Method for preparing calcium fluoride or rare earth doping calcium fluoride film by adopting electrodeposition

A technology of rare earth doping and calcium fluoride, applied in circuits, electrolytic inorganic material coatings, semiconductor devices, etc., can solve the problems that hinder the general application, complex equipment experiment procedures, etc., and achieve simple equipment, fast deposition rate, and low growth temperature Effect

Inactive Publication Date: 2011-07-20
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods require high temperature, high vacuum, complex equipment, and rigorous experimental procedures, which greatly hinder their general application.

Method used

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  • Method for preparing calcium fluoride or rare earth doping calcium fluoride film by adopting electrodeposition
  • Method for preparing calcium fluoride or rare earth doping calcium fluoride film by adopting electrodeposition
  • Method for preparing calcium fluoride or rare earth doping calcium fluoride film by adopting electrodeposition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1) Clean the ITO conductive glass twice with acetone, then clean the ITO conductive glass in an ultrasonic cleaner with deionized water for 10 minutes, then place the ITO conductive glass in a 10% nitric acid solution to activate it for 10 seconds, and finally use Deionized water cleaning, stand-by;

[0020] 2) In the 0.01 mol / liter disodium edetate and calcium ion complex solution, add 0.02 mol / liter sodium ascorbate, then add 0.04 mol / liter ammonium fluoride solution, adjust the pH value of the solution to 6, Obtain electrolyte, stand-by;

[0021] 3) Use ITO conductive glass as the working electrode, the platinum electrode as the counter electrode, and the calomel electrode as the reference electrode to form a three-electrode system, place it in the electrolyte for electrodeposition, and the anode deposition potential relative to the calomel electrode is 0.8V, The deposition temperature is 25° C. to obtain a calcium fluoride film.

Embodiment 2

[0023] 1) Clean the ITO conductive glass with acetone for 3 times, then clean the ITO conductive glass in an ultrasonic cleaner with deionized water for 30 minutes, then put the ITO conductive glass in 10% nitric acid solution to activate for 30 seconds, and finally use Deionized water cleaning, stand-by;

[0024] 2) In the disodium EDTA and calcium ion complex solution of 1 mol / liter, add 2 mol / liter sodium ascorbate, then add 4 mol / liter ammonium fluoride solution, adjust the pH value of the solution to 9, Obtain electrolyte, stand-by;

[0025] 3) Use ITO conductive glass as the working electrode, the platinum electrode as the counter electrode, and the calomel electrode as the reference electrode to form a three-electrode system, which is placed in the electrolyte for electrodeposition. The anode deposition potential relative to the calomel electrode is 1.4V. The deposition temperature is 80° C. to obtain a calcium fluoride film.

Embodiment 3

[0027] 1) Clean the ITO conductive glass twice with acetone, then clean the ITO conductive glass in an ultrasonic cleaner with deionized water for 15 minutes, then place the ITO conductive glass in a 10% nitric acid solution to activate it for 15 seconds, and finally use Deionized water cleaning, stand-by;

[0028] 2) In the 0.02 mol / liter disodium edetate and calcium ion complex solution, add 0.04 mol / liter sodium ascorbate, then add 0.08 mol / liter ammonium fluoride solution, adjust the pH value of the solution to 7, Obtain electrolyte, stand-by;

[0029] 3) Use ITO conductive glass as the working electrode, the platinum electrode as the counter electrode, and the calomel electrode as the reference electrode to form a three-electrode system, which is placed in the electrolyte for electrodeposition. The anode deposition potential relative to the calomel electrode is 1.1V. The deposition temperature is 25° C. to obtain a calcium fluoride film.

[0030] The structure of calciu...

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PUM

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Abstract

The present invention discloses a method for preparing calcium fluoride or rare earth doping calcium fluoride film by adopting electrodeposition, comprising the following steps of: (1) cleaning ITO (indium tin oxide) conducting glass 2-3 times with acetone, then placing the ITO conducting glass into an ultrasonic cleaner to be cleaned with deionized water for 10-30 minutes, then placing the ITO conducting glass into a 10% salpeter solution to be activated for 10-30 seconds, and finally cleaning with the deionized water for standby; (2) adding sodium ascorbate to a compound solution of 0.01-1 mol / L of ethylene diamine tetraacetic acid and calcium ions, then adding an ammonium fluoride solution, and regulating a pH value to 6-9 to obtain electrolyte for later use; and (3) placing the ITO conducting glass used as a working electrode, a platinum electrode used as a counter electrode and a calomel electrode used as a reference electrode into the electrolyte for the electrodeposition so as to obtain the calcium fluoride film, wherein the deposition potential of an anode relative to the calomel electrode is 0.8-1.4 V. The method for preparing calcium fluoride or rare earth doping calcium fluoride film by adopting electrodeposition provided by the present invention has the advantages of simple equipment, low cost, ordinary pressure and low temperature, is not only suitable for scientific research, but also expected to realize the large-scale industrialized production.

Description

technical field [0001] The invention relates to the preparation of thin films, in particular to a method for preparing calcium fluoride or rare earth doped calcium fluoride thin films by electrodeposition. Background technique [0002] Alkaline earth fluorides are widely used in optoelectronic and microelectronic devices. Calcium fluoride is a typical alkaline earth fluoride with a face-centered cubic structure. Calcium fluoride has good stability, does not absorb moisture and has good optical transparency, and can transmit light in a wide range of wavelengths (0.3-8mm), so it is suitable as a fluorescent matrix. When calcium fluoride is doped with an appropriate amount of rare earth elements, it exhibits characteristic luminescent properties and is an excellent laser material. Compared with organic dyes and semiconductor quantum dots, rare earth elements have sharp fluorescence emission peaks, high quantum yields, long lifetimes, and high photostability, and are expected t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25D9/06C25D7/12
Inventor 刘润徐铸德王辉陈科立
Owner ZHEJIANG UNIV
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