CN106702337B - A kind of hard coat stress in-situ control method - Google Patents

A kind of hard coat stress in-situ control method Download PDF

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CN106702337B
CN106702337B CN201611132504.4A CN201611132504A CN106702337B CN 106702337 B CN106702337 B CN 106702337B CN 201611132504 A CN201611132504 A CN 201611132504A CN 106702337 B CN106702337 B CN 106702337B
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temperature
stress
hard coat
control method
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CN106702337A (en
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庞晓露
白燕芸
高克玮
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University of Science and Technology Beijing USTB
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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
    • 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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
    • C23C14/025—Metallic sublayers
    • 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
    • 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
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering

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

Abstract

The present invention relates to technical field of metal material surface modification, provide a kind of hard coat stress in-situ control method；Technique is as follows: being cleaned by ultrasonic to the metallic matrix of polishing, is fixed in magnetron sputtering vacuum chamber；It is evacuated to 5.0 × 10‑3Pa, while heated substrate is to temperature T1；It is passed through Ar deposited metal transition zone, stops deposition after transition region thickness reaches requirement；Substrate temperature is reduced to T2, it is passed through N2Deposited nitride film, film thickness stop deposition after reaching requirement；It is cooled to room temperature.The residual stress in film that the method for the present invention obtains is by metal material and nitride film thermal expansion coefficient, and mismatch between intermediate metal and nitride film and thermal stress generate, the present invention does not need substrate material surface pretreatment and post-processing, improve film-substrate cohesion, there is numerical value higher residual compressive stress appropriate, simple process in obtained film.

