CN108286005A - A kind of preparation method of the tungsten nickel of rare-earth mamem layer - Google Patents

A kind of preparation method of the tungsten nickel of rare-earth mamem layer Download PDF

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Publication number
CN108286005A
CN108286005A CN201810185132.4A CN201810185132A CN108286005A CN 108286005 A CN108286005 A CN 108286005A CN 201810185132 A CN201810185132 A CN 201810185132A CN 108286005 A CN108286005 A CN 108286005A
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rare
earth
mamem
nickel
layer
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瞿凌飞
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
    • C22C29/08—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on tungsten carbide
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
    • C22C29/067—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds comprising a particular metallic binder
    • 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
    • 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
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • 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
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2204/00—End product comprising different layers, coatings or parts of cermet

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

Abstract

The invention discloses a kind of preparation methods of the tungsten nickel of rare-earth mamem layer, tungsten nickel material prepared by this method solves the problems, such as often occur " nickel pond " and hole in traditional fine grained cemented carbide preparation process, the method that the present invention uses magnetron sputtering, and using the means of zerolling, rare-earth mamem layer is formed on tungsten nickel surface, it can will promote the yield strength of the alloy so that the surface even compact of tungsten nickel material, film substrate bond strength height, good mechanical performance.

Description

A kind of preparation method of the tungsten nickel of rare-earth mamem layer
Technical field
The present invention relates to dielectric substance manufacturing fields, and in particular to a kind of system of the tungsten nickel of rare-earth mamem layer Preparation Method.
Background technology
WC-Ni hard alloy has high intensity, high rigidity, excellent abrasion resistance, heat resistance and good corrosion resistance The features such as, therefore it is widely used in the working environments such as high pressure, high rotating speed, high temperature, Korrosionsmedium.Since Ni belongs to face-centered cubic (F.c.c) crystallographic system, plasticity is fine, and plastic deformation is easy to happen during wet-milling, forms the Ni powder balls of sheet.Industrial production with Ni will be grown as the Ball-milling Time of the hard alloy of binder, even in this way, cannot guarantee that the uniform refinement of Ni powder, this is Based on Ni powder, there is the Refining Mechanisms completely different with Co powder.
Mainly WC grain is refined, by stringent technology controlling and process, reduces hole by adding alloying element in the prior art Improve the performance of WC-Ni hard alloy with the methods of defect.The WC-Ni mixtures prepared using conventional method are in vacuum-sintering Under the conditions of often there is " nickel pond " and hole." nickel pond " and hole can seriously affect the comprehensive performance of alloy, such as intensity, wear-resisting Property, corrosion resistance etc..
Marmem（Shape Memory Alloy, SMA）Refer to after suitably deforming, in certain physical condition Change the alloy for descending energy automatic working and restoring shape before deforming.Marmem is because it is with higher restorability shape Become, it has also become a kind of important functional material is applied widely.NiTi system shape memory has reminiscence original shape, nothing Magnetism, wear-and corrosion-resistant, high temperature resistant, avirulent feature.But, the yield strength of current marmem generally exists 700MPa or less.
Invention content
The present invention provides a kind of preparation method of the tungsten nickel of rare-earth mamem layer, tungsten nickel material prepared by this method Solve the problems, such as often occur " nickel pond " and hole in traditional fine grained cemented carbide preparation process, the present invention is using magnetron sputtering Method, and using the means of zerolling, form rare-earth mamem layer on tungsten nickel surface, can will promote the alloy Yield strength so that the surface even compact of tungsten nickel material, film substrate bond strength height, good mechanical performance.
To achieve the goals above, the present invention provides a kind of preparation method of the tungsten nickel of rare-earth mamem layer, This method comprises the following steps：
