CN102409306A - Preparation method of Ti-Mo-N multi-element film - Google Patents

Preparation method of Ti-Mo-N multi-element film Download PDF

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CN102409306A
CN102409306A CN2011103073852A CN201110307385A CN102409306A CN 102409306 A CN102409306 A CN 102409306A CN 2011103073852 A CN2011103073852 A CN 2011103073852A CN 201110307385 A CN201110307385 A CN 201110307385A CN 102409306 A CN102409306 A CN 102409306A
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CN102409306B (en
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韩晓芬
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Inner Mongolia Zhongtian Hongyuan Rare Earth New Material Co ltd
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NINGBO RUITONG NEW MATERIAL TECHNOLOGY Co Ltd
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Abstract

The invention provides a preparation method of a Ti-Mo-N multi-element film. According to the invention, a high-property Ti-Mo-N three-element film is prepared by adopting a magnetic control sputtering method and taking Ti, Mo and N as the basic composition elements of the film; and the high-property Ti-Mo-N three-element film is prepared mainly through optimizing the preparation process parameters of the multi-element film. Compared with the Ti-N two-element film, a filmed sample has smooth appearance and good compactness; the elements on the surface of the film comprise the following components by atom percent: 30.5 of Ti, 28.3 of Mo and 41.2 of N; and the hardness of the film is 29 GPa, and the oxidization weight gain at the temperature of 800 DEG C is only half of that of the Ti-N film.

