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Preparation method for isolated needle point with housing layers wrapped in dual manner

A shell and needle tip technology, applied in the field of scanning probes, can solve problems such as needle tip surface contamination, and achieve the effects of simple preparation method, oxidation prevention, and good universality

Inactive Publication Date: 2017-05-10
XIAMEN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention aims at the problem of surface contamination of the needle tip in the scanning probe technology, and provides a method for preparing a double-coated shell to isolate the needle tip

Method used

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  • Preparation method for isolated needle point with housing layers wrapped in dual manner
  • Preparation method for isolated needle point with housing layers wrapped in dual manner
  • Preparation method for isolated needle point with housing layers wrapped in dual manner

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1: Specific steps of coating 2nm silicon dioxide, aluminum oxide and titanium dioxide. Insert the etched gold needle tip into the special stainless steel base, and then put it into the preheated to 160° (SiO 2 ), 160°(Al 2 o 3 ), 70°(TiO 2 ) into the reaction chamber of the atomic layer deposition system, alternately feed two pulsed silicon sources (or aluminum source, titanium source) and a pulsed water source, and feed high-purity nitrogen for a certain period of time after the source and water source are pulsed. , the source bottle temperature is silicon source (25°), aluminum source (20°), titanium source (20°), water source (25°), ① deposited silica: silicon source pulse time 0.2s, high-purity nitrogen blowing Sweeping for 5s, water source pulse time 0.1s, high-purity nitrogen purging for 5s, 25 cycles can deposit silicon dioxide with a thickness of 2nm. ② Deposition of aluminum oxide: aluminum source pulse time 0.1s, high-purity nitrogen purge 5s, wate...

Embodiment 2

[0029] Example 2: Specific steps of coating 5, 10, 20 nm titanium dioxide. Insert the etched gold needle tip into the special stainless steel base, and then put it into the reaction chamber of the atomic layer deposition system preheated to 70°, alternately feed two pulsed titanium sources and one pulsed water source, the titanium source After pulsing with water source, high-purity nitrogen is flushed for a certain period of time. The temperature of the titanium bottle is set to 20°, the temperature of the water source is 25°, the pulse time of the titanium source is 0.1s, the high-purity nitrogen is purged for 2s, the pulse time of the water source is 0.1s, and the high Purging pure nitrogen for 4s, depositing 50, 134, and 256 cycles respectively can deposit titanium dioxide with a thickness of 5, 10, and 20 nm. Stick the prepared needle tip on the copper ring, and take a high-magnification transmission electron microscope to obtain figure 2 Figure a in figure 2 Figure b ...

Embodiment 3

[0030] Example 3: Electrochemical cyclic voltammetry was performed on a gold needle tip double-coated with a 2nm silica shell layer and polymethylstyrene hot melt adhesive. The CHI electrochemical workstation used for electrochemical testing is in the electrolytic cell of the single-chamber three-electrode system. The counter electrode is a platinum wire, the reference electrode is a saturated calomel electrode, and the working electrode is a gold needle tip and a double-coated gold needle tip. Interval: -0.1~0.5V, sampling interval: 0.0001V, scanning speed: 5mV s -1 , at 10mM K 3 Fe(CN) 6 Cyclic voltammetry scanning was carried out in the electrolyte solution of +0.5M KCl to obtain image 3 and Figure 4 . The cyclic voltammogram of the gold tip ( image 3 ) peak current in the microampere level, while the cyclic voltammogram of the double-coated gold tip ( Figure 4 ) presents a typical "S-shaped curve" of micro-nano electrodes, and the steady-state limiting current is...

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Abstract

The invention provides a preparation method for an isolated needle point with housing layers wrapped in dual manner, which relates to a scanning probe. The method comprises the following steps: 1) using a chemical etching method to prepare a needle point; 2) wrapping the surface of the needle point with a housing layer; and 3) using high polymer materials to package the part of the needle point wrapped by the housing layer in step 2 excluding the needle point end for a second time to obtain an isolated needle point with the housing layers wrapped in a dual manner. According to the invention, an atomic layer deposition technique is adopted and different source precursors are used so that the needle point surface can be wrapped by different inert housings. Through the control over the number of circulation turns of different source precursors, the thickness of the housing layer can be accurately controlled. The wrapping in dual manner can prevent the non-analyte molecules in the solution from interfering with the signal generated at the needle point and can isolate the interference of the Faraday current. Therefore, the method can be applied to electrochemical needle-enhanced Raman spectroscopy, electrochemical scanning tunneling microscope and electrochemical scanning microscope. Capable of being universally applied, the method can also be used to the wrapping of other needle points, like silver needle points, AFM needle points, and platinum iridium needle points. The method is simple to perform and is suitable for large batch production.

Description

technical field [0001] The invention relates to a scanning probe, in particular to a method for preparing a double-coated shell-isolated needle tip applicable to an electrochemical scanning tunneling microscope and an electrochemical tip-enhanced Raman spectrum under complex systems. Background technique [0002] With the development of nanoscience, nano-characterization technology plays an important role in the application of nanomaterials, surface science and other fields. Among them, the scanning probe technology based on the development of nanoprobes (such as scanning tunneling microscope, atomic force microscope, shear force microscope, etc.) ) can obtain atomic-resolution morphology information and nano-scale chemical composition information respectively, which are important components of nano-characterization technology. In these techniques, the tip of the nanostructure is controlled to approach the sample surface for scanning, and the exposed tip is easily polluted ...

Claims

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Application Information

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IPC IPC(8): G01Q70/16G01N21/65C25F3/02C23C16/40C23C16/455
CPCG01Q70/16C23C16/402C23C16/403C23C16/405C23C16/45525C25F3/02G01N21/65
Inventor 李剑锋黄亚萍黄声超
Owner XIAMEN UNIV
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