CN110184574A - A kind for the treatment of process improving steel surface coating adhesion - Google Patents

A kind for the treatment of process improving steel surface coating adhesion Download PDF

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Publication number
CN110184574A
CN110184574A CN201910409232.5A CN201910409232A CN110184574A CN 110184574 A CN110184574 A CN 110184574A CN 201910409232 A CN201910409232 A CN 201910409232A CN 110184574 A CN110184574 A CN 110184574A
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steel
steel surface
treatment
coating adhesion
processing
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CN110184574B (en
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张海涛
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Xi'an Zhiyuan Aviation Technology Co., Ltd
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Anhui Hanjia Mechanical And Electrical Equipment Technology Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B5/00—Cleaning by methods involving the use of air flow or gas flow
    • B08B5/02—Cleaning by the force of jets, e.g. blowing-out cavities
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
    • B08B7/0035—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by radiant energy, e.g. UV, laser, light beam or the like
    • B08B7/0042—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by radiant energy, e.g. UV, laser, light beam or the like by laser
    • 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
    • C23C14/021—Cleaning or etching treatments
    • C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • 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
    • C23C14/35—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
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment
    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • C23F1/30—Acidic compositions for etching other metallic material
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C25D11/10—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/18—After-treatment, e.g. pore-sealing
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/18—Electroplating using modulated, pulsed or reversing current
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00—Electrolytic coating other than with metals
    • C25D9/04—Electrolytic coating other than with metals with inorganic materials

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Optics & Photonics (AREA)
  • Thermal Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Physical Vapour Deposition (AREA)
  • Electroplating Methods And Accessories (AREA)

Abstract

The invention discloses a kind for the treatment of process for improving steel surface coating adhesion; specifically include following processing step: 1) cleaning treatment of steel surface; 2) coating film treatment of steel surface; 3) the pulse electrodeposition processing of steel surface; the present invention is by carrying out special processing method to steel surface; significantly improve the surface characteristic of steel; increase the roughness of steel surface; to improve the adhesive force of steel surface; enhance firmness of the coating in conjunction with steel; it in the protection service life for improving coating, is with a wide range of applications.

Description

A kind for the treatment of process improving steel surface coating adhesion
Technical field
The invention belongs to steel surface processing technical fields, and in particular to a kind of raising steel surface coating adhesion Treatment process.
Background technique
Steel are widely used in the fields such as mechanical equipment, construction and decoration, and the burn into electrostatic charge electromagnetic interference of steel surface is asked Topic is always people's urgent problem to be solved, especially steel because its mechanical strength is good, is widely used in outdoor environment, outdoor Environment temperature, humidity and ultraviolet light can all cause the corrosion of steel surface to cause electrostatic simultaneously because steel are conductors As the security risk in use process.How to extend steel uses birthday noodle, improves its service performance, is one extremely important The problem of.
Steel surface be it is a kind of can repeated action works under dynamic loading environment special rolling-mill section, have repeatability flexible Performance need suitable coating material to prolong its service life steel surface in the exposed environment, to reduce group It is coarse and the problems such as crack to become oxidation, burn into the influence of environment for the outer layer of part in use.
Blasting treatment is substantially carried out to the steel surface before coating at present, although this treatment process can make steel surface Certain cleannes and different roughness are obtained, the mechanical performance of steel surface is improved, but the work of operator Making environment is that a large amount of dust pollutes environment, seriously endangers the health of operator, and steel table is be easy to cause in sandblasting procedures The sand grains in face is unevenly distributed, to bring adverse effect to the binding force of coating and steel surface.
Summary of the invention
The purpose of the present invention is being directed to existing problem, a kind of processing work for improving steel surface coating adhesion is provided Skill.