Description

A kind of preparation method of Ti-Mo-N multi-element film
Technical field
The present invention relates to a kind of preparation method of material surface coating, the preparation method of especially a kind of high performance Ti-Mo-N multi-element film.
Background technology
Ti-N binary film has high hardness, wear resistance and excellent rotproofness, thereby is widely used at surface preparation film coatings such as cutter, moulding stock to improve.Yet along with fast development of modern industry, material property has been proposed increasingly high requirement, an urgent demand improves the use properties of TiN in all respects such as hardness, wear resistance, erosion resistance, high-temperature oxidation resistances.
Mainly be thereby that doping the 3rd in the TiN film, the 4th kind of element are perhaps implemented the performances such as hardness that thermal treatment changes film to passing through to film by the method for generally using now.Yet because alternative alloying element kind is more; And the step of preparation process parameter of film also varies; Therefore select a kind of alloying element of the film of TiN preferably; And find with it preparation technology's method of corresponding a kind of suitable TiN film, for the performance that improves the TiN film and the use range of expanding film and the working conditions using value with reality that has great importance.
Summary of the invention
To the problems referred to above, the object of the invention promptly is to select suitable alloying element with the preparation multi-element film into the TiN film, and optimizes the preparation technology parameter of multi-element film, thereby obtains a kind of preparation method of high performance thin film.
For solving the problems of the technologies described above, the technical scheme that the present invention adopted is following:
At first, be the essentially consist element of film with Ti, Mo, N, adopt the method for magnetron sputtering to prepare the Ti-Mo-N ternary film.
Particularly be, earlier with the substrate material surface polishing, and respectively with dry for standby behind the about 10min of each cleaning in ultrasonic cleaner such as hydrofluoric acid, acetone, alcohol and deionized water;
Subsequently, body material is placed on the sample table in the magnetron sputtering equipment Vakuumkammer, and with pure Ti target and Ti 50Mo 50Alloys target places different negative electrode target position respectively;
Subsequently vacuum tightness in the Vakuumkammer is extracted into≤5 * 10 -4Pa feeds the Ar that flow is 8-10sccm simultaneously, when gas pressure in vacuum is 2-4Pa, and preparatory sputter 2-3min, the power of sputter is 50-70W in advance, with the film formation surface of further cleaning body material;
The flow of keeping Ar subsequently is 8-10sccm; Control body material temperature is 40-50 ℃, when gas pressure in vacuum is 1-1.5Pa, applies the negative bias of 100-150V to body material; Remove the baffle plate of pure Ti target simultaneously; Power with 50-70W carries out sputter, and sputtering time is 5-10min, to form the pure Ti film of one deck;
Begin to feed the N that flow is 0.3-0.6sccm subsequently 2And the flow of keeping Ar is that 8-10sccm, gas pressure in vacuum are that the negative bias of 1-1.5Pa, body material is that the temperature of 100-150V, body material is 40-50 ℃; Power with 50-70W carries out sputter, and sputtering time is 15-25min, to form one deck Ti-N binary film;
The flow of keeping Ar subsequently is 8-10sccm, N 2Flow be that 0.3-0.6sccm, gas pressure in vacuum are that the negative bias of 1-1.5Pa, body material is 100-150V, the temperature of rising body material is 80-100 ℃, closes the baffle plate of pure Ti target simultaneously and removes Ti 50Mo 50The baffle plate of alloys target carries out sputter with the power of 50-70W, and sputtering time is 80-100min, to form the Ti-Mo-N ternary film.
Advantage of the present invention is: formed multilayer Ti-Mo-N multi-element film of different nature at matrix surface, both obtained and matrix good binding performance, had excellent hardness, wear resistance, solidity to corrosion and high-temperature oxidation resistance again.
Embodiment
Below, through concrete embodiment the present invention is elaborated.
The preparation and the heat treating method of a kind of high performance Ti-Mo-N multi-element film, it comprises following preparation process:
It is to be the essentially consist element of film with Ti, Mo, N, adopts the method for magnetron sputtering to prepare the Ti-Mo-N ternary film;
Select for use the W6Mo5Cr4V2 rapid steel as body material, earlier with the substrate material surface polishing, and respectively with dry for standby behind the about 10min of each cleaning in ultrasonic cleaner such as hydrofluoric acid, acetone, alcohol and deionized water;
Subsequently, body material is placed on the sample table in the magnetron sputtering equipment Vakuumkammer, and with pure Ti target and Ti 50Mo 50Alloys target places different negative electrode target position respectively;
Subsequently vacuum tightness in the Vakuumkammer is extracted into≤5 * 10 -4Pa feeds the Ar that flow is 9sccm simultaneously, when gas pressure in vacuum is 3Pa, and preparatory sputter 2min, the power of sputter is 60W in advance, with the film formation surface of further cleaning body material;
The flow of keeping Ar subsequently is 9sccm, and control body material temperature is 40 ℃, when gas pressure in vacuum is 1.5Pa; Apply the negative bias of 150V to body material, remove the baffle plate of pure Ti target simultaneously, carry out sputter with the power of 60W; Sputtering time is 7min, to form the pure Ti film of one deck;
Begin to feed the N that flow is 0.4sccm subsequently 2, and the flow of keeping Ar is that 9sccm, gas pressure in vacuum are that the negative bias of 1.5Pa, body material is that the temperature of 150V, body material is 40 ℃, carries out sputter with the power of 60W, sputtering time is 20min, to form one deck Ti-N binary film;
The flow of keeping Ar subsequently is 9sccm, N 2Flow be that 0.4sccm, gas pressure in vacuum are that the negative bias of 1.5Pa, body material is 150V, the temperature of rising body material is 100 ℃, closes the baffle plate of pure Ti target simultaneously and removes Ti 50Mo 50The baffle plate of alloys target carries out sputter with the power of 60W, and sputtering time is 90min, to form the Ti-Mo-N ternary film.
Compare with Ti-N binary film, the sample appearance surfaces is smooth smooth after the film forming, and compactness is good; Through test; The atoms of elements percentage composition of film surface is 30.5Ti-28.3Mo-41.2N, and the hardness of film surface is 29GPa, and the oxidation weight gain under 800 ℃ of conditions is merely the half the of Ti-N film.

Claims (1)

