CN116695196A - Zinc-nickel plating process for steel material - Google Patents
Zinc-nickel plating process for steel material Download PDFInfo
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- CN116695196A CN116695196A CN202310913789.9A CN202310913789A CN116695196A CN 116695196 A CN116695196 A CN 116695196A CN 202310913789 A CN202310913789 A CN 202310913789A CN 116695196 A CN116695196 A CN 116695196A
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- Prior art keywords
- nickel
- steel material
- zinc
- electroplating
- galvanized
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- 239000000463 material Substances 0.000 title claims abstract description 81
- 238000000034 method Methods 0.000 title claims abstract description 81
- 238000007747 plating Methods 0.000 title claims abstract description 75
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 59
- 239000010959 steel Substances 0.000 title claims abstract description 59
- QELJHCBNGDEXLD-UHFFFAOYSA-N nickel zinc Chemical compound [Ni].[Zn] QELJHCBNGDEXLD-UHFFFAOYSA-N 0.000 title claims abstract description 37
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 98
- 238000009713 electroplating Methods 0.000 claims abstract description 56
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 55
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 44
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 38
- 239000001257 hydrogen Substances 0.000 claims abstract description 38
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000011701 zinc Substances 0.000 claims abstract description 23
- 230000004913 activation Effects 0.000 claims abstract description 22
- 238000004140 cleaning Methods 0.000 claims abstract description 22
- 229910000797 Ultra-high-strength steel Inorganic materials 0.000 claims abstract description 19
- 238000002161 passivation Methods 0.000 claims abstract description 19
- 238000007789 sealing Methods 0.000 claims abstract description 16
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims description 32
- 238000005238 degreasing Methods 0.000 claims description 20
- 239000002253 acid Substances 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 12
- 238000007664 blowing Methods 0.000 claims description 9
- 230000008021 deposition Effects 0.000 claims description 9
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000005246 galvanizing Methods 0.000 claims 4
- 230000003213 activating effect Effects 0.000 claims 2
- 238000012360 testing method Methods 0.000 abstract description 22
- 239000011248 coating agent Substances 0.000 abstract description 21
- 238000000576 coating method Methods 0.000 abstract description 21
- 238000005260 corrosion Methods 0.000 abstract description 19
- 230000007797 corrosion Effects 0.000 abstract description 18
- 239000011159 matrix material Substances 0.000 abstract description 9
- 238000005452 bending Methods 0.000 abstract description 8
- NLBABRCZAOXCEY-UHFFFAOYSA-N [Ti+4].[Cd+2].[C-]#N.[C-]#N.[C-]#N.[C-]#N.[C-]#N.[C-]#N Chemical compound [Ti+4].[Cd+2].[C-]#N.[C-]#N.[C-]#N.[C-]#N.[C-]#N.[C-]#N NLBABRCZAOXCEY-UHFFFAOYSA-N 0.000 abstract description 3
- 230000005587 bubbling Effects 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 39
- 229910052793 cadmium Inorganic materials 0.000 description 13
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 239000011651 chromium Substances 0.000 description 9
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 8
- 230000035882 stress Effects 0.000 description 7
- 238000009864 tensile test Methods 0.000 description 7
- VIROINNDOPNTDI-UHFFFAOYSA-N cadmium titanium Chemical compound [Ti].[Cd] VIROINNDOPNTDI-UHFFFAOYSA-N 0.000 description 6
- 230000007935 neutral effect Effects 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 5
- 238000000861 blow drying Methods 0.000 description 5
- 238000011056 performance test Methods 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 description 4
- 238000005187 foaming Methods 0.000 description 4
- 238000007689 inspection Methods 0.000 description 4
- 229910001453 nickel ion Inorganic materials 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 239000011592 zinc chloride Substances 0.000 description 4
- 235000005074 zinc chloride Nutrition 0.000 description 4
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 3
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 3
- 230000032683 aging Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 description 3
- 229910001350 4130 steel Inorganic materials 0.000 description 2
- 229910021555 Chromium Chloride Inorganic materials 0.000 description 2
- 229910000990 Ni alloy Inorganic materials 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- GGVOVPORYPQPCE-UHFFFAOYSA-M chloronickel Chemical compound [Ni]Cl GGVOVPORYPQPCE-UHFFFAOYSA-M 0.000 description 2
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 description 2
- 229910000151 chromium(III) phosphate Inorganic materials 0.000 description 2
- GRWVQDDAKZFPFI-UHFFFAOYSA-H chromium(III) sulfate Chemical compound [Cr+3].[Cr+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRWVQDDAKZFPFI-UHFFFAOYSA-H 0.000 description 2
- IKZBVTPSNGOVRJ-UHFFFAOYSA-K chromium(iii) phosphate Chemical compound [Cr+3].[O-]P([O-])([O-])=O IKZBVTPSNGOVRJ-UHFFFAOYSA-K 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000002905 metal composite material Substances 0.000 description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- NHMJUOSYSOOPDM-UHFFFAOYSA-N cadmium cyanide Chemical compound [Cd+2].N#[C-].N#[C-] NHMJUOSYSOOPDM-UHFFFAOYSA-N 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 229910001430 chromium ion Inorganic materials 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- -1 hydrogen ions Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- 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
