CN114032530B - Pretreatment method and application of chemical nickel-phosphorus plating of aluminum and aluminum alloy - Google Patents
Pretreatment method and application of chemical nickel-phosphorus plating of aluminum and aluminum alloy Download PDFInfo
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- CN114032530B CN114032530B CN202111286901.8A CN202111286901A CN114032530B CN 114032530 B CN114032530 B CN 114032530B CN 202111286901 A CN202111286901 A CN 202111286901A CN 114032530 B CN114032530 B CN 114032530B
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- 238000007747 plating Methods 0.000 title claims abstract description 61
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 46
- 239000000126 substance Substances 0.000 title claims abstract description 40
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 34
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000002203 pretreatment Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 50
- 230000004913 activation Effects 0.000 claims abstract description 31
- 238000001978 electrochemical passivation Methods 0.000 claims abstract description 30
- 238000005238 degreasing Methods 0.000 claims abstract description 29
- 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 61
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 39
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 32
- 239000008367 deionised water Substances 0.000 claims description 31
- 229910021641 deionized water Inorganic materials 0.000 claims description 31
- 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
- 239000008399 tap water Substances 0.000 claims description 25
- 235000020679 tap water Nutrition 0.000 claims description 25
- JVTAAEKCZFNVCJ-REOHCLBHSA-N L-lactic acid Chemical compound C[C@H](O)C(O)=O JVTAAEKCZFNVCJ-REOHCLBHSA-N 0.000 claims description 18
- 238000005237 degreasing agent Methods 0.000 claims description 18
- 239000013527 degreasing agent Substances 0.000 claims description 18
- 229910052759 nickel Inorganic materials 0.000 claims description 16
- 235000006408 oxalic acid Nutrition 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 11
- 238000005868 electrolysis reaction Methods 0.000 claims description 10
- 238000003860 storage Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 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
- 238000002791 soaking Methods 0.000 claims description 6
- 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
- 235000014655 lactic acid Nutrition 0.000 claims description 4
- 239000004310 lactic acid Substances 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
- 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
- 239000000203 mixture Substances 0.000 claims description 2
- 230000000087 stabilizing effect Effects 0.000 claims description 2
- 238000009736 wetting Methods 0.000 claims 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 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 13
- 230000005587 bubbling Effects 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 238000005516 engineering process Methods 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 5
- 238000002161 passivation Methods 0.000 abstract description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 6
- 238000005336 cracking Methods 0.000 description 6
- 238000007772 electroless plating Methods 0.000 description 6
- 229910052698 phosphorus Inorganic materials 0.000 description 6
- 239000011574 phosphorus Substances 0.000 description 6
- 238000004381 surface treatment Methods 0.000 description 5
- 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
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical class O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 3
- 239000002932 luster Substances 0.000 description 3
- 239000000463 material 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
- 238000004321 preservation Methods 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 230000006641 stabilisation Effects 0.000 description 3
- 238000011105 stabilization Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 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
- 238000002386 leaching Methods 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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 of the pretreatment method in the field of metal material surface protection treatment. The method comprises the steps of organic solvent degreasing, stress relief annealing treatment, chemical degreasing, electrolytic passivation treatment and activation treatment. Production tests prove that: the passivation film layer on the surface of the aluminum and the aluminum alloy prepared by the pretreatment method is very uniform, the binding force of the plating layer is obviously increased, the plating layer has a certain porosity, good metal surface conditions are provided for the later chemical nickel-phosphorus plating process, the occurrence rate of product quality problems such as nickel-phosphorus layer falling and bubbling can be greatly reduced, and 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 of the pretreatment method in the field of metal material surface protection treatment.
Background
Aluminum and aluminum alloy are the most widely used metal materials in nonferrous metals, and have a series of excellent physical, chemical, mechanical and processing properties and characteristics, such as low density, high plasticity, easy reinforcement, good conductivity, corrosion resistance, easy recovery, weldability, easy surface treatment and the like, and are widely applied to industries of aviation, aerospace, ships, automobiles, motorcycles, electronics, instruments, textile machinery, household appliances and the like after being treated by various surface treatment technologies.
