CN102409306B - Preparation method of Ti-Mo-N multi-element film - Google Patents

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

Info

Publication number
CN102409306B
CN102409306B CN 201110307385 CN201110307385A CN102409306B CN 102409306 B CN102409306 B CN 102409306B CN 201110307385 CN201110307385 CN 201110307385 CN 201110307385 A CN201110307385 A CN 201110307385A CN 102409306 B CN102409306 B CN 102409306B
Authority
CN
China
Prior art keywords
film
body material
flow
vacuum
subsequently
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN 201110307385
Other languages
Chinese (zh)
Other versions
CN102409306A (en
Inventor
韩晓芬
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Inner Mongolia Zhongtian Hongyuan Rare Earth New Material Co ltd
Original Assignee
NINGBO RUITONG NEW MATERIAL TECHNOLOGY Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by NINGBO RUITONG NEW MATERIAL TECHNOLOGY Co Ltd filed Critical NINGBO RUITONG NEW MATERIAL TECHNOLOGY Co Ltd
Priority to CN 201110307385 priority Critical patent/CN102409306B/en
Publication of CN102409306A publication Critical patent/CN102409306A/en
Application granted granted Critical
Publication of CN102409306B publication Critical patent/CN102409306B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Physical Vapour Deposition (AREA)

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 more and more higher requirement, an urgent demand improves the use properties of TiN in all respects such as hardness, wear resistance, erosion resistance, high-temperature oxidation resistances.
The method that is commonly used now mainly be in the TiN film, mix the 3rd, the 4th kind of element or to by thereby film is implemented the performances such as hardness that thermal treatment changes film.Yet because alternative doped element kind is more, and the step of preparation process parameter of film also varies, therefore select a kind of doped element of the film of TiN preferably, and find preparation technology's method of a kind of suitable TiN film correspondingly, for the performance that improves the TiN film and expand the use range of film and working conditions has great importance and actual using value.
Summary of the invention
At the problems referred to above, purpose of the present invention namely is to select suitable doped 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 solution adopted in the present invention is as follows:
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 that earlier with the substrate material surface polishing, and each cleans dry for standby behind about 10min in ultrasonic cleaner with hydrofluoric acid, acetone, alcohol and deionized water etc. respectively;
Subsequently, body material is placed on the sample table in the magnetron sputtering equipment vacuum chamber, and with pure Ti target and Ti 50Mo 50Alloys target places different negative electrode target position respectively;
Subsequently vacuum tightness in the vacuum chamber is extracted into≤5 * 10 -4Pa feeds the Ar that flow is 8-10sccm simultaneously, when gas pressure in vacuum is 2-4Pa, and pre-sputter 2-3min, the power of pre-sputter is 50-70W, 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, apply 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, the present invention is described in detail by specific embodiment.
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 each cleans dry for standby behind about 10min in ultrasonic cleaner with hydrofluoric acid, acetone, alcohol and deionized water etc. respectively;
Subsequently, body material is placed on the sample table in the magnetron sputtering equipment vacuum chamber, and with pure Ti target and Ti 50Mo 50Alloys target places different negative electrode target position respectively;
Subsequently vacuum tightness in the vacuum chamber is extracted into≤5 * 10 -4Pa feeds the Ar that flow is 9sccm simultaneously, when gas pressure in vacuum is 3Pa, and pre-sputter 2min, the power of pre-sputter is 60W, 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, after tested, 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 only is half 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 in ultrasonic cleaner, respectively clean dry for standby behind the 10min with hydrofluoric acid, acetone, alcohol and deionized water respectively;
Subsequently, body material is placed on the sample table in the magnetron sputtering equipment vacuum chamber, and with pure Ti target and Ti 50Mo 50Alloys target places different negative electrode target position respectively;
Subsequently vacuum tightness in the vacuum chamber is extracted into≤5 * 10 -4Pa feeds the Ar that flow is 8-10sccm simultaneously, when gas pressure in vacuum is 2-4Pa, and pre-sputter 2-3min, the power of pre-sputter is 50-70W, 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, apply 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)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 201110307385 CN102409306B (en) 2011-10-11 2011-10-11 Preparation method of Ti-Mo-N multi-element film

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 201110307385 CN102409306B (en) 2011-10-11 2011-10-11 Preparation method of Ti-Mo-N multi-element film

Publications (2)

Publication Number Publication Date
CN102409306A CN102409306A (en) 2012-04-11
CN102409306B true CN102409306B (en) 2013-09-25

Family

ID=45911640

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 201110307385 Active CN102409306B (en) 2011-10-11 2011-10-11 Preparation method of Ti-Mo-N multi-element film

