CN110184574B - Treatment process for improving adhesive force of coating on steel surface - Google Patents
Treatment process for improving adhesive force of coating on steel surface Download PDFInfo
- Publication number
- CN110184574B CN110184574B CN201910409232.5A CN201910409232A CN110184574B CN 110184574 B CN110184574 B CN 110184574B CN 201910409232 A CN201910409232 A CN 201910409232A CN 110184574 B CN110184574 B CN 110184574B
- Authority
- CN
- China
- Prior art keywords
- steel
- treatment
- coating
- improving
- sputtering
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Thermal Sciences (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
- Electroplating Methods And Accessories (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a treatment process for improving the adhesive force of a coating on the surface of steel, which specifically comprises the following treatment steps: 1) the method comprises the following steps of (1) cleaning treatment of the surface of the steel, (2) coating treatment of the surface of the steel, and (3) pulse electrodeposition treatment of the surface of the steel.
Description
Technical Field
The invention belongs to the technical field of steel surface treatment and processing, and particularly relates to a treatment process for improving the adhesive force of a steel surface coating.
Background
Steel is widely used in fields such as mechanical equipment, building decoration, and the problem of steel surface's corruption, static charge electromagnetic interference is the problem that people await a urgent need to solve always, and especially steel is because its mechanical strength is good, and the wide application in outdoor environment, outdoor ambient temperature, humidity and ultraviolet ray all can cause the corruption on steel surface, because steel is the conductor, cause static also to become the potential safety hazard in the use simultaneously. It is a very important problem to extend the service life of steel and improve the service performance.
The steel surface is a special steel which can work repeatedly under the dynamic load environment, has repeatable expansion performance, and needs a proper coating material in order to prolong the service life of the steel surface in the exposed environment, so that the problems that the outer layer of the assembly is oxidized, corroded, rough, cracked and the like along with the influence of the environment in the use process are reduced.
At present, the surface of steel before coating is mainly subjected to sand blasting treatment, although the treatment process can ensure that the surface of the steel obtains certain cleanliness and different roughness and the mechanical property of the surface of the steel is improved, the working environment of operators pollutes the environment by a large amount of dust, the health of the operators is seriously harmed, and the sand grains on the surface of the steel are easily distributed unevenly in the sand blasting process, so that the bonding force between a coating and the surface of the steel is adversely affected.
Disclosure of Invention
The invention aims to provide a treatment process for improving the adhesive force of a coating on the surface of a steel product aiming at the existing problems.
The invention is realized by the following technical scheme:
a treatment process for improving the adhesive force of a coating on the surface of steel comprises the following specific treatment methods:
1) cleaning treatment of steel surface
Compressed air is used for blowing the surface of the steel, and dust on the surface of the steel can be effectively removed through blowing; the steel is subjected to heating treatment, and the oxidation reaction on the surface of the steel is more severe and the content of oxygen elements on the surface is higher along with the rise of the temperature of the steel, so that the reflectivity of the surface of the steel is reduced, the reflected part of laser in the subsequent laser treatment process is reduced, and the laser treatment efficiency can be improved; the heated steel is treated on the surface of the steel by using a laser emitter, and oxide skin and rusty materials on the surface of the steel can be removed by using high temperature generated by laser, so that the effect of cleaning the surface of the steel is achieved; in the treatment process, the low-temperature gas is directly sprayed to the cleaning area, and the sprayed low-temperature gas can play a role in cooling and reducing the temperature, so that the change of the steel surface caused by overhigh temperature of the steel surface is avoided;
2) coating treatment of steel surface
S1, putting the cleaned steel into a sample chamber of a magnetron sputtering device, carrying out back-sputtering cleaning on the steel for 10-15min under the condition of 100-150W, and increasing the atomic activity on the surface of the steel through the back-sputtering cleaning so as to be beneficial to the deposition of a film; then, the steel is sent into a main sputtering chamber, the aluminum target material is subjected to 100-150W pre-sputtering treatment for 20-30min, then a layer of aluminum film is plated on the surface of the steel by adopting a radio frequency magnetron sputtering treatment method, the aluminum film is prepared on the surface of the steel by adopting a radio frequency magnetron sputtering method, the aluminum film has the characteristics of strong substrate adhesion and compactness, the film has high crystallinity and regular internal structure, and the formed film has excellent smoothness and uniformity, thereby being beneficial to improving the uniformity of the aperture size and the arrangement order of the subsequently formed porous aluminum oxide film;
