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Silver nanocolumn array vertically at the hole of porous alumina template and its preparation method and application

A technology of porous alumina and alumina template, applied in the direction of ion implantation plating, coating, metal material coating process, etc., can solve the problems of high SERS performance, unfavorable target molecular adsorption and other problems, and achieve improved SERS Activity, improve the electromagnetic field enhancement, and facilitate the effect of effective adsorption

Inactive Publication Date: 2016-01-20
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, both the periodic hexagonal quincunx-shaped silver nano-islands and their preparation methods have shortcomings. First, the nano-units constituting the periodic hexagonal quincunx-shaped silver nano-islands are height-limited silver nano-islands, and their SERS activity Only from the coupled electric field between the nano-islands, the contribution to the enhancement of SERS activity is limited; secondly, the specific surface area of ​​the solid-structured silver nano-islands is low, which is extremely unfavorable for the adsorption of target molecules in SERS detection; thirdly, the preparation method cannot Fabrication of silver nanostructure arrays with high SERS performance

Method used

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  • Silver nanocolumn array vertically at the hole of porous alumina template and its preparation method and application
  • Silver nanocolumn array vertically at the hole of porous alumina template and its preparation method and application
  • Silver nanocolumn array vertically at the hole of porous alumina template and its preparation method and application

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Experimental program
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Embodiment 1

[0029] The concrete steps of preparation are:

[0030] Step 1, first place the aluminum sheet in an oxalic acid solution with a temperature of 6°C and a concentration of 0.2mol / L, and anodize it at a DC voltage of 30V for 4h. Then soak it in a mixed solution of phosphochromic acid at 55° C. for 6 hours to obtain an intermediate product.

[0031] In step 2, the intermediate product is placed in an oxalic acid solution with a temperature of 6°C and a concentration of 0.2 mol / L, and anodized at a DC voltage of 30V for 60s. Then soak it in a phosphoric acid solution with a temperature of 30°C and a concentration of 3wt% for 10 minutes, repeat the above process 10 times, and obtain an alumina template with conical holes.

[0032] Step 3, place the aluminum oxide template with a tapered hole in the ion sputtering device so that the distance between it and the silver target in the ion sputtering device is 8 cm, the current during sputtering is 10 mA, and the time is 30 min. made ap...

Embodiment 2

[0034] The concrete steps of preparation are:

[0035] Step 1, first place the aluminum sheet in an oxalic acid solution with a temperature of 10°C and a concentration of 0.25mol / L, and anodize it at a DC voltage of 35V for 3.5h. Then soak it in a mixed solution of phosphochromic acid at 58° C. for 5 hours to obtain an intermediate product.

[0036] In step 2, the intermediate product is placed in an oxalic acid solution at a temperature of 10° C. and a concentration of 0.25 mol / L, and anodized at a DC voltage of 35 V for 50 seconds. Then soak it in a phosphoric acid solution with a temperature of 35°C and a concentration of 4wt% for 8 minutes, repeat the above process 13 times, and obtain an alumina template with conical holes.

[0037] Step 3, place the aluminum oxide template with a tapered hole in the ion sputtering device so that the distance between it and the silver target in the ion sputtering device is 9 cm, the current during sputtering is 18 mA, and the time is 26 ...

Embodiment 3

[0039] The concrete steps of preparation are:

[0040] Step 1, first place the aluminum sheet in an oxalic acid solution with a temperature of 15°C and a concentration of 0.3mol / L, and anodize it at a DC voltage of 40V for 3h. Then soak it in a mixed solution of phosphochromic acid at 60° C. for 4.5 hours to obtain an intermediate product.

[0041] In step 2, the intermediate product is placed in an oxalic acid solution with a temperature of 15° C. and a concentration of 0.3 mol / L, and anodized at a DC voltage of 40 V for 40 seconds. Then soak it in a phosphoric acid solution with a temperature of 40°C and a concentration of 6wt% for 6 minutes, repeat the above process 15 times, and obtain an alumina template with conical holes.

[0042] Step 3, place the aluminum oxide template with a tapered hole in the ion sputtering device so that the distance between it and the silver target in the ion sputtering device is 10 cm, the current during sputtering is 25 mA, and the time is 21...

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Abstract

The invention discloses a silver nanometer column array erected on the orifice of a porous alumina template and a preparation method and application thereof. The silver nanometer column array is characterized in that silver nanometer columns with the heights of 30-200 nanometers and the diameters of 30-60 nanometers are sequentially hexagonally arrayed on the periphery of the orifice of the porous anodic alumina template with taper holes; and silver nanometer particles with the particle size of 5-40 nanometers are attached to the walls of the taper holes. The preparation method comprises the following steps of: firstly placing an aluminum sheet into an oxalic acid solution, and carrying out anodization at direct-current voltage for at least 2 hours; then placing into a phosphorus-chromium acid mixed solution, and soaking for at least 3 hours to obtain an intermediate product; then firstly placing the intermediate product into the oxalic acid solution, carrying out the anodization at the direct-current voltage for at least 20 seconds, then placing the intermediate product into a phosphorus acid solution, and soaking for at least 1 minute; repeating the process for at least 10 times to obtain the alumina template with the holes in the shape of the taper holes; and then placing the alumina template into an ion sputter for silver sputtering so as to prepare a target product. The silver nanometer column array disclosed by the invention can be used as an active base of surface-enhanced Raman scattering; and the content of rhodamine or tetrachlorobiphenyl which is attached to the silver nanometer column array is measured by using a laser Raman spectrometer.

Description

technical field [0001] The invention relates to a silver nanocolumn array, its preparation method and application, in particular to a silver nanocolumn array perpendicular to the hole of a porous alumina template, its preparation method and application. Background technique [0002] Recently, the Raman (Raman) spectroscopic analysis technology based on the surface-enhanced Raman scattering (SERS) effect of noble metals has the advantages of rapidity and sensitivity, and it has attracted more and more people in the trace analysis of chemistry and biochemistry widespread attention. Practice has proved that one of the keys to the effective application of this technology is to obtain a substrate with a uniform and stable structure, high SERS activity, and good signal repeatability. To this end, people have made unremitting efforts, such as an "ordered and controllable surface-enhanced Raman scattering active substrate and its preparation method" disclosed in the Chinese inventi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25D11/12C23C14/34C23C14/18G01N21/65
Inventor 孙克喜孟国文赵相龙朱储红黄竹林
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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