Description

A kind of hard coat stress in-situ control method
Technical field
The present invention relates to technical field of metal material surface modification, in particular to a kind of hard coat stress in-situ control side Method.
Background technique
Metal material is due to performances such as its excellent corrosion resistance, high intensity, in aerospace, petrochemical industry, automobile, biology Medicine and other fields have a good application prospect.However its weaker wear Characteristics and surface imperfection largely effect on Application in engineering.In order to improve anti-friction abrasion and the fatigue behaviour of material, sandblasting is industrially generallyd use now The method of shot-peening generates compressive stress layer in metal material surface, or makes metal material surface using laser blast wave Plastic deformation forms the hardened layer with the distribution of appropriate residual compressive stress, Lai Tigao fatigue life and anti-friction wear resistance, and This method not only needs to increase in process of production processing links, but also the sample surfaces after sandblasting bead are easy to produce Damage defect, that is, increasing cost again has the possible risk of increase failure during materials'use.
It in metal material surface plated film is to carry out the modified important means in surface using physical deposition method.Ganoine thin film tool There are high-temperature stability, high rigidity, low conductivity, low-friction coefficient, is led in manufacturing industry, biological medicine, aerospace etc. There is important application in domain.But since ganoine thin film is fragile material compared to metallic matrix, residual stress is high, during military service It is also easy to produce defect, causes the failure of material, so the residual pressure for how introducing appropriate numerical value in ganoine thin film deposition process is answered Power, improves the ability of film anti-friction abrasion and fatigue, and the preparation preferable product of mechanical property becomes the emphasis of research and development.
Application No. is 201310752241.7 Chinese patents to propose a kind of PVD preparation work for adjusting TiW membrane stress Substrate to be processed is placed on pedestal by skill, is passed through the hydrogen of first flow, is applied deposition power to DC power supply and is kept the One preset time stops applying DC power supply deposition power and keeps the second preset time, and repeated deposition step and stopping are heavy Product step is until reach required film thickness.The PVD preparation process provided by the invention for adjusting TiW membrane stress, is to pass through The first preset time of deposition is adjusted during the preparation process and stops the second preset time of deposition to adjust membrane stress, is obtained The TiW film controllable to stress.
Application No. is 200810186291.2 Chinese patents to propose a kind of membrane stress control method, is splashed using magnetic control It penetrates film deposition techniques and deposits tin thin film and aluminium film on the polymer film, then vacuumize and heat, make tin thin film and aluminium Sn-Al alloy is formed between film, lattice is made to generate expansion distortions, and the stress to introduce opposite is answered with already existing intrinsic pressure Power contends with.The method is adaptable, and application is wide.
Application No. is 201310170301.4 Chinese patents to provide a kind of preparation side of high pressure stress silicon nitride film Method on the semiconductor device after cvd nitride silicon thin film, closes bias power source, the residual gas in reaction chamber is evacuated, protects It holds that reaction temperature is constant, the protective gas containing argon gas will be passed through in reaction chamber, open direct current power source, set dc power, It is passed through the mixed gas of the enhancing compression containing argon gas simultaneously, silicon nitride film is post-processed, forms high pressure stress nitrogen SiClx film.Last handling process is to complete in situ on the basis of deposition process, and post-processing selectivity is strong, reduces manufacture The complexity of technique.
Studies have shown that the temperature for changing matrix can influence the structure, residual stress and mechanical property of film.Existing research Person points out that substrate temperature when improving ZnO film deposition causes (002) peak ZnO to deflect to desired angle, shows remaining in film The reduction of compression.Due to the hot mispairing between film and matrix, higher film deposition temperature would generally obtain higher residual Residue stress.
Summary of the invention
The object of the invention is to overcome the deficiencies of existing technologies, a kind of hard coat stress in-situ control side is provided Method is modified metal material surface, and this method uses physical deposition techniques, prepares the hard with appropriate residual compressive stress Film.
A kind of hard coat stress in-situ control method of the present invention, including in metal base surface deposited metal transition zone Step and the temperature T the deposited nitride film on the intermediate metal the step of, when depositing the intermediate metal1It is high Temperature T when depositing the nitride film2。
Further, include the following steps:
Step 1: being cleaned by ultrasonic to the metallic matrix polished；
Step 2: the metallic matrix is fixed in magnetron sputtering vacuum chamber, it is evacuated to 5.0 × 10-3Pa adds simultaneously Hot basal body is to temperature T1；It is passed through Ar and deposits the intermediate metal, the stopping when the metal transition layer thickness reaches setting value Deposition；
Step 3: reducing the metallic matrix temperature to T2, T1>T2；It is passed through N2Deposit the nitride film, the nitrogen Compound film thickness stops deposition when reaching setting value, is cooled to room temperature to obtain the final product.
Further, the metallic matrix is TC4 titanium alloy, and the intermediate metal is CrAl transition zone, the nitridation Object film is CrAlN film.
Further, the intermediate metal with a thickness of 70nm, depositing temperature T1It is 300 DEG C；The nitride film With a thickness of 1.5 μm -2.6 μm, depositing temperature T2It is 100 DEG C.
Further, in step 1, the ultrasonic cleaning, cleaning solution used is acetone, scavenging period 5-15min.
