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Preparation method for high-quality TiN thin film

A high-quality, thin-film technology, applied in the direction of ion implantation plating, metal material coating process, coating, etc., can solve the problems of large internal stress, difficult control, and increased difficulty of the coating, and achieve high surface flatness and deposition The effect of high rate and low preparation cost

Inactive Publication Date: 2017-06-23
郭和谦
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, because the working conditions and influencing factors of the mold are much more complicated than those of the tool, the application of the TiN coating prepared under the current conditions on the mold is greatly restricted.
The main reason is that the general mold steel substrate is soft, or the coating and the substrate are not bonded enough, and the internal stress of the coating is relatively large during the preparation process. During the work, the steel substrate cannot strongly support the TiN coating and early failure occurs.
[0006] The application date of Chinese patent (201110425176.8) is 2011.12.16, which discloses a preparation method of an ultra-thick TiN-TiCN multilayer composite thin film material. 20-40sccm, the distance between the target and the substrate is 10-15cm, the initial chamber temperature is 30-40°C, the DC current is 2-4sccm, the duty cycle and negative bias are 60-80% and 0-100W respectively Under certain conditions, by gradually adjusting the flow rate of ammonia and methane, and sputtering pure titanium target, a multilayer composite film with a thickness of 9.5-24.0 μm of TiN-TiCN alternately stacked is prepared, and the deposition time is 100-260min. The film is dense Uniform, smooth surface, good elasticity, good adhesion, high hardness, good wear resistance, but methane gas is used in the preparation process, which is flammable and difficult to control in the experimental operation, and in the preparation process in order to control TiN , the thickness of each layer of TiCN, the ratio of ammonia to methane needs to be strictly adjusted, which increases the difficulty of preparation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A kind of preparation method of high-quality TiN film is characterized in that, comprises the following steps:

[0030] (1) Select Ti ingots with a purity of more than 99.95% to make titanium strips after forging, rolling, heat treatment, leveling and machining; Clean with ionized water and absolute ethanol, dry in vacuum; then engrave the surface of the titanium strips with a laser; finally roll the engraved titanium strips into titanium rings with a rolling machine, and get sputtered titanium rings after cleaning and drying; , the rolling conditions are: the rolling tension is 35MPa, the pass deformation is 10%, and the rolling total deformation is 55%; the heat treatment conditions are: temperature 880°C, holding time 0.5h; the optical engraving conditions are: The pulse width of the laser is 10ns, the pulse frequency is 20kHz, the average laser power is 20W, the engraving line speed is 1000mm / s, and the engraving is engraved in layers, and the thickness of each laye...

Embodiment 2

[0034] A kind of preparation method of high-quality TiN film is characterized in that, comprises the following steps:

[0035] (1) Select Ti ingots with a purity of more than 99.95% to make titanium strips after forging, rolling, heat treatment, leveling and machining; Clean with ionized water and absolute ethanol, dry in vacuum; then engrave the surface of the titanium strips with a laser; finally roll the engraved titanium strips into titanium rings with a rolling machine, and get sputtered titanium rings after cleaning and drying; , the rolling conditions are: the rolling tension is 63MPa, the pass deformation is 20%, and the total rolling deformation is 75%; the heat treatment conditions are: temperature 1200°C, holding time 2h; the optical engraving conditions are: laser The pulse width is 100ns, the pulse frequency is 100kHz, the average laser power is 200W, the engraving line speed is 3000mm / s, the engraving is engraved in layers, and the thickness of each layer is 0.2m...

Embodiment 3

[0039] A kind of preparation method of high-quality TiN film is characterized in that, comprises the following steps:

[0040] (1) Select Ti ingots with a purity of more than 99.95% to make titanium strips after forging, rolling, heat treatment, leveling and machining; Clean with ionized water and absolute ethanol, dry in vacuum; then engrave the surface of the titanium strips with a laser; finally roll the engraved titanium strips into titanium rings with a rolling machine, and get sputtered titanium rings after cleaning and drying; , the rolling conditions are: the rolling tension is 40MPa, the pass deformation is 13%, and the rolling total deformation is 65%; the heat treatment conditions are: temperature 900°C, holding time 0.5h; the optical engraving conditions are: The pulse width of the laser is 40ns, the pulse frequency is 50kHz, the average laser power is 50W, the engraving line speed is 1300mm / s, and the engraving is engraved in layers, and the thickness of each laye...

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Abstract

The invention discloses a method for preparing a high-quality TiN thin film, which comprises the following steps: selecting a Ti ingot to make a titanium strip through forging, rolling, heat treatment, leveling and machining; and then performing laser engraving on it, The engraved titanium strips are rolled into titanium rings with a rolling machine, and after cleaning and drying, the sputtered titanium rings are obtained; the steel sheet is used as the substrate, and the titanium ring and titanium palladium are bonded with conductive adhesive as the target material. TiN thin films were deposited on steel sheets. The invention rationally adjusts the sputtering process, so that the prepared TiN thin film is dense and uniform, has excellent wear resistance and corrosion resistance, smooth and flat surface, strong bonding force with the substrate, and good mechanical properties.

Description

[0001] Technical field: [0002] The invention relates to the field of magnetron sputtering film formation, in particular to a preparation method of a high-quality TiN thin film. [0003] Background technique: [0004] The preparation of TiN coating by physical vapor deposition (PVD) is the most widely used surface strengthening technology. Due to the characteristics of high hardness, high adhesion strength, low friction coefficient and good corrosion resistance, TiN coating has been widely used in various fields, especially in the tool industry. In the 1970s, TiN coating was successfully used on tools such as cutting tools and drill bits, and its service life was increased by an average of 2 to 10 times, which caused a tool revolution. In the 1980s, physical vapor deposition TiN coatings were also successfully tested on forming punches and stamping dies. [0005] However, because the working conditions and influencing factors of the mold are much more complicated than those ...

Claims

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Application Information

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IPC IPC(8): C23C14/06C23C14/35C23C14/02
CPCC23C14/0641C23C14/0036C23C14/021C23C14/3407C23C14/35
Inventor 郭和谦
Owner 郭和谦
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