s2, placing the steel subjected to film coating treatment in a nitrogen environment, heating to 250-350 ℃, and carrying out heat preservation treatment for 2-3h, wherein residual stress remained in the aluminum layer after magnetron sputtering can be eliminated through heat treatment, and the stability of the aluminum film is improved; then putting the coated steel into electrolyte as an anode, a stainless steel plate as a cathode, performing primary anodic oxidation for 4-6h at 5-10 ℃ by adopting 50-80V direct current voltage, then taking out the steel, putting the steel into a phosphorus chromic acid solution, heating to 60-70 ℃, performing constant temperature water bath treatment for 5-10h, cleaning the steel by using deionized water, performing secondary anodic oxidation for 8-10h at 5-10 ℃ by adopting 90-110V direct current voltage, then putting the steel into a phosphoric acid solution with the mass fraction of 10-15% for treatment for 2-3h, performing secondary anodic oxidation treatment to oxidize an aluminum film on the steel surface to form a porous aluminum oxide film with uniform pore size and ordered arrangement, and performing phosphoric acid reaming treatment to enlarge the pore diameter of the aluminum oxide film and improve the carrying capacity of the aluminum oxide film, the pores in the porous oxide film can provide deposition points for the deposition of Ni-SiC in the subsequent pulse electrodeposition treatment, and are beneficial to the uniform distribution of Ni-SiC on the surface of steel;
3) pulse electrodeposition treatment of steel surface
Adding nano silicon carbide into a plating solution, oscillating and dispersing for 30-50min under 300-plus 500W ultrasonic waves, then putting the steel subjected to film coating into the plating solution with a stirring device as a working electrode for pulse electrodeposition, putting the steel into the plating solution containing the nano silicon carbide, taking the coated steel as the working electrode, selecting a platinum sheet as a counter electrode, taking a saturated calomel electrode as an auxiliary electrode for pulse electrodeposition, forming Ni-SiC deposition on the surface of the steel by a pulse electrodeposition method, and accompanying with mechanical stirring in the pulse electrodeposition process, so that the sedimentation and agglomeration of nano SiC particles in the plating solution can be avoided; the method comprises the following steps of slowly dropwise adding a mixed solution consisting of copper chloride with the concentration of 0.1-0.5mol/L and hydrochloric acid with the mass fraction of 20-25% onto the surface of the steel subjected to electroplating treatment until red copper on the surface of the steel is not increased any more, cleaning the copper on the surface of the steel, putting the cleaned copper into a 60-80 ℃ drying oven, drying for 30-40min, and taking out the cleaned copper, wherein an aluminum oxide film and Ni on the surface of the steel can be removed through the mixed solution of the copper chloride and the hydrochloric acid, so that SiC with the same size and uniform distribution is formed on the surface of the steel, the roughness of the surface of the steel is increased, and the adhesive force of a coating on the surface.
Preferably, the treatment process for improving the adhesion of the coating on the surface of the steel comprises the step 1), wherein the steel is heated to 325-395 ℃ in the step 1) for 1-2 hours; the low-temperature gas is cooled in a heat exchanger by liquid nitrogen, the temperature is-80 to-50 ℃, the injection pressure of the cooling gas is 0.5 to 0.8MPa, and the flow rate is 300-500L/min.
Preferably, in the step 1), the laser emitter is a YAG laser, and the process parameters of the laser emitter are as follows: the power is 15-20W, the repetition frequency is 10-20kHz, the scanning speed is 200-1000mm/s, the defocusing amount is 1-3mm, and the scanning times are 2-3.
Preferably, in the step 2), the target material is made of high-purity aluminum alloy, the purity of the aluminum alloy is more than or equal to 99.99%, the working gas is pure argon, the purity of the working gas is more than or equal to 99.9%, and the initial background vacuum degree is 5 × 10- 5Pa-8×10-5Pa。
Preferably, in step 2), the first rf magnetron sputtering process has the following process parameters: the flow rate of argon gas is 50-80sccm, the sputtering pressure is 2-5Pa, the sputtering power is 150-200W, the sputtering time is 120-150min, the diameter of the target material is 65-75mm, and the distance between the target and the steel material is 50-60 mm.
Preferably, the treatment process for improving the adhesion of the coating on the surface of the steel, wherein in the step 2), the purity of the nitrogen is 99.9%; the electrolyte is a mixed acid solution consisting of oxalic acid with the concentration of 0.2-0.4mol/L and phosphoric acid with the mass fraction of 3-6%, and the volume ratio of the oxalic acid to the phosphoric acid is 1: 1; the phosphorus chromic acid solution contains 5-8% of phosphoric acid and 1-3% of chromic acid by mass fraction.