（1）Prepare matrix
Mixed powder is prepared by following composition by weight
Tungsten carbide, 90.1%-92.8%, 0.8-1 μm of Fisher particle size；
Nickel powder, 5%-6%, 0.5-1.0 μm of Fisher particle size；
Chromium carbide, surplus；
The mixed powder of said ratio is subjected to wet-milling；Wherein Ball-milling Time Discrete control；First carbide powder and additive are carbonized Ball grinding cylinder wet-milling 12-16 hours is added in chromium, adds nickel powder wet-milling 14-18 hours；
The mixture slurry drying that ball milling is finished；
Dry pack is pressed into the compacting product of required shape；
Compacting product are placed on high temperature sintering in sintering furnace, sintering temperature is 1450-1470 DEG C, soaking time 70-90min, sintering Pressure is 4.5-5.0Mpa, obtains tungsten nickel matrix；
（2）Substrate pretreated
Described matrix pre-processes, and can be ground polishing, ultrasonic cleaning and ion source cleaning successively；
（3）Prepare rare-earth mamem target
The rare-earth mamem target is made of titanium, nickel, aluminium, yttrium, chromium, element silicon；
Include following component by weight：55-65 parts of titanium, 10-12 parts of nickel；6-9 parts of aluminium；1-3 parts of yttrium, 4-6 parts of chromium；1-2 parts of silicon；
Rare-earth mamem target is prepared using smelting process；
（4）Using above-mentioned alloy target material, using magnetically controlled sputter method, the rare-earth mamem of film-form is formed on above-mentioned matrix Layer：
It is evacuated to 10-4Pa or more is filled with nitrogen, is then evacuated to 10 again-4Pa, adjustment operating voltage are 500V, and sputtering accounts for Sky ratio 65-68%, proceeds by sputtering sedimentation, and control thickness is the 150-250 μm of rare-earth mamem layer for obtaining film-form；
Start rolling machine system, sets the speed ratio of top and bottom rolls as 1.2-1.5, set each rolling deformation amount as 2-3%；It sets low The speed of fast roller is 0.05-0.1m/s, starts the operation of rolling with the tungsten nickel of rare-earth mamem layer；Once rolled Afterwards, repeat to roll 3-5 times, in the operation of rolling, it is -30 to -20 degrees Celsius to keep environment temperature；At 150-200 degrees Celsius Low Temperature Heat Treatment 1-2h is carried out, product is obtained.
The present invention has following advantages：
（1）Tungsten nickel material prepared by this method, which solves, often there is " nickel pond " and hole in traditional fine grained cemented carbide preparation process The problem of, multi-layer film structure can not only hinder the migration of Lacking oxygen；
（2）The method that the present invention uses magnetron sputtering, and using the means of zerolling, rare earth note is formed on tungsten nickel surface Recall alloy-layer, can will promote the yield strength of the alloy so that surface even compact, the film substrate bond strength of tungsten nickel material High, good mechanical performance.
Specific implementation mode
Embodiment one
Mixed powder is prepared by following composition by weight：
Tungsten carbide, 90.1%, 0.8-1 μm of Fisher particle size；
Nickel powder, 5%, 0.5-1.0 μm of Fisher particle size；
Chromium carbide, surplus.
The mixed powder of said ratio is subjected to wet-milling；Wherein Ball-milling Time Discrete control；First by carbide powder and additive Ball grinding cylinder wet-milling 12 hours is added in chromium carbide, adds nickel powder wet-milling 14 hours.
The mixture slurry drying that ball milling is finished.
Dry pack is pressed into the compacting product of required shape.
Compacting product are placed on high temperature sintering in sintering furnace, sintering temperature is 1450 DEG C, soaking time 70-90min, sintering Pressure is 4.5Mpa, obtains tungsten nickel matrix.
Substrate pretreated, described matrix pretreatment can be ground polishing, ultrasonic cleaning and ion source cleaning successively.Institute Grinding and polishing is stated, can matrix be first subjected to corase grinding 10min on the boart boart wheel disc of 600 mesh, then in the Buddha's warrior attendant of 1200 mesh Fine grinding 10min is carried out on stone sand wheel disc, then be polished with the diamond polishing powder of W2.5 it is uniformly bright to specimen surface, it is described It is cleaned by ultrasonic, the matrix after grinding and polishing can be cleaned in the following order, it is clear that acetone is cleaned by ultrasonic 5min → absolute ethyl alcohol ultrasound It is for use to wash 5min → drying, ion source cleaning can be used hall ion source and carry out cleaning 5min to matrix, and pressure is 2 × 10-2Pa, substrate temperature are 300 DEG C, and argon gas flux is 10sccm, and bias is -100V, cathode current 29.5A, and cathode voltage is 19V, anode current 7A, anode voltage 80V improve depositing coating to remove adsorbed gas and the impurity of matrix surface With the bond strength and quality of forming film of matrix.
