CN110804734A - Composite passivation method for stainless steel material - Google Patents
Composite passivation method for stainless steel material Download PDFInfo
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- CN110804734A CN110804734A CN201910971038.6A CN201910971038A CN110804734A CN 110804734 A CN110804734 A CN 110804734A CN 201910971038 A CN201910971038 A CN 201910971038A CN 110804734 A CN110804734 A CN 110804734A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/50—Treatment of iron or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/78—Pretreatment of the material to be coated
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/82—After-treatment
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/82—After-treatment
- C23C22/83—Chemical after-treatment
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Abstract
The invention provides a composite passivation method of a stainless steel material, which comprises the working procedures of organic solvent oil removal, alkali oil removal, acid cleaning, alkali deoxidation, passivation, neutralization, air drying and supplementary treatment. The supplementary treatment process comprises the steps of soaking an air-dried workpiece by adopting a mixed solution of a metal chemical conversion solution and deionized water, and then drying the soaked workpiece; when soaking, the temperature of the mixed solution is 10-35 ℃, the soaking time is 1-1.5 min, the pH value of the mixed solution is 11.1-12.6, the drying temperature is 80-120 ℃, and the drying time is 15-50 min; and performing supplementary treatment on the workpiece, and performing secondary oxidation and hole sealing treatment on the surface passivation layer of the workpiece to improve the compactness of the passivation layer.
Description
Technical Field
The invention belongs to the field of surface treatment of stainless steel materials, and relates to a method for passivating the surface of a stainless steel material.
Background
If no plating or other coating is required, stainless steel parts are generally subjected to pretreatment such as acid washing to remove black skin, polishing and the like, and then are subjected to passivation treatment to be used as finished products or assembled into components. The passivation treatment of the stainless steel can keep the surface of the material in a passive state which is stable for a long time, and the corrosion resistance is improved.
In order to meet the requirement of the airplane on service in severe environment, the environment test of a helicopter of a certain model puts forward the requirements of damp-heat and salt spray tests and the like on stainless steel parts. Performing a damp-heat test according to the part 9 of the GJB150A-2009 military equipment laboratory environment test method, and performing a damp-heat test for 10 periods (264h) in a test box with set temperature and humidity, wherein the surface of the test piece is not rusted; the salt spray test requires GJB150A-2009 laboratory environmental test methods for military equipment, part 11: salt spray test (salt spray test), wherein the salt spray test is carried out for 96h in total, and the surface of a test piece is not rusted; according to ASTM B-117 (laboratory salt spray test method), the 24h test piece has no corrosion and no damp heat test requirements; in the quality test of pickling and passivating of HB5292 stainless steel, the corrosion resistance test can only be carried out for 24h of sodium chloride salt water immersion test, and the requirement of damp and hot test is avoided.
The prior stainless steel passivation treatment technology can not meet the requirements of corrosion resistance, humidity resistance and heat resistance of stainless steel parts in severe environments such as ocean and the like. In order to meet the requirements of environmental tests and improve the humidity resistance, heat resistance and salt spray resistance of stainless steel, the prior stainless steel passivation process is improved.
Disclosure of Invention
The invention aims to provide a composite passivation method for stainless steel materials, which improves the corrosion resistance and the damp and heat resistance of stainless steel material parts.
The technical scheme of the invention is that the composite passivation method of the stainless steel material comprises the working procedures of organic solvent oil removal, alkali oil removal, acid cleaning, alkali deoxidation, passivation, neutralization, air drying and supplementary treatment;
removing oil by using an organic solvent: removing oil by using organic solvent steam or wiping the workpiece by using an organic solvent to remove oil stains on the surface of the workpiece to be passivated;
alkali degreasing: cleaning a workpiece to be passivated by adopting an alkali solution, wherein the alkali solution comprises anhydrous sodium carbonate, anhydrous sodium phosphate, sodium silicate and a surfactant;
at least one treatment process of sand blowing, acid washing or alkali deoxidation, wherein the sand blowing treatment is to treat the surface of a workpiece to be passivated by adopting hydraulic sand blowing or glass microsphere sand blowing and is used for removing an oxide film on the surface of the workpiece; pickling, namely cleaning the workpiece to be passivated by adopting a fluoronitric acid solution if the workpiece to be passivated is made of an austenitic stainless steel material, wherein the fluoronitric acid solution comprises nitric acid and sodium fluoride; performing alkali deoxidation treatment, namely, if the workpiece to be passivated is made of a martensite or ferrite stainless steel material, deoxidizing the workpiece to be passivated by adopting a sodium hydroxide-sodium glucoheptonate solution;
passivation: passivating the surface of a workpiece to be passivated by adopting a nitric acid solution to form a passivation layer on the surface of the workpiece;
neutralizing: cleaning the surface of the passivated workpiece by adopting a sodium carbonate solution to neutralize the residual acid solution;
air drying: removing the residual solution on the surface of the workpiece after neutralization and cleaning by adopting gas blowing;
and (3) supplementary treatment: firstly, soaking an air-dried workpiece by adopting a mixed solution of a metal chemical conversion solution and deionized water, and then drying the soaked workpiece; when soaking, the temperature of the mixed solution is 10-35 ℃, the soaking time is 1-1.5 min, the pH value of the mixed solution is 11.1-12.6, the drying temperature is 80-120 ℃, and the drying time is 15-50 min; and performing supplementary treatment on the workpiece, and performing secondary oxidation and hole sealing treatment on the surface passivation layer of the workpiece to improve the compactness of the passivation layer.
Further, before the oil removal by the organic solvent, the composite passivation method further comprises the steps of removing an oxide film on the surface of the workpiece to be passivated; the surface of the passivated workpiece is free of burrs, cracks or scratches.
Further, when the oil is removed by adopting organic solvent steam, the organic solvent is trichloroethylene.
Further, after the alkali degreasing, the composite passivation method further comprises the step of carrying out water film continuity detection on the surface of the workpiece to be passivated after the alkali degreasing process, wherein a continuous water film 30S formed on the surface of the workpiece is not broken and qualified in degreasing, otherwise, alkali degreasing is carried out again.
Further, the sodium hydroxide-sodium glucoheptonate solution comprises sodium hydroxide, sodium glucoheptonate and deionized water; and the temperature of the sodium hydroxide-sodium glucoheptonate solution is 75-85 ℃ during alkali deoxidation.
Further, preparing a nitric acid solution by using nitric acid and deionized water in a volume ratio of 1: 1; the passivation temperature is 20-25 ℃, and the passivation time is 25-30 min.
Further, before the workpiece is subjected to supplementary treatment and after air drying, the composite passivation method also comprises dehydrogenation, namely dehydrogenation is carried out on the workpiece at the temperature of 190 +/-10 ℃, and the dehydrogenation time t is more than or equal to 3 h.
Further, in the neutralization process, sodium carbonate and deionized water are mixed to prepare a sodium carbonate solution, wherein the concentration of the sodium carbonate solution is 20-50 g/l.
Further, the composite passivation method also comprises the working procedures of organic solvent oil removal, alkali oil removal, acid washing, alkali deoxidation, passivation and neutralization, wherein after each working procedure is finished, the workpiece is cleaned by adopting flowing cooling water or deionized water; and after the neutralization and supplementary treatment processes are finished, the workpiece is cleaned by adopting deionized water.
The invention has the technical effects that:
the invention improves the stainless steel material surface passivation treatment method, adds the procedures of neutralization treatment and supplementary treatment, is used for carrying out reoxidation and hole sealing treatment on the surface passivation layer of the workpiece, and improves the compactness of the passivation layer so as to improve the environmental corrosion resistance of the stainless steel material part.
Detailed Description
The embodiment is a composite passivation method of a stainless steel material, which comprises the working procedures of organic solvent degreasing, alkali degreasing, sand blowing or acid washing or alkali deoxidation, passivation, neutralization, air drying and supplementary treatment;
removing oil by using an organic solvent: and (3) removing oil by adopting organic solvent steam or wiping the oil by using an organic solvent to remove oil stains on the surface of the workpiece to be passivated. Organic solvent degreasing is used to remove unsaponifiable oils.
Alkali degreasing: and cleaning the workpiece to be passivated by adopting an alkali solution, wherein the alkali solution comprises anhydrous sodium carbonate, anhydrous sodium phosphate, sodium silicate and a surfactant. Alkaline degreasing is mainly used for removing saponifiable grease and part of non-saponifiable grease.
Blowing sand: and (3) treating the surface of the workpiece to be passivated by adopting hydraulic sand blowing or glass microsphere sand blowing, and removing an oxide film on the surface of the workpiece.
Acid washing: and if the workpiece to be passivated is made of an austenitic stainless steel material, cleaning the workpiece to be passivated by adopting a fluoronitric acid solution, wherein the fluoronitric acid solution comprises nitric acid and sodium fluoride. The pickling is mainly used for removing an oxide film on the surface of an austenitic material workpiece.
Alkali deoxidation: and if the workpiece to be passivated is made of a martensitic or ferritic stainless steel material, deoxidizing the workpiece to be passivated by adopting a sodium hydroxide-sodium glucoheptonate solution. The alkali deoxidation is mainly used for removing an oxide film on the surface of a ferrite or martensite workpiece.
Passivation: passivating a workpiece to be passivated by adopting a nitric acid solution to form a passivation layer on the surface of the workpiece;
neutralizing: cleaning the surface of the passivated workpiece by adopting a sodium carbonate solution to neutralize the residual acid solution;
air drying: removing the residual solution on the surface of the workpiece after neutralization and cleaning by adopting gas blowing;
and (3) supplementary treatment: firstly, soaking an air-dried workpiece by adopting a mixed solution of a metal chemical conversion solution and deionized water, and then drying the soaked workpiece; when soaking, the temperature of the mixed solution is 10-35 ℃, the soaking time is 1-1.5 min, the pH value of the mixed solution is 11.1-12.6, the drying temperature is 80-120 ℃, and the drying time is 15-50 min; and performing supplementary treatment on the workpiece, and performing secondary oxidation and hole sealing treatment on the surface passivation layer of the workpiece to improve the compactness of the passivation layer. And during the supplementary treatment, the workpiece is dried, so that the stability of the passivation layer is improved. The pH value of the mixed solution is lower than 11.1, and the effective components of the mixed solution are decomposed, so that the content of the effective components is too low, and secondary oxidation and hole sealing treatment cannot be carried out. The pH value of the mixed solution is more than 12.6, the effective components of the mixed solution are too high, and the generated passivation film is easily dissolved by the mixed solution.
In this embodiment, the method for passivating the surface of a stainless steel material is improved, and neutralization treatment and supplementary treatment steps are added for carrying out reoxidation and hole sealing treatment on the surface passivation layer of a workpiece, so that the compactness of the passivation layer is improved, and the environmental corrosion resistance of the stainless steel material part is improved.
Specifically, this embodiment provides a process flow, which includes the following steps: the method comprises the steps of inspection and acceptance before the working procedure, organic solvent oil removal, isolation, loading and hanging, alkali oil removal, flowing cold water washing, sand blowing or acid washing or alkali deoxidation, flowing cold water washing, passivation, flowing cold water washing, neutralization, deionized water washing, air drying, dehydrogenation, deionized water washing, supplement treatment and quality inspection. After each working procedure of organic solvent oil removal, alkali oil removal, acid washing, alkali deoxidation, passivation and neutralization is completed, a workpiece is cleaned by adopting flowing cooling water or deionized water; and after the neutralization treatment process and the supplementary treatment process are finished, cleaning the workpiece by using deionized water.
The specific procedures of this example are described below:
1. acceptance before working procedure
Before the compound passivation, all the working procedures of machining, forming, welding and the like, including the inspection of the working procedures of raw materials, heat treatment, machining, magnetic flaw detection and the like, are finished.
The heat-treated parts are not allowed to carry residual dirt and scale which are not removed to any great extent.
The surface of the part is not allowed to have solder residues, slag and the like which cannot be removed by sand blowing.
The surface of the part should be free of burrs, cracks, scratches, pits, and other mechanical damage.
The sand blown parts are not allowed to have residual scale.
2. Oil removal by organic solvents
The oil can be removed by trichloroethylene steam or wiping with an organic solvent. Trichloroethylene vapor degreasing was performed as TY504SC 0098. And organic solvents such as methyl ethyl ketone, acetone and the like or FSQ-2106A degreasing agents can be adopted to soak the surface of the part or manually wipe the surface of the part to remove oil stains on the surface.
The oil removing parameters and the method of the FSQ-2106A oil removing agent are as follows:
oil removal agent: water 1: 5-10 (volume ratio); temperature: room temperature; soaking time: 5-10 min or 2-3 times of wiping.
The manual wiping method comprises the following steps: the oil removing agent is dipped in clean non-woollen cloth or pure cotton cloth, the surface of the part is uniformly wiped, and the polluted pure cotton cloth is not allowed to be reused.
3. Isolation and mounting hanger
When the assembly or the part with special requirements is passivated, the non-passivated surface and the gap need to be isolated and protected.
The parts and the hanging tool need to be firmly contacted, the surfaces of the parts are ensured not to be stamped and deformed, and the parts are convenient to assemble and disassemble. Air pressure or entrapment of the solution should be avoided as much as possible.
4. Alkali degreasing
And cleaning the workpiece to be passivated by adopting an alkali solution, wherein the alkali solution comprises anhydrous sodium carbonate, anhydrous sodium phosphate, sodium silicate and a surfactant.
The components and the concentrations of the components of the alkaline solution in this example are: 35-45 g/l of anhydrous sodium carbonate, 0.3-0.5 g/l of sodium silicate and 10ml/l of No 631 surfactant. The temperature of alkali degreasing is 55-65 ℃, and the time is 5-15 min.
The preparation method of the No 631 surfactant comprises the following steps: the proportion of No 631 surfactant per liter is as follows: 60g of F68, 30g of 90F, 10g of L61 and the balance of water.
In this embodiment, after the alkali degreasing water is cleaned, the water film continuity is detected, and the continuous water film 30S formed on the surface of the part is not broken and qualified for degreasing, otherwise, the oil is removed again.
5. Sand blasting
And when the surface of the part has more residual oxide films, the precision requirement of the part is not high, and the surface roughness requirement is not high, sand blasting is adopted. When the sand blowing treatment is adopted, the parts are not subjected to acid washing and alkali deoxidation treatment.
In this embodiment, the surface of the part is treated by hydraulic sand blasting or glass microsphere sand blasting, but the requirements of drawing size and surface roughness are met. Attention is paid to the isolation and protection of the non-sand-blowing surface before sand blowing.
Hydraulic sand blasting was performed according to TY504SC0085 production instructions; glass microsphere blowing was performed according to ZT504SC0053 production instructions. The glass microsphere sand blasting is mainly used for the surfaces of parts with higher requirements on surface roughness, and for parts with precision or special requirements, the glass microsphere sand blasting with the granularity of more than 400 meshes can be selected.
6. Acid pickling
And when the workpiece to be passivated is made of austenitic stainless steel, cleaning by using a nitric fluoride solution.
And cleaning a workpiece to be passivated by adopting a fluoronitric acid solution, wherein the fluoronitric acid solution comprises nitric acid and sodium fluoride. The fluorine nitric acid solution comprises the following components in percentage by weight: 190 ml/l-210 ml/l of nitric acid, 20 g/l-25 g/l of sodium fluoride and deionized water.
The pickling temperature is 55-65 ℃, and the pickling time is 4-6 min.
In order to prevent the austenitic stainless steel with strong cold deformation from being over-corroded during the sodium fluoride-nitric acid pickling, the method is adopted only under the condition that the part is proved to have no influence after the pickling through inspection.
7. Alkali deoxidation
When the workpiece material to be passivated is a martensite or ferrite stainless steel material, a sodium hydroxide-sodium glucoheptonate solution is adopted for cleaning.
And deoxidizing the workpiece to be passivated by adopting a sodium hydroxide-sodium glucoheptonate solution. The sodium hydroxide-sodium glucoheptonate solution comprises the following components in percentage by concentration: 300g/l plus or minus 30g/l of sodium hydroxide, 50g/l to 80g/l of sodium glucoheptonate and deionized water. The temperature of the alkali deoxidation is 75-85 ℃.
8. Passivation of
And passivating the workpiece to be passivated by adopting a nitric acid solution to form a passivation layer on the surface of the workpiece. Preparing a nitric acid solution by using nitric acid and deionized water in a volume ratio of 1: 1; the passivation temperature is 20-25 ℃, and the passivation time is 25-30 min.
9. Neutralization
And cleaning the passivated workpiece surface by using a sodium carbonate solution to neutralize the residual acid solution. The concentration of the sodium carbonate solution is 20-50 g/l.
10. Air drying
And (4) removing the residual solution on the surface of the workpiece after the neutralization and cleaning by adopting gas blowing. The air is dried by compressed air without oil and water, and the temperature of the air is not more than 70 ℃. The compressed air should meet the requirements of TY504SC0104 surface treatment plant compressed air. The dried parts are strictly forbidden to be taken by bare hands, and the parts are taken by wearing clean pure cotton gloves.
11. Dehydrogenation
And (3) passivating the parts with the strength value of more than or equal to 1050MPa, and then removing hydrogen at 190 +/-10 ℃ after air drying, wherein the hydrogen removal time is more than or equal to 3 h. The time interval between the part after passivation treatment and hydrogen removal is not allowed to exceed 24 h.
12. Supplemental treatment
Firstly, soaking an air-dried workpiece by adopting a mixed solution of a metal chemical conversion solution and deionized water, and then drying the soaked workpiece; when soaking, the temperature of the mixed solution is 10-35 ℃, the soaking time is 1-1.5 min, the pH value of the mixed solution is 11.1-12.6, the drying temperature is 80-120 ℃, and the drying time is 15-50 min; and performing supplementary treatment on the workpiece, and performing secondary oxidation and hole sealing treatment on the surface passivation layer of the workpiece to improve the compactness of the passivation layer.
The metal chemical conversion liquids of this example were Bonderite S-FN 3000 and Bonderite S-FN 3001. In this embodiment, the ratio of the metal chemical conversion solution to the deionized water is: bonderite S-FN 3000 (200g/l to 500g/l), Bonderite S-FN 3000: bonderite S-FN 3001 ≈ 10: 1 (volume ratio), deionized water.
13. Quality inspection
After the above procedures are carried out, the quality of the parts is inspected, including appearance inspection, corrosion resistance inspection and damp-heat test.
The appearance inspection requirements are as follows: the surface of the part after the composite passivation treatment is visually checked and should be silvery white, grey white or steel grey.
a) Allowing for defects:
1) allowing slight color changes in the weld area;
2) slight color unevenness of the surface of the part is allowed;
3) because the surface states of the parts are different, the same part has different colors and gloss.
b) Defects are not allowed:
1) ash is hung on the surface of the part;
2) no retentate is allowed on the inner surface and the outer surface of the part socket and the cavity;
3) the surface of the part has an exposed crystal structure, pits and other over-corrosion phenomena.
The corrosion resistance test requirements are as follows: according to GJB150.11A-2009 military equipment laboratory environmental test method part 11: salt spray test, the neutral salt spray test was carried out using the specified test procedure and method, using a single cycle period of 48h (24h continuous spray and 24h dry) with a cycle number of 2/4 days (96 h). A test procedure of 48h continuous spraying and 48h drying was also used. After the test is finished, the surface of the test piece is qualified without rusty spots, and the machined edge of the part is not used as the inspection basis.
The damp heat test requirements are as per section 9 of the military equipment laboratory environmental test method GJB150.9A-2009: the test method defined in Damp-Heat test was conducted.
The film integrity inspection requires that the parts after composite passivation are immersed into a test solution with the following components at room temperature, kept for 5 minutes, taken out and checked for copper deposition on the surfaces. Or dripping 1-2 drops of test solution on the surface of the part to be detected, wiping the test solution after 5 minutes, and detecting whether the part has contact copper. The components and concentrations of the test solution were as follows:
copper sulfate (CuSO4.5H2O) chemical purity concentration 16g/l
Sulfuric acid (H2SO4 weight ratio 1.84) chemical purity concentration 4ml/l
The balance of deionized water.
Claims (9)
1. The composite passivation method of the stainless steel material is characterized by comprising at least one of organic solvent degreasing, alkali degreasing, sand blowing, acid washing or alkali deoxidation, passivation, neutralization, air drying and supplementary treatment processes; wherein the content of the first and second substances,
removing oil by using an organic solvent: removing oil by using organic solvent steam or wiping the workpiece by using an organic solvent to remove oil stains on the surface of the workpiece to be passivated;
alkali degreasing: cleaning a workpiece to be passivated by adopting an alkali solution, wherein the alkali solution comprises anhydrous sodium carbonate, anhydrous sodium phosphate, sodium silicate and a surfactant;
at least one treatment process of sand blowing, acid washing or alkali deoxidation, wherein the sand blowing treatment is to treat the surface of a workpiece to be passivated by adopting hydraulic sand blowing or glass microsphere sand blowing and is used for removing an oxide film on the surface of the workpiece; pickling, namely cleaning the workpiece to be passivated by adopting a fluoronitric acid solution if the workpiece to be passivated is made of an austenitic stainless steel material, wherein the fluoronitric acid solution comprises nitric acid and sodium fluoride; performing alkali deoxidation treatment, namely, if the workpiece to be passivated is made of a martensite or ferrite stainless steel material, deoxidizing the workpiece to be passivated by adopting a sodium hydroxide-sodium glucoheptonate solution;
passivation: passivating a workpiece to be passivated by adopting a nitric acid solution to form a passivation layer on the surface of the workpiece;
neutralizing: cleaning the surface of the passivated workpiece by adopting a sodium carbonate solution to neutralize the residual acid solution;
air drying: removing the residual solution on the surface of the workpiece after neutralization and cleaning by adopting gas blowing;
and (3) supplementary treatment: firstly, soaking an air-dried workpiece by adopting a mixed solution of a metal chemical conversion solution and deionized water, and then drying the soaked workpiece; when soaking, the temperature of the mixed solution is 10-35 ℃, the soaking time is 1-1.5 min, the pH value of the mixed solution is 11.1-12.6, the drying temperature is 80-120 ℃, and the drying time is 15-50 min; and performing supplementary treatment on the workpiece, and performing secondary oxidation and hole sealing treatment on the surface passivation layer of the workpiece to improve the compactness of the passivation layer.
2. The composite passivation method according to claim 1, characterized in that, before degreasing with organic solvent, the method further comprises removing oxide film and contaminants on the surface of the workpiece to be passivated; the surface of the passivated workpiece is free of burrs, cracks or scratches.
3. The composite passivation method of claim 1, characterized in that, when vapor of organic solvent is used for removing oil, the organic solvent is trichloroethylene.
4. The composite passivation method of claim 1, characterized in that after the alkali degreasing, the method further comprises a water film continuity check of the workpiece surface to be passivated after the alkali degreasing process, a continuous water film is formed on the workpiece surface, the water film 30S is not broken and qualified for degreasing, otherwise, alkali degreasing is carried out again.
5. The composite passivation method of claim 1, characterized in that the sodium hydroxide-sodium glucoheptonate solution comprises sodium hydroxide, sodium glucoheptonate complex and deionized water; and the temperature of the sodium hydroxide-sodium glucoheptonate solution is 75-85 ℃ during alkali deoxidation.
6. The composite passivation method of claim 1, characterized in that a nitric acid solution is prepared by using nitric acid and deionized water in a volume ratio of 1: 1; the composite passivation temperature is 20-25 ℃, and the passivation time is 25-30 min.
7. The composite passivation method of claim 1, characterized in that before the workpiece is subjected to the additional treatment and after the air drying, the method further comprises dehydrogenation, and the workpiece is dehydrogenated at 190 ℃ ± 10 ℃, and the dehydrogenation time t is more than or equal to 3 h.
8. The composite passivation method of claim 1, characterized in that during the neutralization process, sodium carbonate and deionized water are mixed to prepare a sodium carbonate solution, and the concentration of the sodium carbonate solution is 20-50 g/l.
9. The composite passivation method of claim 1, further comprising the steps of degreasing with an organic solvent, degreasing with an alkali, pickling, deoxidizing with an alkali, passivating, and neutralizing, wherein after each step is completed, the workpiece is cleaned with flowing cooling water or deionized water; and after the neutralization process is finished, cleaning the workpiece by using deionized water.
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| CN115896769A (en) * | 2023-02-03 | 2023-04-04 | 广东腐蚀科学与技术创新研究院 | Inter-production-sequence protection passivation treating fluid for coated steel plate and preparation method and film forming process thereof |
| CN116197092A (en) * | 2022-12-09 | 2023-06-02 | 哈尔滨哈飞航空工业有限责任公司 | Surface treatment method for stainless steel sheet before cementing |
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