The present invention is achieved by the following technical solutions:
A kind for the treatment of process improving steel surface coating adhesion, specific processing method are as follows:
1) cleaning treatment of steel surface
Steel surface is purged using compressed air, the dust of steel surface can be effectively removed by purging；To steel Material is heated, and by heating to steel, with the raising of steel temperature, the oxidation reaction of steel surface is got over Acutely, the content of surface oxygen element is higher, so that the reflectivity of steel surface is reduced, to advantageously reduce subsequent laser treatment The part that laser is reflected in the process, so as to improve the efficiency of laser treatment；Steel after heating are used into Laser emission Device handles steel surface, and the oxide skin and rust of steel surface can be removed using the high temperature that laser generates, is played Clean the effect of steel surface；During processing, cryogenic gas is directly injected into cleaning area, the cryogenic gas of injection can be with Play the role of cooling, avoids steel surface temperature is excessively high steel surface is caused to change；
2) coating film treatment of steel surface
S1, the steel through over cleaning are put into the specimen chamber of magnetron sputtering apparatus, 10- is cleaned to steel backwash at 100-150W 15min can increase the atom active of steel surface by backwash cleaning, be conducive to the deposition of film；Then steel are sent into In main sputtering chamber, the pre-sputtering for first carrying out 100-150W to aluminium target is handled, and the sputter process time is 20-30min, is then used The method of rf magnetron sputtering processing plates one layer of aluminium film in steel surface, using radio-frequency magnetron sputter method in steel surface system Standby aluminium film, the aluminium film have the characteristics that substrate adhesion and compactness are strong, and film crystal unity is high, internal structure rule Whole, the film planarization and excellent in uniformity of formation are conducive to improve the porous alumina membrane pore size being subsequently formed Uniformity and the order of arrangement；
S2, the steel Jing Guo coating film treatment are placed under nitrogen environment, are heated to 250-350 DEG C of isothermal holding 2-3h, pass through heat Processing remains in the residual stress in aluminium layer after can eliminating magnetron sputtering, improves the stability of aluminium film；Then by plated film Steel are put into electrolyte as anode, and stainless steel plate is as cathode, using 50-80V DC voltage progress the at 5-10 DEG C Anodic oxidation 4-6h, then takes out steel, is put into phosphorus chromic acid solution, is heated to 60-70 DEG C, water bath with thermostatic control handles 5- 10h after then being cleaned up with deionized water, carries out two-step anodization 8- using 90-110V DC voltage at 5-10 DEG C Then 10h is placed it in the phosphoric acid solution that mass fraction is 10-15% and is handled 2-3h, at two-step anodization Reason, can make the aluminium film in steel face aoxidize the porous alumina membrane to form that pore size is uniform, orderly aligned, then again through phosphorus Sour expanding treatment, so that the aperture increases of aluminum oxide film, improve the carrying capability of aluminum oxide film, in the porous oxide film Hole can provide saltation point for the deposition of Ni-SiC in the processing of subsequent pulse electrodeposition, be conducive to the Ni-SiC of steel surface It is evenly distributed；
3) the pulse electrodeposition processing of steel surface
Nanometer silicon carbide is added in plating solution, the vibrating dispersion 30-50min under 300-500W ultrasonic wave, it then will be by plating The steel of film process are put into the plating solution with agitating device progress pulse electrodeposition processing as working electrode, by by steel It is put into the plating solution containing nanometer silicon carbide, using plated film steel as working electrode, selects platinized platinum to be used as to electrode, be saturated calomel Electrode is auxiliary electrode, carries out pulse electrodeposition, forms Ni-SiC deposition, pulse on the surface of steel by pulse electrodeposition method With mechanical stirring in electrodeposition process, sedimentation can occur to avoid nano SiC particle in plating solution and reunite；It is 0.1- with concentration The mixed liquor that the hydrochloric acid that the copper chloride and mass fraction of 0.5mol/L is 20-25% forms is slowly dropped to by electroplating processes Steel surface is put into 60-80 DEG C of baking oven after cleaning the copper of steel surface until the red copper of steel surface no longer increases It is taken out after middle drying process 30-40min, it can be by the aluminum oxide film of steel surface by copper chloride and hydrochloric acid mixed solution And Ni removal, thus, the SiC that is evenly distributed identical in steel surface formation size, thus increase the roughness of steel surface, Improve steel surface coating adhesion.
Preferably, a kind for the treatment of process improving steel surface coating adhesion, wherein in step 1), the heat steel Processing is by heat steel to 325-395 DEG C, heat treatment time 1-2h；The cryogenic gas be by liquid nitrogen in a heat exchanger Cooled, for temperature at -80--50 DEG C, the injection pressure of cooling gas is 0.5-0.8MPa, flow 300-500L/min.
Preferably, a kind for the treatment of process improving steel surface coating adhesion, wherein in step 1), the Laser emission Device is YAG laser, the technological parameter of laser emitter are as follows: power 15-20W, repetition rate 10-20kHz, scanning speed For 200-1000mm/s, defocusing amount 1-3mm, scanning times 2-3 times.