Further, in step 2, the flow for being passed through Ar is 30sccm；In step 3, it is passed through N2Flow be 5sccm.
Further, in step 3, CrAlN film crystal structure is column crystal, sedimentation time 180min-300min.
Further, film deposition apparatus is rf magnetron sputtering coating machine, and target used is CrAl metallic target, Cr:Al =30:70at%.
The invention has the benefit that
(1) in metal material surface Direct precipitation ganoine thin film, material surface pretreatment, simple process are not needed；
(2) present invention deposits one layer of transition zone first on matrix, improves film-substrate cohesion；
(3) film residual stress value is improved by changing the temperature of deposition transition zone, is not needed after depositing ganoine thin film Preferable film quality and mechanical property can be reached by post-processing, and without departing from vacuum environment in coating process, film quality is high；
(4) preparation facilities of the invention is simple, controllable, low in cost, realizes very well；
(5) film plating process simple process of the invention, pollution-free, gained ganoine thin film structure is uniform column crystal, at This is low；
(6) present invention, which has the development of metal surface properties modification, inspires meaning.
Detailed description of the invention
Fig. 1 show the CrAlN film sections FESEM shape appearance figure that sedimentation time in the embodiment of the present invention is 300min.
Fig. 2 show the CrAlN film residual stress value figure of different sedimentation times and transition zone depositing temperature.
Fig. 3 show CrAlN film scratch experiment load-friction resistance curve, and CrAlN film sedimentation time is 180min, 1.5 μm of film thickness, TC4 matrix.
Fig. 4 show CrAlN film scratch experiment load-friction resistance curve, and CrAlN film sedimentation time is 240min, 2 μm of film thickness, TC4 matrix.
Fig. 5 show CrAlN film scratch experiment load-friction resistance curve, and CrAlN film sedimentation time is 300min, 2.6 μm of film thickness, TC4 matrix.
Fig. 6 show CrAlN film scratch appearance in early stage figure, 100 DEG C of CrAl transition zone depositing temperature, when CrAlN silence Between 300min, TC4 matrix.
Fig. 7 show CrAlN film scratch mid-term shape appearance figure, 100 DEG C of CrAl transition zone depositing temperature, when CrAlN silence Between 300min, TC4 matrix.
Fig. 8 show CrAlN film scratch appearance in early stage figure, 300 DEG C of CrAl transition zone depositing temperature, when CrAlN silence Between 300min, TC4 matrix.
Fig. 9 show CrAlN film scratch mid-term shape appearance figure, 300 DEG C of CrAl transition zone depositing temperature, when CrAlN silence Between 300min, TC4 matrix.
Figure 10 show metallic matrix, intermediate metal and ceramic film residual stress schematic diagram.
Figure 11 show intermediate metal depositing temperature be higher than ceramic film when, metallic matrix, intermediate metal and Ceramic film residual stress schematic diagram.
In figure: it is 100 DEG C that 100-100, which represents CrAl transition zone depositing temperature, and CrAlN film deposition temperature is 100 DEG C；
It is 300 DEG C that 300-100, which represents CrAl transition zone depositing temperature, and CrAlN film deposition temperature is 100 DEG C；
TC4 and TC21 is basis material.
Specific embodiment
Below in conjunction with specific attached drawing the present invention is described in detail specific embodiment.It should be noted that in following embodiments The combination of the technical characteristic or technical characteristic of description is not construed as isolated, they can be combined with each other to reaching To superior technique effect.In the drawings of the following embodiments, the identical label that each attached drawing occurs represent identical feature or Person's component, can be apply to different embodiments.
The thermal expansion coefficient of metal material is more ceramic big.Such as: such as iron 12 × 10-6/ DEG C, austenitic stainless steel be 1.6 × 10-6/ DEG C, ordinary carbon steel, martensitic stain less steel thermal expansion coefficient be 1.01 × 10-6/ DEG C, aluminium alloy is about 22-25 × 10-6/ DEG C, nickel-chromium steel is about 13-15 × 10-6/ DEG C, titanium alloy is about 8.5-9.7 × 10-6/℃.And the thermal expansion coefficient very little of ceramics, Some ceramics at an elevated temperature, hardly happen geometrical property variation, thermal expansion coefficient is close to 0.
As shown in Figure 10, in low temperature depositing transition zone and ceramic film, (in this application, " ceramic film " refers to nitridation Object film layer) room temperature is cooled to later, due to the difference of metal material and ceramic membrane thermal expansion coefficient, metallic matrix and metal The deformation of transition zone is big, can generate shear stress with the interface of ceramic film, is transmitted in film layer and translates into pressure and answer Power.When the depositing temperature of transition zone is higher than ceramic film, as shown in figure 11, also have in transition zone by the same token residual Overbottom pressure stress generates, and passes to ceramic film.Again since the mismatch of intermediate metal and ceramic film increases, heat is answered Power increases, therefore the residual compressive stress of gained film is higher than the film that transition zone and ceramic film are deposited at identical temperature.
The embodiment of the present invention deposits one layer of intermediate metal before metal base surface deposits ganoine thin film first.It is heavy The temperature of product transition zone is higher, then cools down, and deposits ganoine thin film layer at low temperature.The ganoine thin film layer of deposition is nitride.
A kind of hard coat stress in-situ control method of the embodiment of the present invention, is included in metal base surface deposited metal mistake The step of crossing layer and the temperature the deposited nitride film on the intermediate metal the step of, when depositing the intermediate metal Spend T1Temperature T when higher than the deposition nitride film2。
Preferably, include the following steps:
Step 1: being cleaned by ultrasonic to the metallic matrix polished；
Step 2: the metallic matrix is fixed in magnetron sputtering vacuum chamber, it is evacuated to 5.0 × 10-3Pa adds simultaneously Hot basal body is to temperature T1；It is passed through Ar and deposits the intermediate metal, the stopping when the metal transition layer thickness reaches setting value Deposition；