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/565—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of zinc
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
-
- 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
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/36—Pretreatment of metallic surfaces to be electroplated of iron or steel
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Automation & Control Theory (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The invention discloses a zinc and nickel plating process for steel materials, which comprises the following steps: s1, cleaning a steel material; s2, electroplating zinc and nickel: putting the steel material cleaned in the step S1 into zinc-nickel electroplating solution, wherein the electroplating current density is 3-3.5A/dm 2 The electroplating time is 20-30 min, and after the electroplating is finished, the galvanized nickel steel material is obtained by cleaning; s3, removing hydrogen; s4, surface activation; s5, passivating; s6, sealing: and (3) placing the galvanized nickel steel material after passivation in the step (S5) into hot water for sealing, and obtaining the sealed galvanized nickel steel material. The corrosion resistance of the galvanized nickel ultrahigh-strength steel material prepared by the process is not lower than 360 hours; the hydrogen embrittlement performance is not broken after 200 hours; the binding force between the coating and the matrix should be good, and bending binding force test is performed, so that the peeling and bubbling phenomena of the coating and the matrix can not occur; low hydrogen embrittlement plating with fatigue strength superior to that of the same material platingCadmium process and non-cyanide cadmium-titanium plating process.
Description
Technical Field
The invention relates to a steel material surface protection process method, in particular to a steel material zinc-nickel plating process.
Background
The ultra-high strength steel material is widely applied to the field of aviation manufacturing at present, and basically adopts processes of low-hydrogen embrittlement cadmium plating, titanium plating and the like for surface protection in order to improve the corrosion resistance of the material and provide a good bottom layer for paint spraying, so that the cost is high, and the environmental protection requirements of heavy metals chromium and cadmium cannot be met. In contrast, the zinc-nickel plating process has the advantages of strong corrosion resistance, environmental protection, strong plating solution dispersing capability, weak corrosiveness, convenient wastewater treatment, low production cost and the like, is rapidly developed in recent years, and has wide application in the automobile industry and the foreign aerospace manufacturing industry. The research of the ultra-high strength steel zinc-nickel plating process is developed, and the ultra-high strength steel zinc-nickel plating process is applied to the field of domestic aviation, becomes a replacement process for cadmium plating (cyanided cadmium plating and low-hydrogen brittle cadmium plating) and cadmium-titanium plating, and is a technical problem to be solved in the technical urgent need in the art.
The patent with publication number CN106637315A discloses an automatic electroplating process of zinc-nickel alloy without chromium ions, which comprises the following steps: pretreatment: removing greasy dirt and rust on the surface of a rubber metal composite part or a metal part to be plated by adopting acid washing, electrolytic degreasing and high-temperature degreasing modes (the high-temperature degreasing temperature is 50-60 ℃, the concentration is 40-60g/L, the time is 3-5min, the electrolytic degreasing voltage is 4-8V, the concentration is 20-40g/L, the temperature is 40-60 ℃, the time is 2-3min, the acid washing concentration is 300-500g/L, and the acid washing time is 2-3 min). Electroplating: the electrochemical reaction is utilized to make zinc and nickel metal ions co-deposit on the metal surface to form a plating layer; closing: penetrating into the coating gap by using a sealing liquid, forming an organic or inorganic protective layer on the surface of the coating, wherein the sealing time is 50-80S, and the temperature of the sealing liquid is 40-50 ℃; blow-drying; drying; and (5) packaging. The invention has short neutral salt fog resistance time. The process is only suitable for common metal composite parts, because the ultra-high strength steel material is particularly sensitive to hydrogen embrittlement, if the acid with high concentration of 300-500g/L is used for long-time treatment for 2-3min to remove rust in the electroplating pretreatment, the process has great corrosion function on the material, and a large amount of hydrogen is generated, so that the risk of hydrogen embrittlement fracture is greatly increased. Therefore, the alloy can be used for common metal material pieces and cannot be used for ultra-high strength steel materials.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a zinc and nickel plating process for a steel material, which has the advantages of strong corrosion resistance, excellent hydrogen embrittlement performance, good binding force between a plating layer and a matrix and good fatigue strength.