However, some of the chemical properties of aluminum and aluminum alloys also create significant difficulties in production during industrial applications. Firstly, aluminum and aluminum alloy have high affinity to oxygen, a layer of thinner loose oxide film is easy to generate in the air, and a layer of new oxide film can be generated in a very short time after the oxide film is removed, so that the binding force of a plating layer is seriously affected; secondly, the standard potential of aluminum is too low and the negative value is too large (-1.67V), so that the aluminum is easy to carry out displacement reaction with other metal ions with higher positive potential in the plating solution, and the plating binding force is also affected; in addition, the expansion coefficients of aluminum and aluminum alloys are different from those of most metal plating layers, for example, the expansion coefficients of aluminum and aluminum alloys are large, the expansion coefficients of nickel are small, when the temperature is changed greatly in the electroplating process, the stress generated between the plating layers can cause product quality problems such as plating layer falling and surface bubbling due to the great difference of the expansion degrees of the aluminum and the aluminum alloys, or the product can generate the conditions in the use process after cooling. Therefore, if the pretreatment process is not ideal in the surface treatment process of aluminum and aluminum alloy, a large amount of products will be reworked or scrapped, thereby reducing the production efficiency and improving the processing cost.
At present, a plurality of processes for surface treatment of aluminum and aluminum alloy, such as anodic oxidation process, micro-arc oxidation process, chemical plating and the like, are adopted. The chemical nickel-phosphorus plating process is a common surface treatment technology for aluminum alloy, and in order to meet the quality requirement of the chemical nickel-phosphorus plating of the aluminum alloy, the conventional zinc dipping is generally adopted for preplating (pretreatment), so that the natural oxide film on the surface of the aluminum is rapidly and effectively removed, and meanwhile, a zinc layer can be deposited to prevent the surface of the aluminum from being oxidized again, thereby changing the electrode potential of the aluminum. Although the method has good effect and wide application range, the method has some defects, on one hand, the operation is complicated, the process flow is complex, the method needs to dip zinc twice, and in order to improve the stability of the chemical nickel plating solution, an alkaline nickel dipping procedure is added after the second zinc dipping; on the other hand, the process standardization is poor, the product quality is unstable, the processing cost is high, if the zinc dipping procedure and the alkaline nickel dipping procedure are not standard in operation, the surface quality of the pretreated product is not high, the binding force of a plating layer and the stability of bath solution can be directly influenced, the product plating layer is stripped, and even the serious consequence of decomposition and scrapping of the bath solution can be caused.
In summary, in order to overcome the defects of complicated process flow, high processing cost, unstable product quality, high pollution and the like of the traditional zinc dipping process, the pretreatment process of the chemical nickel-phosphorus plating of the aluminum and the aluminum alloy is further improved. At present, a new pretreatment method for chemical nickel-phosphorus plating of aluminum and aluminum alloy, which has the advantages of simple process, low production cost and stable product quality, is needed in the chemical industry.
