CN103009697A - Self-lubricating gradient composite superhard film and preparation method thereof - Google Patents
Self-lubricating gradient composite superhard film and preparation method thereof Download PDFInfo
- Publication number
- CN103009697A CN103009697A CN2012105515359A CN201210551535A CN103009697A CN 103009697 A CN103009697 A CN 103009697A CN 2012105515359 A CN2012105515359 A CN 2012105515359A CN 201210551535 A CN201210551535 A CN 201210551535A CN 103009697 A CN103009697 A CN 103009697A
- Authority
- CN
- China
- Prior art keywords
- workpiece
- film
- preparation
- targets
- target
- 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.)
- Granted
Links
Images
Landscapes
- Cutting Tools, Boring Holders, And Turrets (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a self-lubricating gradient composite superhard film and a preparation method thereof. The superhard film comprises a CrN priming layer, a TiN transition layer and a Ti (C, N) working layer which are sequentially arranged. The preparation method comprises the steps of preparing vacuum coating equipment; workpiece pretreatment; workpiece heating and ion etching; preparing the CrN priming layer; preparing the TiN transition layer; and preparing the Ti (C, N) working layer. According to the superhard film prepared by the invention, crystal phases of TiN, TiC and Ti (C, N) and an amorphous phase C are contained in the Ti (C, N) working phase, so that the film is excellent in toughness and simultaneously has ultra-high hardness, the hardness value can reach up to 62 GPa, simultaneously the emergence of the amorphous phase C in the film enables the friction coefficient of the film to be maintained in a range from 0.4 to 0.5, and the film has the excellent comprehensive performance.
Description
Technical field
What the present invention relates to is a kind of ultra-hard abrasive material of utilizing the preparation of multi-arc ion coating method, in particular a kind of self-lubricating gradient compounded superhard film and preparation method thereof.
Background technology
Along with the develop rapidly of new and high technology, more and more higher to the requirement of die surface performance, the precision die of especially under the conditions such as high temperature, high pressure, heavy duty, working.Mould often lost efficacy because of wearing and tearing, fracture and fatigue etc. in the process under arms.This mainly is because effect and die hardness, the intensity of high temperature, high pressure, high friction, alternate stress and stress raisers, rigidity is on the low side and poor lubrication etc. causes.For avoiding the mould premature failure, its working face necessarily requires to have high rigidity, self-lubricity, high thermal stability and corrosion resistance etc.The multi-arc ion coating membrane technology has had the development of advancing by leaps and bounds in the time of decades, the self-lubricating superhard film of this technology preparation can make performance, the service life of zero die surface obtain economically optimized effect, thereby holds out broad prospects in coating market.
Ti(C, N) have the advantage of TiC and TiN bi-material concurrently, it can be by the one-tenth that continuously changes C, N assign to control Ti(C, N in coating procedure) performance, and form the sandwich construction of heterogeneity, reduce the internal stress of coating, improve toughness.Some instruments of producing at present recommend the GC4000 series blade for the machined steel material, T715X and the T725X coated chip of Toshiba Corp all to contain Ti(C, N such as Sweden Sandvik company) coating composition.Ti(C, N) preparation technology of coating have multiple, early stage industrial quarters high temperature CVD method depositing Ti (C, N) coating commonly used, depositing temperature up to 900 ℃～1100 ℃, matrix is mainly resistant to elevated temperatures Hardmetal materials.At present, middle temperature Ti(C, N) coating has many application in the cast-aluminum die surface protection.But in 700 ℃～900 ℃ scope behind depositing Ti (C, the N) film, steel matrix need be heat-treated toward contact, so low temperature Ti(C, N) preparation research obtains to pay attention to gradually, physical vapour deposition (PVD) particularly.
Utilizing physical vapour deposition (PVD) to prepare TiCN series self-lubricating gradient superhard thin film is the effective ways that improve the die surface performance.On the one hand, the existence of the amorphous C phase in the film effectively reduces the coefficient of friction of film, has avoided the scuffing of die surface to workpiece; On the other hand, TiC phase and Ti(C, N in the film) efficiently solve mutually the hardness problem of bringing mutually because of amorphous C; The graded of composition has guaranteed the adhesion that film is good in addition.
