CN114032530A - Pretreatment method and application of chemical nickel-phosphorus plating on aluminum and aluminum alloy - Google Patents
Pretreatment method and application of chemical nickel-phosphorus plating on aluminum and aluminum alloy Download PDFInfo
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- 238000007747 plating Methods 0.000 title claims abstract description 53
- 239000000126 substance Substances 0.000 title claims abstract description 42
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 36
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 34
- 238000002203 pretreatment Methods 0.000 title claims abstract description 18
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 60
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 54
- 230000004913 activation Effects 0.000 claims abstract description 30
- 238000001978 electrochemical passivation Methods 0.000 claims abstract description 30
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 27
- 239000003960 organic solvent Substances 0.000 claims abstract description 20
- 239000007769 metal material Substances 0.000 claims abstract description 7
- 238000000137 annealing Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 47
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 39
- 238000005406 washing Methods 0.000 claims description 31
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 26
- 239000008367 deionised water Substances 0.000 claims description 26
- 229910021641 deionized water Inorganic materials 0.000 claims description 26
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 26
- 239000008399 tap water Substances 0.000 claims description 25
- 235000020679 tap water Nutrition 0.000 claims description 25
- 238000005238 degreasing Methods 0.000 claims description 23
- 235000014655 lactic acid Nutrition 0.000 claims description 13
- 239000004310 lactic acid Substances 0.000 claims description 13
- 235000006408 oxalic acid Nutrition 0.000 claims description 13
- 238000003860 storage Methods 0.000 claims description 13
- 238000005237 degreasing agent Methods 0.000 claims description 12
- 239000013527 degreasing agent Substances 0.000 claims description 12
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 230000001680 brushing effect Effects 0.000 claims description 4
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims description 3
- 239000003085 diluting agent Substances 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 claims description 3
- 239000003502 gasoline Substances 0.000 claims description 2
- 239000003350 kerosene Substances 0.000 claims description 2
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 230000003213 activating effect Effects 0.000 claims 1
- 230000001681 protective effect Effects 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 28
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 14
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 14
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 14
- 239000011574 phosphorus Substances 0.000 abstract description 14
- 229910052725 zinc Inorganic materials 0.000 abstract description 14
- 239000011701 zinc Substances 0.000 abstract description 14
- 238000007598 dipping method Methods 0.000 abstract description 12
- 230000005587 bubbling Effects 0.000 abstract description 10
- 238000000576 coating method Methods 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 239000011248 coating agent Substances 0.000 abstract description 8
- 229910052751 metal Inorganic materials 0.000 abstract description 8
- 239000002184 metal Substances 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000002161 passivation Methods 0.000 abstract description 5
- 238000005336 cracking Methods 0.000 description 6
- 238000005868 electrolysis reaction Methods 0.000 description 6
- 238000004381 surface treatment Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 230000008595 infiltration Effects 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- 239000002932 luster Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1837—Multistep pretreatment
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1848—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by electrochemical pretreatment
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
Abstract
The invention belongs to the fields of chemical technology and metal material surface protection treatment methods, and particularly relates to a pretreatment method for chemical nickel-phosphorus plating of aluminum and aluminum alloy and application thereof in the field of metal material surface protection treatment. The method comprises the steps of organic solvent oil removal, stress relief annealing treatment, chemical oil removal, electrolytic passivation treatment and activation treatment. Production tests prove that: the aluminum and aluminum alloy surface passivation film layer prepared by the pretreatment method is very uniform, the coating binding force is obviously increased, and the aluminum and aluminum alloy surface passivation film layer has certain porosity, so that good metal surface conditions are provided for a chemical nickel and phosphorus plating process in the later period, the incidence rate of product quality problems such as falling off and bubbling of a nickel and phosphorus layer can be greatly reduced, in addition, the pretreatment method has the advantages of simple process flow, stable product quality, lower production cost and obviously reduced pollution compared with the traditional zinc dipping process.
Description
Technical Field
The invention belongs to the fields of chemical technology and metal material surface protection treatment methods, and particularly relates to a pretreatment method for chemical nickel-phosphorus plating of aluminum and aluminum alloy and application thereof in the field of metal material surface protection treatment.