Preferably, a kind for the treatment of process improving steel surface coating adhesion, wherein in step 2), the target is used Raffinal closes, purity >=99.99%；Working gas is pure argon, purity >=99.9%；Initial background vacuum degree is 5 × 10- 5Pa-8×10-5Pa。
Preferably, a kind for the treatment of process improving steel surface coating adhesion, wherein in step 2), the first time The technological parameter of rf magnetron sputtering processing are as follows: argon flow 50-80sccm, sputtering pressure 2-5Pa, sputtering frequency are 150- 200W, sputtering time 120-150min, target diameter are 65-75mm, and target is 50-60mm at a distance from steel.
Preferably, a kind for the treatment of process improving steel surface coating adhesion, wherein in step 2), the nitrogen gas purity 99.9%；The nitration mixture that the phosphoric acid that the oxalic acid and mass fraction that the electrolyte is 0.2-0.4mol/L by concentration are 3-6% forms is molten Liquid, the volume ratio of the two are 1:1；The phosphorus chromic acid solution contains the phosphoric acid that mass fraction is 5-8% and mass fraction is 1-3%'s Chromic acid.
Preferably, a kind for the treatment of process improving steel surface coating adhesion, wherein in step 3), the plating solution includes Nickel sulfate 250-300g/L, nickel chloride 30-60g/L, boric acid 30-40g/L；The additive amount of the nanometer silicon carbide is plating solution weight 0.3-0.8%；The volume ratio of copper chloride and hydrochloric acid is 1:1 in the mixed liquor.
Preferably, a kind for the treatment of process improving steel surface coating adhesion, wherein in step 3), the pulse electricity is heavy Product selects platinized platinum to be used as to electrode, and saturated calomel electrode is auxiliary electrode, current density 0.1-0.5A/cm2, temperature 50- 60 DEG C, electrodeposition time 40-60min, stirring rate 300-400r/min, pulse frequency 1000-2000Hz, between electrode Away from for 30-50mm.
The present invention has the advantage that compared with prior art
Steel processing method provided by the invention, by being started the cleaning processing to steel, at coating film treatment and pulse electrodeposition Reason, hence it is evident that the surface characteristic for improving steel increases the roughness of steel surface, to improve the adhesive force of steel surface, increases Strong firmness of the coating in conjunction with steel, improves the protection service life of coating, is with a wide range of applications.
Specific embodiment
Below with reference to specific implementation method, the present invention is described further.
Embodiment 1
A kind for the treatment of process improving steel surface coating adhesion, specific processing method are as follows:
1) cleaning treatment of steel surface
Steel surface is purged using compressed air, then steel are heated, the steel after heating are used Laser emitter handles steel surface, during processing, cryogenic gas is directly injected into cleaning area；
2) coating film treatment of steel surface
S1, the steel through over cleaning are put into the specimen chamber of magnetron sputtering apparatus, 15min are cleaned to steel backwash at 100W, Then steel to be sent into main sputtering chamber, the pre-sputtering for first carrying out 100W to aluminium target is handled, and the sputter process time is 30min, Then one layer of aluminium film is plated in steel surface using the method for rf magnetron sputtering processing；
S2, the steel Jing Guo coating film treatment are placed under nitrogen environment, 250 DEG C of isothermal holding 3h are heated to, then by plated film Steel are put into electrolyte as anode, and stainless steel plate carries out sun for the first time using 50V DC voltage at 5 DEG C as cathode Pole aoxidizes 6h, then takes out steel, is put into phosphorus chromic acid solution, is heated to 60 DEG C, and water bath with thermostatic control handles 10h, then spends After ionized water cleans up, two-step anodization 15h is carried out using 90V DC voltage at 5 DEG C, then places it in quality point Number is processing 3h in 10% phosphoric acid solution；
3) the pulse electrodeposition processing of steel surface
Nanometer silicon carbide is added in plating solution, the vibrating dispersion 50min under 300W ultrasonic wave, it then will be by coating film treatment Steel are put into progress pulse electrodeposition processing in the plating solution with agitating device as working electrode, are then with concentration The mixed liquor that the hydrochloric acid that the copper chloride and mass fraction of 0.1mol/L is 20% forms is slowly dropped to the steel by electroplating processes Surface is put into 60 DEG C of baking ovens after then cleaning the copper of steel surface until the red copper of steel surface no longer increases It is taken out after being dried 40min.