Step 3: reducing the metallic matrix temperature to T2, T1>T2；It is passed through N2Deposit the nitride film, the nitrogen Compound film thickness stops deposition when reaching setting value, is cooled to room temperature to obtain the final product.
Metal material (metallic matrix) of the present invention, can be a variety of different metals, such as copper, iron, chromium, no Generality is lost, only selects titanium alloy as example in embodiment, it should not be using the content of embodiment as the scope of the present invention Limitation.
The metallic matrix selects TC4 titanium alloy, and the intermediate metal is CrAl transition zone, and the nitride film is CrAlN film.In order to make intermediate metal and nitride film layer that there is better binding force, it is preferred that in intermediate metal Metallic element it is identical as metallic element included in nitride film；For example, intermediate metal and nitridation in the present embodiment The metallic element of object film is CrAl.
The intermediate metal with a thickness of 70nm, depositing temperature T1It is 300 DEG C；The nitride film is with a thickness of 1.5 μ M-2.6 μm, depositing temperature T2It is 100 DEG C.
In step 1, the ultrasonic cleaning, cleaning solution used is acetone, scavenging period 5-15min.
In step 2, the flow for being passed through Ar is 30.0sccm；In step 3, it is passed through N2Flow be 5.0sccm.
In step 3, CrAlN film crystal structure is column crystal, sedimentation time 180min-300min.
Film deposition apparatus be rf magnetron sputtering coating machine, target used be CrAl metallic target, Cr:Al=30: 70at%.
Embodiment
In the present embodiment, CrAl transition zone is deposited first in TC4 titanium alloy surface, depositing temperature is set in 300 DEG C, transition Thickness degree is about 70nm.Then temperature is reduced, control CrAlN film deposition temperature is 100 DEG C, and film thickness is respectively 1.5 μm, 2 μm and 2.6 μm.Obtain the titanium alloy surface coating with higher residual stresses.
Use equipment:
Film deposition apparatus is rf magnetron sputtering coating machine, and CrAl metallic target is connected with radio-frequency power supply, cold by recycling But water is cooling.Sample is fixed on the specimen holder above vacuum chamber, and rotation is driven by motor in specimen holder in film deposition process, To guarantee the uniformity of deposition.Thermocouple is used to measure the temperature of matrix in film deposition process.Vacuum chamber is cylinder, is connect Ground is to guarantee the electroneutral of system.
The rf magnetron sputtering plated film mode, corresponding technological parameter are as follows:
Operating air pressure 0.28Pa；Power 300W；Automatic bias 500V；Ar flow 30sccm；N2Flow 5sccm；
Target used is CrAl metallic target, Cr:Al=30:70at%.
Nitride film preparation method includes the following steps:
(1) the TC4 titanium alloy surface of polishing is cleaned by ultrasonic, cleaning solution is acetone, scavenging period 10min.Gu Random sample product are evacuated to 5.0 × 10 in vacuum chamber, being warming up to 300 DEG C-3Pa。
(2) control Ar flow is 30.0sccm, according to parameter deposition film shown in table 1, CrAl transition zone sedimentation time Then 10min is cooled to 100 DEG C, deposit CrAlN film, N2Flow control is 5.0sccm, and sedimentation time is set as 180min, 240min and 300min is cooled to room temperature after plated film, takes out sample, obtain three cluster film samples.
1 coating process parameter of table
(3) film sections pattern is observed using FESEM, measures film thickness.CrAlN film crystal structure is column crystal, Film thickness corresponding to sedimentation time difference (180min, 240min, 300min) is respectively 1.5 μm, 2 μm and 2.6 μm.
Film residual stress is measured using XRD method.It can be seen that, CrAlN film is residual from 2 experimental data of table and Fig. 3 Residue stress is both less than zero, is expressed as compression, and there are the film sample of 300 DEG C of high temperature deposition CrAl transition zones bigger remnants to answer Power, and the residual compressive stress of the film sample of 100 DEG C of low temperature deposition CrAl transition zones is smaller.Illustrate to deposit CrAl under hot conditions Transition zone has positive effect to the generation of film residual stress, so that the mechanical property to film plays active influence.
2 CrAlN film residual stress value of table
Thin film mechanical performance is measured using scarification.It can see from scratch experiment load-friction resistance curve, in film In the case that thickness is different, the critical load of the CrAlN film of 300 DEG C of high temperature deposition CrAl transition zones is deposited than 100 DEG C of low temperature The critical load of the CrAlN film of CrAl transition zone is big, it was demonstrated that improves the depositing temperature of film transition layer to different-thickness Film all has the function of improving thin film mechanical performance.
The invention has the benefit that
(1) in metal material surface Direct precipitation ganoine thin film, material surface pretreatment, simple process are not needed；
(2) present invention deposits one layer of transition zone first on matrix, improves film-substrate cohesion；
(3) film residual stress value is improved by changing the temperature of deposition transition zone, is not needed after depositing ganoine thin film Preferable film quality and mechanical property can be reached by post-processing, and without departing from vacuum environment in coating process, film quality is high；
(4) preparation facilities of the invention is simple, controllable, low in cost, realizes very well；
(5) film plating process simple process of the invention, pollution-free, gained ganoine thin film structure is uniform column crystal, at This is low；
(6) present invention, which has the development of metal surface properties modification, inspires meaning.
Although having been presented for several embodiments of the present invention herein, it will be appreciated by those of skill in the art that Without departing from the spirit of the invention, the embodiments herein can be changed.Above-described embodiment is only exemplary, no It should be using the embodiments herein as the restriction of interest field of the present invention.

Claims (7)

1. a kind of hard coat stress in-situ control method, which is characterized in that be included in metal base surface deposited metal transition The step of layer and the temperature the deposited nitride film on the intermediate metal the step of, when depositing the intermediate metal T1Temperature T when higher than the deposition nitride film2；The metallic matrix is TC4 titanium alloy, and the intermediate metal is CrAl transition zone, the nitride film are CrAlN film.
2. hard coat stress in-situ control method as described in claim 1, which comprises the steps of:
Step 1: being cleaned by ultrasonic to the metallic matrix polished；
Step 2: the metallic matrix is fixed in magnetron sputtering vacuum chamber, it is evacuated to 5.0 × 10-3Pa, while heating base Body is to temperature T1；It is passed through Ar and deposits the intermediate metal, stop deposition when the metal transition layer thickness reaches setting value；
Step 3: reducing the metallic matrix temperature to T2, T1>T2；It is passed through N2The nitride film is deposited, the nitride is thin Film thickness stops deposition when reaching setting value, is cooled to room temperature to obtain the final product.
3. hard coat stress in-situ control method as described in claim 1, which is characterized in that the thickness of the intermediate metal Degree is 70nm, depositing temperature T1It is 300 DEG C；The nitride film is with a thickness of 1.5 μm -2.6 μm, depositing temperature T2It is 100 DEG C.
4. hard coat stress in-situ control method as claimed in claim 2, which is characterized in that in step 1, the ultrasound Cleaning, cleaning solution used are acetone, scavenging period 5-15min.
5. hard coat stress in-situ control method as claimed in claim 2, which is characterized in that in step 2, be passed through Ar's Flow is 30.0sccm；In step 3, it is passed through N2Flow be 5.0sccm.
6. hard coat stress in-situ control method as claimed in claim 2, which is characterized in that in step 3, CrAlN film Crystal structure is column crystal, sedimentation time 180min-300min.
7. hard coat stress in-situ control method as described in claim 1, which is characterized in that film deposition apparatus is radio frequency Magnetron sputtering coater, target used are CrAl metallic target, Cr:Al=30:70at%.
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CN103022290A (en) * 2012-12-19 2013-04-03 湘能华磊光电股份有限公司 Light-emitting diode (LED) epitaxial structure with quaternary InAlGaN and method for preparing same
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