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Sea urchin shaped nano-hemisphere array as well as preparation method and application thereof

A silver nano, sea urchin-shaped technology, applied in the field of sea urchin-shaped silver nano hemisphere array and its preparation, can solve the problems of low cost performance, few layers, inaccessibility, etc., and achieves scientific preparation method, high surface roughness, and wide detection range. Effect

Inactive Publication Date: 2015-04-22
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are unsatisfactory aspects in both the product and its preparation method and application. First, the product has few layers in the morphology, only three layers of silver film, silver nano-hemisphere and gold nano-particles, resulting in the surface The change in roughness is not too large; secondly, the SERS activity of the precious metal gold is lower than that of silver, and the price is much higher than that of silver, resulting in low cost performance; thirdly, the preparation method cannot obtain products with higher surface roughness and SERS cost performance; Finally, the product failed to serve as an active substrate for surface-enhanced Raman scattering, and the content of trace plasticizers dibutyl phthalate or PCB 77 attached to it was measured using a laser Raman spectrometer

Method used

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  • Sea urchin shaped nano-hemisphere array as well as preparation method and application thereof
  • Sea urchin shaped nano-hemisphere array as well as preparation method and application thereof
  • Sea urchin shaped nano-hemisphere array as well as preparation method and application thereof

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Effect test

Embodiment 1

[0043] The concrete steps of preparation are:

[0044] Step 1: First place the aluminum sheet in a 0.2mol / L phosphoric acid solution at -4°C, anodize it at a DC voltage of 190V for 8 minutes, and then soak it in a phosphochromic acid mixture at 50°C for 16 hours. Then, put it again under the same process conditions for the second anodic oxidation for 8 minutes, first use tin chloride solution to remove the unoxidized aluminum on the back, and then place it in 4wt% phosphoric acid solution at 45°C for 55 minutes to remove barrier layer and reaming, to obtain an approximate figure 1 A through-hole alumina template with a pore diameter of 150 nm is shown.

[0045] Step 2, sputtering the silver film on one side of the through-hole alumina template; wherein, the current of the sputtering silver film is 4mA, and the time is 35min, so that one side is covered with a silver film, and there is a silver film between the silver film and the orifice. An alumina template with a hexagonal...

Embodiment 2

[0048] The concrete steps of preparation are:

[0049] Step 1: First place the aluminum sheet in a 0.25mol / L phosphoric acid solution at -5°C, anodize it at a DC voltage of 193V for 7 minutes, and then soak it in a phosphochromic acid mixture at 55°C for 13.5 hours. Next, place it again under the same process conditions for the second anodic oxidation for 9.5 minutes, first remove the unoxidized aluminum on the back with a tin chloride solution, and then place it in a 4.5wt% phosphoric acid solution at 46°C 53min to remove the barrier layer and reaming, to obtain such as figure 1 A through-hole alumina template with a pore diameter of 180 nm is shown.

[0050] Step 2, the silver film is sputtered on one side of the through-hole aluminum oxide template; wherein, the current when sputtering the silver film is 4.5mA, and the time is 33min, so that one side is covered with a silver film, and the distance between the silver film and the orifice is Alumina template with silver hex...

Embodiment 3

[0053] The concrete steps of preparation are:

[0054] Step 1: First place the aluminum sheet in a 0.3mol / L phosphoric acid solution at -6°C, anodize it at a DC voltage of 195V for 6 minutes, and then soak it in a phosphochromic acid mixture at 60°C for 11 hours. Then, put it again under the same process conditions for the second anodic oxidation for 11 minutes, first use tin chloride solution to remove the unoxidized aluminum on the back, and then place it in 5wt% phosphoric acid solution at 48°C for 50 minutes to remove barrier layer and reaming, to obtain an approximate figure 1 A through-hole alumina template with a pore diameter of 200 nm is shown.

[0055] Step 2, the silver film is sputtered on one side of the through-hole alumina template; wherein, the current of the sputtering silver film is 5mA, and the time is 30min, so that one side is covered with a silver film, and the silver film and the hole are covered with a silver film. An alumina template with a hexagonal...

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Abstract

The invention discloses a sea urchin shaped nano-hemisphere array as well as a preparation method and an application thereof. According to the array, a silver hexagonal bottom-side frustum which is sequentially and hexagonally arrayed and a silver hemisphere are sequentially adhered to a silver membrane on a hot melt adhesive substrate; silver nanoparticles are modified on the surfaces of the silver membrane, the silver hexagonal bottom-side frustum and the silver hemisphere. The method comprises the steps: performing a secondary anode oxidization method to obtain a through hole aluminum oxide template; sputtering on one side of the through hole aluminum oxide template to obtain an aluminum oxide template of which one side is coated with the silver membrane, the middle of the silver membrane and a hole opening is the silver hexagonal bottom-side frustum and the middle of the hole is the silver hemisphere; coating t the surface of the silver membrane of the aluminum oxide template with the hot melt adhesive; curing and putting the cured aluminum oxide template into an alkali solution for eating off the aluminum oxide template to obtain a hot melt adhesive substrate on which the silver membrane is sequentially adhered to the hexagonal and sequentially-arrayed silver hexagonal bottom-side frustum and the silver hemisphere; and putting the hot melt adhesive substrate into silver electrolyte for performing electric deposition to prepare a target product. The product can be used as a surface enhanced Raman scattering active substrate, and the content of R6G or DBP or PCB-77 attached on the active substrate is measured by using a laser Raman spectrometer.

Description

technical field [0001] The invention relates to a nano-hemisphere array and its preparation method and application, in particular to a sea urchin-shaped silver nano-hemisphere array and its preparation method and application. Background technique [0002] Theoretical and experimental studies on surface-enhanced Raman scattering (SERS) have shown that the size and shape of noble metal nanostructures have a great influence on the SERS activity of the substrate. For example, changes in surface roughness of just a few atomic layers thick can cause redshifts in surface plasmon longitudinal vibration modes. Therefore, the research on the preparation of gold and silver nanoparticles and microparticles with rough surface and their SERS activity has been widely concerned at home and abroad. For example, a gold nanoparticle published on December 18, 2013 in the Chinese invention patent application -Array of silver nano hemispheres and its preparation method and use. The array disclo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23F17/00C23C14/34C25D3/46B82Y40/00G01N21/65
Inventor 唐海宾孟国文李中波朱储红黄竹林
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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