In order to solve the technical problems, the invention adopts the following technical scheme: a zinc-nickel plating process for steel materials comprises S1, cleaning the steel materials; s2, electroplating zinc and nickel; the method also comprises the following steps:
s3, removing hydrogen: heating the galvanized nickel steel material in the step S2 to remove hydrogen;
s4, surface activation: adding acid into the electroplating solution in the step S2, and placing the galvanized nickel steel material subjected to the dehydrogenation in the step S3 into the electroplating solution for activation, and cleaning after the activation is completed to obtain an activated galvanized nickel steel material;
s5, passivating: putting the activated zinc-nickel plated steel material prepared in the step S4 into Cr 3+ Passivating in the solution, and cleaning after the passivation is finished to obtain a passivated zinc-nickel plated steel material;
s6, sealing: placing the galvanized nickel steel material after passivation in the step S5 into hot water for sealing to obtain a sealed galvanized nickel steel material, wherein the thickness of a plating layer of the sealed galvanized nickel steel material is 10-20 mu m;
wherein, S2, electroplated zinc nickel specifically comprises: putting the steel material cleaned in the step S1 into zinc-nickel electroplating solution, wherein the electroplating current density is 3-3.5A/dm 2 And the electroplating time is 20-30 min, and after the electroplating is finished, the galvanized nickel steel material is obtained by cleaning.
In the design of the technological process, the invention adopts the steps of firstly removing hydrogen and then carrying out Cr after electroplating 3+ And (5) passivating the solution. Firstly removing hydrogen and then passivating, firstly preventing the passivation film layer which is passivated and then densified from obstructing the overflow of hydrogen molecules, and effectively reducing the risk of hydrogen embrittlement fracture; and secondly, the passivation film layer is effectively protected from discoloration, aging and damage caused by the influence of the dehydrogenation temperature, and the appearance and the corrosion resistance of the plating layer are ensured. According to the process, zinc-nickel electroplating of the ultra-high strength steel material can be realized, and the method is also suitable for common steel materials.
The invention adopts the method of post-treatment technology, and the deionized hot water is used for sealing immediately after passivation. After the passivated zinc-nickel coating is sealed by hot water, pinholes generated by electroplating can be blocked, the binding force between the passivation film layer and the electroplated layer is improved, and the brightness and corrosion resistance of the passivation film layer are improved.
Zinc and nickel ions together undergo oxidation-reduction reaction deposition on the cathode to form an alloy coating, but because the standard electrode potential (-0.762V) of zinc is much more negative than the standard electrode potential (-0.246V) of nickel, hydrogen is evolved from the cathode surface during electroplating to form Zn (OH) 2 The adsorption layer blocks the passage of nickel ions so that zinc ions are preferentially deposited. However, the invention mainly adopts low current density to carry out electroplating, so that the reaction speed is reduced, the hydrogen evolution amount is reduced, and Zn (OH) cannot be caused 2 The effect on the deposition of nickel ions forms a zinc-nickel co-deposit.
The accurate control of the current density effectively ensures the plating thickness of the enclosed galvanized nickel steel material, thereby further ensuring the good fatigue strength of the galvanized nickel steel material.
In a preferred embodiment of the invention, the zinc-nickel plating solution of S2 contains Zn 2+ The concentration is 0.1mol/L to 0.17mol/L; ni (Ni) 2+ ：0.017mol/L～0.024mol/L；Zn 2+ concentration/Ni 2+ Concentration=6:1 to 7:1; the NaOH concentration is as follows: 100-140 g/L; na (Na) 2 CO 3 Concentration: 60-80 g/L; electroplating temperature: 20-28 ℃; deposition rate: 0.5-0.8 mu m/min.
Control of Zn 2+ Concentration and Ni 2+ Concentration of Zn is favorable to 2+ And Ni 2+ And the common electroplating can ensure good deposition of the plating layer in the electroplating process.
In a preferred embodiment of the invention, the temperature of the heating dehydrogenation in S3 is 180-200 ℃ for 20-25 hours.
When the part is kept at 180-200 ℃ for at least 20-25 h, hydrogen ions among the metal lattices are combined into hydrogen molecules to overflow from the plating layer. When the temperature of dehydrogenation is higher than 200 ℃, zinc embrittlement occurs. Further preferably, the temperature of the heating dehydrogenation in S3 is 180℃to 190 ℃.
In a preferred embodiment of the invention, the concentration of acid in S4 is 10g/L to 30g/L, the activation temperature is 20 ℃ to 30 ℃ and the activation time is 1min to 2min.
Under the surface activation condition, the surface activation is reacted under the alkaline condition, so that the oxide layer is removed, the surface layer is not corroded, and the thickness of the plating layer is not influenced.
In a preferred embodiment of the invention, cr in S5 3+ The concentration of the solution is 0.035mol/L to 0.045mol/L, the pH is 4 to 4.4, the temperature is 23 ℃ to 28 ℃ and the time is 20s to 30s. Ensuring the continuity of the film after passivation.
In a preferred embodiment of the invention, the temperature of the hot water in S6 is 100℃and the closing time is 1min to 2min.
The hot water at 100 ℃ can effectively block pinholes generated by electroplating. The hot water sealing can improve the corrosion resistance of the plating layer to more than 1500 hours, and the aging and falling of the passivation film layer can not be caused.