Preferably, the treatment process for improving the adhesive force of the coating on the surface of the steel, wherein in the step 3), the plating solution comprises 250-300g/L of nickel sulfate, 30-60g/L of nickel chloride and 30-40g/L of boric acid; the addition amount of the nano silicon carbide is 0.3-0.8% of the weight of the plating solution; the volume ratio of the copper chloride to the hydrochloric acid in the mixed solution is 1:1.
Preferably, in the step 3), the pulse electrodeposition selects a platinum sheet as a counter electrode, a saturated calomel electrode as an auxiliary electrode, and the current density is 0.1-0.5A/cm2The temperature is 50-60 ℃, the electro-deposition time is 40-60min, the stirring speed is 300-400r/min, the pulse frequency is 1000-2000Hz, and the electrode spacing is 30-50 mm.
Compared with the prior art, the invention has the following advantages:
according to the steel processing method provided by the invention, the steel is subjected to cleaning treatment, film coating treatment and pulse electrodeposition treatment, so that the surface characteristics of the steel are obviously improved, and the roughness of the steel surface is increased, thereby improving the adhesive force of the steel surface, enhancing the firmness of the combination of the coating and the steel, prolonging the service life of the coating, and having wide application prospects.
Detailed Description
The present invention will be further described with reference to specific embodiments.
Example 1
A treatment process for improving the adhesive force of a coating on the surface of steel comprises the following specific treatment methods:
1) cleaning treatment of steel surface
Blowing the surface of the steel by using compressed air, then heating the steel, treating the surface of the heated steel by using a laser emitter, and directly spraying low-temperature gas into a cleaning area in the treatment process;
2) coating treatment of steel surface
S1, putting the cleaned steel into a sample chamber of a magnetron sputtering device, carrying out back sputtering cleaning on the steel for 15min at 100W, then sending the steel into a main sputtering chamber, carrying out pre-sputtering treatment on an aluminum target material at 100W for 30min, and then plating an aluminum film on the surface of the steel by adopting a radio frequency magnetron sputtering treatment method;
s2, placing the steel subjected to film coating treatment in a nitrogen environment, heating to 250 ℃, carrying out heat preservation treatment for 3h, then placing the steel subjected to film coating in an electrolyte as an anode, taking a stainless steel plate as a cathode, carrying out primary anodic oxidation for 6h at 5 ℃ by adopting 50V direct current voltage, then taking the steel out, placing the steel in a phosphorus chromic acid solution, heating to 60 ℃, carrying out constant-temperature water bath treatment for 10h, then cleaning with deionized water, carrying out secondary anodic oxidation for 15h at 5 ℃ by adopting 90V direct current voltage, and then placing the steel in a phosphoric acid solution with the mass fraction of 10% for 3 h;
3) pulse electrodeposition treatment of steel surface
Adding nano silicon carbide into a plating solution, oscillating and dispersing for 50min under 300W ultrasonic waves, then putting the steel subjected to film coating into the plating solution with a stirring device as a working electrode for pulse electrodeposition, slowly dropwise adding a mixed solution consisting of copper chloride with the concentration of 0.1mol/L and hydrochloric acid with the mass fraction of 20% onto the surface of the steel subjected to electroplating until red copper on the surface of the steel is not increased any more, then cleaning the copper on the surface of the steel, putting the cleaned copper into a 60 ℃ drying oven, and drying for 40min, and taking out the steel.
Preferably, in the step 1), the steel is heated to 325 ℃ for 2 h; the low-temperature gas is cooled in a heat exchanger by liquid nitrogen, the temperature is-80 ℃, the injection pressure of the cooling gas is 0.5MPa, and the flow rate is 300L/min.
Preferably, in step 1), the laser emitter is a YAG laser, and the process parameters of the laser emitter are as follows: the power is 15W, the repetition frequency is 10kHz, the scanning speed is 200mm/s, the defocusing amount is 1mm, and the scanning times are 3 times.
Preferably, in the step 2), the target material is high-purity aluminum with the purity of more than or equal to 99.99 percent, the working gas is pure argon with the purity of more than or equal to 99.9 percent, and the initial background vacuum degree is 5 × 10-5Pa。
Preferably, in step 2), the process parameters of the first rf magnetron sputtering process are as follows: the argon flow is 50sccm, the sputtering pressure is 2Pa, the sputtering power is 150W, the sputtering time is 150min, the target diameter is 65mm, and the distance between the target and the steel is 50 mm.