Generally speaking, utilize the method for physical vapour deposition (PVD), prepare at low temperatures have ultrahigh hardness, the hard coat of low-friction coefficient, high-bond, for the development important in inhibiting of processing manufacturing industry.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of self-lubricating gradient compounded superhard film and preparation method thereof is provided, in the deposition process of film, change the flow of gas by linearity, thereby obtain the superhard film that component gradient changes.
The present invention is achieved by the following technical solutions, superhard film of the present invention comprises CrN prime coat, TiN transition zone and Ti(C, the N that sets gradually) working lining, described Ti(C, N) working lining comprises crystal phase TiN, TiC, Ti(C, N) and amorphous phase C; Ti(C, N) in the working lining, the content of amorphous phase C by superhard film surface to TiN transition zone and Ti(C, N) the at the interface gradually reduction of working lining, the content of crystal phase TiC by superhard film surface to TiN transition zone and Ti(C, N) the at the interface gradually increase of working lining.
The gross thickness of described superhard film is 5～7 μ m, and CrN prime coat and TiN transition zone gross thickness are 2.5～4 μ m, Ti(C, N) working lining thickness is 1.5～3 μ m.
A kind of preparation method of self-lubricating gradient compounded superhard film may further comprise the steps:
(1) prepares vacuum coating equipment
Two row negative electrode multi sphere Ti targets and one are listed as three sides that the Cr target is installed in respectively the vacuum coating locular wall, four targets of every row, the angle of adjacent two row targets is 120 °;
(2) workpiece preliminary treatment
Surface of the work is carried out blasting treatment, then blow away the sand on surface with air gun, again workpiece is put into the pure water Ultrasonic Cleaning, then workpiece is put into the ultrasonic processing of the cleaning machine that is added with antirust solution, at last workpiece is dried;
(3) workpiece heating and ion etching
Pretreated clamping workpiece on the turntable of vacuum film coating chamber, is evacuated to 4 * 10
-3Behind the Pa, pass into N
2With Ar gas, make the vacuum in the coating chamber maintain 1.5Pa, make simultaneously the plated film indoor temperature maintain 450 ℃, workpiece is applied 600～800V Dc bias, start the Cr target, the high energy electron and the ion that are produced by arc discharge and glow discharge effect in the coating chamber bombard surface of the work under electric field action, workpiece was carried out etching 20～50 minutes;
(4) preparation of CrN prime coat
Back bias voltage on the workpiece is adjusted to 150V, stops Ar gas and pass into N
2Gas flow is made as 380～400sccm, makes the pressure in the coating chamber remain on 0.8Pa, makes simultaneously the coating chamber temperature maintain 480 ℃, and the Cr target is opened, and two row Ti targets are closed, and the target current of Cr target is 80A, and sedimentation time is 10～15 minutes;
(5) preparation of TiN transition zone
Close the Cr target of opening in the step (4), then open two row Ti targets, the Ti target current is adjusted to 80A, with N
2Throughput is adjusted into 700sccm, and sedimentation time is 30～40 minutes;
(6) Ti(C, N) preparation of working lining
Keep the N in the step (5)
2Throughput and Ti target current pass into C
2H
2Gas,
At first make the C that passes into
2H
2Gas flow remains on 25～40sccm, and sedimentation time is 25 minutes;
Then with C
2H
2Gas flow is by the 90～400sccm that increases to of 25～40sccm linearity, and preparation has Ti(C, the N that component gradient changes) layer, sedimentation time is 30 minutes, coating chamber is cooled to room temperature taking-up workpiece and gets final product.
In the described step (1), two row negative electrode multi sphere Ti targets are made by Ti simple substance, and purity is that 99.9%, one row Cr target is made by Cr simple substance, and purity is 99.9%.
