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Aluminum oxide nano-needles and preparation method and application of aluminum oxide nano-needle and hole composite array structure

A technology of alumina nano-composite arrays, applied in the field of material science, can solve the problems of limited and unreachable surface enhancement performance, and achieve the effects of low cost, high strength and good reproducibility

Active Publication Date: 2017-08-01
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the traditional anodic oxidation can only obtain the ordinary post-hole AAO film, and the surface enhancement performance of this structure is limited, which is far from achieving the ideal effect.

Method used

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  • Aluminum oxide nano-needles and preparation method and application of aluminum oxide nano-needle and hole composite array structure
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Embodiment 1

[0023] As one of the more preferred embodiments, the method may include: using a low-temperature (5-18°C) oxalic acid solution as the electrolyte, with an oxalic acid concentration of 0.1-1M, and performing a mild (current density 2 ) Oxidation for 3h, and then use a mixed solution of 6wt% phosphoric acid solution and 1.8wt% chromic acid solution to soak and peel off the oxide layer to obtain hexagonal ordered pits to manufacture the pre-patterned aluminum surface, and the period of the pits is 80~ 110nm, the period of the pit determines the period of the final hole; then the initiation point formed by using the pit as a hole is subjected to mild oxidation for 25~250s under the same conditions as above to obtain a columnar hole structure with a height of 50~500nm, and finally the The obtained alumina column holes are immersed in a phosphoric acid solution with a temperature of 20-70°C and a concentration of 0.1-4M and corroded for 10-100 minutes, so that the pore walls are just ...

Embodiment 2

[0032] 1) Remove the organic grease and inorganic impurities on the surface of the aluminum foil by cleaning or grinding, or use the aluminum foil without any treatment;

[0033] 2) Use aluminum foil as anode, platinum electrode as cathode, sulfuric acid and oxalic acid mixed solution as electrolyte, sulfuric acid concentration is 0.012M, oxalic acid concentration is 0.3M, firstly oxidize at 35V for 8min (current density2 ), and then increase the voltage to 110V at a rate of 0.5V / s for high-intensity (current density>30mA / cm 2 ) oxidation, the entire oxidation time is 1.5h, and the temperature is -2°C; after the completion, the sample is immersed in a mixed solution of 1.8wt% chromic acid and 6wt% phosphoric acid at a temperature of 65°C for 3h, so that the alumina is completely denuded Drop the pit structure with a pitch of 200 nm;

[0034] 3) Take the pit as the initiation point of the hole formation, use the phosphoric acid solution with a concentration of 0.23M as the elec...

Embodiment 3

[0037] 1) Remove organic grease and inorganic impurities on the surface of aluminum foil by cleaning or grinding;

[0038] 2) Use aluminum as the anode, graphite electrode as the cathode, and 0.3 M sulfuric acid solution as the electrolyte, at 25V, 10°C for 6h (current density 2 ); After the completion, the sample is immersed in a mixed solution of 1.8wt% chromic acid and 6wt% phosphoric acid at a temperature of 3h for 3h, so that the aluminum oxide is completely eroded away and the pit structure with a spacing of 60 nm is left;

[0039] 3) Use the pit as the initiation point of hole formation, use phosphoric acid solution with a concentration of 0.23M as the electrolyte, and perform high-intensity oxidation at 25V for 1800s at a temperature of 40°C, so that the corrosion of the top hole and the formation of branch holes proceed simultaneously , to obtain a composite array structure of nanoneedles and pillar holes with a height of nano needle cones of 100nm and a height of pill...

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Abstract

The invention belongs to the technical field of material science and discloses aluminum oxide nano-needles, a preparation method of an aluminum oxide nano-needle and hole composite array structure and application of the structure to surface enhanced Raman scattering. The structure is achieved particularly by ingeniously cooperatively controlling the corrosion process and the oxidation process of aluminum oxide to enable the joints of whole hole walls or the joints of top hole walls to be completely broken. The aluminum oxide nano-needles are independently vertical to a substrate and are located at the positions of vertexes of substrate pits or vertexes of holes, the bottom composite holes can be adjusted to be in a column shape or a horn shape or a funnel shape or a cone shape or a branch shape, the top sizes of the aluminum oxide nano-needles can be adjusted within the range of 5-100 nm, the heights of the aluminum oxide nano-needles can be adjusted within the range of 0-1,000 nm, and the distances between the composite holes can be adjusted within the range of 50-1,000 nm. The structure can serve as an active Raman substrate after being compounded with gold or silver or other precious metals to be used for molecular structure and trace substance detection and the like, and has wide application prospects in the aspects of biology, medicine, food, environment and the like.

Description

technical field [0001] The invention belongs to the technical field of material science, and relates to a method for preparing an alumina nanoneedle and a composite array structure with holes, and the application of the structure to surface-enhanced Raman scattering. Background technique [0002] Surface-enhanced Raman scattering (SERS) is a very effective method for detecting interface properties and intermolecular interactions, and characterizing surface molecular adsorption behavior and molecular structure. The surface of the metal structure can excite high local electromagnetic field strength, thereby greatly improving the intensity of the Raman signal of the immobilized molecules. Both theory and experiments have shown that the highly ordered metal nanoneedle array structure is an ideal SERS active substrate; on the one hand, the extremely small curvature radius of the top can generate extremely high excitation local field strength and thus produce an ideal signal enhan...

Claims

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Application Information

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IPC IPC(8): C25D11/04C25D11/16C25D11/24G01N21/65
CPCC25D11/045C25D11/16C25D11/24G01N21/658
Inventor 李娟孙润广李雨欣张中月
Owner SHAANXI NORMAL UNIV
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