Preferably, wherein in step 1), the heat steel processing is by heat steel to 325 DEG C, heat treatment time For 2h；The cryogenic gas be it is cooled in a heat exchanger by liquid nitrogen, temperature is at -80 DEG C, the injection pressure of cooling gas For 0.5MPa, flow 300L/min.
Preferably, the laser emitter is YAG laser, the technological parameter of laser emitter wherein in step 1) Are as follows: power 15W, repetition rate 10kHz, scanning speed 200mm/s, defocusing amount 1mm, scanning times 3 times.
Preferably, the target uses raffinal, purity >=99.99% wherein in step 2)；Working gas is Pure argon, purity >=99.9%；Initial background vacuum degree is 5 × 10-5Pa。
Preferably, wherein in step 2), the technological parameter of the rf magnetron sputtering processing of the first time are as follows: argon gas stream Amount is 50sccm, and sputtering pressure 2Pa, sputtering frequency is 150W, and sputtering time 150min, target diameter is 65mm, target and steel The distance of material is 50mm.
Preferably, wherein in step 2), the nitrogen gas purity 99.9%；The electrolyte is 0.2mol/L's by concentration The mixed acid solution that the phosphoric acid that oxalic acid and mass fraction are 3% forms, the volume ratio of the two are 1:1；The phosphorus chromic acid solution contains matter Measure the phosphoric acid that score is 5% and the chromic acid that mass fraction is 1%.
Preferably, the plating solution includes nickel sulfate 250g/L, nickel chloride 30g/L, boric acid 30g/L wherein in step 3)； The additive amount of the nanometer silicon carbide is the 0.3% of plating solution weight；The volume ratio of copper chloride and hydrochloric acid is 1:1 in the mixed liquor.
Preferably, the pulse electrodeposition selects platinized platinum to be used as to electrode, and saturated calomel electrode is wherein in step 3) Auxiliary electrode, current density 0.1A/cm2, temperature is 50 DEG C, electrodeposition time 60min, stirring rate 300r/min, Pulse frequency is 1000Hz, electrode spacing 30mm.
Embodiment 2
A kind for the treatment of process improving steel surface coating adhesion, specific processing method are as follows:
1) cleaning treatment of steel surface
Steel surface is purged using compressed air, then steel are heated, the steel after heating are used Laser emitter handles steel surface, during processing, cryogenic gas is directly injected into cleaning area；
2) coating film treatment of steel surface
S1, the steel through over cleaning are put into the specimen chamber of magnetron sputtering apparatus, 12min are cleaned to steel backwash at 130W, Then steel to be sent into main sputtering chamber, the pre-sputtering for first carrying out 130W to aluminium target is handled, and the sputter process time is 25min, Then one layer of aluminium film is plated in steel surface using the method for rf magnetron sputtering processing；
S2, the steel Jing Guo coating film treatment are placed under nitrogen environment, 300 DEG C of isothermal holding 2.5h are heated to, then by plated film Steel be put into electrolyte as anode, stainless steel plate carries out first time using 70V DC voltage at 7 DEG C as cathode Anodic oxidation 5h, then takes out steel, is put into phosphorus chromic acid solution, is heated to 65 DEG C, and water bath with thermostatic control handles 8h, then spends After ionized water cleans up, two-step anodization 13h is carried out using 100V DC voltage at 7 DEG C, then places it in quality 2.5h is handled in the phosphoric acid solution that score is 12%；
3) the pulse electrodeposition processing of steel surface
Nanometer silicon carbide is added in plating solution, the vibrating dispersion 40min under 400W ultrasonic wave, it then will be by coating film treatment Steel are put into progress pulse electrodeposition processing in the plating solution with agitating device as working electrode, are then with concentration The mixed liquor that the hydrochloric acid that the copper chloride and mass fraction of 0.3mol/L is 23% forms is slowly dropped to the steel by electroplating processes Surface is put into 70 DEG C of baking ovens after then cleaning the copper of steel surface until the red copper of steel surface no longer increases It is taken out after being dried 35min.
Preferably, wherein in step 1), the heat steel processing is by heat steel to 360 DEG C, heat treatment time For 1.5h；The cryogenic gas be it is cooled in a heat exchanger by liquid nitrogen, temperature is at -60 DEG C, the jet pressure of cooling gas Power is 0.7MPa, flow 400L/min.