In the described step (3), the rotating speed of turntable is 3rpm, before etching, is evacuated to 4 * 10
-3Behind the Pa, all cathode targets are in closed condition, pass into N
2With residual air in the further eliminating coating chamber, N
2Gas flow is 100sccm, passes into simultaneously Ar gas, and the Ar gas flow is 50sccm, N
2It is 1～3 minute that gas passes into the time, and Ar gas keeps passing into state;
When surface of the work was carried out etching, the back bias voltage on front 10～25 minutes workpiece was 800V, and the back bias voltage on rear 10～25 minutes workpiece is 600V; Surface of the work is carried out in the etching process, and the Ar throughput was adjusted into 30sccm by 50sccm in rear 10～25 minutes, and again passed into N
2Gas, flow are 50sccm; In the etching process, four Cr targets, two targets separately that are arranged in the same side are one group, open simultaneously, close; Two groups of adjacent successively open and close, target current is 60～80A.
In the described step (4), N
2Throughput is 380～450sccm.
The present invention has the following advantages compared to existing technology: the present invention carries out in two steps to the etching of workpiece, respectively carrying out under the 800V back bias voltage with under the 600V back bias voltage, when back bias voltage is adjusted into 600V, passes into the N of 50sccm
2Gas helps further to strengthen the adhesion of CrN prime coat and matrix;
The present invention controls C when preparation Ti (C, N) working lining
2H
2Flow, it was increased and linear increasing with the plated film time, crystal phase TiC content from outward appearance to inner essence increases in gradient in the coating of acquisition, amorphous phase C then reduces, so that the surface of film has lower coefficient of friction;
The superhard thin film that the present invention is prepared, at Ti (C, N) comprise crystal phase TiN, TiC, Ti (C in the working lining, N) and amorphous phase C, make film have excellent toughness, have simultaneously ultrahigh hardness concurrently, hardness number can be up to 62GPa, the appearance of amorphous phase C has good combination property so that the coefficient of friction of this film can remain on 0.4～0.5 in the film simultaneously.
Description of drawings
Fig. 1 is with the analysis result of glancing incidence small angle X-ray diffraction to the film phase;
Fig. 2 is that embodiment 1 gained film is without the C1s x-ray photoelectron energy spectrogram on the As-deposited film surface of Ar ion etching;
Fig. 3 is that embodiment 2 gained films are without the C1s x-ray photoelectron energy spectrogram on the As-deposited film surface of Ar ion etching;
Fig. 4 is that embodiment 3 gained films are without the C1s x-ray photoelectron energy spectrogram on the As-deposited film surface of Ar ion etching;
Fig. 5 is that embodiment 1 gained film is through the C1s x-ray photoelectron energy spectrogram at 50 seconds following 10nm place, As-deposited film surface of Ar ion etching;
Fig. 6 is that embodiment 2 gained films are through the C1s x-ray photoelectron energy spectrogram at 50 seconds following 10nm place, As-deposited film surface of Ar ion etching;
Fig. 7 is that embodiment 3 gained films are through the C1s x-ray photoelectron energy spectrogram at 50 seconds following 10nm place, As-deposited film surface of Ar ion etching;
Fig. 8 is the hardness that adopts the film that nano impress equipment continuous stiffness measurement records;
Fig. 9 is that embodiment 1 adopts scratching instrument to the test result of film adhesion;
Figure 10 is that embodiment 2 adopts scratching instrument to the test result of film adhesion;
Figure 11 is that embodiment 3 adopts scratching instrument to the test result of film adhesion.