Rare-earth mamem target is prepared, which is made of titanium, nickel, aluminium, yttrium, chromium, element silicon；It presses Parts by weight include following component：55 parts of titanium, 10 parts of nickel；6 parts of aluminium；1 part of yttrium, 4 parts of chromium；1 part of silicon；It is prepared using smelting process dilute Native memorial alloy target.
Using above-mentioned alloy target material, using magnetically controlled sputter method, the rare earth memory that film-form is formed on above-mentioned matrix is closed Layer gold：It is evacuated to 10-4Pa or more is filled with nitrogen, is then evacuated to 10 again-4Pa, adjustment operating voltage are 500V, sputtering Duty ratio 65%, proceeds by sputtering sedimentation, and control thickness is 150 μm of rare-earth mamem layers for obtaining film-form.
Start rolling machine system, sets the speed ratios of top and bottom rolls as 1.2, set each rolling deformation amount as 2%；Set low speed The speed of roller is 0.05m/s, starts the operation of rolling with the tungsten nickel of rare-earth mamem layer；After primary rolling, weight Rolling 3 times is carried out again, and in the operation of rolling, it is -30 to -20 degrees Celsius to keep environment temperature；It is carried out at Low Temperature Thermal at 150 degrees Celsius 1h is managed, product is obtained.
Embodiment two
Mixed powder is prepared by following composition by weight：
Tungsten carbide, 92.8%, 0.8-1 μm of Fisher particle size；
Nickel powder, 6%, 0.5-1.0 μm of Fisher particle size；
Chromium carbide, surplus.
The mixed powder of said ratio is subjected to wet-milling；Wherein Ball-milling Time Discrete control；First by carbide powder and additive Ball grinding cylinder wet-milling 16 hours is added in chromium carbide, adds nickel powder wet-milling 18 hours.
The mixture slurry drying that ball milling is finished.
Dry pack is pressed into the compacting product of required shape.
Compacting product are placed on high temperature sintering in sintering furnace, sintering temperature is 1470 DEG C, soaking time 90min, sintering pressure For 5.0Mpa, tungsten nickel matrix is obtained.
Substrate pretreated, described matrix pretreatment can be ground polishing, ultrasonic cleaning and ion source cleaning successively.Institute Grinding and polishing is stated, can matrix be first subjected to corase grinding 10min on the boart boart wheel disc of 600 mesh, then in the Buddha's warrior attendant of 1200 mesh Fine grinding 10min is carried out on stone sand wheel disc, then be polished with the diamond polishing powder of W2.5 it is uniformly bright to specimen surface, it is described It is cleaned by ultrasonic, the matrix after grinding and polishing can be cleaned in the following order, it is clear that acetone is cleaned by ultrasonic 5min → absolute ethyl alcohol ultrasound It is for use to wash 5min → drying, ion source cleaning can be used hall ion source and carry out cleaning 5min to matrix, and pressure is 2 × 10-2Pa, substrate temperature are 300 DEG C, and argon gas flux is 10sccm, and bias is -100V, cathode current 29.5A, and cathode voltage is 19V, anode current 7A, anode voltage 80V improve depositing coating to remove adsorbed gas and the impurity of matrix surface With the bond strength and quality of forming film of matrix.
Rare-earth mamem target is prepared, which is made of titanium, nickel, aluminium, yttrium, chromium, element silicon；It presses Parts by weight include following component：65 parts of titanium, 12 parts of nickel；9 parts of aluminium；3 parts of yttrium, 6 parts of chromium；2 parts of silicon；It is prepared using smelting process dilute Native memorial alloy target.
Using above-mentioned alloy target material, using magnetically controlled sputter method, the rare earth memory that film-form is formed on above-mentioned matrix is closed Layer gold：It is evacuated to 10-4Pa or more is filled with nitrogen, is then evacuated to 10 again-4Pa, adjustment operating voltage are 500V, sputtering Duty ratio 68%, proceeds by sputtering sedimentation, and control thickness is 250 μm of rare-earth mamem layers for obtaining film-form.
Start rolling machine system, sets the speed ratios of top and bottom rolls as 1.5, set each rolling deformation amount as 3%；Set low speed The speed of roller is 0.1m/s, starts the operation of rolling with the tungsten nickel of rare-earth mamem layer；After primary rolling, repeat Rolling 5 times is carried out, in the operation of rolling, it is -20 degrees Celsius to keep environment temperature；Low Temperature Heat Treatment 2h is carried out at 200 degrees Celsius, is obtained To product.