Preferably, the laser emitter is YAG laser, the technological parameter of laser emitter wherein in step 1) Are as follows: power 18W, repetition rate 15kHz, scanning speed 600mm/s, defocusing amount 2mm, scanning times 2 times.
Preferably, the target uses raffinal, purity >=99.99% wherein in step 2)；Working gas is Pure argon, purity >=99.9%；Initial background vacuum degree is 6 × 10-5Pa。
Preferably, wherein in step 2), the technological parameter of the rf magnetron sputtering processing of the first time are as follows: argon gas stream Amount is 65sccm, and sputtering pressure 3Pa, sputtering frequency is 180W, and sputtering time 135min, target diameter is 70mm, target and steel The distance of material is 55mm.
Preferably, wherein in step 2), the nitrogen gas purity 99.9%；The electrolyte is 0.3mol/L's by concentration The mixed acid solution that the phosphoric acid that oxalic acid and mass fraction are 5% forms, the volume ratio of the two are 1:1；The phosphorus chromic acid solution contains matter Measure the phosphoric acid that score is 7% and the chromic acid that mass fraction is 2%.
Preferably, the plating solution includes nickel sulfate 280g/L, nickel chloride 50g/L, boric acid 35g/L wherein in step 3)； The additive amount of the nanometer silicon carbide is the 0.5% of plating solution weight；The volume ratio of copper chloride and hydrochloric acid is 1:1 in the mixed liquor.
Preferably, the pulse electrodeposition selects platinized platinum to be used as to electrode, and saturated calomel electrode is wherein in step 3) Auxiliary electrode, current density 0.3A/cm2, temperature is 55 DEG C, electrodeposition time 50min, stirring rate 350r/min, Pulse frequency is 1500Hz, electrode spacing 40mm.
Embodiment 3
A kind for the treatment of process improving steel surface coating adhesion, specific processing method are as follows:
1) cleaning treatment of steel surface
Steel surface is purged using compressed air, then steel are heated, the steel after heating are used Laser emitter handles steel surface, during processing, cryogenic gas is directly injected into cleaning area；
2) coating film treatment of steel surface
S1, the steel through over cleaning are put into the specimen chamber of magnetron sputtering apparatus, 10min are cleaned to steel backwash at 150W, Then steel to be sent into main sputtering chamber, the pre-sputtering for first carrying out 150W to aluminium target is handled, and the sputter process time is 20min, Then one layer of aluminium film is plated in steel surface using the method for rf magnetron sputtering processing；
S2, the steel Jing Guo coating film treatment are placed under nitrogen environment, 350 DEG C of isothermal holding 2h are heated to, then by plated film Steel are put into electrolyte as anode, and stainless steel plate carries out sun for the first time using 80V DC voltage at 10 DEG C as cathode Pole aoxidizes 4h, then takes out steel, is put into phosphorus chromic acid solution, is heated to 70 DEG C, and water bath with thermostatic control handles 5h, then spend from After sub- water cleans up, two-step anodization 10h is carried out using 110V DC voltage at 10 DEG C, then places it in quality point Number is processing 2h in 15% phosphoric acid solution；
3) the pulse electrodeposition processing of steel surface
Nanometer silicon carbide is added in plating solution, the vibrating dispersion 50min under 500W ultrasonic wave, it then will be by coating film treatment Steel are put into progress pulse electrodeposition processing in the plating solution with agitating device as working electrode, are then with concentration The mixed liquor that the hydrochloric acid that the copper chloride and mass fraction of 0.5mol/L is 25% forms is slowly dropped to the steel by electroplating processes Surface is put into 80 DEG C of baking ovens after then cleaning the copper of steel surface until the red copper of steel surface no longer increases It is taken out after being dried 30min.
Preferably, wherein in step 1), the heat steel processing is by heat steel to 395 DEG C, heat treatment time For 1h；The cryogenic gas be it is cooled in a heat exchanger by liquid nitrogen, temperature is at -50 DEG C, the injection pressure of cooling gas For 0.8MPa, flow 500L/min.
Preferably, the laser emitter is YAG laser, the technological parameter of laser emitter wherein in step 1) Are as follows: power 20W, repetition rate 20kHz, scanning speed 1000mm/s, defocusing amount 3mm, scanning times 2 times.