Disclosure of Invention
In order to overcome the defects of the traditional aluminum and aluminum alloy surface chemical nickel-phosphorus plating pretreatment technology, the invention provides a feasible solution, and the production test proves that: the passivation film layer on the surface of the aluminum and the aluminum alloy prepared by the pretreatment method is very uniform, the binding force of the plating layer is obviously increased, the plating layer has a certain porosity, good metal surface conditions are provided for the later chemical nickel-phosphorus plating process, the occurrence rate of product quality problems such as nickel-phosphorus layer falling and bubbling can be greatly reduced, and 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 relates to a pretreatment method for chemical nickel-phosphorus plating of aluminum and aluminum alloy, which specifically comprises the following steps:
step one: deoiling with organic solvents
Soaking or brushing the surface of an aluminum or aluminum alloy workpiece with an organic solvent at room temperature to remove oil, degreasing the surface of the workpiece, and drying;
step two: stress relief annealing
Placing the workpiece with the surface oil stain removed into a constant temperature oven for stress removal 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 completed;
step three: chemical degreasing
Degreasing the workpiece treated in the second step in aluminum piece degreasing agent solution at 30-60 ℃ for 10-30min, and washing the workpiece clean by hot water at 40-80 ℃ and running tap water at room temperature in sequence after degreasing;
step four: electrolytic passivation treatment
Placing the workpiece treated in the third step into electrolytic passivation tank liquor for electrolytic passivation treatment, adopting a voltage stabilizing and power supplying mode, controlling the voltage range to be 15-20V, the electrolysis temperature to be less than or equal to 20 ℃ and the electrolysis time to be 5-15min, and washing the workpiece cleanly by tap water and deionized water in sequence after the treatment is finished;
wherein the electrolytic passivation tank solution consists of sulfuric acid, industrial oxalic acid, lactic acid and deionized water with the conductivity of less than 30us/cm for a storage battery;
step five: activation treatment
Placing the workpiece subjected to the treatment in an activation tank liquid for activation treatment, wherein the treatment temperature is room temperature, the treatment time is 1-3min, and after the activation treatment is finished, the workpiece is sequentially washed by tap water and deionized water and immediately transferred into a chemical nickel plating tank for plating treatment;
wherein the activation tank liquid consists of industrial grade nitric acid and tap water.
Preferably, the organic solvent in the step one of the method of the present invention is any one or a mixture of several of the following organic solvents: gasoline, kerosene, ethanol, acetone, trichloroethylene, carbon tetrachloride and a universal quick-drying diluent.
Further, the surface of the workpiece washed clean in the third step of the method is in a soaked state, a continuous water film is displayed, and the water film is not broken within at least 30 seconds.
Further, in the electrolytic passivation tank solution in the fourth step of the method, the storage battery contains 140-200g/L of sulfuric acid, 15-25g/L of industrial oxalic acid, 3-10ml/L of lactic acid and the balance deionized water with the conductivity less than 30 us/cm.
Preferably, in the electrolytic passivation tank solution, the storage battery contains 140g/L sulfuric acid, 15g/L industrial oxalic acid, 3ml/L lactic acid and deionized water with conductivity less than 30 us/cm.
It is also preferable that in the electrolytic passivation tank solution, the storage battery contains 160g/L sulfuric acid, 20g/L industrial oxalic acid, 4ml/L lactic acid and deionized water with conductivity less than 30 us/cm.
It is also preferable that in the electrolytic passivation tank solution, the storage battery contains 200g/L sulfuric acid, 25g/L industrial oxalic acid, 5ml/L lactic acid and deionized water with conductivity less than 30 us/cm.
Further, in the activation tank liquid 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 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 summary, the pretreatment method for electroless nickel phosphorus plating of 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 a comparison of the traditional zinc leaching 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, hanging, chemical degreasing, hot water washing, cold water washing, alkali corrosion, hot water washing, cold water washing, chemical activation, 2 times of cold water washing, one time of zinc dipping, 2 times of cold water washing, zinc removing, 2 times of cold water washing, secondary zinc dipping, 2 times of cold water washing, hot deionized water washing, cold deionized water washing, alkaline nickel dipping, 2 times of cold water washing, cold deionized water washing, hot deionized water washing and chemical nickel and phosphorus plating (total 25 steps).
The process flow of the invention comprises the following steps: pre-inspection, organic solvent degreasing, stress relief treatment, local protection, hanging, chemical degreasing, hot water washing, cold water washing, alkali corrosion, hot water washing, cold water washing, chemical activation, 2 times of cold water washing, electrolytic passivation, 2 times of cold water washing, chemical activation, 2 times of cold water washing, cold deionized water washing and chemical nickel and phosphorus plating (total 19 steps).