The specific embodiment
The below elaborates to embodiments of the invention, and present embodiment is implemented under take technical solution of the present invention as prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
The preparation method of the self-lubricating gradient compounded superhard film of present embodiment may further comprise the steps:
(1) prepares vacuum coating equipment
Two row negative electrode multi sphere Ti targets and one are listed as three sides that the Cr target is installed in respectively the vacuum coating locular wall, four targets of every row, the angle of adjacent two row targets is 120 °, two row negative electrode multi sphere Ti targets are made by Ti simple substance, purity is that 99.9%, one row Cr target is made by Cr simple substance, and purity is 99.9%;
(2) workpiece preliminary treatment
Surface of the work is carried out blasting treatment, remove surperficial burr, then blow away the sand on surface with air gun, again workpiece is put into the pure water Ultrasonic Cleaning, then workpiece is put into the ultrasonic processing of the cleaning machine that is added with antirust solution, at last workpiece is dried;
(3) workpiece heating and ion etching
On the turntable of vacuum film coating chamber, the rotating speed of turntable is 3rpm, is evacuated to 4 * 10 with pretreated clamping workpiece
-3Behind the Pa, pass into N
2With Ar gas, make the vacuum in the coating chamber maintain 1.5Pa, open simultaneously firing equipment, make the plated film indoor temperature maintain 450 ℃, workpiece is applied the 800V back bias voltage, pass into N
2With residual air in the further eliminating coating chamber, N
2Gas flow is 100sccm, passes into simultaneously Ar gas, and the Ar gas flow is 50sccm, N
2It is 1 minute that gas passes into the time, and Ar gas keeps passing into state, so that the pressure of vacuum chamber remains on 1.5Pa;
Stop to pass into N
2Gas, the Ar gas flow is constant, keeps passing into state, keeps the pressure of vacuum chamber at 1.5Pa, and first group of two target separately opened simultaneously on the Cr target, and target current is 70A, etching 8 minutes;
Then close first group of two target separately on the Cr target, open second group of two target separately on the Cr target, target current is 70A, etching 8 minutes;
The Ar throughput is adjusted into 30sccm by 50sccm, and again passes into N
2Gas, flow are 50sccm, and pressure keeps 0.75Pa in the coating chamber, and the back bias voltage on the workpiece is adjusted to 600V, and the target current of second group of two target separately is 60A on the Cr target, etching 10 minutes;
Close second group of two target separately on the Cr target, open first group of two target separately on the Cr target, target current is 60A, etching 10 minutes;
(4) preparation of CrN prime coat
Back bias voltage on the workpiece is adjusted to 150V, stops Ar gas and pass into, regulate N
2Throughput is 380sccm, makes the pressure in the coating chamber remain on 0.8Pa, makes simultaneously the coating chamber temperature maintain 480 ℃, and four Cr targets that are positioned at same row are held open state simultaneously, and target current is 80A, and sedimentation time is 1 minute;
Then with N
2Throughput is adjusted to 400sccm, deposits 11 minutes;
(5) preparation of TiN transition zone
Close the Cr target of opening in the step (4), then open two row Ti targets, the Ti target current is adjusted to 80A, with N
2Throughput is adjusted into 700sccm, and sedimentation time is 33 minutes;
(6) Ti(C, N) preparation of working lining
Keep the N in the step (5)
2Throughput and Ti target current pass into C
2H
2Gas,
At first make the C that passes into
2H
2Gas flow remains on 35sccm, and sedimentation time is 25 minutes;
Then with C
2H
2Gas flow is by the 100sccm that increases to of 35sccm linearity, and sedimentation time is 30 minutes, and preparation has Ti(C, the N that component gradient changes) layer, coating chamber is cooled to room temperature taking-up workpiece and gets final product.
The gross thickness of the superhard film that present embodiment makes is 5 μ m, and Ti (C, N) Thickness of Gradient Layer is 2.5 μ m, and the gross thickness of CrN prime coat and TiN transition zone is 2.5 μ m, and hardness is 62GPa, and adhesion is 50N.
Embodiment 2
In the present embodiment step (6), C
2H
2Gas flow is by the 230sccm that increases to of 35sccm linearity, and the gross thickness of the superhard film that present embodiment makes is 6 μ m, Ti (C, N) Thickness of Gradient Layer is 2.5 μ m, the gross thickness of CrN prime coat and TiN transition zone is 3.5 μ m, and hardness is 48GPa, and adhesion is 60N.Other embodiments are identical with embodiment 1.
Embodiment 3
In the present embodiment step (6), C
2H
2Gas flow is by the 350sccm that increases to of 35sccm linearity, and the gross thickness of the superhard film that present embodiment makes is 7 μ m, Ti (C, N) Thickness of Gradient Layer is 4 μ m, the gross thickness of CrN prime coat and TiN transition zone is 4 μ m, and hardness is 31GPa, and adhesion is 76N.Other embodiments are identical with embodiment 1.