Claims (1)

1. a kind of preparation method of the tungsten nickel of rare-earth mamem layer, this method comprises the following steps：
（1）Prepare matrix
Mixed powder is prepared by following composition by weight
Tungsten carbide, 90.1%-92.8%, 0.8-1 μm of Fisher particle size；
Nickel powder, 5%-6%, 0.5-1.0 μm of Fisher particle size；
Chromium carbide, surplus；
The mixed powder of said ratio is subjected to wet-milling；Wherein Ball-milling Time Discrete control；First carbide powder and additive are carbonized Ball grinding cylinder wet-milling 12-16 hours is added in chromium, adds nickel powder wet-milling 14-18 hours；
The mixture slurry drying that ball milling is finished；
Dry pack is pressed into the compacting product of required shape；
Compacting product are placed on high temperature sintering in sintering furnace, sintering temperature is 1450-1470 DEG C, soaking time 70-90min, sintering Pressure is 4.5-5.0Mpa, obtains tungsten nickel matrix；
（2）Substrate pretreated
Described matrix pre-processes, and can be ground polishing, ultrasonic cleaning and ion source cleaning successively；
（3）Prepare rare-earth mamem target
The rare-earth mamem target is made of titanium, nickel, aluminium, yttrium, chromium, element silicon；
Include following component by weight：55-65 parts of titanium, 10-12 parts of nickel；6-9 parts of aluminium；1-3 parts of yttrium, 4-6 parts of chromium；1-2 parts of silicon；
Rare-earth mamem target is prepared using smelting process；
（4）Using above-mentioned alloy target material, using magnetically controlled sputter method, the rare-earth mamem of film-form is formed on above-mentioned matrix Layer：
It is evacuated to 10-4Pa or more is filled with nitrogen, is then evacuated to 10 again-4Pa, adjustment operating voltage are 500V, and sputtering accounts for Sky ratio 65-68%, proceeds by sputtering sedimentation, and control thickness is the 150-250 μm of rare-earth mamem layer for obtaining film-form；
Start rolling machine system, sets the speed ratio of top and bottom rolls as 1.2-1.5, set each rolling deformation amount as 2-3%；It sets low The speed of fast roller is 0.05-0.1m/s, starts the operation of rolling with the tungsten nickel of rare-earth mamem layer；Once rolled Afterwards, repeat to roll 3-5 times, in the operation of rolling, it is -30 to -20 degrees Celsius to keep environment temperature；At 150-200 degrees Celsius Low Temperature Heat Treatment 1-2h is carried out, product is obtained.
CN201810185132.4A 2018-03-07 2018-03-07 A kind of preparation method of the tungsten nickel of rare-earth mamem layer Pending CN108286005A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105695837A (en) * 2014-11-26 2016-06-22 自贡硬质合金有限责任公司 Preparation method of WC-Ni fine grain cemented carbide
CN105951047A (en) * 2016-06-26 2016-09-21 苏州思创源博电子科技有限公司 Preparation method for tungsten-nickel alloy with nitrogen-yttrium-zirconium hard coating
CN106119785A (en) * 2016-06-26 2016-11-16 苏州思创源博电子科技有限公司 A kind of preparation method possessing wear-and corrosion-resistant coating tungsten nickel
CN106591627A (en) * 2016-12-31 2017-04-26 镇江市丹徒区硕源材料科技有限公司 High-strength shape memory alloy and preparing method and application thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105695837A (en) * 2014-11-26 2016-06-22 自贡硬质合金有限责任公司 Preparation method of WC-Ni fine grain cemented carbide
CN105951047A (en) * 2016-06-26 2016-09-21 苏州思创源博电子科技有限公司 Preparation method for tungsten-nickel alloy with nitrogen-yttrium-zirconium hard coating
CN106119785A (en) * 2016-06-26 2016-11-16 苏州思创源博电子科技有限公司 A kind of preparation method possessing wear-and corrosion-resistant coating tungsten nickel
CN106591627A (en) * 2016-12-31 2017-04-26 镇江市丹徒区硕源材料科技有限公司 High-strength shape memory alloy and preparing method and application thereof

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Application publication date: 20180717

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