Country Status (1)

Country Link
CN (1) CN102409306B (en)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103898463B (en) * 2014-03-07 2015-11-11 浙江大学 A kind of polynary high-entropy alloy film and preparation method thereof
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
JP6868426B2 (en) * 2016-03-29 2021-05-12 東北特殊鋼株式会社 Titanium alloy coating film and its manufacturing method, and titanium alloy target material manufacturing method
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

Citations (2)

* Cited by examiner, † Cited by third party
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
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

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
"Wear resistant TiMoN coatings deposited by magnetron sputtering";Q.Yang, et al.;《WEAR》;20050825;第261卷;119-125 *
Q.Yang, et al.."Wear resistant TiMoN coatings deposited by magnetron sputtering".《WEAR》.2005,第261卷119-125.
于翔，等."中频对靶磁控溅射合成TiN/Ti多层膜".《金属学报》.2006,第42卷(第6期),第662-666页.
于翔,等."中频对靶磁控溅射合成TiN/Ti多层膜".《金属学报》.2006,第42卷(第6期),第662-666页. *

Also Published As

Publication number Publication date
CN102409306A (en) 2012-04-11

Similar Documents

Publication Publication Date Title
CN102409306B (en) Preparation method of Ti-Mo-N multi-element film
CN107130212B (en) High-hardness wear-resistant thermal-shock-resistant thick tantalum coating and preparation method thereof
CN103522627B (en) The composite coating on a kind of valve sealing element surface and preparation method thereof
CN103572207A (en) Plated piece and preparation method thereof
CN104264116B (en) A kind of technique preparing AlTiCrNiTa high-entropy alloy coating at X80 pipe line steel substrate surface
CN102899622A (en) Film-coated component and preparation method thereof
CN102409308B (en) Preparation and heat treatment method of Ti-Mo-N multi-element film
CN110670029A (en) High-hardness wear-resistant TiN/TiAlSiN composite coating on surface of aluminum alloy and preparation method thereof
CN105385997B (en) A kind of Cr2O3Thin film system and preparation method thereof
CN104532190A (en) Preparation method of Zr-Cu metal glass film
TW201243069A (en) Coated article and method for making the same
CN102409290B (en) Hard Ti-Mo-N multi-element thin film
CN203697597U (en) Composite coating on surface of valve sealing element
CN104032269A (en) NbN-Ag hard thin film and preparation method thereof
CN102409307B (en) Cutting tool with Ti-Mo-N multi-element surface film
CN109487214A (en) A kind of magnesium-alloy surface coating method and Corrosion-resistant magnesia alloy prepared therefrom
CN113025958B (en) Composite film layer for aluminum alloy surface and preparation method thereof
CN112941463B (en) Nano multilayer oxynitride corrosion-resistant protective coating and preparation method and application thereof
CN101660160A (en) Nitride compound protective coating with high hardness and high thermal shock stability
CN104073770A (en) Tiwaln hard thin film and preparation method thereof
CN102534480A (en) Coating piece and preparation method thereof
CN113913747A (en) Coating, method for producing the same and device
CN111118465A (en) Sintered neodymium-iron-boron magnet surface functional film layer and preparation method thereof
CN102994954A (en) Plated film member and preparation method
CN112301400B (en) Preparation method of hard protection micro-arc oxidation film layer on surface of titanium alloy ball valve

Legal Events

Date Code Title Description
C06 Publication
DD01 Delivery of document by public notice

Addressee: NINGBO RUITONG NEW MATERIAL TECHNOLOGY Co.,Ltd.

Document name: Notification of Passing Preliminary Examination of the Application for Invention

PB01 Publication
C10 Entry into substantive examination
DD01 Delivery of document by public notice

Addressee: NINGBO RUITONG NEW MATERIAL TECHNOLOGY Co.,Ltd.

Document name: Notification of Publication of the Application for Invention

SE01 Entry into force of request for substantive examination
DD01 Delivery of document by public notice

Addressee: NINGBO RUITONG NEW MATERIAL TECHNOLOGY Co.,Ltd.

Document name: Notification of Patent Invention Entering into Substantive Examination Stage

DD01 Delivery of document by public notice

Addressee: NINGBO RUITONG NEW MATERIAL TECHNOLOGY Co.,Ltd.

Document name: the First Notification of an Office Action

DD01 Delivery of document by public notice

Addressee: NINGBO RUITONG NEW MATERIAL TECHNOLOGY Co.,Ltd.

Document name: Notification to Go Through Formalities of Registration

C14 Grant of patent or utility model
GR01 Patent grant
ASS Succession or assignment of patent right

Owner name: INNER ZHONGTIAN HONGYUAN TECHNOLOGY CO., LTD.

Free format text: FORMER OWNER: GUANGDONG HUABO ENTERPRISE MANAGEMENT CONSULTING CO., LTD.

Effective date: 20140515

Owner name: GUANGDONG HUABO ENTERPRISE MANAGEMENT CONSULTING C

Free format text: FORMER OWNER: NINGBO RUITONG NEW MATERIAL TECHNOLOGY CO., LTD.

Effective date: 20140515

C41 Transfer of patent application or patent right or utility model
COR Change of bibliographic data

Free format text: CORRECT: ADDRESS; FROM: 510640 GUANGZHOU, GUANGDONG PROVINCE TO: 014000 BAOTOU, INNER MONGOLIA AUTONOMOUS REGION

Free format text: CORRECT: ADDRESS; FROM: 315177 NINGBO, ZHEJIANG PROVINCE TO: 510640 GUANGZHOU, GUANGDONG PROVINCE

TR01 Transfer of patent right

Effective date of registration: 20140515

Address after: 510640 Guangdong city of Guangzhou province Tianhe District gold Yinglu No. 1 was 1106 room two

Patentee after: GUANGDONG HUABO ENTERPRISE MANAGEMENT CONSULTING Co.,Ltd.

Address before: 315177 Zhejiang province Ningbo city Yinzhou District town water village turnip

Patentee before: NINGBO RUITONG NEW MATERIAL TECHNOLOGY Co.,Ltd.

Effective date of registration: 20140515

Address after: 014000 the Inner Mongolia Autonomous Region Baotou rare earth hi tech Zone Software Park D Part 411

Patentee after: Inner Mongolia Zhongtian Hongyuan Technology Co.,Ltd.

Address before: 510640 Guangdong city of Guangzhou province Tianhe District gold Yinglu No. 1 was 1106 room two

Patentee before: GUANGDONG HUABO ENTERPRISE MANAGEMENT CONSULTING Co.,Ltd.

CP01 Change in the name or title of a patent holder

Address after: 014000 D software part of rare earth hi tech Zone, Baotou, the Inner Mongolia Autonomous Region, Part 411

Patentee after: INNER MONGOLIA ZHONGTIAN HONGYUAN REMANUFACTURING CO.,LTD.

Address before: 014000 D software part of rare earth hi tech Zone, Baotou, the Inner Mongolia Autonomous Region, Part 411

Patentee before: Inner Mongolia Zhongtian Hongyuan Technology Co.,Ltd.

CP01 Change in the name or title of a patent holder
PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of invention: Preparation method of Ti-Mo-N multi-element film

Effective date of registration: 20191008

Granted publication date: 20130925

Pledgee: Inner Mongolia Productivity Promotion Center Co.,Ltd.

Pledgor: INNER MONGOLIA ZHONGTIAN HONGYUAN REMANUFACTURING CO.,LTD.

Registration number: Y2019150000010

PE01 Entry into force of the registration of the contract for pledge of patent right
PC01 Cancellation of the registration of the contract for pledge of patent right

Date of cancellation: 20191126

Granted publication date: 20130925

Pledgee: Inner Mongolia Productivity Promotion Center Co.,Ltd.

Pledgor: INNER MONGOLIA ZHONGTIAN HONGYUAN REMANUFACTURING CO.,LTD.

Registration number: Y2019150000010

PC01 Cancellation of the registration of the contract for pledge of patent right
CP01 Change in the name or title of a patent holder

Address after: 014000 D software part of rare earth hi tech Zone, Baotou, the Inner Mongolia Autonomous Region, Part 411

Patentee after: Inner Mongolia Zhongtian Hongyuan rare earth new material Co.,Ltd.

Address before: 014000 D software part of rare earth hi tech Zone, Baotou, the Inner Mongolia Autonomous Region, Part 411

Patentee before: INNER MONGOLIA ZHONGTIAN HONGYUAN REMANUFACTURING Co.,Ltd.

CP01 Change in the name or title of a patent holder
PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of invention: A Preparation Method of Ti Mo N Multivariate Thin Films

Effective date of registration: 20230728

Granted publication date: 20130925

Pledgee: Baotou Branch of Inner Mongolia Hohhot Jingu Rural Commercial Bank Co.,Ltd.

Pledgor: Inner Mongolia Zhongtian Hongyuan rare earth new material Co.,Ltd.

Registration number: Y2023150000119

PE01 Entry into force of the registration of the contract for pledge of patent right