Preferably, in the step 2), the nitrogen purity is 99.9%; the electrolyte is a mixed acid solution consisting of oxalic acid with the concentration of 0.2mol/L and phosphoric acid with the mass fraction of 3%, and the volume ratio of the oxalic acid to the phosphoric acid is 1: 1; the phosphorus chromic acid solution contains 5 mass percent of phosphoric acid and 1 mass percent of chromic acid.
Preferably, in the step 3), the plating solution comprises 250g/L of nickel sulfate, 30g/L of nickel chloride and 30g/L of boric acid; the addition amount of the nano silicon carbide is 0.3 percent of the weight of the plating solution; the volume ratio of the copper chloride to the hydrochloric acid in the mixed solution is 1:1.
Preferably, in the step 3), the platinum sheet is selected as a counter electrode in the pulse electrodeposition, the saturated calomel electrode is taken as an auxiliary electrode, and the current density is 0.1A/cm2The temperature is 50 ℃, the electro-deposition time is 60min, the stirring speed is 300r/min, the pulse frequency is 1000Hz, and the electrode spacing is 30 mm.
Example 2
A treatment process for improving the adhesive force of a coating on the surface of steel comprises the following specific treatment methods:
1) cleaning treatment of steel surface
Blowing the surface of the steel by using compressed air, then heating the steel, treating the surface of the heated steel by using a laser emitter, and directly spraying low-temperature gas into a cleaning area in the treatment process;
2) coating treatment of steel surface
S1, putting the cleaned steel into a sample chamber of a magnetron sputtering device, carrying out back sputtering cleaning on the steel for 12min at 130W, then sending the steel into a main sputtering chamber, carrying out pre-sputtering treatment on an aluminum target material at 130W for 25min, and then plating an aluminum film on the surface of the steel by adopting a radio frequency magnetron sputtering treatment method;
s2, placing the steel subjected to film coating treatment in a nitrogen environment, heating to 300 ℃, carrying out heat preservation treatment for 2.5h, then placing the steel subjected to film coating in an electrolyte as an anode, using a stainless steel plate as a cathode, carrying out primary anodic oxidation for 5h at 7 ℃ by adopting 70V direct current voltage, then taking out the steel, placing the steel into a phosphorus chromic acid solution, heating to 65 ℃, carrying out constant-temperature water bath treatment for 8h, then cleaning with deionized water, carrying out secondary anodic oxidation for 13h at 7 ℃ by adopting 100V direct current voltage, and then placing the steel in a phosphoric acid solution with the mass fraction of 12% for treatment for 2.5 h;
3) pulse electrodeposition treatment of steel surface
Adding nano silicon carbide into a plating solution, oscillating and dispersing for 40min under 400W ultrasonic waves, then putting the steel subjected to film coating as a working electrode into the plating solution with a stirring device for pulse electrodeposition, slowly dropwise adding a mixed solution consisting of copper chloride with the concentration of 0.3mol/L and hydrochloric acid with the mass fraction of 23% onto the surface of the steel subjected to electroplating until red copper on the surface of the steel is not increased any more, then cleaning the copper on the surface of the steel, putting the cleaned copper into a 70 ℃ drying oven, and drying for 35min, and taking out the steel.
Preferably, in the step 1), the steel is heated to 360 ℃ for 1.5 h; the low-temperature gas is cooled in a heat exchanger by liquid nitrogen, the temperature is-60 ℃, the injection pressure of the cooling gas is 0.7MPa, and the flow is 400L/min.
Preferably, in step 1), the laser emitter is a YAG laser, and the process parameters of the laser emitter are as follows: the power is 18W, the repetition frequency is 15kHz, the scanning speed is 600mm/s, the defocusing amount is 2mm, and the scanning times are 2 times.
Preferably, in the step 2), the target material is high-purity aluminum with the purity of more than or equal to 99.99 percent, the working gas is pure argon with the purity of more than or equal to 99.9 percent, and the initial background vacuum degree is 6 × 10-5Pa。
Preferably, in step 2), the process parameters of the first rf magnetron sputtering process are as follows: the argon flow is 65sccm, the sputtering pressure is 3Pa, the sputtering power is 180W, the sputtering time is 135min, the target material diameter is 70mm, and the distance between the target and the steel material is 55 mm.