In a preferred embodiment of the present invention, S1 includes organic solvent washing, deionized cold water washing, steam degreasing, aluminum oxide blowing, electrochemical degreasing, hot water washing, deionized cold water washing, acid activation, and deionized cold water washing, respectively.
The clean steel material in S1 can effectively ensure that the surface of the sample piece before electroplating has no signs of greasy dirt, oxide skin, over corrosion and the like.
In a preferred embodiment of the invention, the medium for steam degreasing in S1 is trichloroethylene, the temperature is 86-90 ℃, and the steam degreasing time is 3-5min.
In a preferred embodiment of the invention, the medium for blowing aluminum oxide in S1 is 150 mesh aluminum oxide sand grains, and the wind pressure is 0.3Mpa to 0.5Mpa; the distance between the nozzle and the surface of the sample is 100 mm-300 mm.
In a preferred embodiment of the invention, the acid activation in S1 is carried out by placing the steel material into 30mL/L to 50mL/L hydrochloric acid at a temperature of 20 ℃ to 30 ℃ for 20 to 40 seconds. The pretreatment has the aluminum oxide blowing treatment, the possibility of rusting the surface of the part is very small after electrochemical degreasing, but under natural conditions, an oxide film layer can be generated on the surface after sand blowing in the electroplating process, so that the surface of the part is activated for 20-40 s by using 30-50 mL/L low-concentration hydrochloric acid, the slight oxide film layer can be removed, the fresh surface before electroplating is achieved, a large amount of hydrogen is not generated, and the possibility of hydrogen embrittlement is greatly reduced.
In a preferred embodiment of the invention, the current density in S2 is controlled by means of a current control device comprising a hanger, the lower part of which is in electrically conductive connection with an ammeter, the lower part of which is in electrically conductive connection with a conductive element.
In a preferred embodiment of the invention, the conductive member comprises a connecting rod connected with the lower part of the ammeter, the other end of the connecting rod is fixedly connected with the conductive hanging plate, a plurality of groups of conductive connecting members are respectively arranged on the lower surface of the conductive hanging plate, and each conductive connecting member comprises a unidirectional screw rod fixed with the lower surface of the conductive hanging plate and a connecting nut fixed at the lower end of the unidirectional screw rod.
The hanger is a conductive rod, and in the use process, the hanger is hung on the cathode. The surface of the connecting nut is sprayed with insulating materials, and organic paint is used for spraying (anti-corrosion effect). And steel materials are connected below the connecting nuts and electroplated in electroplating liquid.
By using a set of accurate current control device, the invention can accurately display the actual current value reaching the surface of the plated sample piece. In general, in the electroplating process, a current value reaching the surface of a plated part has a great relationship with the measuring range of a power supply device, and the larger the measuring range of the power supply device is, the more the current is lost. For small piece electroplating there is therefore a large error in the set current on the power supply device and the actual current actually reaching the surface of the plated piece, which is determined by the accuracy error of the power supply device. The current control device is connected with the plating piece at the current output end, and can directly display the actual current value reaching the surface of the plating piece.
The current control device has the current precision of 0.01A, and can more accurately monitor and control the actual current value reaching the surface of the plating piece.
In a preferred embodiment of the present invention, the steel material comprises a steel material and an ultra-high strength steel material, the ultra-high strength steel material having a yield strength of greater than 1180MPa and a tensile strength of greater than 1380MPa.
The ultra-high strength steel is very sensitive to hydrogen embrittlement, so the process of the invention is suitable for being applied to zinc-nickel plating of ultra-high strength steel materials.
The invention innovates the optimal technological parameters of zinc-nickel electroplating of steel materials. Including the current density and time relationship of electroplating, the temperature of the electroplating solution, the temperature and time of dehydrogenation, the temperature and time of passivation, and the temperature and time of hot water sealing; according to the technological parameters of the invention, the effective deposition of nickel and zinc ions in the zinc-nickel plating process can be effectively ensured, and the effect on the deposition of nickel ions due to the large difference between the electrode potential of zinc ions and the electrode potential of nickel ions is avoided; the appearance of the coating is uniform and fine, and the phenomena of coarse coating, charring, pitting, foaming or falling off, discontinuous coating, partial no coating and the like are avoided; the coating has good dispersion capability and uniform thickness; the plating layer has good hydrogen embrittlement performance, binding force and fatigue strength.