Film to embodiment 1～3 gained is labeled as respectively C1, C2 and C3.
Fig. 1 is the glancing incidence small angle x-ray diffraction (SAXD) collection of illustrative plates of embodiment 1～3 gained film, utilizes Jade software that it is analyzed, the result show all contain TiN, TiC, Ti(C, N in the gained film) the crystal phase.
Fig. 2～4 are respectively the C1s x-ray photoelectron energy spectrogram of embodiment 1～3 gained film, the comparative example 1～3, utilize XPS that C element chemistry attitude in the film is analyzed, all contain C-C sp2 key in embodiment 1～3 gained film, studies show that widely sp2 amorphous phase C can effectively reduce the coefficient of friction of film.
Fig. 5～7 are respectively embodiment 1～3 gained film at the C1s x-ray photoelectron energy spectrogram of Ar ion etching after 50 seconds, and etch rate is 0.2nm/S.With Fig. 5～7 difference comparison diagrams 2～4, the percentage that the corresponding peak area of each bond energy accounts for the gross area can be thought the percentage of this bond energy, can find out: Ti(C, N) in the working lining, the content of amorphous phase C is surperficial to TiN transition zone and Ti(C by superhard film, N) reducing gradually at the interface of working lining, the content of crystal phase TiC by the superhard film surface to TiN transition zone and Ti(C, N) the at the interface gradually increase of working lining.
As shown in Figure 8, comparative example 1～embodiment 3, the hardness of the film that employing nano impress equipment continuous stiffness measurement records.Can find out that embodiment 1 gained film hardness can reach more than the 60GPa, embodiment 3 gained films are owing to the increase of amorphous phase C content, and hardness decreases.
Shown in Fig. 9～11, adopt scratching instrument that the film adhesion is tested, comparative example 1～embodiment 3 adopts scratching instrument that the film adhesion is tested.The graded of composition and the preparation of transition zone are so that film can obtain good binding ability, and three embodiment adhesions are all above 50N.
C among three embodiment
2H
2The difference of gas flow, deposition effect show above the performance of film, shown in Fig. 8～11: because final step C
2H
2Gas flow adds to 350 of C3 by 100 of C1, and analyzing and drawing structure aspects TiC content is C1〉C2〉C3, amorphous phase C content C1＜C2＜C3 causes hardness C1〉C2〉C3, but adhesion C1＜C2＜C3.
Claims (6)
1. a self-lubricating gradient compounded superhard film is characterized in that, described superhard film comprises CrN prime coat, TiN transition zone and the Ti(C that sets gradually, N) working lining, described Ti(C, N) working lining comprises crystal phase TiN, TiC, Ti(C, N) and amorphous phase C; Ti(C, N) in the working lining, the content of amorphous phase C by superhard film surface to TiN transition zone and Ti(C, N) the at the interface gradually reduction of working lining, the content of crystal phase TiC by superhard film surface to TiN transition zone and Ti(C, N) the at the interface gradually increase of working lining.
2. self-lubricating gradient compounded superhard film according to claim 1, it is characterized in that: the gross thickness of described superhard film is 5～7 μ m, CrN prime coat and TiN transition zone gross thickness are 2.5～4 μ m, Ti(C, N) working lining thickness is 1.5～3 μ m.
3. the preparation method of a self-lubricating gradient compounded superhard film as claimed in claim 1 or 2 is characterized in that: may further comprise the steps:
(1) prepares vacuum coating equipment
Two row negative electrode multi sphere Ti targets and one are listed as three sides that the Cr target is installed in respectively the vacuum coating locular wall, four targets of every row, the angle of adjacent two row targets is 120 °;
(2) workpiece preliminary treatment
Surface of the work is carried out blasting treatment, then blow away the sand on surface with air gun, again workpiece is put into the pure water Ultrasonic Cleaning, then workpiece is put into the ultrasonic processing of the cleaning machine that is added with antirust solution, at last workpiece is dried;
(3) workpiece heating and ion etching
Pretreated clamping workpiece on the turntable of vacuum film coating chamber, is evacuated to 4 * 10
-3Behind the Pa, pass into N
2With Ar gas, make the vacuum in the coating chamber maintain 1.5Pa, make simultaneously the plated film indoor temperature maintain 450 ℃, workpiece is applied 600～800V Dc bias, start the Cr target, the high energy electron and the ion that are produced by arc discharge and glow discharge effect in the coating chamber bombard surface of the work under electric field action, workpiece was carried out etching 20～50 minutes;
(4) preparation of CrN prime coat
Back bias voltage on the workpiece is adjusted to 150V, stops Ar gas and pass into N
2Gas flow is made as 380～400sccm, makes the pressure in the coating chamber remain on 0.8Pa, makes simultaneously the coating chamber temperature maintain 480 ℃, and the Cr target is opened, and two row Ti targets are closed, and the target current of Cr target is 80A, and sedimentation time is 10～15 minutes;
(5) preparation of TiN transition zone
Close the Cr target of opening in the step (4), then open two row Ti targets, the Ti target current is adjusted to 80A, with N
2Throughput is adjusted into 700sccm, and sedimentation time is 30～40 minutes;
(6) Ti(C, N) preparation of working lining
Keep the N in the step (5)
2Throughput and Ti target current pass into C
2H
2Gas,
At first make the C that passes into
2H
2Gas flow remains on 25～40sccm, and sedimentation time is 25 minutes;
Then with C
2H
2Gas flow is by the 90～400sccm that increases to of 25～40sccm linearity, and preparation has Ti(C, the N that component gradient changes) layer, sedimentation time is 30 minutes, coating chamber is cooled to room temperature taking-up workpiece and gets final product.
4. the preparation method of a kind of self-lubricating gradient compounded superhard film according to claim 3, it is characterized in that: in the described step (1), two row negative electrode multi sphere Ti targets are made by Ti simple substance, and purity is that 99.9%, one row Cr target is made by Cr simple substance, and purity is 99.9%.
5. the preparation method of a kind of self-lubricating gradient compounded superhard film according to claim 3, it is characterized in that: in the described step (3), the rotating speed of turntable is 3rpm, before etching, is evacuated to 4 * 10
-3Behind the Pa, all cathode targets are in closed condition, pass into N
2With residual air in the further eliminating coating chamber, N
2Gas flow is 100sccm, passes into simultaneously Ar gas, and the Ar gas flow is 50sccm, N
2It is 1～3 minute that gas passes into the time, and Ar gas keeps passing into state;
When surface of the work was carried out etching, the back bias voltage on front 10～25 minutes workpiece was 800V, and the back bias voltage on rear 10～25 minutes workpiece is 600V; Surface of the work is carried out in the etching process, and the Ar throughput was adjusted into 30sccm by 50sccm in rear 10～25 minutes, and again passed into N
2Gas, flow are 50sccm;
In the etching process, four Cr targets, two targets separately that are arranged in the same side are one group, open simultaneously, close; Two groups of adjacent successively open and close, target current is 60～80A.
6. the preparation method of a kind of self-lubricating gradient compounded superhard film according to claim 3 is characterized in that: in the described step (4), and N
2Throughput is 380～450sccm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210551535.9A CN103009697B (en) | 2012-12-18 | 2012-12-18 | Self-lubricating gradient composite superhard film and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210551535.9A CN103009697B (en) | 2012-12-18 | 2012-12-18 | Self-lubricating gradient composite superhard film and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103009697A true CN103009697A (en) | 2013-04-03 |
| CN103009697B CN103009697B (en) | 2014-09-24 |
Family
ID=47959057
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210551535.9A Active CN103009697B (en) | 2012-12-18 | 2012-12-18 | Self-lubricating gradient composite superhard film and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103009697B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104846340A (en) * | 2015-05-29 | 2015-08-19 | 山东大学 | Mo-S-N-Cr self-lubricating gradient-coated cutting tool and preparation process thereof |
| CN105463372A (en) * | 2015-12-11 | 2016-04-06 | 西北有色金属研究院 | Preparation method of multi-layer composite super-thick self-lubricating hard coating |
| CN105714244A (en) * | 2016-03-30 | 2016-06-29 | 青岛滨海学院 | Titanium alloy surface ceramic/metal gradient high-temperature composite coating and preparing method thereof |
| CN111893421A (en) * | 2020-08-12 | 2020-11-06 | 常熟市绿一电器配件制造有限公司 | Wear-resistant mold surface nanocrystal pattern layer and preparation method thereof |
| CN112725792A (en) * | 2020-12-28 | 2021-04-30 | 成都美奢锐新材料有限公司 | Preparation method of chromium nitride-titanium carbonitride base metal ceramic composite coating |
| CN115110033A (en) * | 2022-07-27 | 2022-09-27 | 南京真合材料科技有限公司 | Method for manufacturing super-hard film layer |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0550473A (en) * | 1991-08-28 | 1993-03-02 | Toshiba Corp | Injection mold |
| CN1454869A (en) * | 2003-06-04 | 2003-11-12 | 山东大学 | Gradient function ceramic cutter material and preparing method thereof |
| CN1962942A (en) * | 2006-11-27 | 2007-05-16 | 河海大学 | Process for in-situ formation of TiC/metal composite cladding layer controlled by plasma |
| CN101033842A (en) * | 2007-04-19 | 2007-09-12 | 湖南工业大学陶瓷研究所 | Ceramics coal-water slurry nozzle having two-way gradient function and method for making same |
| CN101554790A (en) * | 2009-05-18 | 2009-10-14 | 浙江大学 | Ultra-hard carbon film and preparation method thereof |
| CN101698362A (en) * | 2009-10-30 | 2010-04-28 | 华南理工大学 | Self-lubricating hard nanocomposite laminated coating and preparation method thereof |
| CN101712215A (en) * | 2009-10-30 | 2010-05-26 | 华南理工大学 | TiCN series nanometer gradient compound multi-layer coating and method for preparing same |
| US20120052276A1 (en) * | 2010-08-30 | 2012-03-01 | Hon Hai Precision Industry Co., Ltd. | Coating, article coated with coating, and method for manufacturing article |
| CN102390980A (en) * | 2011-08-12 | 2012-03-28 | 山东轻工业学院 | Gradient self-lubricating ceramic cutter material and preparation method thereof |
-
2012
- 2012-12-18 CN CN201210551535.9A patent/CN103009697B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0550473A (en) * | 1991-08-28 | 1993-03-02 | Toshiba Corp | Injection mold |
| CN1454869A (en) * | 2003-06-04 | 2003-11-12 | 山东大学 | Gradient function ceramic cutter material and preparing method thereof |
| CN1962942A (en) * | 2006-11-27 | 2007-05-16 | 河海大学 | Process for in-situ formation of TiC/metal composite cladding layer controlled by plasma |
| CN101033842A (en) * | 2007-04-19 | 2007-09-12 | 湖南工业大学陶瓷研究所 | Ceramics coal-water slurry nozzle having two-way gradient function and method for making same |
| CN101554790A (en) * | 2009-05-18 | 2009-10-14 | 浙江大学 | Ultra-hard carbon film and preparation method thereof |
| CN101698362A (en) * | 2009-10-30 | 2010-04-28 | 华南理工大学 | Self-lubricating hard nanocomposite laminated coating and preparation method thereof |
| CN101712215A (en) * | 2009-10-30 | 2010-05-26 | 华南理工大学 | TiCN series nanometer gradient compound multi-layer coating and method for preparing same |
| US20120052276A1 (en) * | 2010-08-30 | 2012-03-01 | Hon Hai Precision Industry Co., Ltd. | Coating, article coated with coating, and method for manufacturing article |
| CN102390980A (en) * | 2011-08-12 | 2012-03-28 | 山东轻工业学院 | Gradient self-lubricating ceramic cutter material and preparation method thereof |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104846340A (en) * | 2015-05-29 | 2015-08-19 | 山东大学 | Mo-S-N-Cr self-lubricating gradient-coated cutting tool and preparation process thereof |
| CN104846340B (en) * | 2015-05-29 | 2017-06-16 | 山东大学 | Mo S N Cr self-lubricating gradient coating cutters and its preparation technology |
| CN105463372A (en) * | 2015-12-11 | 2016-04-06 | 西北有色金属研究院 | Preparation method of multi-layer composite super-thick self-lubricating hard coating |
| CN105463372B (en) * | 2015-12-11 | 2018-05-11 | 西北有色金属研究院 | A kind of preparation method of MULTILAYER COMPOSITE super thick self-lubricating hard coating |
| CN105714244A (en) * | 2016-03-30 | 2016-06-29 | 青岛滨海学院 | Titanium alloy surface ceramic/metal gradient high-temperature composite coating and preparing method thereof |
| CN111893421A (en) * | 2020-08-12 | 2020-11-06 | 常熟市绿一电器配件制造有限公司 | Wear-resistant mold surface nanocrystal pattern layer and preparation method thereof |
| CN112725792A (en) * | 2020-12-28 | 2021-04-30 | 成都美奢锐新材料有限公司 | Preparation method of chromium nitride-titanium carbonitride base metal ceramic composite coating |
| CN112725792B (en) * | 2020-12-28 | 2022-07-26 | 成都美奢锐新材料有限公司 | Preparation method of chromium nitride-titanium carbonitride base metal ceramic composite coating |
| CN115110033A (en) * | 2022-07-27 | 2022-09-27 | 南京真合材料科技有限公司 | Method for manufacturing super-hard film layer |
| CN115110033B (en) * | 2022-07-27 | 2024-01-23 | 南京真合材料科技有限公司 | Method for manufacturing superhard film layer |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103009697B (en) | 2014-09-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103009697B (en) | Self-lubricating gradient composite superhard film and preparation method thereof | |
| CN105112858B (en) | A kind of nano combined cutter coat of sandwich construction | |
| CN104131256B (en) | Multilayer nanometer composite cutting tool coating and preparation method thereof | |
| CN100506527C (en) | Metallic carbide/adamantine (MeC/DLC) nanometer multi-layer film material and preparation method thereof | |
| CN107523790B (en) | A kind of AlCrSiCuN nano laminated coating and preparation method thereof | |
| CN103160783B (en) | TiCuN nano composite coating and preparation method thereof | |
| CN101831608B (en) | Nano composite titanium-aluminum-silicon nitride cutter coating and preparation method thereof | |
| CN104928638A (en) | AlCrSiN-based multilayer nanometer composite cutter coating layer and preparation method thereof | |
| CN103212729B (en) | A kind of have NC cutting tool of CrAlTiN superlattice coating and preparation method thereof | |
| CN104508171A (en) | High performance tools exhibiting reduced crater wear in particular by dry machining operations | |
| CN101831615B (en) | Nano composite titanium-chromium-aluminum-silicon nitride cutter coat and preparation method thereof | |
| CN107747093B (en) | A kind of flexible hard composite coating and preparation method thereof and coated cutting tool | |
| CN105584148A (en) | Hard high-temperature resistant self-lubricating coating product and preparation method thereof | |
| CN103160781A (en) | Manufacture method of multilayer gradient nano-composite diamond film of surface of die steel | |
| CN105803393A (en) | Tough abrasion-resistant coating and preparation method thereof | |
| CN107937873A (en) | Transition metal boride coating, carbon transition metal boride composite coating, preparation method and application and the cutting element of carbon doping | |
| CN108251797A (en) | A kind of titanium alloy cutting cutter TiAlN/CrN laminated coatings and preparation method thereof | |
| CN103215544A (en) | Coating applied to thread forming tap | |
| CN105177498A (en) | AlCrSiON nano-composite cutting tool coating and preparation method thereof | |
| CN108977775B (en) | TiAlSiN coating cutter preparation process | |
| CN103938157B (en) | A kind of ZrNbAlN superlattice coating and preparation method | |
| CN102286726A (en) | Surface wear-resistance coating applied to automobile ordinary carbon steel movement friction pair | |
| CN104928639B (en) | A kind of superpower tough carbon based surfaces protective coating and preparation method thereof | |
| CN103741100B (en) | A kind of containing high silicon PVD hard coat technique | |
| KR101727420B1 (en) | Laminated coating film having excellent abrasion resistance |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |