Special electrode for in-vivo voltammetry analysis and preparation method thereof
A micro-electrode and potential technology, which is applied in the analysis of materials, material analysis by electromagnetic means, and electrochemical variables of materials, etc., to achieve wide application prospects, good stability, and high selectivity.
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Embodiment 1
[0027] Embodiment 1, the preparation of the carbon fiber of surface covering carbon nanomaterial
[0028] Carbon fiber (T650-35, 7 μm in diameter) (Fabric Development Inc.). Put the carbon fiber into a high-temperature furnace at 1100 ° C, and put SiCl 4 Inject a mixed flow of 300mL / min argon and 40mL / min hydrogen into a high-temperature furnace containing oxygen at atmospheric pressure for 20 minutes. 4 Reacts with carbon fibers to generate SiO on the surface of carbon fibers 2 TLC. The prepared carbon fiber and 0.1 ~ 0.3g iron phthalocyanine (FeC 32 N 8 h 16 ) respectively placed in the same quartz glass tube, under Ar / H 2 (The volume ratio is 1:1~1:2, the flow rate is 20~40cm 3 / min) atmosphere, different heat treatments were carried out for carbon fiber and iron phthalocyanine. For the heat treatment of carbon fiber, it is heated at a temperature of 800-1100°C for 2-15 minutes, and for the heat treatment of iron phthalocyanine, it is heated at a temperature of 500-...
Embodiment 2
[0029] Embodiment 2, the preparation of the carbon fiber microelectrode of surface covering carbon nanometer material
[0030] The carbon fiber of the surface covering carbon nanomaterial of 1~2cm of embodiment 1 is micro-adhered on the copper wire of 5~10cm with conductive glue, and it is penetrated in the glass capillary tube (internal diameter is 1.5 mm, the length is 10cm), the inner diameter of the thin end opening is 30-50μm, and the length of the exposed carbon fiber at this end is about 1mm. The thick end of the glass tube exposes the copper wire. After the openings at both ends of the glass tube were sealed with insulating glue, the prepared electrode was baked at 100° C. for 1 hour to obtain a carbon fiber microelectrode covered with carbon nanomaterials.
Embodiment 3
[0031] Example 3. Preparation Method 1 of Special Electrode for Vivo Voltammetric Analysis of Physiologically Active Substances
[0032] 1) The carbon fiber electrode whose surface is covered with carbon nanomaterials prepared in Example 2 is successively dissolved in acetone, ethanol, 1.0-3.0M HNO 3 , 1.0~2.0M KOH solution and ultrasonic in secondary water. The ultrasonic intensity is 20W / cm 2 , the ultrasonic frequency is 50kHz, the ultrasonic action mode is 20s at intervals of 15s, and the ultrasonic time is 2 to 5 minutes;
[0033] 2) Electrochemically activate the carbon fiber electrode in step 1) in 0.5M sulfuric acid solution, that is, firstly apply +2.0V potential polarization on the electrode for 30-50s, and then apply -1.0V potential polarization for 10-30s. The obtained electrodes are then subjected to a 0.05-0.2V s -1 The scan speed is cyclically scanned within the potential range of 0.0-1.0V until a stable cyclic voltammogram is obtained. The schematic diagram...
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