Compared with the prior art, the invention has the following beneficial effects: the invention forms the technological process, the technological method and the technological parameters of the zinc-nickel plating of the ultra-high strength steel material through exploring the zinc-nickel alloy plating process of the ultra-high strength steel material. The nickel content in the plating layer can be effectively controlled to be 12% -15%, and the corrosion resistance of the plating layer is far higher than that of other surface plating layers (cadmium layer and cadmium-titanium layer) through a neutral salt spray test, and can reach more than 1500 hours, which is about 5 times of that of a common plating layer; the zinc-nickel coating formed by the process has good hydrogen embrittlement performance, and is subjected to notch tensile test, so that the sample is not broken for 200 hours; the binding force between the coating and the matrix is good, and the bending binding force test is carried out, so that the phenomena of stripping and foaming of the coating and the matrix are avoided. Compared with other electroplating processes (low-hydrogen brittle cadmium plating and non-cyanide cadmium plating titanium) for the same materials, the fatigue strength is more excellent, and can reach 20775 times at the maximum stress level of 1375 Mpa. The invention is also suitable for being used as a common steel material for zinc and nickel plating.
Drawings
FIG. 1 is a process flow diagram of an embodiment of the present invention.
FIG. 2 is a schematic diagram of the structure of a hydrogen embrittlement notch tensile specimen in the performance test of the present invention.
Wherein, 1) the material of the sample is 300M steel, 4 pieces of the sample are in each group, and the ultimate tensile strength of the notch is 1900 Mpa-2100 Mpa.
2) All surface roughness Ra0.8μm.
FIG. 3 is a front view of a corrosion resistant test specimen in the performance test of the present invention.
Wherein, the material of 1) the sample is 4130 steel, each group of 2 pieces of samples.
2) All surface roughness Ra0.8μm.
FIG. 4 is a left side view of a corrosion resistant test specimen in the performance test of the present invention.
FIG. 5 is a front view of a bond specimen in a performance test of the present invention.
Wherein, the material of 1) the sample is 4130 steel, each group of 2 pieces of samples.
2) All surface roughness Ra0.8μm.
FIG. 6 is a left side view of a bond test specimen in the performance test of the present invention.
FIG. 7 is a graph comparing fatigue strength of low hydrogen embrittlement cadmium plating, non-cyanide cadmium titanium plating, and zinc nickel plating.
Fig. 8 is a schematic diagram of a current control device.
Detailed Description
Example 1
The process flow of the invention comprises 24 stepsThe method comprises the following steps: pre-plating acceptance (step 1), organic solvent cleaning (step 2), deionized cold water cleaning (step 3), stress relief (step 4), steam degreasing (step 5), aluminum oxide blowing (step 6), hanging and protecting (step 7), electrochemical degreasing (step 8), hot water cleaning (step 9), deionized cold water cleaning (step 10), acid activation (step 11), deionized cold water cleaning (step 12), 30s water film continuity check (step 13), electrogalvanized nickel (step 14), deionized cold water cleaning (step 15), compressed air blow-drying (step 16), dehydrogenation (step 17), surface activation (step 18), deionized cold water cleaning (step 19), cr 3+ Solution passivation (step 20), deionized cold water washing (step 21), hot water sealing (step 22), compressed air blow-drying (step 23), and inspection (step 24).
The main flow of the electroplating process of the embodiment is as follows: manual cleaning with organic solvent (step 2), stress relief (step 4), steam degreasing (step 5), aluminum oxide blowing (step 6), hanging and protecting (step 7), electrochemical degreasing (step 8), acid activation (step 11), electrogalvanizing nickel (step 14), dehydrogenation (step 17), activation (step 18), passivation (step 20), and hot water sealing (step 22); pre-treating the plating piece to ensure that the surface of the plating piece has no greasy dirt, oxide skin and the like; after the last water washing before zinc and nickel plating, 30s of water film continuity check is carried out to ensure that the water film 30s is not broken; and (3) carrying out dehydrogenation treatment on the plating piece, wherein the temperature is 190 ℃, and the time is more than or equal to 23h.
The specific process steps and parameters are as follows:
1) Acceptance before plating (step 1): before electroplating, the surface of the part is inspected, and impurities such as sharp corners, burrs, knocks and other surface defects and excessive substances are avoided.
2) Washing with organic solvent (step 2) using 180 # The surface of the part is cleaned by aviation washing gasoline or equivalent organic solvent until cleaned.
3) Deionized cold water washing (step 3): at room temperature, the parts are rinsed for at least 1min by using deionized A-level water, and then 30s of water film continuity check is carried out to ensure that the surfaces of the parts are free of greasy dirt.
4) Stress relief (step 4): for steel pieces with strength greater than 1300Mpa, the stress is relieved for at least 4 hours at 190+ -14 ℃.
5) Steam degreasing (process step 5): steam degreasing is carried out in trichloroethylene at 86 ℃ for 3-5min.
6) Blowing aluminum oxide (process step 6): medium: 150 mesh alumina grit; wind pressure: 0.3Mpa; nozzle to sample surface distance: 100mm.
7) And (step 7) hanging and protecting: the parts are hung by using special tools or materials with good conductivity, and the surfaces of the parts which do not need to be electroplated and the surfaces of the clamps which enter the electroplating solution are shielded and protected by using insulating materials such as electroplating protection adhesive tapes. The mounting and hanging of the parts must ensure good electrical conductivity.