Background
Aluminum and aluminum alloys are metal materials with the largest usage amount and the widest application range in nonferrous metals, have a series of excellent physical, chemical, mechanical and processing properties and characteristics, such as low density, high plasticity, easy reinforcement, good electric conduction, corrosion resistance, easy recovery, weldability, easy surface treatment and the like, and are widely applied to industries such as aviation, aerospace, ships, automobiles, motorcycles, electronics, instruments, textile machinery, household appliances and the like after being treated by various surface treatment technologies.
However, in industrial applications, some of the chemical properties of aluminum and aluminum alloys also pose significant difficulties in production. Firstly, aluminum and aluminum alloy have high affinity to oxygen, a thin loose oxide film is easily generated in the air, and a new oxide film is generated in a very short time after the oxide film is removed, so that the binding force of a plating layer is seriously influenced; secondly, the standard potential of the aluminum is too low, and the negative value is too large (-1.67V), so that the aluminum is easy to perform a displacement reaction with other metal ions with higher positive potential in the plating solution, and the bonding force of the plating layer can be influenced; in addition, the expansion coefficients of aluminum and aluminum alloys are different from those of most metal coatings, for example, the expansion coefficients of aluminum and aluminum alloys are large, the expansion coefficient of nickel is small, and when the temperature is greatly changed in the electroplating process, the expansion degrees of the aluminum and aluminum alloys are greatly different, so that the stress generated between the coatings can cause product quality problems such as coating falling and surface bubbling, or the like, or the product can be used in the process after being cooled. Therefore, in the surface treatment process of aluminum and aluminum alloy, if the pretreatment process is not ideal, a large amount of products can be reworked or scrapped, so that the production efficiency is reduced and the processing cost is increased.
At present, many process methods for surface treatment of aluminum and aluminum alloys, such as anodic oxidation process, micro-arc oxidation process, chemical plating, and the like, are available. The chemical nickel-phosphorus plating process is a surface treatment technology commonly used for aluminum alloy, and in order to meet the quality requirements of chemical nickel-phosphorus plating of aluminum alloy, the traditional zinc dipping is generally adopted for pre-plating (pretreatment), so that the natural oxide film on the surface of aluminum can be quickly and effectively removed, a zinc layer can be deposited at the same time, the surface of aluminum can be prevented from being oxidized again, and the electrode potential of aluminum can be changed. Although the method has good effect and wide application range, the method still has some defects, on one hand, the operation is complicated, the process flow is complex, the method needs to carry out zinc dipping twice, and in order to improve the stability of the chemical nickel plating solution, an alkaline nickel dipping procedure needs to be added after the secondary zinc dipping; on the other hand, the process specification is not good, the product quality is unstable, the processing cost is high, if the operations of the zinc dipping procedure and the alkaline nickel dipping procedure are not standard, the surface quality of the pretreated product is not high, the binding force of a coating and the stability of bath solution can be directly influenced, the coating of the product is stripped, and even the serious consequence of bath solution decomposition and scrapping can be caused.
In conclusion, in order to overcome the defects of complicated process, high processing cost, unstable product quality, high pollution and the like of the traditional zinc dipping process, the pretreatment process of chemical nickel-phosphorus plating on aluminum and aluminum alloy needs to be further improved. At present, a new pretreatment method for chemically plating nickel and phosphorus on aluminum and aluminum alloy, which has the advantages of simple process, low production cost and stable product quality, is urgently needed in the chemical industry.
Disclosure of Invention
In order to overcome the defects of the traditional pretreatment technology for chemically plating nickel and phosphorus on the surfaces of aluminum and aluminum alloy, the invention provides a feasible solution, and production tests prove that: the aluminum and aluminum alloy surface passivation film layer prepared by the pretreatment method is very uniform, the coating binding force is obviously increased, and the aluminum and aluminum alloy surface passivation film layer has certain porosity, so that good metal surface conditions are provided for a chemical nickel and phosphorus plating process in the later period, the incidence rate of product quality problems such as falling off and bubbling of a nickel and phosphorus layer can be greatly reduced, in addition, the pretreatment method has the advantages of simple process flow, stable product quality, lower production cost and obviously reduced pollution compared with the traditional zinc dipping process.
The invention discloses a pretreatment method for chemically plating nickel phosphorus on aluminum and aluminum alloy, which comprises the following steps:
the method comprises the following steps: oil removal by organic solvents
Soaking the surface of an aluminum or aluminum alloy workpiece at room temperature or brushing the surface of the workpiece with an organic solvent to remove oil, removing oil stains on the surface of the workpiece completely, and drying;
step two: stress relief annealing treatment
Placing the workpiece with the surface oil stain removed completely into a constant-temperature oven for stress relief treatment, wherein the temperature of the oven is 100-150 ℃, the treatment time is 1-3 hours, and slowly cooling to room temperature after the treatment is finished;
step three: chemical degreasing
Degreasing the workpiece treated in the second step in an aluminum part degreasing agent solution at the temperature of 30-60 ℃ for 10-30min, and then sequentially washing the workpiece with hot water at the temperature of 40-80 ℃ and flowing tap water at room temperature;
step four: electrolytic passivation treatment
Placing the workpiece treated in the third step in electrolytic passivation bath solution for electrolytic passivation treatment, adopting a voltage-stabilizing power supply mode, controlling the voltage range to be 15-20V, the electrolytic temperature to be less than or equal to 20 ℃, and the electrolytic time to be 5-15min, and sequentially washing the workpiece with tap water and deionized water after the treatment is finished;
the electrolytic passivation bath solution consists of sulfuric acid for the storage battery, industrial oxalic acid, lactic acid and deionized water with the conductivity of less than 30 us/cm;
step five: activation treatment
Placing the workpiece treated in the fourth step into an activation bath solution for activation treatment, wherein the treatment temperature is room temperature, the treatment time is 1-3min, and after the activation treatment is finished, sequentially washing the workpiece with tap water and deionized water, and immediately transferring the workpiece into a chemical nickel plating bath for plating treatment;
wherein the activation bath solution consists of industrial-grade nitric acid and tap water.
Preferably, the organic solvent in step one of the method of the present invention is a mixed solvent composed of any one or more of the following organic solvents: gasoline, kerosene, ethanol, acetone, trichloroethylene, carbon tetrachloride and a general quick-drying diluent.
Furthermore, the surface of the workpiece washed clean in the third step of the method is in a wetting state, a continuous water film is presented, and the water film is not broken within at least 30 seconds.
Furthermore, in the electrolytic passivation bath solution in the fourth step of the method, the sulfuric acid content for the storage battery is 140-200g/L, the industrial oxalic acid content is 15-25g/L, the lactic acid content is 3-10ml/L, and the balance is deionized water with the conductivity of less than 30 us/cm.
Preferably, in the electrolytic passivation bath solution, the content of sulfuric acid for the storage battery is 140g/L, the content of industrial oxalic acid is 15g/L, the content of lactic acid is 3ml/L, and the balance is deionized water with the conductivity of less than 30 us/cm.
Still preferably, in the electrolytic passivation bath solution, the content of sulfuric acid for the storage battery is 160g/L, the content of industrial oxalic acid is 20g/L, the content of lactic acid is 4ml/L, and the balance is deionized water with the conductivity of less than 30 us/cm.
Preferably, in the electrolytic passivation bath solution, the content of sulfuric acid for the storage battery is 200g/L, the content of industrial oxalic acid is 25g/L, the content of lactic acid is 5ml/L, and the balance is deionized water with the conductivity of less than 30 us/cm.
Furthermore, in the activation bath solution in the fifth step of the method, the content of industrial-grade nitric acid is 300-650g/L, and the balance is tap water.
In addition, the invention also relates to the application of the pretreatment method for chemically plating nickel and phosphorus on aluminum and aluminum alloy in the field of surface protection treatment of metal materials.
In conclusion, the pretreatment method for chemically plating nickel and phosphorus on aluminum and aluminum alloy has the following characteristics:
(1) the process flow is simple, the operation time is saved, the production efficiency is improved, and the production cost is reduced; the following is the comparison of the traditional zinc dipping process and the process flow of the invention:
the traditional zinc dipping process flow comprises the following steps: pre-inspection → organic solvent degreasing → local protection → mounting → chemical degreasing → hot washing → cold washing → alkali corrosion → hot washing → cold washing → chemical activation → 2 times of cold washing → one time of zinc immersion → 2 times of cold washing → zinc removal → 2 times of cold washing → secondary zinc immersion → 2 times of cold washing → hot washing with deionized water → cold washing with deionized water → alkaline nickel immersion → 2 times of cold washing with cold water → hot washing with deionized water → chemical nickel phosphorus plating (25 steps in total).
The process flow of the invention is as follows: pre-inspection → degreasing by organic solvent → destressing treatment → local protection → mounting → chemical degreasing → hot washing → cold washing water → alkaline corrosion → hot washing water → cold washing water → chemical activation → 2 times cold washing water → electrolytic passivation → 2 times cold washing water → chemical activation → 2 times cold washing water → chemical nickel phosphorus plating (19 steps in total).
(2) The surface passivation film layer of the aluminum and aluminum alloy products treated by the method is very uniform, the binding force of the plating layer is obviously increased, and the plating layer has certain porosity, so that good metal surface conditions are provided for the chemical nickel and phosphorus plating process in the later period, the incidence rate of product quality problems such as the falling off and bubbling of the nickel and phosphorus layer can be greatly reduced, the product quality is stable, and the defective rate is obviously reduced.
(3) The method has the advantages of environmental protection, simple process, low pollution discharge, and no pollution to the chemical nickel and phosphorus plating solution compared with the traditional zinc dipping process.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to specific embodiments. It is to be understood that the embodiments described are merely illustrative of some, but not all, of the present invention and that the invention may be embodied or carried out in various other specific forms, and that various modifications and changes in the details of the specification may be made without departing from the spirit of the invention.
Also, it should be understood that the scope of the invention is not limited to the particular embodiments described below; it is also to be understood that the terminology used in the examples is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the present invention.
Unless otherwise defined, all technical terms used in the present invention have the same meaning as commonly understood by one of ordinary skill in the art. In addition to the specific methods, devices, and materials used in the examples, any methods, devices, and materials similar or equivalent to those described in the examples may be used in the practice of the invention, in addition to the specific methods, devices, and materials used in the examples, in keeping with the knowledge of one skilled in the art and with the description of the invention.
In the present invention, all materials, reagents and the like are commercially available or commonly used in the industry, if not specified otherwise. The methods in the following examples are conventional in the art unless otherwise specified.
The operation steps and the effect of the pretreatment method of the present invention will be described in detail with reference to the following specific examples.
Example 1: a pretreatment method for chemically plating nickel phosphorus on aluminum and aluminum alloy comprises the following steps:
the method comprises the following steps: oil removal by organic solvents
Soaking the surface of an aluminum alloy workpiece by using an organic solvent at room temperature for degreasing, wherein the workpiece has the size of 100x50x5 and the treatment area of 1dm2Removing oil stains on the surface of the workpiece and drying; the organic solvent is commercial oil removal agent trichloroethylene;
step two: stress relief annealing treatment
Placing the workpiece with the surface oil stain removed completely into a constant-temperature oven for stress relief treatment, wherein the temperature of the oven is 150 ℃, the treatment time is 1 hour, and slowly cooling to room temperature after the treatment is finished;
step three: chemical degreasing
Placing the workpiece treated in the second step into an aluminum part degreasing agent solution for degreasing, wherein the aluminum part degreasing agent is a PA30-IM commodity steel part special degreasing agent with the mass fraction of 100%, the solution temperature is 30 ℃, the degreasing time is 10min, and after the degreasing is finished, the workpiece is washed clean by hot water at 60 ℃ and flowing tap water at room temperature in sequence; the surface of the workpiece which is washed clean is in an infiltration state, a continuous water film is presented, and the water film is not broken within 30 seconds;
step four: electrolytic passivation treatment
Putting the workpiece treated in the third step into electrolytic passivation bath solution for electrolytic passivation, wherein the electrolytic passivation bath solution contains 140g/L of sulfuric acid for a storage battery, 15g/L of industrial oxalic acid, 3ml/L of lactic acid and the balance of deionized water with the conductivity of less than 30 us/cm; a voltage-stabilizing power supply mode is adopted, the voltage is 15V, the electrolysis temperature is 20 ℃, the electrolysis time is 5min, and tap water and deionized water are sequentially used for washing after the treatment is finished;
step five: activation treatment
Putting the workpiece treated in the fourth step into an activation tank solution for activation treatment, wherein the content of industrial nitric acid in the activation tank solution is 300g/L, and the balance is tap water; the treatment temperature is room temperature, the treatment time is 1min, tap water and deionized water are sequentially used for washing after the activation treatment is finished, and the treated product is immediately transferred into a chemical nickel plating bath for plating treatment.
In the example, after pretreatment, the surface of the workpiece is darker than the original metal luster; after chemical nickel and phosphorus plating, the plating layer is bright, flat, uniform and compact, and the thickness of the plating layer is 15 mu m (chemical nickel plating for 1 hour). The phenomenon of bubbling, peeling and cracking of the coating is avoided through the observation of an optical microscope; and (3) carrying out a thermal shock test on the plated workpiece, keeping the temperature at 200 ℃ for 1.5 hours, taking out the workpiece, putting the workpiece into tap water for cooling, and repeating for 5 times, wherein the plated layer has no bubbling, stripping and cracking phenomena.
Example 2: a pretreatment method for chemically plating nickel phosphorus on aluminum and aluminum alloy comprises the following steps:
the method comprises the following steps: oil removal by organic solvents
Brushing and degreasing the surface of an aluminum alloy workpiece by using an organic solvent at room temperature, wherein the size of the workpiece is 100x50x5, and the treatment area is 1dm2Removing oil stains on the surface of the workpiece and drying; the organic solvent is commercial degreasing agent carbon tetrachloride;
step two: stress relief annealing treatment
Placing the workpiece with the surface oil stain removed completely into a constant-temperature oven for stress relief treatment, wherein the temperature of the oven is 120 ℃, the treatment time is 2 hours, and slowly cooling to room temperature after the treatment is finished;
step three: chemical degreasing
Placing the workpiece treated in the second step into an aluminum part degreasing agent solution for degreasing, wherein the aluminum part degreasing agent is a PA30-IM commodity steel part special degreasing agent with the mass fraction of 100%, the solution temperature is 30 ℃, the degreasing time is 20min, and after the degreasing is finished, the workpiece is washed clean by hot water at 60 ℃ and flowing tap water at room temperature in sequence; the surface of the workpiece which is washed clean is in an infiltration state, a continuous water film is presented, and the water film is not broken within 30 seconds;
step four: electrolytic passivation treatment
Putting the workpiece treated in the third step into electrolytic passivation bath solution for electrolytic passivation, wherein the electrolytic passivation bath solution contains 160g/L of sulfuric acid for a storage battery, 20g/L of industrial oxalic acid, 4ml/L of lactic acid and the balance of deionized water with the conductivity of less than 30 us/cm; a voltage-stabilizing power supply mode is adopted, the voltage is 18V, the electrolysis temperature is 15 ℃, the electrolysis time is 10min, and tap water and deionized water are sequentially used for washing after the treatment is finished;
step five: activation treatment
Putting the workpiece treated in the fourth step into an activation tank solution for activation treatment, wherein the content of industrial nitric acid in the activation tank solution is 500g/L, and the balance is tap water; the treatment temperature is room temperature, the treatment time is 2min, after the activation treatment is finished, tap water and deionized water are sequentially used for washing, and the treated product is immediately transferred into a chemical nickel plating bath for plating treatment.
In the example, after pretreatment, the surface of the workpiece is darker than the original metal luster; after chemical nickel and phosphorus plating, the plating layer is bright, flat, uniform and compact, and the thickness of the plating layer is 40 mu m (chemical nickel plating for 2 hours). The phenomenon of bubbling, peeling and cracking of the coating is avoided through the observation of an optical microscope; and (3) carrying out a thermal shock test on the plated workpiece, keeping the temperature at 200 ℃ for 1.5 hours, taking out the workpiece, putting the workpiece into tap water for cooling, and repeating for 5 times, wherein the plated layer has no bubbling, stripping and cracking phenomena.
Example 3: a pretreatment method for chemically plating nickel phosphorus on aluminum and aluminum alloy comprises the following steps:
the method comprises the following steps: oil removal by organic solvents
Brushing and degreasing the surface of an aluminum alloy workpiece by using an organic solvent at room temperature, wherein the size of the workpiece is 100x50x5, and the treatment area is 1dm2Removing oil stains on the surface of the workpiece and drying; the organic solvent is a commercial universal quick-drying diluent;
step two: stress relief annealing treatment
Placing the workpiece with the surface oil stain removed completely into a constant-temperature oven for stress relief treatment, wherein the temperature of the oven is 150 ℃, the treatment time is 1 hour, and slowly cooling to room temperature after the treatment is finished;
step three: chemical degreasing
Placing the workpiece treated in the second step into an aluminum part degreasing agent solution for degreasing, wherein the aluminum part degreasing agent is a PA30-IM commodity steel part special degreasing agent with the mass fraction of 100%, the solution temperature is 30 ℃, the degreasing time is 30min, and after the degreasing is finished, the workpiece is washed clean by hot water at 60 ℃ and flowing tap water at room temperature in sequence; the surface of the workpiece which is washed clean is in an infiltration state, a continuous water film is presented, and the water film is not broken within 30 seconds;
step four: electrolytic passivation treatment
Putting the workpiece treated in the third step into electrolytic passivation bath solution for electrolytic passivation, wherein in the electrolytic passivation bath solution, the sulfuric acid content of the storage battery is 200g/L, the industrial oxalic acid content is 25g/L, the lactic acid content is 5ml/L, and the balance is deionized water with the conductivity of less than 30 us/cm; a voltage-stabilizing power supply mode is adopted, the voltage is 20V, the electrolysis temperature is 18 ℃, the electrolysis time is 15min, and tap water and deionized water are sequentially used for washing after the treatment is finished;
step five: activation treatment
Putting the workpiece treated in the fourth step into an activation tank solution for activation treatment, wherein the industrial nitric acid content in the activation tank solution is 650g/L, and the balance is tap water; the treatment temperature is room temperature, the treatment time is 3min, tap water and deionized water are sequentially used for washing after the activation treatment is finished, and the treated product is immediately transferred into a chemical nickel plating bath for plating treatment.
In the example, after pretreatment, the surface of the workpiece is darker than the original metal luster; after chemical nickel and phosphorus plating, the plating layer is bright, flat, uniform and compact, and the thickness of the plating layer is 70 mu m (chemical nickel plating for 4 hours). The phenomenon of bubbling, peeling and cracking of the coating is avoided through the observation of an optical microscope; and (3) carrying out a thermal shock test on the plated workpiece, keeping the temperature at 200 ℃ for 1.5 hours, taking out the workpiece, putting the workpiece into tap water for cooling, and repeating for 5 times, wherein the plated layer has no bubbling, stripping and cracking phenomena.
The above description is only an example of the present invention, and is not intended to limit the present invention. Various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, replacement, or the like that comes within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.