Preferably, in the step 2), the nitrogen purity is 99.9%; the electrolyte is a mixed acid solution consisting of oxalic acid with the concentration of 0.3mol/L and phosphoric acid with the mass fraction of 5%, and the volume ratio of the oxalic acid to the phosphoric acid is 1: 1; the phosphorus chromic acid solution contains 7 mass percent of phosphoric acid and 2 mass percent of chromic acid.
Preferably, in the step 3), the plating solution comprises 280g/L of nickel sulfate, 50g/L of nickel chloride and 35g/L of boric acid; the addition amount of the nano silicon carbide is 0.5 percent of the weight of the plating solution; the volume ratio of the copper chloride to the hydrochloric acid in the mixed solution is 1:1.
Preferably, in the step 3), the platinum sheet is selected as a counter electrode in the pulse electrodeposition, the saturated calomel electrode is taken as an auxiliary electrode, and the current density is 0.3A/cm2The temperature is 55 ℃, the electro-deposition time is 50min, the stirring speed is 350r/min, the pulse frequency is 1500Hz, and the electrode spacing is 40 mm.
Example 3
A treatment process for improving the adhesive force of a coating on the surface of steel comprises the following specific treatment methods:
1) cleaning treatment of steel surface
Blowing the surface of the steel by using compressed air, then heating the steel, treating the surface of the heated steel by using a laser emitter, and directly spraying low-temperature gas into a cleaning area in the treatment process;
2) coating treatment of steel surface
S1, putting the cleaned steel into a sample chamber of a magnetron sputtering device, carrying out back sputtering cleaning on the steel for 10min at 150W, then sending the steel into a main sputtering chamber, carrying out pre-sputtering treatment on an aluminum target material at 150W for 20min, and then plating an aluminum film on the surface of the steel by adopting a radio frequency magnetron sputtering treatment method;
s2, placing the steel subjected to film coating treatment in a nitrogen environment, heating to 350 ℃, carrying out heat preservation treatment for 2h, then placing the steel subjected to film coating in an electrolyte as an anode, taking a stainless steel plate as a cathode, carrying out primary anodic oxidation for 4h at 10 ℃ by adopting 80V direct current voltage, then taking the steel out, placing the steel in a phosphorus chromic acid solution, heating to 70 ℃, carrying out constant-temperature water bath treatment for 5h, then cleaning with deionized water, carrying out secondary anodic oxidation for 10h at 10 ℃ by adopting 110V direct current voltage, and then placing the steel in a phosphoric acid solution with the mass fraction of 15% for treatment for 2 h;
3) pulse electrodeposition treatment of steel surface
Adding nano silicon carbide into a plating solution, oscillating and dispersing for 50min under 500W ultrasonic waves, then putting the steel subjected to film coating into the plating solution with a stirring device as a working electrode for pulse electrodeposition, slowly dropwise adding a mixed solution consisting of copper chloride with the concentration of 0.5mol/L and hydrochloric acid with the mass fraction of 25% onto the surface of the steel subjected to electroplating until red copper on the surface of the steel is not increased any more, then cleaning the copper on the surface of the steel, putting the cleaned copper into an oven with the temperature of 80 ℃, drying for 30min, and taking out.
Preferably, in the step 1), the steel is heated to 395 ℃ for 1 h; the low-temperature gas is cooled in a heat exchanger by liquid nitrogen, the temperature is-50 ℃, the injection pressure of the cooling gas is 0.8MPa, and the flow is 500L/min.
Preferably, in step 1), the laser emitter is a YAG laser, and the process parameters of the laser emitter are as follows: the power is 20W, the repetition frequency is 20kHz, the scanning speed is 1000mm/s, the defocusing amount is 3mm, and the scanning times are 2 times.
Preferably, in the step 2), the target material is high-purity aluminum with the purity of more than or equal to 99.99 percent, the working gas is pure argon with the purity of more than or equal to 99.9 percent, and the initial background vacuum degree is 8 × 10-5Pa。
Preferably, in step 2), the process parameters of the first rf magnetron sputtering process are as follows: the argon flow is 80sccm, the sputtering pressure is 5Pa, the sputtering power is 200W, the sputtering time is 120min, the target diameter is 75mm, and the distance between the target and the steel is 60 mm.
Preferably, in the step 2), the nitrogen purity is 99.9%; the electrolyte is a mixed acid solution consisting of oxalic acid with the concentration of 0.4mol/L and phosphoric acid with the mass fraction of 6%, and the volume ratio of the oxalic acid to the phosphoric acid is 1: 1; the phosphorus chromic acid solution contains 8 mass percent of phosphoric acid and 3 mass percent of chromic acid.
Preferably, in the step 3), the plating solution comprises 300g/L of nickel sulfate, 60g/L of nickel chloride and 40g/L of boric acid; the addition amount of the nano silicon carbide is 0.8 percent of the weight of the plating solution; the volume ratio of the copper chloride to the hydrochloric acid in the mixed solution is 1:1.
Preferably, in the step 3), the platinum sheet is selected as a counter electrode in the pulse electrodeposition, the saturated calomel electrode is taken as an auxiliary electrode, and the current density is 0.5A/cm2The temperature is 60 ℃, the electro-deposition time is 40min, the stirring speed is 400r/min, the pulse frequency is 2000Hz, and the electrode spacing is 50 mm.
Comparative example 1: the same as in example 1 except that the steel material heat treatment in step 1) was removed.
Comparative example 2: the low-temperature gas injected in step 1) was removed, and the process was the same as in example 1.
Comparative example 3: the heating and heat-insulating treatment in the step 2) is removed, and the rest is the same as that in the example 1.
Comparative example 4: the stirring was performed during the pulse electrodeposition in the removal step 3), and the rest was the same as in example 1.
Comparative example 5: the existing sand blasting technology is adopted to carry out sand blasting treatment on the steel for 10 min.
Test example: a commercially available No. 45 steel test piece having a thickness of 5mm was used as a test object and treated in the same manner as in examples 1 to 3 and comparative examples 1 to 4, respectively, and 100g of bisphenol A epoxy resin E51 was charged into a container according to the epoxy group: adding 17.5g of 1, 2-cycloh mutexanediamine curing agent into an active hydrogen ratio of 1:1.2, mechanically stirring until the system is uniform, then roller-coating the mixture on the surface of a steel sheet by using an applicator, curing at room temperature for 14h, curing at 50 ℃ for 4h, and curing at 80 ℃ for 6h, then coating a high-performance two-component polyurethane adhesive PU8804 produced by Shanghai Yangxing practical Limited company on a spindle, pasting the adhesive on a resin coating, curing at a greenhouse for 15h and curing at 50 ℃ for 15h, and then selecting a PosittAT-A full-automatic adhesion tester to perform adhesion test, wherein the results are shown in the following table:
| average adhesion MPa | |
| Example 1 | 12.36 |
| Example 2 | 13.25 |
| Example 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 table above, the steel treatment method provided by the invention can effectively improve the adhesive force of the coating on the surface of the steel, enhance the firmness of the combination of the coating and the steel, prolong the service life of the coating and have wide application prospects.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that are not thought of through the inventive work should be included in the scope of the present invention.
Claims (8)
1. A treatment process for improving the adhesive force of a coating on the surface of steel is characterized by comprising the following specific treatment methods:
1) cleaning treatment of steel surface
Blowing the surface of the steel by using compressed air, then heating the steel, treating the surface of the heated steel by using a laser emitter, and directly spraying low-temperature gas into a cleaning area in the treatment process;
2) coating treatment of steel surface
S1, putting the cleaned steel into a sample chamber of a magnetron sputtering device, carrying out back sputtering cleaning on the steel for 10-15min under the condition of 100-;
s2, placing the steel subjected to film coating treatment in a nitrogen environment, heating to 250-350 ℃, performing heat preservation treatment for 2-3h, then placing the steel subjected to film coating in an electrolyte as an anode, using a stainless steel plate as a cathode, performing first anodic oxidation for 4-6h at 5-10 ℃ by adopting 50-80V direct current voltage, then taking out the steel, placing the steel in a phosphorus chromic acid solution, heating to 60-70 ℃, performing constant temperature water bath treatment for 5-10h, then cleaning with deionized water, performing secondary anodic oxidation for 10-15h at 5-10 ℃ by adopting 90-110V direct current voltage, and then placing the steel in a phosphoric acid solution with the mass fraction of 10-15% for treatment for 2-3 h;
3) pulse electrodeposition treatment of steel surface
Adding nano silicon carbide into a plating solution, oscillating and dispersing for 30-50min under 300-500W ultrasonic waves, then putting the steel subjected to film coating as a working electrode into the plating solution with a stirring device for pulse electrodeposition, slowly dropwise adding a mixed solution consisting of copper chloride with the concentration of 0.1-0.5mol/L and hydrochloric acid with the mass fraction of 20-25% onto the surface of the steel subjected to electroplating until red copper on the surface of the steel is not increased any more, cleaning the copper on the surface of the steel, putting the cleaned copper into a 60-80 ℃ drying oven, and drying for 30-40min, and then taking out the steel.
2. The treatment process for improving the adhesion of the coating on the steel product as claimed in claim 1, wherein in the step 1), the steel product is heated to 325 ℃ and 395 ℃ for 1-2 h; the low-temperature gas is cooled in a heat exchanger by liquid nitrogen, the temperature is-80 to-50 ℃, the injection pressure of the cooling gas is 0.5 to 0.8MPa, and the flow rate is 300-500L/min.
3. The process for improving the adhesion of a coating on a steel surface according to claim 1, wherein in the step 1), the laser emitter is a YAG laser, and the process parameters of the laser emitter are as follows: the power is 15-20W, the repetition frequency is 10-20kHz, the scanning speed is 200-1000mm/s, the defocusing amount is 1-3mm, and the scanning times are 2-3.
4. The process of claim 1, wherein the step of treating the steel surface to improve the adhesion of the coating2) The target material is high-purity aluminum with the purity of more than or equal to 99.99 percent, the working gas is pure argon with the purity of more than or equal to 99.9 percent, and the initial background vacuum degree is 5 × 10-5Pa-8×10-5Pa。
5. The treatment process for improving the adhesion of the coating on the steel surface according to claim 1, wherein in the step 2), the process parameters of the first radio frequency magnetron sputtering treatment are as follows: the flow rate of argon gas is 50-80sccm, the sputtering pressure is 2-5Pa, the sputtering power is 150-200W, the sputtering time is 120-150min, the diameter of the target material is 65-75mm, and the distance between the target and the steel material is 50-60 mm.
6. The process for improving the adhesion of a coating on a steel product according to claim 1, wherein in the step 2), the purity of the nitrogen is 99.9%; the electrolyte is a mixed acid solution consisting of oxalic acid with the concentration of 0.2-0.4mol/L and phosphoric acid with the mass fraction of 3-6%, and the volume ratio of the oxalic acid to the phosphoric acid is 1: 1; the phosphorus chromic acid solution contains 5-8% of phosphoric acid and 1-3% of chromic acid by mass fraction.
7. The treatment process for improving the adhesion of the coating on the steel surface as claimed in claim 1, wherein in the step 3), the plating solution comprises nickel sulfate 250-300g/L, nickel chloride 30-60g/L, boric acid 30-40 g/L; the addition amount of the nano silicon carbide is 0.3-0.8% of the weight of the plating solution; the volume ratio of the copper chloride to the hydrochloric acid in the mixed solution is 1:1.
8. The process for improving the adhesion of a coating on a steel product as claimed in claim 1, wherein in step 3), the pulse electrodeposition uses a platinum sheet as a counter electrode, a saturated calomel electrode as an auxiliary electrode, and the current density is 0.1-0.5A/cm2The temperature is 50-60 ℃, the electro-deposition time is 40-60min, the stirring speed is 300-400r/min, the pulse frequency is 1000-2000Hz, and the electrode spacing is 30-50 mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910409232.5A CN110184574B (en) | 2019-05-17 | 2019-05-17 | Treatment process for improving adhesive force of coating on steel surface |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910409232.5A CN110184574B (en) | 2019-05-17 | 2019-05-17 | Treatment process for improving adhesive force of coating on steel surface |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110184574A CN110184574A (en) | 2019-08-30 |
| CN110184574B true CN110184574B (en) | 2020-09-01 |
Family
ID=67716530
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910409232.5A Active CN110184574B (en) | 2019-05-17 | 2019-05-17 | Treatment process for improving adhesive force of coating on steel surface |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110184574B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111185441B (en) * | 2020-03-06 | 2022-02-22 | 东莞宜安新材料研究院有限公司 | Low-power high-efficiency integrated laser cleaning method for amorphous alloy surface |
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103757647A (en) * | 2013-08-16 | 2014-04-30 | 南通瑞丽精密机电设备科技有限公司 | Steel material acid-washing and phosphorization method |
| CN104694896A (en) * | 2015-02-11 | 2015-06-10 | 宁波金鼎紧固件有限公司 | Surface treatment method for heavy anticorrosive bolt |
| CN108034978A (en) * | 2017-12-14 | 2018-05-15 | 马鞍山新徽铝业有限公司 | A kind of processing method for lifting aluminum alloy materials corrosion resistant characteristic |
| CN108707869A (en) * | 2018-04-03 | 2018-10-26 | 瑞信五金(河源)有限公司 | A kind of surface treatment method of 316 stainless steel watchband |
-
2019
- 2019-05-17 CN CN201910409232.5A patent/CN110184574B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103757647A (en) * | 2013-08-16 | 2014-04-30 | 南通瑞丽精密机电设备科技有限公司 | Steel material acid-washing and phosphorization method |
| CN104694896A (en) * | 2015-02-11 | 2015-06-10 | 宁波金鼎紧固件有限公司 | Surface treatment method for heavy anticorrosive bolt |
| CN108034978A (en) * | 2017-12-14 | 2018-05-15 | 马鞍山新徽铝业有限公司 | A kind of processing method for lifting aluminum alloy materials corrosion resistant characteristic |
| CN108707869A (en) * | 2018-04-03 | 2018-10-26 | 瑞信五金(河源)有限公司 | A kind of surface treatment method of 316 stainless steel watchband |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110184574A (en) | 2019-08-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110184574B (en) | Treatment process for improving adhesive force of coating on steel surface | |
| CN110055496B (en) | Preparation process for preparing Cr coating on surface of nuclear zirconium alloy substrate | |
| CN108570703B (en) | Preparation method of tungsten/copper laminated composite material based on tungsten sheet surface nanocrystallization | |
| CN109137035A (en) | A kind of preparation method of aluminum-based copper-clad plate | |
| CN109576679A (en) | A kind of fuel battery double plates carbon coating continuous deposition system and its application | |
| CN106835132A (en) | A kind of preparation method of double-layer high-strength corrosion resistant iron base amorphous composite coating | |
| CN112680090A (en) | Preparation method of corrosion-resistant self-repairing coating on surface of magnesium alloy | |
| CN113462911B (en) | Preparation method of tough corrosion-resistant AZ80 magnesium alloy | |
| CN110468381A (en) | A kind of higher-order of oscillation pulsed magnetron sputtering method | |
| CN106929793B (en) | Composite material, method for spraying coating on metal substrate and anticorrosive coating | |
| CN110777413B (en) | Method for laser remelting of surface of plasma cathode electrolytic deposition ceramic coating | |
| CN102330057B (en) | Method for preparing metal ruthenium film for hard semiconductor component | |
| US20200199734A1 (en) | Magnesium alloy surface coating method and corrosion-resistant magnesium alloy prepared thereby | |
| CN110318050A (en) | A kind of aluminium base/anode oxide film composite coating and its preparation method and application | |
| CN113403577B (en) | Method for improving binding force of Cu matrix and carbon-based film | |
| CN113046811B (en) | Micro-arc oxidation electrolyte, application method thereof and workpiece | |
| CN113308693A (en) | High-strength corrosion-resistant stainless steel pipe fitting and machining process thereof | |
| CN109811389B (en) | Preparation method of titanium niobium nitride nanotube array and nitriding layer composite structure | |
| CN109504996B (en) | Cathode micro-arc oxidation solution and method for preparing DLC composite oxide film on steel surface | |
| CN106435442A (en) | Metal surface gradient coating cladding method | |
| CN102485955A (en) | Method for preparing thin silicon steel strip through vacuum film plating | |
| CN106521431A (en) | Preparation method of nickel-plated Mo/Ti target | |
| CN111334752A (en) | Method for preparing CrCN thin film | |
| TWI835152B (en) | Manufacturing method of preparing ceramic membrane on stainless steel surface | |
| CN113215636B (en) | Surface treatment method for pickled plate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20200807 Address after: 710600 1st floor, building a, building 13, yuanqinguang electromechanical R & D base, middle section of Qinwang 2nd Road, Weibei Industrial Zone, Lintong District, Xi'an City, Shaanxi Province Applicant after: Xi'an Zhiyuan Aviation Technology Co., Ltd Address before: 230012 Room 703, 40 Building, Haotianyuan Garden, Northeast corner of the intersection of Huainan Road and Tangshan Road, Xinzhan District, Hefei City, Anhui Province Applicant before: ANHUI HANJIA ELECTROMECHANICAL EQUIPMENT TECHNOLOGY Co.,Ltd. |
|
| TA01 | Transfer of patent application right | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |