CN105925946B - A method of using magnetron sputtering method TiN or CrN films are prepared in aluminum alloy surface - Google Patents

A method of using magnetron sputtering method TiN or CrN films are prepared in aluminum alloy surface Download PDF

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CN105925946B
CN105925946B CN201610294033.0A CN201610294033A CN105925946B CN 105925946 B CN105925946 B CN 105925946B CN 201610294033 A CN201610294033 A CN 201610294033A CN 105925946 B CN105925946 B CN 105925946B
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film
alloy matrix
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aluminum
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CN105925946A (en
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王亚男
陈东旭
陈琦
周艳文
张力元
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University of Science and Technology Liaoning USTL
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0617—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641—Nitrides

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

A method of using magnetron sputtering method TiN or CrN films are prepared in aluminum alloy surface.Plasma enhancing unbalanced magnetron sputter equipment is the present invention relates to the use of, using Ti, Cr metallic target, TiN the and CrN films of the atomic transition layer containing Ti and Cr are prepared respectively in aluminum alloy surface.The method not only ensure that the self-strength of alloy matrix aluminum, while also improve the hardness and corrosion resistance of aluminum alloy surface, and film and basal body binding force are good, and important reference frame can be provided for aluminum alloy surface modified technique.

Description

A method of using magnetron sputtering method TiN or CrN films are prepared in aluminum alloy surface
Technical field
The present invention relates to magnetron sputtering methods to prepare film applications, specifically a kind of to utilize magnetron sputtering method in 7A04 aluminium alloys The method that surface prepares TiN or CrN films.
Background technology
7A04 aluminium alloys have the characteristics that high intensity, low-density, are widely used in aviation field.In order to improve aluminium Ganoine thin film can be prepared on its surface in case hardness and corrosion resistance of alloy etc..Ganoine thin film not only remains basis material original Some excellent properties, while also improving mechanical property, high temperature stability performance, corrosion resistance and the abrasion resistance properties of material Deng.It can be said that the preparation of material surface ganoine thin film occupies particularly important status in modern industrial production.
Magnetron sputtering has been widely used as a kind of technology of preparing of surface hard film.Its technical characterstic exists In：First, in coating process, film thickness, deposition rate and film consistency etc. may be by change sputtering time and Sputtering power controls.In addition, when preparing film using magnetically controlled sputter method, the shape of target is unrestricted, can be as needed It is selected, to advantageously ensure that the quality of film.Studies have shown that the film prepared using magnetically controlled sputter method, with base The bond strength of body is relatively high, and can reach evaporation coating ten times are even higher.Further, since the energy of sputtering particle is higher, It can continue to spread around after hitting outer surface of matrix, to obtain fine and close and uniform ganoine thin film.
About ganoine thin film, there are more correlative study and report.But both at home and abroad about in aluminum alloy surface system The report of standby TiN or CrN films is less, can be for reference without relevant preparation technology parameter and standard.
Invention content
Technical problem to be solved by the invention is to provide a kind of using magnetron sputtering technique in 7A04 aluminum alloy surface systems The method of standby TiN or CrN films, makes the binding force of film and matrix increase, Thin Film Tissue even compact, hardness and corrosion resistance carry It is high.
