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Method for preparing single structure ferricyanide film using single-stage pulse electrodeposition

A unipolar pulse and cyanide technology, applied in the direction of circuits, electrical components, electrolytic inorganic material coatings, etc., can solve the problems of unstable composition and structure of MHCF films, poor uniformity and stability, and achieve excellent selectivity and sensitivity , The preparation process is simple and the effect of strong controllability

Inactive Publication Date: 2009-02-04
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention proposes a method for preparing a single-structure ferricyanide thin film unipolar pulse electrodeposition to solve the problem of unstable composition and structure of the MHCF thin film due to the influence of the composition of the film-making solution in the existing film-making method and mixed-structure metal ferricyanide. Thin film and poor film uniformity and stability

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Take a platinum sheet as the working electrode, a large-area platinum sheet or a platinum mesh as the counter electrode, and a saturated calomel electrode as the reference electrode. -1 Potassium ferricyanide, 0.002mol L -1 Nickel sulfate and 0.25mol L -1 After applying a constant pulse deposition voltage of 0.2V (vs. SCE) for a certain period of time in the solution of sodium sulfate, the current is controlled to be zero within the cut-off time for unipolar pulse electrodeposition, and the pulse frequency is controlled at 5 / s and the pulse on-off time ratio t on / t off 1:1, pulse deposition 2000 times, on the surface of platinum substrate made "insoluble" structure of nickel ferricyanide thin film. at 1mol L -1 KNO 3 After cyclic scanning in the solution, the composition ratio of the film in the oxidized state was measured as: K:Ni:Fe=0.01:1.44:1.

Embodiment 2

[0014] Take a platinum sheet as the working electrode, a large-area platinum sheet or a platinum mesh as the counter electrode, and a saturated calomel electrode as the reference electrode. -1 Potassium ferricyanide, 0.004mol L -1 Nickel nitrate and 0.25mol L -1 After applying a constant pulse deposition voltage of 0.6V (vs. SCE) for a certain period of time in the solution of sodium nitrate, control the current to zero within the cut-off time for unipolar pulse electrodeposition, control the pulse frequency 2 / s, and the pulse on-off time ratio t on / t off 1.5:1, pulse deposition 3000 times, on the surface of the platinum substrate made of "soluble" structure of nickel ferricyanide thin film. at 1mol L -1 KNO 3 The composition ratio of the film in the oxidized state measured after circular scanning in the solution is: K:Ni:Fe=1.12:1.08:1.

Embodiment 3

[0016] Conductive glass was used as the working electrode, a large-area platinum sheet or platinum mesh was used as the counter electrode, and a saturated calomel electrode was used as the reference electrode. -1 Potassium ferricyanide, 0.01mol·L -1 Nickel chloride and 0.5mol L -1 After applying a constant pulse deposition voltage of 0.6V (vs. SCE) for a certain period of time in the solution of potassium nitrate, control the current to zero within the cut-off time for unipolar pulse electrodeposition, control the pulse frequency 3 / s, and the pulse on-off time ratio t on / t off 3:1, pulse deposition 5000 times, on the surface of the graphite substrate, the nickel ferricyanide film with "insoluble" structure was prepared. at 1mol L -1 KNO 3 The cyclic voltammogram in the solution is a single peak (0.41V low potential peak), which corresponds to the "insoluble" structure of the film.

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Abstract

The invention discloses a preparation method for single-structure ferricyanide film monopolar pulse electro-deposition, which adopts a monopolar pulse electro-deposition method to prepare semi-conductive metal ferricyanide film on the surface of a conductive matrix, i.e. feeds a certain period of pulse deposition voltage and then controls the current to be zero within the interruption time to realize monopolar pulse, and prepares soluble or insoluble single-structure inorganic semi-conductive metal ferricyanide film by regulating the pulse voltage, pulse frequency, pulse make-break time (duty ratio) and other parameters in the solution containing potassium ferricyanide, transition metal salt and supporting electrolyte. The preparation method is simple and has strong operability; and the prepared single-structure metal ferricyanide film has excellent selectivity and sensitivity, and is the preferred material for the preparation of sensitive sensors and the electrical control ion separation technology.

Description

technical field [0001] The invention relates to a method for preparing an inorganic semiconductor thin film, in particular to a method for preparing a metal ferricyanide thin film with a single structure by unipolar pulse electrodeposition. Background technique [0002] Transition metal ferricyanide or transition metal analogs of Prussian blue (Metal Hexacyanoferrate, MHCF, molecular formula A h m k [Fe(CN) 6 ] l mH 2 O, h, k, l, m are stoichiometric coefficients, A is an alkali metal ion, M is a transition metal ion) has a cubic framework structure similar to molecular sieves, and is centered on electrochemically reversible iron (II / III), through Cyanide bond (CN - ) is an inorganic coordination compound formed by linking with transition metal ions. Due to their unique solid-state chemical and structural features, these compounds are promising in electrocatalysis (synthesis), photoelectrocatalysis, electrochromism, imaging, ion exchange, ion detection (chemical and bi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D9/08C25D5/18H01L21/36
Inventor 郝晓刚马旭莉王忠德张忠林李永国刘世斌孙彦平
Owner TAIYUAN UNIV OF TECH
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