Claims (9)
1. A pretreatment method for chemically plating nickel phosphorus on aluminum and aluminum alloy is characterized by comprising the following steps:
the method comprises the following steps: oil removal by organic solvents
Soaking the surface of an aluminum or aluminum alloy workpiece at room temperature or brushing the surface of the workpiece with an organic solvent to remove oil, removing oil stains on the surface of the workpiece completely, and drying;
step two: stress relief annealing treatment
Placing the workpiece with the surface oil stain removed completely into a constant-temperature oven for stress relief treatment, wherein the temperature of the oven is 100-150 ℃, the treatment time is 1-3 hours, and slowly cooling to room temperature after the treatment is finished;
step three: chemical degreasing
Degreasing the workpiece treated in the second step in an aluminum part degreasing agent solution at the temperature of 30-60 ℃ for 10-30min, and then sequentially washing the workpiece with hot water at the temperature of 40-80 ℃ and flowing tap water at room temperature;
step four: electrolytic passivation treatment
Placing the workpiece treated in the third step in electrolytic passivation bath solution for electrolytic passivation treatment, adopting a voltage-stabilizing power supply mode, controlling the voltage range to be 15-20V, the electrolytic temperature to be less than or equal to 20 ℃, and the electrolytic time to be 5-15min, and sequentially washing the workpiece with tap water and deionized water after the treatment is finished;
the electrolytic passivation bath solution consists of sulfuric acid for the storage battery, industrial oxalic acid, lactic acid and deionized water with the conductivity of less than 30 us/cm;
step five: activation treatment
Placing the workpiece treated in the fourth step into an activation bath solution for activation treatment, wherein the treatment temperature is room temperature, the treatment time is 1-3min, and after the activation treatment is finished, sequentially washing the workpiece with tap water and deionized water, and immediately transferring the workpiece into a chemical nickel plating bath for plating treatment;
wherein the activation bath solution consists of industrial-grade nitric acid and tap water.
2. The method according to claim 1, wherein the organic solvent in the first step is a mixed solvent of any one or more of the following organic solvents: gasoline, kerosene, ethanol, acetone, trichloroethylene, carbon tetrachloride and a general quick-drying diluent.
3. The method of claim 1, wherein the surface of the workpiece rinsed clean in step three is wet, exhibits a continuous film of water, and does not break for at least 30 seconds.
4. The method as claimed in claim 1, wherein in the electrolytic passivation bath solution in the fourth step, the sulfuric acid content for the storage battery is 140-200g/L, the oxalic acid content for industrial grade is 15-25g/L, the lactic acid content is 3-10ml/L, and the rest is deionized water with the conductivity of less than 30 us/cm.
5. The method as claimed in claim 4, wherein the electrolytic passivation bath solution contains 140g/L of sulfuric acid for storage batteries, 15g/L of oxalic acid for industrial grade, 3ml/L of lactic acid and the balance of deionized water with the conductivity of less than 30 us/cm.
6. The method as claimed in claim 4, wherein the electrolytic passivation bath solution contains 160g/L of sulfuric acid for storage batteries, 20g/L of oxalic acid for industrial grade, 4ml/L of lactic acid and the balance of deionized water with the conductivity of less than 30 us/cm.
7. The method as claimed in claim 4, wherein the electrolytic passivation bath solution contains 200g/L of sulfuric acid for storage batteries, 25g/L of oxalic acid for industrial grade, 5ml/L of lactic acid and the balance of deionized water with the conductivity of less than 30 us/cm.
8. The method as claimed in claim 1, wherein the activating bath solution in the fifth step contains 300-650g/L industrial-grade nitric acid and tap water.
9. Use of the pretreatment method for electroless nickel-phosphorus plating on aluminum and aluminum alloys according to any one of claims 1 to 8 in the field of surface protective treatment of metal materials.
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| CN112695358A (en) * | 2020-11-25 | 2021-04-23 | 云南昆船机械制造有限公司 | Electrochemical conductive oxidation process method for aluminum and aluminum alloy |
| CN113122845A (en) * | 2021-04-03 | 2021-07-16 | 郑小宝 | Preparation method of aluminum alloy metal plated part |
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| CN112695358A (en) * | 2020-11-25 | 2021-04-23 | 云南昆船机械制造有限公司 | Electrochemical conductive oxidation process method for aluminum and aluminum alloy |
| CN113122845A (en) * | 2021-04-03 | 2021-07-16 | 郑小宝 | Preparation method of aluminum alloy metal plated part |
Non-Patent Citations (1)
| Title |
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| 范建凤等: "铝及铝合金直接化学镀镍前处理工艺研究", 《忻州师范学院学报》, vol. 23, no. 2, pages 7 - 9 * |
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