8) Electrochemical degreasing (process step 8): oakite90:50g/L; temperature: 84 ℃. Current density: 6A/dm 2 The method comprises the steps of carrying out a first treatment on the surface of the Time: anode for 0.5min.
9) Hot water washing (step 9): solution: deionized grade a water; temperature: 40 ℃; time: less than or equal to 1min.
10 Deionized cold water washing (process step 10): temperature: room temperature; time: 1min.
11 Acid activation (step 11): hydrochloric acid (HCl, ρ=1.19 g/ml): 30mL/L; temperature: room temperature; time: 30s.
12 Deionized cold water washing (process step 12): temperature: room temperature; time: 1min.
13 30s water film continuity check (step 13): after the last water washing before electroplating, the part is subjected to 30s water film continuity inspection, so that the surface of the part is clean and free of greasy dirt.
14 Electrogalvanized nickel (step 14): zn (zinc) 2+ ：8.5g/L；Ni 2+ ：1.2g/L；NaOH：120g/L；Na 2 CO 3 :70g/L; temperature: 23 ℃; current density: 3A/dm 2 The method comprises the steps of carrying out a first treatment on the surface of the Electroplating time: 20min; deposition rate: 0.65 μm/min. Wherein Zn is 2+ Is zinc oxide (ZnO) or zinc chloride (ZnCl) 2 )，Ni 2+ Is nickel chloride (NiCl) 2 ) Or nickel sulfate.
15 Deionized cold water washing (step 15): temperature: room temperature; time: 2min.
16 Compressed air blow-drying (step 16): the parts are dried by using clean and oil-free compressed air, and the temperature of the compressed air cannot be more than 50 ℃.
17 Hydrogen removal (step 17): and (3) carrying out dehydrogenation baking on the steel piece with the strength of more than 1300Mpa within 3 hours after electroplating at 190+/-14 ℃ for at least 23 hours.
18 Surface activation (step 18): sulfuric acid: 10g/L; temperature: room temperature; time: 5s.
19 Deionized cold water washing (step 19): temperature: room temperature; time: 1min.
20)Cr 3+ Solution passivation (process step 20): cr (Cr) 3+ :1.84g/L; pH 4; temperature: 23 ℃; time: 20s. Wherein Cr is 3+ The source of (a) is chromium chloride, chromium sulfate, chromium nitrate or chromium phosphate.
21 Deionized cold water washing (step 21): temperature: room temperature; time: 1min.
22 Hot water closed (process step 22): temperature: 100 ℃; time: 1min.
23 Compressed air blow-drying (step 23): the parts are dried by using clean and oil-free compressed air, and the temperature of the compressed air cannot be more than 50 ℃.
24 Inspection (step 24): appearance and thickness inspection was performed on the parts.
The current density in S2 is controlled by a current control device, the current control device comprises a hook 1, the lower part of the hook 1 is in conductive connection with an ammeter 3, and the lower part of the ammeter 3 is in conductive connection with a conductive piece.
The electric conduction piece includes with connecting rod 4 that ampere meter 3 below is connected, the other end and the conductive link plate 5 fixed connection of connecting rod 4, conductive link plate 5 lower surface is equipped with multiunit connecting piece respectively, the connecting piece include with conductive link plate 5 lower surface fixed's unidirectional screw rod 6 and be fixed in the coupling nut 7 of unidirectional screw rod 6 lower extreme.
Example 2
The specific process parameters are as follows:
1) Organic solvent cleaning (process step 2) medium: 180 # Aviation washing gasoline; time: removing the cleaning stop.
2) Deionized cold water washing (step 3): temperature: room temperature; time: 2min.
3) Steam degreasing (process step 5): medium: trichloroethylene; temperature: 90 ℃; time: 5min.
4) Blowing aluminum oxide (process step 6): medium: 150 mesh alumina grit; wind pressure: 0.5Mpa; nozzle to sample surface distance: 300mm;
5) Electrochemical degreasing (process step 8): oakite90:80g/L; temperature: 90 ℃; current density: 8A/dm 2 The method comprises the steps of carrying out a first treatment on the surface of the Time: anode for 1min.
6) Hot water washing (step 9): solution: deionized grade a water; temperature: 60 ℃; time: less than or equal to 1min.
7) Deionized cold water washing (process step 10): temperature: room temperature; time: 2min.
8) Acid activation (step 11): hydrochloric acid (HCl, ρ=1.19 g/ml): 50mL/L; temperature: room temperature; time: 30s.
9) Deionized cold water washing (process step 12): temperature: room temperature; time: 2min.
10 Electrogalvanized nickel (step 14): zn (zinc) 2+ ：8.5g/L；Ni 2+ ：1.2g/L；NaOH：120g/L；Na 2 CO 3 :70g/L; temperature: 26 ℃; current density: 3.5A/dm 2 The method comprises the steps of carrying out a first treatment on the surface of the Electroplating time: 30min; deposition rate: 0.65 μm/min.
Wherein Zn is 2+ Is zinc oxide (ZnO) or zinc chloride (ZnCl) 2 )，Ni 2+ Is nickel chloride (NiCl) 2 ) Or nickel sulfate.
11 Deionized cold water washing (step 15): temperature: room temperature; time: 5min.
12 Surface activation (step 18): sulfuric acid: 10g/L to 30g/L; temperature: room temperature; time: 10s.
13 Deionized cold water washing (step 19): temperature: room temperature; time: 2min.
14)Cr 3+ Solution passivation (process step 20): cr (Cr) 3+ :2.36g/L; PH 4.4; temperature: 28 ℃; time: 30s. Wherein Cr is 3+ The source of (a) is chromium chloride, chromium sulfate, chromium nitrate or chromium phosphate.
15 Deionized cold water washing (step 21): temperature: room temperature; time: 2min.
16 Hot water closed (process step 22): temperature: 100 ℃; time: 2min.
The galvanized nickel ultrahigh-strength steel material prepared in example 1 was subjected to performance testing according to the following steps:
1. the 300M ultra-high strength steel material hydrogen embrittlement notch tensile test sample, corrosion resistance test sample and binding force test sample are subjected to electroplating treatment according to the process flow of FIG. 1. The whole electroplating process mainly comprises four stages, wherein the first stage is pretreatment cleaning of a sample (comprising a process step 2 to a process step 13); the second stage is electro-plating zinc-nickel (including steps 14 to 16); the third stage is the dehydro-baking of the sample (including step 17); the fourth stage is the post-treatment passivation and sealing of the sample (including steps 18-23).
2. The hydrogen embrittlement tensile test was performed on 4 samples as shown in fig. 2 (length l=50.8 mm, thread m=9.525 mm, notch diameter Φ= 4.445 mm). And (3) vertically installing the sample piece on tensile test equipment in a straight line, ensuring that the center of the sample piece is coaxial with the tensile center of the test equipment, and applying a force value with the notch limit tensile strength of 75% to carry out static load stretching until no fracture occurs in 200 hours.
3. The corrosion resistance test (neutral salt spray test) was performed on 2 samples as shown in fig. 3 to 4 (length l=150 mm, width w=100 mm, thickness h=1 mm). The sample surface is scrubbed clean and supported or suspended at an angle of between 15 deg. and 25 deg. from vertical and preferably parallel to the main face being tested and the main direction of fog flow through the fog box, and the sample is tested in a neutral salt fog environment, and the condition of the sample surface is observed and recorded every 8 hours.
4. The bending bonding force test was performed on 2 samples as shown in fig. 5 to 6 (length l=100 mm, width w=50 mm, thickness h=1 mm). Clamping the tested test piece by pliers, and repeatedly bending 180 degrees (bending 90 degrees to two sides) until the test piece breaks; the fracture is inspected under the condition of 5 times magnification, and the coating should not peel, fall off or foam.
5. As shown in FIG. 7, the fatigue strength test was performed on the low-hydrogen embrittlement cadmium plating fatigue strength specimen, the cyanide-free cadmium titanium plating fatigue strength specimen, and the zinc-nickel plating fatigue strength specimens in the three bath concentration ranges (upper, middle, lower) at the stress level of 1375Mpa at the maximum, and the results showed that the fatigue strength of the zinc-nickel plating specimens was superior to those of the low-hydrogen embrittlement cadmium plating specimens and the cyanide-free cadmium titanium plating specimens.
6. According to the method shown in fig. 8, in the electroplating process, when the plated part is hung on the 7-connection nut, a current value is applied through the power supply device, and the actual current reaching the plated part can be truly displayed through the ammeter on the current control device, so that the actual current error caused by the precision error of the power supply device when the power supply range is large is avoided, and the thickness and the quality of the plated layer are effectively ensured.
7. Electroplating of certain ultra-high strength steel material parts is achieved according to the determined flow and the optimal technological parameters and methods (see flow and description) in the invention. The performance parameters obtained by the detection are as follows:
1. the invention uses high temperature deionized water sealing technology in the post-treatment process of the plating layer, which can not cause aging and falling of the passivation film layer, and the corrosion resistance is far higher than other surface plating layers (cadmium layer and cadmium-titanium layer), which can reach more than 1500 hours, which is about 5 times of the corrosion resistance of common plating layers.
2. The hydrogen embrittlement performance is good, and the notch tensile test can not break after 200 hours.
3. The binding force between the coating and the matrix is good, and the bending binding force test is carried out without the phenomena of coating and matrix stripping and foaming.
4. The fatigue strength is superior to other electroplating processes (low-hydrogen brittle cadmium plating and non-cyanide cadmium titanium plating) of the same material, and can reach 20775 times at the maximum stress level of 1375Mpa (the fatigue strength comparison is shown in table 1).
Table 1 fatigue strength comparison table
The galvanized nickel ultra-high strength steel material prepared in example 1 was tested for corrosion resistance GB/T10125 (neutral salt spray test), hydrogen embrittlement performance ASTM F519 (notch tensile test), adhesion test of coating and substrate GB/T5270 (bending adhesion test):
the nickel content in the plating layer can be effectively controlled to be 12% -15%, and the corrosion resistance of the plating layer is far higher than that of other surface plating layers (cadmium layer and cadmium-titanium layer) through a neutral salt spray test, and can reach more than 1500 hours, which is about 5 times of that of a common plating layer; the zinc-nickel coating formed by the process has good hydrogen embrittlement performance, and is subjected to notch tensile test, so that the sample is not broken for 200 hours; the binding force between the coating and the matrix is good, and the bending binding force test is carried out, so that the phenomena of stripping and foaming of the coating and the matrix are avoided.
Claims (10)
1. A zinc-nickel plating process for steel materials comprises S1, cleaning the steel materials; s2, electroplating zinc and nickel; the method is characterized by further comprising the following steps:
s3, removing hydrogen: heating the galvanized nickel steel material in the step S2 to remove hydrogen;
s4, surface activation: adding acid into the electroplating solution in the step S2, and placing the galvanized nickel steel material subjected to the dehydrogenation in the step S3 into the electroplating solution for activation, and cleaning after the activation is completed to obtain an activated galvanized nickel steel material;
s5, passivating: putting the activated zinc-nickel plated steel material prepared in the step S4 into Cr 3+ Passivating in the solution, and cleaning after the passivation is finished to obtain a passivated zinc-nickel plated steel material;
s6, sealing: placing the galvanized nickel steel material after passivation in the step S5 into hot water for sealing to obtain a sealed galvanized nickel steel material, wherein the thickness of a plating layer of the sealed galvanized nickel steel material is 10-20 mu m;
wherein, S2, electroplated zinc nickel specifically comprises: putting the steel material cleaned in the step S1 into zinc-nickel electroplating solution, wherein the electroplating current density is 3-3.5A/dm 2 And the electroplating time is 20-30 min, and after the electroplating is finished, the galvanized nickel steel material is obtained by cleaning.
2. According to claim 1The zinc-nickel plating process of the steel material is characterized in that Zn in the zinc-nickel plating solution of S2 2+ The concentration is 0.1mol/L to 0.17mol/L; ni (Ni) 2+ ：0.017mol/L～0.024mol/L；Zn 2+ concentration/Ni 2+ Concentration=6:1 to 7:1; the NaOH concentration is as follows: 100-140 g/L; na (Na) 2 CO 3 Concentration: 60-80 g/L; electroplating temperature: 20-28 ℃; deposition rate: 0.5-0.8 mu m/min.
3. The process for galvanizing nickel on steel materials according to claim 1, wherein the temperature of heating and dehydrogenation in S3 is 180-200 ℃ for 20-25 h.
4. The process for galvanizing nickel on steel materials according to claim 1, wherein the concentration of acid in S4 is 10 g/L-30 g/L, the activating temperature is 20-30 ℃, and the activating time is 1-2 min.
5. The process for galvanization and nickel plating steel material according to claim 1, wherein Cr in S5 3+ The concentration of the solution is 0.035mol/L to 0.045mol/L, the PH is 4 to 4.4, the temperature is 23 ℃ to 28 ℃ and the time is 20s to 30s.
6. The process for galvanization and nickel plating steel material according to claim 1, wherein the temperature of hot water in S6 is 100 ℃ and the closing time is 1 min-2 min.
7. The process for galvanizing nickel on steel materials according to claim 1, wherein S1 comprises organic solvent cleaning, deionized cold water washing, steam degreasing, aluminum oxide blowing, electrochemical degreasing, hot water washing, deionized cold water washing, acid activation, and deionized cold water washing, respectively.
8. The zinc-nickel plating process of steel materials according to claim 1, characterized in that the current density in S2 is controlled by a current control device comprising a hanger (1), the lower part of the hanger (1) is electrically connected with an ammeter (3), and the lower part of the ammeter (3) is electrically connected with a conductive member.
9. The steel material zinc-nickel plating process according to claim 8, wherein the conductive member comprises a connecting rod (4) connected with the lower part of the ammeter (3), the other end of the connecting rod (4) is fixedly connected with a conductive hanging plate (5), a plurality of groups of conductive connecting members are respectively arranged on the lower surface of the conductive hanging plate (5), and each conductive connecting member comprises a unidirectional screw rod (6) fixed with the lower surface of the conductive hanging plate (5) and a connecting nut (7) fixed at the lower end of the unidirectional screw rod (6).
10. The process of galvanising nickel of a steel material according to claim 1, characterized in that the steel material comprises a steel material and an ultra high strength steel material, the ultra high strength steel material having a yield strength of more than 1180MPa and a tensile strength of more than 1380MPa.
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