CN101768724B - Method for preparing film on stainless steel - Google Patents

Method for preparing film on stainless steel Download PDF

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Publication number
CN101768724B
CN101768724B CN2008101429964A CN200810142996A CN101768724B CN 101768724 B CN101768724 B CN 101768724B CN 2008101429964 A CN2008101429964 A CN 2008101429964A CN 200810142996 A CN200810142996 A CN 200810142996A CN 101768724 B CN101768724 B CN 101768724B
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China
Prior art keywords
stainless steel
film
diamond
octadecylene
carbon film
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CN101768724A (en
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张俊彦
王舟
宋仕永
张斌
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Lanzhou Institute of Chemical Physics LICP of CAS
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Lanzhou Institute of Chemical Physics LICP of CAS
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Abstract

The invention discloses a method for preparing a stainless steel/diamond-like carbon/organic film composite structure coating with the characteristics of low friction, high load-bearing and long service life. The method adopts the magnetron sputtering vapor deposition technology, firstly deposits a Ti transition layer on a stainless steel substrate, then deposits a diamond-like carbon film, and uses organic molecules (octadecylene) to decorate the surface. The method is easy to be operated. The prepared film is uniform. And the film has excellent friction and wear characteristics.

Description

The method that on stainless steel, prepares film
Technical field
The present invention relates to a kind of low friction high-mechanic long lifetime stainless steel/quasi-diamond/organic film composite structure coating preparation method.
Technical background
Stainless steel be in air or the chemical corrosion medium in can resist a kind of high quality steel of corrosive because stainless steel has corrosion resistance and good, the intensity height, high temperature oxidation resisting, plastic working is easily safeguarded simple, highly polished, characteristics such as good welding performance have been widely used in household supplies at present, auto parts machinery, medical apparatus, building materials, chemistry, foodstuffs industry, agricultural, fields such as ship components.And more and more higher to the requirement of stainless steel wear-resistant corrosion-resistant energy of (such as cutter, mould) under some high strength work condition environments in recent years, this can have higher requirement to the wear-resistant corrosion-resistant on the stainless steel surface.By deposition one deck or which floor protective film on the stainless steel-based end is a kind of method commonly used that improves its wear-resistant corrosion-resistant energy, and diamond-like carbon film is a kind of thin-film material that can improve its mechanical property that occurs in recent years.
Diamond-like carbon (diamond-like carbon, DLC) therefore film is with a wide range of applications in fields such as machinery, tribology, aerospace owing to have high hardness, fabulous unreactiveness, extremely low frictional coefficient, good resistance to abrasion and good excellent specific properties such as heat conductivity.But the surface energy of diamond like carbon film is higher, and hydrophobicity is relatively poor, and this has limited it and has had the application of (as MEMS) in the particular requirement environment at some.
With organic molecule the diamond like carbon film surface being modified is a kind of effective ways that improve its surface property.Organic film be coated with the reduction that is beneficial to the diamond like carbon film surface energy, strengthen its surface hydrophobicity, being in contact with one another between antithesis when the long-chain flexility of organic molecule is reduced friction improved its friction wear performance.
Summary of the invention
The object of the present invention is to provide a kind of method that on stainless steel, prepares film.
The present invention adopts the magnetron sputtering gas phase deposition technology, deposits one deck Ti transition layer earlier on the stainless steel-based end, and depositing diamond-like carbon film uses organic molecule (octadecylene) that its surface is modified then again.This method is operated easily, and the film of preparation is even, and film has the excellent friction wearing character.
A kind of method for preparing film on stainless steel adopts the medium frequency magnetron sputtering gas phase deposition technology, it is characterized in that this method may further comprise the steps:
The stainless steel substrates of A after with precleaning put into acetone, ethanol ultrasonic cleaning successively, is transferred to then in the vacuum chamber, and substrate disk links to each other with the pulsed negative bias power supply; Vacuumize up to vacuum tightness less than 2.0 * 10 -3Pa;
B depositing Ti transition layer: argon flow amount 160sccm, electric current of intermediate frequency 2.0A, pulsed bias 2000V, dutycycle 0.15;
C deposition DLC film: argon flow amount 120sccm, methane flow 60sccm, electric current of intermediate frequency 2.0A, pulsed bias 800V, dutycycle 0.15;
The D organic molecule is modified the diamond like carbon film surface: octadecylene is spun to the diamond like carbon film surface, uses the medium pressure mercury lamp UV-irradiation then under nitrogen protection; Take out sample, ultrasonic cleaning is five minutes in toluene, in order to remove unreacted octadecylene.
The present invention is spun to the diamond like carbon film surface with octadecylene, can effectively reduce the surface energy of film, increases its hydrophobicity, can improve the tribological property of film.
The structure of the film of the present invention's preparation characterizes with Raman spectrum (Raman), infrared spectra (FTIR), x-ray photoelectron spectroscopy (XPS) and transmission electron microscope (TEM).Structure shows, has successfully prepared diamond-like carbon film on the stainless steel-based end, and this film is an amorphous structure, and has the excellent friction polishing machine.
The used substrate of the present invention is a stainless steel, and adds the Ti transition layer to increase the bonding force of film and steel base in process of plating.
The film that the present invention obtains has the structure of diamond-like carbon film, is a kind of high rigidity that has, the film of high recovery of elasticity and the effect of excellent anti-attrition anti-friction.
The film surface that the present invention obtains is modified through organic molecule (octadecylene), and the surface energy that this helps reducing the diamond like carbon film surface increases its surface hydrophobicity, and this can improve the corrosion resistance of laminated film; The long-chain of organic molecule (octadecylene) has snappiness simultaneously, the resistance in the time of reducing friction between antithesis, the friction life-span of improving laminated film.
The diamond-like carbon film of modifying through organic molecule (octadecylene) that the present invention obtains has excellent tribological property, and under nitrogen environment, after 30000 frictions, its average friction coefficient is 0.026.
Embodiment
For a better understanding of the present invention, describe by example.
Embodiment 1:
At first select three of the stainless steel substrates of any surface finish, use tap water pre-washing, wait to put it in acetone, the ethanol ultrasonic cleaning after its drying again each 20 minutes, take out stainless steel substrates, change over to rapidly in the vacuum chamber after drying up with nitrogen, be placed on the substrate disk, begin to vacuumize.Treat that vacuum is extracted into less than 2.0 * 10 -3During handkerchief, feeding argon gas (160sccm), is 0.15 in 2000 volts of pulsed bias, dutycycle, and under the condition of sputtering current 2.0A (Ti target), the deposition transition layer continues 20 minutes; After finishing, feed methane (60sccm), the adjustment argon flow amount is 120sccm, in 800 volts of pulsed bias, dutycycle 0.15, and the condition deposit film of sputtering current 2.0A (graphite target), depositing time 2 hours.
On CSM tribo-D-0000 friction wear testing machine, estimate the tribological property of film.Test conditions is as follows: normal load is 5N, toward covering frequency 8Hz, amplitude 5mm, nitrogen atmosphere, relative humidity 40~60%, room temperature.Test result shows: having excellent tribological property under the situation of diamond like carbon film at 5N after organic molecule (octadecylene) is modified, is 0.026 at the average friction coefficient through 30000 friction rear films.

Claims (1)

1. a method for preparing film on stainless steel adopts the medium frequency magnetron sputtering gas phase deposition technology, it is characterized in that this method may further comprise the steps:
The stainless steel substrates of A after with precleaning put into acetone, ethanol ultrasonic cleaning successively, is transferred to then in the vacuum chamber, and substrate disk links to each other with the pulsed negative bias power supply; Vacuumize up to vacuum tightness less than 2.0 * 10 -3Pa;
B depositing Ti transition layer: argon flow amount 160sccm, electric current of intermediate frequency 2.0A, pulsed bias 2000V, dutycycle 0.15;
C deposition DLC film: argon flow amount 120sccm, methane flow 60sccm, electric current of intermediate frequency 2.0A, pulsed bias 800V, dutycycle 0.15;
The D organic molecule is modified the diamond like carbon film surface: octadecylene is spun to the diamond like carbon film surface, uses the medium pressure mercury lamp UV-irradiation then under nitrogen protection; Take out sample, ultrasonic cleaning is five minutes in toluene, in order to remove unreacted octadecylene.
CN2008101429964A 2008-12-29 2008-12-29 Method for preparing film on stainless steel Expired - Fee Related CN101768724B (en)

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CN101768724A CN101768724A (en) 2010-07-07
CN101768724B true CN101768724B (en) 2011-08-03

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Publication number Priority date Publication date Assignee Title
CN103160801B (en) * 2011-12-16 2016-06-15 中国科学院兰州化学物理研究所 In the method that metallic interior surface prepares diamond-like carbon film
CN103952663A (en) * 2014-05-02 2014-07-30 合肥永信等离子技术有限公司 Metal bottoming technology in diamond like coating
CN111876754A (en) * 2020-08-04 2020-11-03 中国科学院兰州化学物理研究所 Method for realizing macroscopic super-lubricity by matching nano metal coated steel ball and hydrogen-carbon-containing film
CN112210417B (en) * 2020-10-21 2021-11-12 中国科学院兰州化学物理研究所 Friction catalysis design method for realizing ultralow friction of carbon film
CN113305463B (en) * 2021-06-15 2022-07-22 广东谛思纳为新材料科技有限公司 Process for preventing stainless steel from discoloring during welding
RU2764041C1 (en) * 2021-06-22 2022-01-13 Федеральное государственное бюджетное учреждение науки Институт сильноточной электроники Сибирского отделения Российской академии наук (ИСЭ СО РАН) Method for increasing wear resistance and anti-corrosion properties of steel products

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CN101081557A (en) * 2007-06-26 2007-12-05 广州有色金属研究院 Metallic carbide/adamantine (MeC/DLC) nanometer multi-layer film material and method for preparing the same

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