To achieve the above object, the present invention is realized using following technical scheme：
A method of TiN or CrN films being prepared in aluminum alloy surface using magnetron sputtering method, are as follows：
1. cutting sample before plated film：Alloy matrix aluminum is cut by required specification；
2. pretreatment before sputtering：Sample is cleaned before plated film, is divided into two steps of exterior washings and internal washing；
1) exterior washings the specific steps are：Alloy matrix aluminum is placed in absolute ethyl alcohol, with 15~20 points of ultrasonic cleaning Clock, then alloy matrix aluminum is placed in deionized water, with ultrasonic cleaning 20~25 minutes, alloy matrix aluminum is finally taken out, it is fast Speed drying；
2) internal washing the specific steps are：Alloy matrix aluminum is linked into plasma enhancing unbalanced magnetron sputtering equipment cavity In, after cavity vacuumizes, preheating first is carried out 10~15 minutes to alloy matrix aluminum, backward vacuum chamber in be passed through argon gas, argon gas Flow is more than 200sccm, chamber pressure control be 10~30A and adds 50 in 0.5~1.0Pa, control tungsten filament electric current~ The pulsed bias of 150V, pulse power power is 100~300W, frequency 60KHz, generates enhancing plasma, to workpiece into Row plasma clean, scavenging period are controlled at 20~25 minutes or so；
3. four walls set rectangular metal target, metal targets respectively in plasma enhancing unbalanced magnetron sputtering equipment vacuum chamber For Ti or Cr；
4. plating film：
1) plating TiAlN thin film is as follows：
1. alloy matrix aluminum is once purged, reduce argon flow amount to 150~180sccm, adjust chamber pressure be 0.2~ 1.0Pa opens magnetic control target power supply, target is preheated under 2~4A target currents 10~15 minutes；
2. adjustment target current carries out 20~25 minutes pre-sputterings to 4~6A to target after preheating；
3. it is 1~5KW, frequency 60KHz, plated film 1~10 minute, in alloy matrix aluminum table to adjust target power output after pre-sputtering Face depositing Ti atom forms one layer of Ti atomic transition layer；
4. opening nitrogen flow to 5~15sccm, continue plated film 15~60 minutes；
5. adjusting argon gas and nitrogen flow, make argon flow amount/nitrogen flow (FAr/FN2) it is 1~5, target current is 4~6A, Chamber pressure is 0.4~0.6Pa, and substrate bias is -80~-100V, continues plated film 4~9 hours, aluminium alloy matrix surface deposition Go out TiAlN thin film；
2) plating CrN films are as follows：
1. alloy matrix aluminum is once purged, reduce argon flow amount to 150~180sccm, adjust chamber pressure be 0.2~ 1.0Pa opens magnetic control target power supply, target is preheated under 2~4A target currents 10~15 minutes；
2. adjustment target current carries out 20~25 minutes pre-sputterings to 4~6A to target after preheating；
3. it is 1~5KW, frequency 60KHz, plated film 1~10 minute, in alloy matrix aluminum table to adjust target power output after pre-sputtering Face deposits Cr atoms, forms one layer of Cr atomic transition layer；
4. opening nitrogen flow to 5~15sccm, continue plated film 15~60 minutes；
5. adjusting argon gas and nitrogen flow, make argon flow amount/nitrogen flow (FAr/FN2) it is 0.5~1.5, target current 4 ~5A, chamber pressure are 0.4~0.6Pa, and substrate bias is -80~-100V, continues plated film 4~9 hours, alloy matrix aluminum table Face deposits CrN films；
In the step 4, it is preferable that plating TiAlN thin film is as follows：
1. alloy matrix aluminum is once purged, argon flow amount is reduced to 150sccm, adjusting chamber pressure is 0.2~1.0Pa, Magnetic control target power supply is opened, target is preheated under 2A target currents 10 minutes；
2. adjustment target current carries out 20 minutes pre-sputterings to 4A to target after preheating；
3. it is 1~5KW, frequency 60KHz, plated film 1~10 minute, in alloy matrix aluminum table to adjust target power output after pre-sputtering Face depositing Ti atom forms one layer of Ti atomic transition layer；
4. opening nitrogen flow to 5~15sccm, continue plated film 15~60 minutes；
5. adjusting argon gas and nitrogen flow, make argon flow amount/nitrogen flow (FAr/FN2) it is 3.13, target current 4A, chamber Body pressure is 0.4Pa, and substrate bias is -80V, continues plated film 6 hours, aluminium alloy matrix surface deposits TiAlN thin film；
In the step 4, it is preferable that plating CrN films are as follows：
1. alloy matrix aluminum is once purged, argon flow amount is reduced to 150sccm, adjusting chamber pressure is 0.2~1.0Pa, Magnetic control target power supply is opened, target is preheated under 2A target currents 10 minutes；
2. adjustment target current carries out 20 minutes pre-sputterings to 5A to target after preheating；
3. it is 1~5KW, frequency 60KHz, plated film 1~10 minute, in alloy matrix aluminum table to adjust target power output after pre-sputtering Face deposits Cr atoms, forms one layer of Cr atomic transition layer；
4. opening nitrogen flow to 5~15sccm, continue plated film 15~60 minutes；
5. adjusting argon gas and nitrogen flow, make argon flow amount/nitrogen flow (FAr/FN2) it is 1.07, target current 5A, chamber Body pressure is 0.4Pa, and substrate bias is -80V, continues plated film 6 hours, aluminium alloy matrix surface deposits CrN films；
The argon gas and nitrogen gas purity is 99.99%.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention not only ensure that the self-strength of alloy matrix aluminum, and using magnetron sputtering technique in 7A04 aluminium alloys There is the atomic transition layer of Ti or Cr in TiN the or CrN films that surface is prepared, the binding force of film and matrix is made to increase accordingly Add, Thin Film Tissue even compact, hardness and corrosion resistance improve.Important reference frame is provided for surface modification technology.
