A kind of preparation method of tin film

A thin film and electrolyte technology, applied in the field of TiN thin film preparation, can solve the problems of difficult process control, complex sputtering equipment, slow deposition speed, etc., and achieve the effect of convenient and flexible production, low cost and simple equipment

Active Publication Date: 2020-04-14
JIANGXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Physical vapor deposition films mostly use sputtering coating, but there are complex sputtering equipment, vacuum systems and high-voltage devices are required, the deposition speed is slow, and the cost is high
Chemical vapor deposition technology is a technology that uses gaseous precursor reactions to form solid films through chemical reactions between atoms and molecules. Its devices mainly include gas generation, purification, mixing and transportation devices, reaction chambers, substrate heating devices and exhaust. Gas device, complex equipment, difficult process control, poor repeatability, difficult operation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Mix LiCl and KCl uniformly at a molar ratio of 0.42:1, add aluminum nitride with a mass fraction of 0.5% to the LiCl-KCl supporting electrolyte and mix uniformly to obtain a mixed molten salt electrolyte, and place the mixed molten salt electrolyte in the electrolytic cell , use titanium sheet as anode, aluminum sheet as cathode, control cathode current density to 20mA / cm 2 , the electrolysis temperature is 430°C, after electrolysis for 10 hours, a flat, smooth and dense TiN film is obtained on the surface of the anode, the thickness of the TiN film is 10-15 μm, the atomic percentage of N is 50.5%, and the rest is Ti.

Embodiment 2

[0020] Mix LiCl and KCl uniformly at a molar ratio of 1.9:1, add aluminum nitride with a mass fraction of 2.0% to the LiCl-KCl supporting electrolyte and mix uniformly to obtain a mixed molten salt electrolyte, and place the mixed molten salt electrolyte in the electrolytic cell , using titanium sheet as anode and aluminum sheet as cathode, control the cathode current density to 100mA / cm 2 , the electrolysis temperature is 450°C, and after 20 hours of electrolysis, a flat, smooth and dense TiN film is obtained on the surface of the anode. The thickness of the TiN film is 65-70 μm, the atomic percentage of N is 52.5%, and the rest is Ti.

Embodiment 3

[0022] Mix LiCl and KCl uniformly at a molar ratio of 1.5:1, add aluminum nitride with a mass fraction of 1.0% to the LiCl-KCl supporting electrolyte and mix uniformly to obtain a mixed molten salt electrolyte, and place the mixed molten salt electrolyte in the electrolytic cell , using a titanium sheet as the anode, an aluminum sheet as the cathode, and controlling the cathode current density to 60mA / cm 2 , the electrolysis temperature is 440°C, and after electrolysis for 15 hours, a flat, smooth and dense TiN film is obtained on the surface of the anode. The thickness of the TiN film is 35-40 μm, the atomic percentage of N is 51.4%, and the rest is Ti.

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Abstract

The invention provides a preparation method of TiN film. The method comprises the following steps: adding 0.5-2.0 mass percentage of aluminum nitride into LiCl-KCl supporting electrolyte, uniformly mixing to obtain mixed molten salt electrolyte, adding the mixed molten salt electrolyte in an electrolytic tank and increasing the temperature to 430-450 DEG C, carrying out electrolysis by taking metallic titanium as an anode and taking metallic aluminum as a cathode, wherein the anode current density is 20-100mA / cm<2> and the electrolysis time is 10-20 hours; and obtaining dense TiN film on the surface of the anode. The preparation method of the TiN film is short in process, simple in equipment, convenient to operate and low in cost; the bonding strength between the TiN film and the substrateis high; the TiN film with different thicknesses can be obtained by controlling the current density or the electrolysis time.

Description

technical field [0001] The invention relates to the technical field of substrate surface treatment, in particular to a method for preparing a TiN thin film. Background technique [0002] Hard film materials are generally used to improve the wear resistance and corrosion resistance of the substrate surface, including thin film materials such as nitrides, carbides, and borides. Titanium nitride (TiN) film has high hardness, wear resistance and corrosion resistance, and is an ideal film material for the surface of cemented carbide tools and molds. Depositing TiN film on workpieces such as turning tools, milling cutters, drill bits, bearings, gears, and forming technology tools can increase the surface hardness and wear resistance of the workpiece, and its service life and durability are significantly improved. TiN thin films are not only used in tools, molds and other workpieces, but also widely used in diffusion barriers, optical films and decorative films in the semiconducto...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25D11/00
CPCC25D11/00
Inventor 李亮星黄茜琳黄金堤钟银生艾翔徐迎春
Owner JIANGXI UNIV OF SCI & TECH
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