All-solid-state nano-probe for scanning electrochemical cell microscope, preparation method and application of all-solid-state nano-probe
A scanning electrochemical and nano-probe technology, applied in the field of electrochemical detection, can solve problems such as non-negligible volatilization or easy salt precipitation at the tip of the probe, difficulty in co-localization of different technologies, etc., to achieve a stable shape effect of size
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Embodiment 1
[0040] Preparation of solid electrolyte probes
[0041] In this paper, solid electrolyte probes were prepared by photoinitiated free radical polymerization. The formula in one embodiment is: 350 mg of acrylamide: 75 mg of hydroxyethyl acrylate: 75 mg of polyethylene glycol diacrylate, 500 mg of water, and 10 mg of 2-hydroxy-2-methyl-1-phenylacetone to prepare a solution. The glass tube is drawn by a P-2000 needle pulling instrument, and the parameters are line1: HEAT 800FIL5VEL 60DEL 128PUL 50; line 2: HEAT 850FIL 4VEL 50DEL 130PUL 175. After pouring the prepared solution into the glass tube, use an air pump to pressurize the probe, so that the internal pressure of the probe is 0.2 MPa, carry out ultraviolet light polymerization under pressure, turn off the light source after 5 minutes of light, and release the pressure. The light source is a 365nm ultraviolet light source with a power of 6W. The probes were characterized by optical microscopy (Nikon Ti) and SEM (S-4800). T...
Embodiment 2
[0047] The characterization of embodiment two solid-state probes
[0048] Electrochemical test
[0049] When carrying out the ion current test, the solution concentration of the electrochemical cell is 500mM KCl, the solution concentration in the probe is 500mM KCl, and the final ion concentration in the solid electrolyte probe is 500mM KCl. The ion current test voltage is 0.2V, and a two-electrode system is adopted, and both electrodes are Ag / AgCl electrodes.
[0050] When carrying out the CV test, the solution concentration is 500mM KCl, 100mM potassium ferrocyanide, and 100mM potassium ferricyanide. A two-electrode system is adopted, the working electrode is an ITO electrode, and the counter electrode is an Ag / AgCl electrode. The scanning range is -0.2~0.7V, and the scanning speed is 50mV / s.
[0051] Reference to electrochemical test results for solid-state probes Figure 4 : CV test results, the solution is 500mM KCl, 100mM potassium ferrocyanide, 100mM potassium ferri...
Embodiment 3
[0052] Example 3 Detection of wrinkled graphene by SECCM all-solid-state probe
[0053] Preparation of graphene samples
[0054] Graphene samples were purchased from Xianfeng Nano, and multi-layer graphene was prepared on the surface of Cu substrate by CVD method. Cut 2mm*2mm graphene-loaded Cu foil and float it on the surface of 1M FeCl3 for 1h, the copper foil will be dissolved. Use ITO to carry the graphene film floating on the surface of the solution, then wash it with water for 3 times, wash it with ethanol for 3 times, and dry it with nitrogen gas for later use.
[0055] SECCM scan
[0056] When performing resolution verification experiments, the solid electrolyte probe was used as a reference electrode containing 500mM KCl solution. The working electrode is an ITO electrode, and an Au layer film is prepared on the surface of the ITO with an evaporation apparatus, the evaporation current is 15mA, and the evaporation time is 120s. A voltage of 2V was applied to the wo...
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Abstract
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