Description of the drawings
Fig. 1 (a) is difference F in embodiment 1Ar/FN2Under the conditions of prepare TiAlN thin film and matrix binding force result.
Fig. 1 (b) is F in embodiment 1Ar/FN2When for 3.13, sputtering time be 6 hours, target current is 4A, TiAlN thin film is cut Surface scan electron microscopic picture.
Fig. 2 (a) is that the continuation of embodiment 1 plated film time is to prepare within 4 hours TiAlN thin film tissue topography scanning electron microscopic picture.
Fig. 2 (b) is that the continuation of embodiment 1 plated film time is to prepare within 6 hours TiAlN thin film tissue topography scanning electron microscopic picture.
Fig. 2 (c) is that the continuation of embodiment 1 plated film time is to prepare within 9 hours TiAlN thin film tissue topography scanning electron microscopic picture.
Fig. 3 is F in embodiment 1Ar/FN2When for 3.13, sputtering time be 6 hours, target current is 4A, TiAlN thin film and matrix Electrochemical tests measurement result.
Fig. 4 (a) is difference F in embodiment 2Ar/FN2Under the conditions of prepare the binding force result of CrN films and matrix.
Fig. 4 (b) is F in embodiment 2Ar/FN2When for 1.07, sputtering time be 6 hours, target current is 5A, film sections Scanning electron microscopic picture.
Fig. 5 is F in embodiment 2Ar/FN2When for 1.07, sputtering time be 6 hours, target current is 5A, CrN films and matrix Electrochemical tests measurement result.
Fig. 6 is the XRD results of the film object phase composition prepared in two embodiments of the invention.
Specific implementation mode
The specific implementation mode of the present invention is further illustrated below in conjunction with the accompanying drawings：
Embodiment 1
The present embodiment prepares TiAlN thin film using magnetron sputtering method in 7A04 aluminum alloy surfaces, and working gas selection purity is 99.99% argon gas and nitrogen；
It is as follows：
1. cutting sample before plated film：Cut Φ 45mm × 2mm alloy matrix aluminums；
2. pretreatment before sputtering：Sample is cleaned before plated film, is divided into two steps of exterior washings and internal washing；
1) exterior washings the specific steps are：Alloy matrix aluminum is placed in absolute ethyl alcohol, with 15~20 points of ultrasonic cleaning Clock, then alloy matrix aluminum is placed in deionized water, with ultrasonic cleaning 20~25 minutes, alloy matrix aluminum is finally taken out, it is fast Speed drying；
2) internal washing the specific steps are：Alloy matrix aluminum is linked into plasma enhancing unbalanced magnetron sputtering equipment cavity In, after cavity vacuumizes, preheating first is carried out 10~15 minutes to alloy matrix aluminum, backward vacuum chamber in be passed through argon gas, argon gas Flow is more than 200sccm, chamber pressure control be 10~30A and adds 50 in 0.5~1.0Pa, control tungsten filament electric current~ The pulsed bias of 150V, pulse power power is 100~300W, frequency 60KHz, generates enhancing plasma, to workpiece into Row plasma clean, scavenging period are controlled at 20~25 minutes or so；
3. in plasma enhancing unbalanced magnetron sputtering equipment vacuum chamber four walls set respectively 549mm × 180mm × 12.5mm rectangular metal targets, metal targets Ti；
4. plating TiAlN thin film is as follows：
1. alloy matrix aluminum is once purged, argon flow amount is reduced to 150sccm, adjusting chamber pressure is 0.2~1.0Pa, Magnetic control target power supply is opened, target is preheated under 2A target currents 10 minutes；
2. adjustment target current carries out 20 minutes pre-sputterings to 4~6A to target after preheating；
3. it is 1~5KW, frequency 60KHz, plated film 1~10 minute, in alloy matrix aluminum table to adjust target power output after pre-sputtering Face depositing Ti atom forms one layer of Ti atomic transition layer；
4. opening nitrogen flow to 5~15sccm, continue plated film 15~60 minutes；
5. adjusting argon gas and nitrogen flow, make argon flow amount/nitrogen flow (FAr/FN2) it is 1~5, target current is 4~6A, Chamber pressure is 0.4Pa, and substrate bias is -80V, continues plated film 4~9 hours, aluminium alloy matrix surface deposits TiAlN thin film；
Argon gas and nitrogen flow are adjusted, argon flow amount/nitrogen flow (F is madeAr/FN2) be respectively 1.46,1.57,2.63, 2.94,3.13,3.33,3.75,3.95,4.29 and 4.69；Target current is respectively 4A, 6A, and it is respectively 4 small to continue plated film time When, 6 hours, 9 hours, deposit TiAlN thin film in aluminium alloy matrix surface respectively.
Tissue topography, mechanical property and corrosion proof test are carried out to the film prepared.
As shown in Figure 1, the binding force of film is with FAr/FN2Increase and enhance, work as FAr/FN2For 3.13, sputtering time 6 When hour, target current are 4A, no matter in the junction of matrix and film, or in thin film growth process, all do not find apparent Hole, be in the form of a column growth.The TiAlN thin film dense uniform, transition zone are smooth and apparent.Film thickness reaches 9.29 μm, organizes shape Looks are ideal.
As shown in Fig. 2, when becoming 6 hours when sputtering time is small from 4, the tissue topography of film is by three prismatic (Fig. 2 (a)) Become spherical (Fig. 2 (b)), film quality improves.But Thin Film Tissue pattern becomes three prismatic again when sputtering time extends to 9 hours (Fig. 2 (c)).When sputtering time is 6 hours, the binding force and hardness highest of film respectively reach 21.76N and 337.24HV；When Film binding force and hardness are decreased to 12.77N and 192.11HV when sputtering time is 9 hours.
As shown in figure 3, being 4A, F in target currentAr/FN2After being sputtered 6 hours under the conditions of being 3.13, gained TiAlN thin film is certainly rotten It loses current potential and is higher than matrix, illustrate the thermodynamic tendency corroded after plated film reduction.Simultaneously anodic attack current density again smaller than Matrix, after illustrating plated film under this condition, corrosion resistance improves.
To sum up, the present embodiment optimization magnetron sputtering parameter is：It is 6 hours, target current 4A to control the magnetron sputtering time, FAr/FN2It is 3.13.At this point, the TiAlN thin film that surface compact, hardness are high, corrosion resistance is good, can very well be combined with matrix can be obtained.
Embodiment 2
The present embodiment prepares CrN films using magnetron sputtering method in 7A04 aluminum alloy surfaces, and working gas selection purity is 99.99% argon gas and nitrogen；
It is as follows：
1. cutting sample before plated film：Φ 50mm × 3mm alloy matrix aluminums are cut by required specification；
2. pretreatment before sputtering：Sample is cleaned before plated film, is divided into two steps of exterior washings and internal washing；
1) exterior washings the specific steps are：Alloy matrix aluminum is placed in absolute ethyl alcohol, with 15~20 points of ultrasonic cleaning Clock, then alloy matrix aluminum is placed in deionized water, with ultrasonic cleaning 20~25 minutes, alloy matrix aluminum is finally taken out, it is fast Speed drying；
2) internal washing the specific steps are：Alloy matrix aluminum is linked into plasma enhancing unbalanced magnetron sputtering equipment cavity In, after cavity vacuumizes, preheating first is carried out 10~15 minutes to alloy matrix aluminum, backward vacuum chamber in be passed through argon gas, argon gas Flow is more than 200sccm, chamber pressure control be 10~30A and adds 50 in 0.5~1.0Pa, control tungsten filament electric current~ The pulsed bias of 150V, pulse power power is 100~300W, frequency 60KHz, generates enhancing plasma, to workpiece into Row plasma clean, scavenging period are controlled at 20~25 minutes or so；
3. in plasma enhancing unbalanced magnetron sputtering equipment vacuum chamber four walls set respectively 549mm × 180mm × 12.5mm rectangular metal targets, metal targets Cr；
4. plating CrN films are as follows：
1. alloy matrix aluminum is once purged, argon flow amount is reduced to 150sccm, adjusting chamber pressure is 0.2~1.0Pa, Magnetic control target power supply is opened, target is preheated under 2A target currents 10 minutes；
2. adjustment target current carries out 20 minutes pre-sputterings to 4~6A to target after preheating；
3. it is 1~5KW, frequency 60KHz, plated film 1~10 minute, in alloy matrix aluminum table to adjust target power output after pre-sputtering Face deposits Cr atoms, forms one layer of Cr atomic transition layer；
4. opening nitrogen flow to 5~15sccm, continue plated film 15~60 minutes；
5. adjusting argon gas and nitrogen flow, make argon flow amount/nitrogen flow (FAr/FN2) it is 0.5~1.5, target current is 5A, chamber pressure 0.4Pa, substrate bias are -80, continue plated film 6 hours, alloy matrix aluminum deposits CrN films；
Argon gas and nitrogen flow are adjusted, argon flow amount/nitrogen flow (F is madeAr/FN2) be respectively 0.75,0.83,0.94, 1.07 and 1.25, alloy matrix aluminum deposits CrN films；
As shown in figure 4, the binding force of film is first with FAr/FN2Raising and enhance, work as FAr/FN2When being 1.07, film knot Resultant force is most strong.And work as FAr/FN2When being 1.25, film binding force declines.
Work as FAr/FN2When for 1.07, sputtering time be 6 hours, target current is 5A, the CrN Thin Film Tissues prepared cause the most It is close uniformly, with matrix binding ability is most strong, hardness highest.
FAr/FN2When increasing to 1.07 from 0.75, N, Cr atomic ratio in film decline, and film thickness increases, deposition rate Increase.And work as FAr/FN2When increasing to 1.25, N, Cr atomic ratio are begun to ramp up in film, and film thickness reduces, deposition rate drop It is low.
As shown in figure 5, being 5A, F in target currentAr/FN2After being sputtered 6 hours under the conditions of being 1.07, gained CrN films are certainly rotten It loses current potential and is higher than matrix, illustrate the thermodynamic tendency corroded after plated film reduction.Simultaneously anodic attack current density again smaller than Matrix, after illustrating plated film under this condition, corrosion resistance improves.
To sum up, the present embodiment optimization magnetron sputtering parameter is：It is 6 hours, target current 5A to control the magnetron sputtering time, FAr/FN2It is 1.07.At this point, the CrN films that surface compact, hardness are high, corrosion resistance is good, can very well be combined with matrix can be obtained.
In embodiment 1 of the present invention and embodiment 2, in order to make film be combined more preferably with matrix, in coating process In, the atomic transition layer first in one layer of pure Ti or pure Cr of substrate deposit, redeposition TiN or CrN films later.Such as Fig. 1 (b) With shown in Fig. 4 (b), there is transition zone in the film of preparation.Meanwhile film object phase composition measurement result is presented in Fig. 6.
Described above is only the basic principle of the present invention, is not imposed any restrictions to the present invention, every right according to the present invention It carries out equivalent variations and modification, within the scope of the art of this patent protection scheme.

Claims (1)

1. a kind of method being film-made in aluminum alloy surface using magnetron sputtering method, the film layer is TiN film, which is characterized in that film Thickness reaches 9.29 μm, and the binding force 21.76N of film, hardness 337.24HV, being organized as film is spherical, is as follows：
1) sample before cutting plated film：Alloy matrix aluminum is cut by required specification；
2) pretreatment before sputtering：Sample is cleaned before plated film, is divided into two steps of exterior washings and internal washing；
A. exterior washings the specific steps are：Alloy matrix aluminum is placed in absolute ethyl alcohol, with ultrasonic cleaning 15~20 minutes, then Alloy matrix aluminum is placed in deionized water, with ultrasonic cleaning 20~25 minutes, alloy matrix aluminum is finally taken out, blows rapidly It is dry；
B. internal washing the specific steps are：Alloy matrix aluminum is linked into plasma enhancing unbalanced magnetron sputtering equipment cavity, After cavity vacuumizes, preheating first is carried out 10~15 minutes to alloy matrix aluminum, backward vacuum chamber in be passed through argon gas, argon flow amount To be more than 200sccm, chamber pressure control is 10~30A and adds 50~150V's in 0.5~1.0Pa, control tungsten filament electric current Pulsed bias, pulse power power is 100~300W, frequency 60KHz, generates enhancing plasma, to workpiece carry out etc. from Daughter is cleaned, and scavenging period was controlled at 20~25 minutes；
3) four walls set rectangular metal target respectively in plasma enhancing unbalanced magnetron sputtering equipment vacuum chamber, and metal targets are Ti；
4) film is plated
1. alloy matrix aluminum is once purged, argon flow amount is reduced to 150sccm, adjusting chamber pressure is 0.2~1.0Pa, is opened Magnetic control target power supply, preheats target 10 minutes under 2A target currents；
2. adjustment target current carries out 20 minutes pre-sputterings to 4A to target after preheating；
3. adjusting target power output after pre-sputtering as 1~5KW, frequency 60KHz, plated film 1~10 minute sinks in aluminium alloy matrix surface Product Ti atoms, form one layer of Ti atomic transition layer；
4. opening nitrogen flow to 5~15sccm, continue plated film 15~60 minutes；
5. adjusting argon gas and nitrogen flow, make argon flow amount/nitrogen flow (FAr/FN2) it is 3.13, target current 4A, chamber pressure For 0.4Pa, substrate bias is -80V, continues plated film 6 hours, aluminium alloy matrix surface deposits TiAlN thin film.
CN201610294033.0A 2016-05-06 2016-05-06 A method of using magnetron sputtering method TiN or CrN films are prepared in aluminum alloy surface Expired - Fee Related CN105925946B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08296039A (en) * 1995-04-25 1996-11-12 Nippon Steel Corp Production of iron-nickel alloy thin sheet with aluminum thin film coated surface
CN104862657A (en) * 2015-04-17 2015-08-26 东北大学 Titanium alloy surface nano Ti/TiN gradient film and preparation method thereof
CN104878359A (en) * 2015-06-12 2015-09-02 浙江金盾链条制造有限公司 High-hardness and high-abrasion-resisting TiA1N/ZrSiN nano-structure protective coating and preparation method thereof
CN105177498A (en) * 2015-05-21 2015-12-23 广东工业大学 AlCrSiON nano-composite cutting tool coating and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08296039A (en) * 1995-04-25 1996-11-12 Nippon Steel Corp Production of iron-nickel alloy thin sheet with aluminum thin film coated surface
CN104862657A (en) * 2015-04-17 2015-08-26 东北大学 Titanium alloy surface nano Ti/TiN gradient film and preparation method thereof
CN105177498A (en) * 2015-05-21 2015-12-23 广东工业大学 AlCrSiON nano-composite cutting tool coating and preparation method thereof
CN104878359A (en) * 2015-06-12 2015-09-02 浙江金盾链条制造有限公司 High-hardness and high-abrasion-resisting TiA1N/ZrSiN nano-structure protective coating and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
ZL101A铝合金表面磁控溅射镀TiN薄膜的研究;吴义志;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20110815;第15-23,31-40页 *

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