CN116103644A - Phosphating process of chromium-free super-strong steel material - Google Patents
Phosphating process of chromium-free super-strong steel material Download PDFInfo
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- CN116103644A CN116103644A CN202211713399.9A CN202211713399A CN116103644A CN 116103644 A CN116103644 A CN 116103644A CN 202211713399 A CN202211713399 A CN 202211713399A CN 116103644 A CN116103644 A CN 116103644A
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- phosphating
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- 239000000463 material Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 37
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 36
- 239000010959 steel Substances 0.000 title claims abstract description 36
- 238000007789 sealing Methods 0.000 claims abstract description 36
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000004140 cleaning Methods 0.000 claims abstract description 30
- 238000000227 grinding Methods 0.000 claims abstract description 30
- 230000007797 corrosion Effects 0.000 claims abstract description 22
- 238000005260 corrosion Methods 0.000 claims abstract description 22
- 230000003750 conditioning effect Effects 0.000 claims abstract description 16
- 239000000126 substance Substances 0.000 claims abstract description 16
- 230000007935 neutral effect Effects 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 41
- 239000000243 solution Substances 0.000 claims description 26
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 18
- 238000005238 degreasing Methods 0.000 claims description 17
- 238000002791 soaking Methods 0.000 claims description 17
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000013527 degreasing agent Substances 0.000 claims description 11
- 238000005237 degreasing agent Methods 0.000 claims description 11
- 238000005498 polishing Methods 0.000 claims description 11
- 239000011550 stock solution Substances 0.000 claims description 10
- 239000012190 activator Substances 0.000 claims description 9
- 239000003112 inhibitor Substances 0.000 claims description 9
- 239000012530 fluid Substances 0.000 claims description 8
- 239000002199 base oil Substances 0.000 claims description 7
- 239000012286 potassium permanganate Substances 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- 239000004615 ingredient Substances 0.000 claims description 6
- 238000006386 neutralization reaction Methods 0.000 claims description 6
- 235000006408 oxalic acid Nutrition 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims description 3
- 230000000996 additive effect Effects 0.000 claims description 3
- 150000002191 fatty alcohols Chemical class 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims description 3
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 3
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 abstract description 18
- 229910052751 metal Inorganic materials 0.000 abstract description 7
- 239000002184 metal Substances 0.000 abstract description 7
- 238000004381 surface treatment Methods 0.000 abstract description 6
- 239000007788 liquid Substances 0.000 description 11
- 238000012360 testing method Methods 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 10
- 239000013081 microcrystal Substances 0.000 description 10
- 239000007921 spray Substances 0.000 description 10
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 7
- 230000002378 acidificating effect Effects 0.000 description 6
- 238000002161 passivation Methods 0.000 description 6
- 229910052804 chromium Inorganic materials 0.000 description 5
- 239000011651 chromium Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000003814 drug Substances 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- CPSYWNLKRDURMG-UHFFFAOYSA-L hydron;manganese(2+);phosphate Chemical compound [Mn+2].OP([O-])([O-])=O CPSYWNLKRDURMG-UHFFFAOYSA-L 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910000423 chromium oxide Inorganic materials 0.000 description 2
- 239000008139 complexing agent Substances 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- -1 iron ions Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 230000001131 transforming effect Effects 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- SCYYUUINVKYGRP-UHFFFAOYSA-K P(=O)([O-])([O-])[O-].[Zn+2].[Mn+2] Chemical compound P(=O)([O-])([O-])[O-].[Zn+2].[Mn+2] SCYYUUINVKYGRP-UHFFFAOYSA-K 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- 239000002981 blocking agent Substances 0.000 description 1
- IQBJFLXHQFMQRP-UHFFFAOYSA-K calcium;zinc;phosphate Chemical compound [Ca+2].[Zn+2].[O-]P([O-])([O-])=O IQBJFLXHQFMQRP-UHFFFAOYSA-K 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000003642 hunger Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910000398 iron phosphate Inorganic materials 0.000 description 1
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 239000012224 working solution Substances 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
Classifications
-
- 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
- C23C22/07—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 containing phosphates
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The invention discloses a phosphating process of a chromium-free super-strong steel material, belonging to the technical field of metal surface treatment methods. Sequentially carrying out magnetic grinding, chemical rust removal, ultrasonic oil removal cleaning, surface conditioning treatment, phosphating treatment and oily sealing treatment on the material; the corrosion resistance of the novel super-strong steel material is improved, so that the neutral salt fog can at least pass through 8 hours, and the limit salt fog rusting time exceeds 120 hours.
Description
Technical Field
The invention relates to the technical field of metal surface treatment methods, in particular to a phosphating process of a chromium-free super-strong steel material.
Background
The common stainless steel has strong corrosion resistance mainly because an obvious chromium oxide film is formed on the surface of the stainless steel, and the content of oxygen element and chromium element has minimum requirement (10.5 percent) to obtain a continuous protective film so as to inhibit the occurrence of corrosion; if the protective film is damaged, it can recover naturally; increasing the chromium content increases the corrosion resistance of the stainless steel and enhances its ability to self-repair when the chromium oxide film is damaged. However, when the components do not contain chromium element, the salt fog can not meet the 8-hour requirement by adopting the common conventional passivation technology, and other conventional coating technologies such as PVD (physical vapor deposition), spraying and electroplating are high in cost, and the generated film is additionally added on the metal substrate.
Phosphating is classified by the phosphate used: zinc phosphate, zinc calcium phosphate, iron phosphate, zinc manganese phosphate, and manganese phosphate; the classification according to the temperature of phosphating is: high temperature (over 80 ℃) phosphating, medium temperature (50-70 ℃) phosphating, low temperature phosphating (about 40 ℃) and normal temperature phosphating (10-30 ℃). For example, the Chinese patent publication No. CN107099792A discloses a steel surface phosphating process, which specifically comprises deslagging, polishing, degreasing, surface conditioning and phosphating, wherein the phosphating is carried out at a lower temperature, and the requirement on the wear resistance of a phosphating film cannot be met. The phosphating film is thin, but is a non-metal non-conductive isolation layer, so that the excellent conductor on the surface of the metal workpiece can be converted into a poor conductor, the formation of micro cells on the surface of the metal workpiece is inhibited, and further, the corrosion of a coating film is effectively prevented. The phosphating film has porosity, and the salt spray test directly after phosphating cannot meet the test requirement.
Therefore, there is an urgent need to develop a new process capable of satisfying the salt spray requirements while simultaneously spontaneously growing a plating process from the substrate with low cost of chromium.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a phosphating process for chromium-free super-strong steel materials, which is low in cost and meets the salt spray test requirements.
In order to solve the technical problems, the invention adopts the following technical scheme: a phosphating process of a chromium-free super-strong steel material, comprising the following steps:
s1, magnetic grinding: magnetically grinding the material by using grinding fluid;
s2, chemical rust removal: chemically derusting the magnetically grinded material by using a treating agent;
s3, ultrasonic degreasing and cleaning: 10-15% of alkaline or neutral degreasing agent by weight is used for ultrasonic degreasing and cleaning of the chemically derusted material;
s4, table adjustment processing: performing surface conditioning treatment on the material subjected to ultrasonic degreasing and cleaning by using a surface conditioning agent;
s5, phosphating: phosphating the surface-modified material by using phosphating solution;
s6, oily sealing treatment: and (3) carrying out oily sealing treatment on the phosphated material by using a sealing agent.
The invention has the beneficial effects that: in the phosphating process of the chromium-free super-strong steel material, the physical rust removal and chemical rust removal processes are added before phosphating, and the phosphating technology and the sealing technology are combined to be applied to the chromium-free super-strong steel material, so that the corrosion resistance of a new material of the super-strong steel can be greatly improved, and at least 8 hours can be passed in a neutral salt spray test.
Detailed Description
In order to describe the technical contents, the achieved objects and effects of the present invention in detail, the following description will be made with reference to the embodiments.
The most critical concept of the invention is as follows: by adding physical rust removal and chemical rust removal processes before phosphating, the corrosion resistance of the novel super-strong steel material is improved, so that the requirements of salt spray testing are met.
The invention relates to a phosphating process of a chromium-free super-strong steel material, which comprises the following steps of:
sequentially carrying out magnetic grinding, chemical rust removal, ultrasonic oil removal cleaning, surface conditioning treatment, phosphating treatment and oily sealing treatment on the material; the material is super-strong steel with the hardness of 500-600 HV, is suitable for being used as a rotating shaft of a folding screen mobile phone, and contains 8-9wt% of cobalt, 16-17wt% of nickel and 7-8wt% of molybdenum as main alloy components, and does not contain chromium.
The invention relates to a phosphating process of a chromium-free super-strong steel material, which specifically comprises the following steps:
s1, magnetic grinding: magnetically grinding the material by using grinding fluid;
s2, chemical rust removal: chemically derusting the magnetically grinded material by using a treating agent;
s3, ultrasonic degreasing and cleaning: 10-15% of alkaline or neutral degreasing agent by weight is used for ultrasonic degreasing and cleaning of the chemically derusted material;
s4, table adjustment processing: performing surface conditioning soaking treatment on the material subjected to ultrasonic degreasing and cleaning by using a surface conditioning agent;
s5, phosphating: carrying out phosphating soaking treatment on the material subjected to the surface conditioning treatment by using phosphating solution;
s6, oily sealing treatment: and (3) carrying out oily sealing soaking treatment on the phosphated material by using a sealing agent.
From the above description, the beneficial effects of the invention are as follows: by adding physical rust removal and chemical rust removal processes before phosphating and combining the phosphating technology and the sealing technology on the chromium-free super-strong steel material, the corrosion resistance of the super-strong steel material can be greatly improved, so that the neutral salt fog can at least pass 8 hours, the limit salt fog rust time exceeds 120 hours, and the corrosion resistance of the passivation process is far exceeded.
Further, in step S1, the grinding parameters of the magnetic grinding are: rotational speed: 15-20 Hz; grinding time: 20-30 mm; size of steel needle: 0.4 x 8mm/10mm or 0.5 x 8mm/10mm; grinding fluid: neutral or alkaline grinding fluid.
As can be seen from the above description, the magnetic grinding means that the workpiece is mixed with water, abrasive and grinding agent, friction force is generated by high-speed rotation of a machine, so that the surface and the size of the workpiece reach the standard of quality requirements, and the magnetic grinding can make the surface of the product rough, sharp-angle, burr, sharp-edge, large-size and other defective workpiece to achieve brightness, smoothness, size and the like, so that the workpiece meets the quality requirements.
Furthermore, the magnetic grinding is carried out by pure water, 4-6L of pure water is added and 200-300 mL of alkaline grinding liquid is added when each magnetic grinding barrel is singly ground, tap water or circulating water is forbidden, and otherwise, the workpiece is blackened.
Further, the polishing slurry was purchased from Shenzhen Shunjia polishing technology Co., ltd.
From the above description, it is understood that the pH of the polishing liquid is 7 or more, and the polished workpiece is directly blackened if an acidic polishing liquid is used, which has a great influence on the subsequent salt spray performance.
Further, in step S2, the chemical rust removing treatment is a rust removing treatment using a treating agent immersing material, and the rust removing temperature must be 80 ℃ or higher, and the rust removing time at this temperature is at least 10 minutes. The specific parameters of chemical rust removal are as follows: treating agent: 10-15% alkaline potassium permanganate solution; derusting temperature: at a temperature of more than 80 ℃; derusting time: and not less than 10min.
From the above description, it is known that the rust remover prohibits the use of acidic rust removers, such as hydrofluoric acid, hydrochloric acid, nitric acid, citric acid, sulfuric acid, etc., and rust removal with these acidic chemical agents can cause serious corrosion of the workpiece directly, resulting in blackening, starving, and even scrapping.
Further, the treating agent contains potassium permanganate, sodium hydroxide and a corrosion inhibitor, wherein the potassium permanganate comprises the following components in parts by weight: sodium hydroxide is 2:1.
from the above description, it is known that the corrosion inhibitor includes benzotriazole, hydrogen peroxide or polyethylene glycol.
Further, in step S3, the ultrasonic degreasing cleaning step includes: soaking a workpiece by adopting an oil removing agent, cleaning the workpiece by 2 times of pure water, and then carrying out acid washing neutralization by using 5% -10% oxalic acid solution, wherein the temperature is normal temperature, and the time is 2-3 min; after neutralization of oxalic acid, 2 times of pure water is used for cleaning, and then the cleaning is further carried out, wherein the cleaning temperature is 80-90 ℃.
From the above description, the workpiece is further cleaned using an automatic cleaning line.
Further, in step S3, the degreasing agent is purchased from Shenzhen Xiang Hebangtai Lubricant Co., ltd. And is composed of the following ingredients in parts by weight: 6-11 parts of fatty alcohol polyoxyethylene ether, 8-13 parts of nonionic activator, 10-15 parts of sodium carbonate, 8-12 parts of surfactant and 5-10 parts of sodium tripolyphosphate.
From the above description, the ultrasonic degreasing refers to ultrasonic degreasing cleaning by using a degreasing agent with the concentration of 10-15%, wherein the degreasing agent comprises the following ingredients in parts by weight: 6 to 11 parts of fatty alcohol polyoxyethylene ether, 8 to 13 parts of nonionic activator, 10 to 15 parts of sodium carbonate, 8 to 12 parts of surfactant and 5 to 10 parts of sodium tripolyphosphate, wherein the cleaning temperature is 80 to 90 ℃; the degreasing agent must be alkaline or neutral, prohibiting the use of an acidic degreasing agent.
Further, in step S4, the surface conditioning process is to soak the workpiece with a surface conditioning agent, where the surface conditioning agent is used as a stock solution, and the temperature is normal temperature, and the soaking time is: 40-70 s, pH value: 8-10.
From the above description, the surface regulator is called as microcrystal activator, which has the main functions of overcoming the roughening phenomenon of the coating, eliminating the defects of uneven corrosion and the like caused by degreasing or rust removal of the metal workpiece with strong alkalinity, improving the microcrystal conversion (phosphating) speed, shortening the treatment time, enabling the metal workpiece to generate a compact and uniform film layer in the microcrystal conversion (phosphating) process, enhancing the corrosion resistance, improving the coating adhesive force, reducing the sediment and the like. When the pH of the microcrystal activator is reduced due to the mixing of acidic substances, the pH value of the tank liquor is kept about 8-10 during operation by taking care of timely supplementing fresh medicament, and when the microcrystal activator tank liquor exceeds the working range or the mixed impurities turn into yellow brown or brown, the microcrystal activator tank liquor is discarded in time and the tank is re-established.
Further, in step S5, the phosphating treatment is performed by soaking in a phosphating solution, wherein the phosphating solution is a high Wen Meng series phosphating solution, the stock solution is used, the use temperature is higher than 90 ℃, and the soaking time is as follows: 4-7 min, the density is 1.402+/-0.04 kg/m 3 The total acidity, namely the acidity of phosphoric acid and dimanganese hydrogen phosphate is 6-150 PT, and the free acidity, namely the concentration of phosphoric acid is 8-30 PT.
From the above description, the main component of the phosphating film formed after phosphating is a manganese phosphate film, and during phosphating, acidic substances in the phosphating solution are continuously consumed and the effect of carried objects on the workpiece is affected because the phosphating solution is in a high-temperature state for a long time, so that the liquid medicine should be timely added every half a day according to the liquid level drop of the liquid medicine. The sediment in the tank liquor is removed by using an overhead tank or a filtering pump, so that the tank liquor components are stabilized, the service life is prolonged, and the consumption of the stock liquor is reduced. For better control of the components of the liquid medicine, 3 repeated liquid medicine titration tests should be carried out every 3 days, and sediment and tank liquor can be properly discharged and water is replenished when the total acid is more than 150 pT. When the total acidity is less than 60, all the components should be replaced; the content mass fraction of the product is changed by 1%, and the acidity is changed by about 0.5PT. Practice proves that: the working solution is used for a long time, when the total acidity content in the solution is less than 60PT, the performance can be drastically reduced, no matter how the new solution is added, the requirement is difficult to be met, and the tank solution is poured out to replace the new solution. To maintain the stability of the passivating liquid, it is suggested to examine the acidity of the bath every 2 to 3 days, which is the most effective control method. The phosphating solution is sensitive to the content of iron ions, so that the conversion solution is forbidden to be in direct contact with all iron containers or hangers in the production process.
Further, in step S6, the blocking agent is composed of the following ingredients in parts by weight: 25 parts of base oil and 75 parts of additive, wherein the stock solution is used, the soaking time is 10-60 s, and the temperature is normal temperature; the sealer 7d was filtered once and the base oil was replaced once at 30 d.
Preferably, the sealing agent is an oily sealing agent, wherein the oily sealing agent is an oily sealing agent 'Fe-1 oily sealing agent' developed by Huishuka surface treatment materials Co-Ltd, the base oil accounts for 25% and the additive accounts for 75% of the oily sealing agent, the low-viscosity refined mineral oil is used as the base oil, and a plurality of high-quality rust inhibitors, cosolvents and antioxidants are added, and the sealing agent is prepared by adopting a special production process, wherein the main rust inhibitor is an independently developed high-efficiency oil-soluble corrosion inhibitor.
As is apparent from the above description, the pore sealing agent is classified into an aqueous pore sealing agent and an oily pore sealing agent according to the type of solvent, and the aqueous pore sealing agent is composed of a long-chain alkane compound containing sulfur or silicon element, a corrosion inhibitor, water, an organic solvent, and the like. The oily hole sealing agent consists of base oil, corrosion inhibitor, diluent (alkane) and the like. In contrast, oily hole-sealing agents are used more frequently with a fast film formation rate, good stability, and good functionality. After phosphating, the product is soaked in the oily hole sealing agent, a layer of thin oily hole sealing agent can be adhered to the phosphating film, the holes of the phosphating film can be well adhered, and then the solvent is removed by high-temperature baking, so that a uniform and compact film can be obtained on the surface of the phosphating film, and the film can isolate the phosphating layer from contacting with the environment, and the corrosion resistance of the plating layer is improved.
Example 1 of the present invention is:
a phosphating process of a chromium-free super-strong steel material, comprising the following steps:
s1, magnetic grinding: magnetically grinding the material by using grinding fluid;
the magnetic grinding parameters are as follows: frequency: 15HZ; time: 10mm; steel needle: steel needle with phi 0.5 mm by 10mm; grinding fluid: the alkaline polishing liquid is purchased from alkaline polishing liquid SJ-Y115 manufactured by Shenzhen Shunjia polishing technology Co., ltd;
s2, chemical rust removal: chemically derusting the magnetically grinded material by using a treating agent, wherein the derusting temperature is 80 ℃, and the derusting time is 10 minutes at the temperature; the specific parameters of chemical rust removal are as follows: treating agent: 12.5% alkaline potassium permanganate solution; derusting temperature: 80 ℃; derusting time: for 10min;
s3, ultrasonic degreasing and cleaning: soaking a chemically derusted material by using 12.5% neutral degreasing agent in parts by weight, cleaning by using 2 pure water, and then carrying out acid washing neutralization by using 12.5% oxalic acid solution at normal temperature for 2min; 2 times of pure water is used for cleaning after oxalic acid neutralization, and then an automatic cleaning line is used for further cleaning, wherein the cleaning temperature is 85 ℃;
the ultrasonic degreasing parameters are as follows: concentration: 12.5%; temperature: 85 ℃; time: 5 minutes; the degreasing agent is an alkaline degreasing agent BTO-2018 manufactured by Shenzhen Xiang Hebangtai lubricating material Co., ltd;
s4, table adjustment processing: performing surface conditioning treatment on the material subjected to ultrasonic degreasing cleaning in a surface conditioning tank by using a surface conditioning agent;
the parameters of the meter-adjusting groove are as follows: the model of the surface regulator is a microcrystal activator KM200, and the microcrystal activator KM200 is a surface regulator specially developed by Dongguan Kai allied surface treatment technology development limited company for the novel chromium-free super-strength steel material; the stock solution is used at normal temperature, the soaking time is 60 seconds, and the pH value is 10;
s5, phosphating: phosphating the surface-modified material in a phosphating tank by using phosphating solution;
the parameters of the phosphating tank are as follows: the phosphating solution is high Wen Meng phosphating solution, the model of the phosphating solution is a microcrystal transforming agent KM0501, and the microcrystal transforming agent KM0501 is phosphating solution specially developed by the Dongguan, kaban surface treatment technology development limited company aiming at the novel chromium-free super-strong steel material; the stock solution is used, the use temperature is 95 ℃, the soaking time is 4 minutes, the density (25 ℃) is 1.402, the total acidity is 62PT (the acidity of phosphoric acid and manganese hydrogen phosphate), and the free acidity is 15PT (the concentration of phosphoric acid);
s6, oily sealing treatment: using a sealing agent to carry out oily sealing treatment on the phosphatized material in a sealing groove;
the parameters of the closed groove are as follows: the sealing agent is Fe-1 oily sealing agent, and the Fe-1 oily sealing agent is an oily sealing agent developed by Huizhou SiKai surface treatment materials Co.Ltd; the temperature is normal temperature; the soaking time is 30 seconds;
the work piece produced by the process is subjected to neutral salt spray test, the work piece still does not rust after 8 hours of test time, the salt spray limit test is performed, and finally the rust phenomenon occurs after 120 hours.
Comparative example 1
Comparative example 1 differs from example 1 only in that the phosphating temperature in the S5 phosphating treatment is 85 deg.c, and the effect of the phosphating temperature on the salt spray is compared, and the test result shows that the rust phenomenon occurs after 6 hours of the salt spray.
Comparative example 2
Comparative example 1 differs from example 1 only in that the passivation process was used instead of the S4 conditioning and S5 phosphating, and the test results showed that the rusting phenomenon occurred after 4 hours of salt fog.
The specific steps of comparative example 2 are:
s1, S2 and S3 are all identical to those of example 1;
s4, passivating the workpiece subjected to ultrasonic degreasing and cleaning in a passivation tank;
the parameters of the passivation tank are as follows: the model of the passivating agent is DunHua400C, the use temperature of the stock solution is 60 ℃, and the soaking time is 30 minutes.
S5, carrying out coordination treatment on the passivated workpiece in a coordination groove;
the parameters of the coordination groove are as follows: the complexing agent is DunHua401A, the stock solution is used at 60 ℃ and the soaking time is 30 minutes. The complexing agent consists of the following ingredients in parts by weight: 2-5 parts of inorganic acid, 3-7 parts of chromate and 1-6 parts of corrosion inhibitor;
s6, carrying out oily sealing treatment on the workpiece subjected to coordination treatment, wherein the specific operation steps are the same as those in the embodiment 1.
In summary, in the phosphating process of the super-strong steel material without chromium, physical rust removal and chemical rust removal processes are added before phosphating, and the phosphating technology and the sealing technology are combined to be applied to the super-strong steel material without chromium, so that the corrosion resistance of the novel material of the super-strong steel can be greatly improved, the neutral salt fog can be at least 8 hours, the limit salt fog rust time is more than 120 hours, and the corrosion resistance of the passivation process is far exceeded.
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent modifications made by the present invention or directly or indirectly applied to the related technical field are included in the scope of the present invention.
Claims (10)
1. A phosphating process of a chromium-free super-strong steel material, which is characterized by comprising the following steps:
and sequentially carrying out magnetic grinding, chemical rust removal, ultrasonic oil removal cleaning, surface conditioning treatment, phosphating treatment and oily sealing treatment on the material.
2. The process for phosphating a chromium-free super-strong steel material according to claim 1, wherein in step S1, the grinding parameters of the magnetic grinding are: rotational speed: 15-20 Hz; grinding time: 20-30 mm; size of steel needle: 0.4 x 8mm/10mm or 0.5 x 8mm/10mm; grinding fluid: neutral or alkaline grinding fluid.
3. The process according to claim 2, wherein in step S1, the polishing slurry is obtained from alkaline polishing slurry SJ-Y115 of Shenzhen Shunja polishing technology Co.
4. The process for phosphating a chromium-free super-strong steel material according to claim 1, wherein in step S2, the parameters of the chemical rust removal are: treating agent: 10-15% alkaline potassium permanganate solution; derusting temperature: at a temperature of more than 80 ℃; derusting time: and not less than 10min.
5. The phosphating process of a chromium-free super-strong steel material according to claim 1, wherein the treating agent comprises potassium permanganate, sodium hydroxide and a corrosion inhibitor, and the potassium permanganate comprises the following components in parts by weight: sodium hydroxide is 2:1.
6. the phosphating process of a chromium-free super strong steel material according to claim 1, wherein in step S3, the ultrasonic degreasing cleaning step is: after ultrasonic degreasing, cleaning by 2 times of pure water, and then carrying out acid washing neutralization by 5% -10% oxalic acid solution, wherein the temperature is normal temperature, and the time is 2-3 min; after neutralization of oxalic acid, 2 times of pure water is used for cleaning, and then the cleaning is further carried out, wherein the cleaning temperature is 80-90 ℃.
7. The phosphating process of chromium-free super-strong steel material according to claim 1, wherein in step S3, the degreasing agent is composed of the following ingredients in parts by weight: 6-11 parts of fatty alcohol polyoxyethylene ether, 8-13 parts of nonionic activator, 10-15 parts of sodium carbonate, 8-12 parts of surfactant and 5-10 parts of sodium tripolyphosphate.
8. The phosphating process of a chromium-free super strong steel material according to claim 1, wherein in the step S4, the surface conditioner is used as a stock solution, the temperature is normal temperature, and the soaking time is: 40-70 s, pH value: 8-10.
9. A chromium-free super-strength steel according to claim 1The phosphating process of the material is characterized in that in the step S5, the phosphating solution is high Wen Meng series phosphating solution, the stock solution is used, the use temperature is higher than 90 ℃, and the soaking time is as follows: 4-7 min, the density is 1.402+/-0.04 kg/m 3 The total acidity, namely the acidity of phosphoric acid and dimanganese hydrogen phosphate is 6-150 PT, and the free acidity, namely the concentration of phosphoric acid is 8-30 PT.
10. The phosphating process of chromium-free super-strong steel material according to claim 1, wherein in step S6, the sealer consists of the following ingredients in parts by weight: 25 parts of base oil and 75 parts of additive, wherein the stock solution is used, the soaking time is 10-60 s, and the temperature is normal temperature; the sealer 7d was filtered once and the base oil was replaced once at 30 d.
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