1. the preparation method of a Ti-Mo-N multi-element film, it is to be the essentially consist element of film with Ti, Mo, N, adopts the method for magnetron sputtering to prepare the Ti-Mo-N ternary film; Specifically comprise following preparation process:
Earlier with the substrate material surface polishing, and respectively with dry for standby behind the about 10min of each cleaning in ultrasonic cleaner such as hydrofluoric acid, acetone, alcohol and deionized water;
Subsequently, body material is placed on the sample table in the magnetron sputtering equipment Vakuumkammer, and with pure Ti target and Ti 50Mo 50Alloys target places different negative electrode target position respectively;
Subsequently vacuum tightness in the Vakuumkammer is extracted into≤5 * 10 -4Pa feeds the Ar that flow is 8-10sccm simultaneously, when gas pressure in vacuum is 2-4Pa, and preparatory sputter 2-3min, the power of sputter is 50-70W in advance, with the film formation surface of further cleaning body material;
The flow of keeping Ar subsequently is 8-10sccm; Control body material temperature is 40-50 ℃, when gas pressure in vacuum is 1-1.5Pa, applies the negative bias of 100-150V to body material; Remove the baffle plate of pure Ti target simultaneously; Power with 50-70W carries out sputter, and sputtering time is 5-10min, to form the pure Ti film of one deck;
Begin to feed the N that flow is 0.3-0.6sccm subsequently 2And the flow of keeping Ar is that 8-10sccm, gas pressure in vacuum are that the negative bias of 1-1.5Pa, body material is that the temperature of 100-150V, body material is 40-50 ℃; Power with 50-70W carries out sputter, and sputtering time is 15-25min, to form one deck Ti-N binary film;
The flow of keeping Ar subsequently is 8-10sccm, N 2Flow be that 0.3-0.6sccm, gas pressure in vacuum are that the negative bias of 1-1.5Pa, body material is 100-150V, the temperature of rising body material is 80-100 ℃, closes the baffle plate of pure Ti target simultaneously and removes Ti 50Mo 50The baffle plate of alloys target carries out sputter with the power of 50-70W, and sputtering time is 80-100min, to form the Ti-Mo-N ternary film.
CN 201110307385 2011-10-11 2011-10-11 Preparation method of Ti-Mo-N multi-element film Active CN102409306B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103898463A (en) * 2014-03-07 2014-07-02 浙江大学 Multi-element high-entropy alloy film and preparation method thereof
CN104602438A (en) * 2014-12-29 2015-05-06 中国原子能科学研究院 Preparation method of tritium impregnated target slice
CN108884553A (en) * 2016-03-29 2018-11-23 大同特殊钢株式会社 Titanium alloy overlay film and titanium alloy target
CN109440065A (en) * 2018-11-09 2019-03-08 南昌大学 A kind of preparation method of Mg alloy surface tungsten molybdenum nanoscale anticorrosion film

Citations (2)

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Publication number Priority date Publication date Assignee Title
CN101386976A (en) * 2008-10-31 2009-03-18 上海工程技术大学 Technique for magnetron sputtering TiN film on magnesium alloy surface
CN102115872A (en) * 2009-12-30 2011-07-06 沈阳天贺新材料开发有限公司 Preparation method for magnetron sputtering TiMo film on titanium alloy surface

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Publication number Priority date Publication date Assignee Title
CN101386976A (en) * 2008-10-31 2009-03-18 上海工程技术大学 Technique for magnetron sputtering TiN film on magnesium alloy surface
CN102115872A (en) * 2009-12-30 2011-07-06 沈阳天贺新材料开发有限公司 Preparation method for magnetron sputtering TiMo film on titanium alloy surface

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Q.YANG, ET AL.: ""Wear resistant TiMoN coatings deposited by magnetron sputtering"", 《WEAR》 *
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103898463A (en) * 2014-03-07 2014-07-02 浙江大学 Multi-element high-entropy alloy film and preparation method thereof
CN104602438A (en) * 2014-12-29 2015-05-06 中国原子能科学研究院 Preparation method of tritium impregnated target slice
CN104602438B (en) * 2014-12-29 2017-07-14 中国原子能科学研究院 One kind inhales tritium target piece preparation method
CN108884553A (en) * 2016-03-29 2018-11-23 大同特殊钢株式会社 Titanium alloy overlay film and titanium alloy target
CN108884553B (en) * 2016-03-29 2021-02-23 大同特殊钢株式会社 Titanium alloy coating and titanium alloy target
CN109440065A (en) * 2018-11-09 2019-03-08 南昌大学 A kind of preparation method of Mg alloy surface tungsten molybdenum nanoscale anticorrosion film
CN109440065B (en) * 2018-11-09 2020-07-14 南昌大学 Preparation method of nano-scale corrosion-resistant molybdenum-tungsten film on surface of magnesium alloy

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