[0035] (3) 3ml of silver precursor solution B is added in the above-mentioned trimanganese tetraoxide dispersion A, fully stirred and mixed;

[0036] (4) Then add 4 mmol of formaldehyde and place it in a water bath at 50°C for reaction;

[0037] (5) Take out the sample after 6 hours of reaction, add ethanol to settle, centrifuge, wash and redisperse in cyclohexane after repeating three times, obtain the silver-trimanganese tetraoxide nanocomposite containing silver about 30% (mass percentage) . According to ultra-high resolution scanning electron microscope (Ultra-HRSEM) analysis, th...

Embodiment 3

[0039] (1) Disperse 250mg of nanometer zirconia (5nm) and 25mg of octadecylamine into 200mL of toluene solvent, and ultrasonically treat it for 10min to obtain a stable zirconia dispersion A;

[0040] (2) Take by weighing 0.17g silver nitrate and 1.2g octadecylamine and join in 10ml toluene, fully stir until completely dissolving, obtain silver precursor solution B;

[0041] (3) 7ml silver precursor solution B is added in the above-mentioned zirconium dioxide dispersion liquid A, fully stirs and mixes;

[0042] (4) Then add 2.3mmol of formaldehyde and place it in a water bath at 50°C for reaction;

[0043] (5) After reacting for 9 hours, take out the sample, add ethanol for sedimentation, centrifuge, wash and repeat three times, and then redisperse in cyclohexane to obtain a silver-zirconia nanocomposite with a silver content of about 50% (mass percentage). According to ultra-high resolution scanning electron microscopy (Ultra-HRSEM) analysis, the average size of silver nanoc...

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Abstract

The invention discloses a method for preparing a nano-composite by controllable deposition of silver atoms on the surface of nano-oxide. The nano-composite is composed of transition metal or rare-earth oxide and silver cluster which is deposited and grows on the surface of transition metal or rare-earth oxide. The method is realized through an organic amine improved silver mirror reaction. That is to say, silver atoms generated by reducing a silver amine complex with aldehyde are controllably deposited on the surface of nano-oxide. By using organic amine as a complexing agent, the silver mirror reaction can be carried out in a mild and controllable way. The method comprises the following specific steps: dispersing surfactant-wrapped nano-oxide into an organic solvent to obtain a system A; dissolving silver salt and organic amine in an organic solvent to obtain a silver amine complex solution B; and adding the solution B into the system A, adding an excessive amount of aldehyde and keeping for 1-30 h, precipitating a product with ethanol, centrifuging and washing to obtain the nano-composite. By changing addition amount of the silver source and effectively controlling reaction time, size of silver species in the nano-composite is controlled within 0.3-3 nm.

Description

technical field [0001] The invention belongs to the field of nanotechnology, and in particular relates to a method for preparing nanocomposites by controllable deposition of silver atoms on the surface of nanometer oxides. technical background [0002] In recent years, nanocomposites formed by transition metals and their nanoclusters uniformly distributed on the surface of nanoscale oxides have attracted widespread attention as a very valuable nanomaterial. Especially in the field of catalysis, it has very good catalytic performance as a catalyst. Compared with the traditional metal salt impregnation method, an obvious advantage of the in-situ reduction deposition method is that it can effectively control the entire reduction deposition process, so that the size of the metal particles loaded on the surface of the oxide can be controlled and distributed uniformly, and the impregnation method can be avoided. Aggregation occurs during high temperature pyrolysis, making size co...

Claims

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Application Information

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IPC IPC(8): C23C18/44B82Y40/00B82Y30/00B01J23/50B01J23/68B01J23/89
Inventor 程谟杰王鑫
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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