Preferably, the target uses raffinal, purity >=99.99% wherein in step 2)；Working gas is Pure argon, purity >=99.9%；Initial background vacuum degree is 8 × 10-5Pa。
Preferably, wherein in step 2), the technological parameter of the rf magnetron sputtering processing of the first time are as follows: argon gas stream Amount is 80sccm, and sputtering pressure 5Pa, sputtering frequency is 200W, and sputtering time 120min, target diameter is 75mm, target and steel The distance of material is 60mm.
Preferably, wherein in step 2), the nitrogen gas purity 99.9%；The electrolyte is 0.4mol/L's by concentration The mixed acid solution that the phosphoric acid that oxalic acid and mass fraction are 6% forms, the volume ratio of the two are 1:1；The phosphorus chromic acid solution contains matter Measure the phosphoric acid that score is 8% and the chromic acid that mass fraction is 3%.
Preferably, the plating solution includes nickel sulfate 300g/L, nickel chloride 60g/L, boric acid 40g/L wherein in step 3)； The additive amount of the nanometer silicon carbide is the 0.8% of plating solution weight；The volume ratio of copper chloride and hydrochloric acid is 1:1 in the mixed liquor.
Preferably, the pulse electrodeposition selects platinized platinum to be used as to electrode, and saturated calomel electrode is wherein in step 3) Auxiliary electrode, current density 0.5A/cm2, temperature is 60 DEG C, electrodeposition time 40min, stirring rate 400r/min, Pulse frequency is 2000Hz, electrode spacing 50mm.
Comparative example 1: the steel heat treatment in removal step 1), remaining is same as Example 1.
Comparative example 2: the injection cryogenic gas in removal step 1), remaining is same as Example 1.
Comparative example 3: the heating and thermal insulation processing in removal step 2, remaining is same as Example 1.
Comparative example 4: it is stirred during the pulse electrodeposition in removal step 3), remaining is same as Example 1.
Comparative example 5: blasting treatment 10min is carried out to steel using existing grit blasting techniques.
Test example: selecting commercially available No. 45 steel test pieces is subjects, with a thickness of 5mm, be respectively adopted embodiment 1-3 and The method that comparative example 1-4 is provided is handled, and then takes 100g bisphenol A epoxide resin E51 to be added in container, according to epoxy Base: active hydrogen ratio is that 1,2- cyclohexanediamine curing agent 17.5g is added in 1:1.2, and mechanical stirring is uniform to system, then with coating Device roller coating is in steel disc surface, room temperature curing 14h, 50 DEG C of solidifications 4h, 80 DEG C of solidification 6h, then by Shanghai Shou Xing Industrial Co., Ltd. The high-performance dual-component polyurethane adhesive PU8804 of production is coated on spindle, is pasted on resinous coat, and greenhouse solidifies 15h, Then 50 DEG C of solidification 15h select the full-automatic adhesion-force tester of PosiTestAT-A to carry out adhesive force test, as a result such as following table institute Show:
Average adhesive force MPa
Embodiment 1 12.36
Embodiment 2 13.25
Embodiment 3 12.71
Comparative example 1 11.32
Comparative example 2 10.98
Comparative example 3 9.32
Comparative example 4 10.10
Comparative example 5 6.93
As can be seen from the above table, steel processing method provided by the invention can effectively improve the attachment of steel surface coating Power enhances firmness of the coating in conjunction with steel, improves the protection service life of coating, be with a wide range of applications.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any It transforms or replaces, should be covered by the scope of protection of the present invention without what creative work was expected.

Claims (8)

1. a kind for the treatment of process for improving steel surface coating adhesion, which is characterized in that specific processing method is as follows:
1) cleaning treatment of steel surface
Steel surface is purged using compressed air, then steel are heated, the steel after heating are used Laser emitter handles steel surface, during processing, cryogenic gas is directly injected into cleaning area；
2) coating film treatment of steel surface
S1, the steel through over cleaning are put into the specimen chamber of magnetron sputtering apparatus, 10- is cleaned to steel backwash at 100-150W Then steel are sent into main sputtering chamber by 15min, the pre-sputtering for first carrying out 100-150W to aluminium target is handled, when sputter process Between be 20-30min, then using rf magnetron sputtering processing method plate one layer of aluminium film in steel surface；
S2, the steel Jing Guo coating film treatment are placed under nitrogen environment, are heated to 250-350 DEG C of isothermal holding 2-3h, then will The steel of plated film are put into electrolyte as anode, and stainless steel plate uses 50-80V DC voltage as cathode at 5-10 DEG C First time anodic oxidation 4-6h is carried out, then steel are taken out, are put into phosphorus chromic acid solution, are heated to 60-70 DEG C, water bath with thermostatic control 5-10h is handled, after then being cleaned up with deionized water, secondary anode is carried out using 90-110V DC voltage at 5-10 DEG C 10-15h is aoxidized, then places it in the phosphoric acid solution that mass fraction is 10-15% and handles 2-3h；
3) the pulse electrodeposition processing of steel surface
Nanometer silicon carbide is added in plating solution, the vibrating dispersion 30-50min under 300-500W ultrasonic wave, it then will be by plating The steel of film process are put into progress pulse electrodeposition processing in the plating solution with agitating device as working electrode, then use concentration The mixed liquor for the hydrochloric acid composition that copper chloride and mass fraction for 0.1-0.5mol/L are 20-25% is slowly dropped to by plating The steel surface of processing is put into after then cleaning the copper of steel surface until the red copper of steel surface no longer increases It is taken out after being dried 30-40min in 60-80 DEG C of baking oven.
2. a kind for the treatment of process for improving steel surface coating adhesion as described in claim 1, which is characterized in that step 1) In, heat steel processing is by heat steel to 325-395 DEG C, heat treatment time 1-2h；The cryogenic gas be by Liquid nitrogen is cooled in a heat exchanger, and for temperature at -80--50 DEG C, the injection pressure of cooling gas is 0.5-0.8MPa, flow For 300-500L/min.
3. a kind for the treatment of process for improving steel surface coating adhesion as described in claim 1, which is characterized in that step 1) In, the laser emitter is YAG laser, the technological parameter of laser emitter are as follows: power 15-20W, repetition rate are 10-20kHz, scanning speed 200-1000mm/s, defocusing amount 1-3mm, scanning times 2-3 times.
4. a kind for the treatment of process for improving steel surface coating adhesion as described in claim 1, which is characterized in that step 2) In, the target uses raffinal, purity >=99.99%；Working gas is pure argon, purity >=99.9%；Initial background Vacuum degree is 5 × 10-5Pa-8×10-5Pa。
5. a kind for the treatment of process for improving steel surface coating adhesion as described in claim 1, which is characterized in that step 2) In, the technological parameter of the rf magnetron sputtering processing of the first time are as follows: argon flow 50-80sccm, sputtering pressure 2- 5Pa, sputtering frequency are 150-200W, and sputtering time 120-150min, target diameter is 65-75mm, and target is at a distance from steel For 50-60mm.
6. a kind for the treatment of process for improving steel surface coating adhesion as described in claim 1, which is characterized in that step 2) In, the nitrogen gas purity 99.9%；The phosphorus that the oxalic acid and mass fraction that the electrolyte is 0.2-0.4mol/L by concentration are 3-6% The mixed acid solution of acid composition, the volume ratio of the two are 1:1；The phosphorus chromic acid solution contains the phosphoric acid and matter that mass fraction is 5-8% Measure the chromic acid that score is 1-3%.
7. a kind for the treatment of process for improving steel surface coating adhesion as described in claim 1, which is characterized in that step 3) In, the plating solution includes nickel sulfate 250-300g/L, nickel chloride 30-60g/L, boric acid 30-40g/L；The nanometer silicon carbide Additive amount is the 0.3-0.8% of plating solution weight；The volume ratio of copper chloride and hydrochloric acid is 1:1 in the mixed liquor.
8. a kind for the treatment of process for improving steel surface coating adhesion as described in claim 1, which is characterized in that step 3) In, the pulse electrodeposition selects platinized platinum to be used as to electrode, and saturated calomel electrode is auxiliary electrode, current density 0.1- 0.5A/cm2, temperature is 50-60 DEG C, electrodeposition time 40-60min, stirring rate 300-400r/min, and pulse frequency is 1000-2000Hz, electrode spacing 30-50mm.
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CN111607816A (en) * 2020-06-03 2020-09-01 暨南大学 Method for pulse electrodeposition of Ni-SiC composite coating on surface of aluminum alloy

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