(2) The passivation film layer on the surface of the aluminum and aluminum alloy products treated by the method is very uniform, the binding force of the plating layer is obviously increased, the plating layer has a certain porosity, good metal surface conditions are provided for the later chemical nickel-phosphorus plating process, the occurrence rate of product quality problems such as nickel-phosphorus layer falling and bubbling can be greatly reduced, the product quality is stable, and the defective rate is obviously reduced.
(3) The method is environment-friendly, has simple process, low pollution discharge amount and obviously reduced pollution compared with the traditional zinc dipping process, and can not pollute the chemical nickel-phosphorus plating solution.
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 in the following in connection with specific embodiments. It is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and the present invention may be implemented or applied by different specific embodiments, and that various modifications or changes may be made in the details of the present description based on different points of view and applications without departing from the spirit of the present invention.
Meanwhile, it should be understood that the scope of the present invention is not limited to the following specific embodiments; it is also to be understood that the terminology used in the examples of the invention is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the invention.
Unless defined otherwise, 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, materials used in the embodiments, any methods, devices, and materials of the prior art similar or equivalent to those described in the embodiments of the present invention may be used to practice the present invention according to the knowledge of one skilled in the art and the description of the present invention.
In the present invention, unless otherwise specified, all materials, reagents, etc. are commercially available or commonly used in the industry. The methods in the following examples are conventional in the art unless otherwise specified.
The following describes the operation steps and effects of the pretreatment method according to the present invention in detail with reference to specific examples.
Example 1: a pretreatment method for chemical nickel-phosphorus plating of aluminum and aluminum alloy comprises the following steps:
step one: deoiling with organic solvents
Soaking the surface of an aluminum alloy workpiece in an organic solvent at room temperature for degreasing, wherein the workpiece size is 100x50x5, and the treatment area is 1dm 2 Removing greasy dirt on the surface of the workpiece and drying; the organic solvent is commercial degreasing agent trichloroethylene;
step two: stress relief annealing
Placing the workpiece with the surface oil stain removed into a constant temperature oven for stress removal 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 completed;
step three: chemical degreasing
Degreasing the workpiece treated in the second step in an aluminum piece degreasing agent solution, wherein the aluminum piece degreasing agent is a degreasing agent special for PA30-IM commercial steel pieces, the mass fraction of the aluminum piece degreasing agent is 100%, the solution temperature is 30 ℃, the degreasing time is 10min, and the aluminum piece degreasing agent is sequentially washed clean by hot water at 60 ℃ and running tap water at room temperature after degreasing; the surface of the washed workpiece is in a soaking state, a continuous water film is formed, and the water film is not broken within 30 seconds;
step four: electrolytic passivation treatment
Placing the workpiece treated in the third step into electrolytic passivation tank liquor for electrolytic passivation treatment, wherein in the electrolytic passivation tank liquor, the storage battery contains 140g/L sulfuric acid, 15g/L industrial oxalic acid, 3ml/L lactic acid and the balance deionized water with the conductivity less than 30 us/cm; adopting a voltage stabilization power supply mode, wherein 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 completed;
step five: activation treatment
The workpiece treated in the fourth step is placed in an activation tank liquid for activation treatment, wherein the content of industrial grade nitric acid in the activation tank liquid 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 activated water and deionized water are immediately transferred into an electroless nickel plating tank for plating treatment.
After pretreatment in this example, the surface of the workpiece is darker than the original metallic luster; after electroless plating with nickel and phosphorus, the plating layer is bright, flat, uniform and compact, and the thickness of the plating layer is 15 mu m (electroless plating for 1 hour). The plating layer has no phenomena of bubbling, flaking and cracking when observed by an optical microscope; and (3) carrying out a thermal shock test on the plated workpiece, taking out the workpiece after heat preservation for 1.5 hours at 200 ℃, putting the workpiece into tap water for cooling, and reciprocating for 5 times, wherein the plating layer has no bubbling, peeling and cracking phenomena.
Example 2: a pretreatment method for chemical nickel-phosphorus plating of aluminum and aluminum alloy comprises the following steps:
step one: deoiling with organic solvents
Brushing and degreasing the surface of the aluminum alloy workpiece at room temperature by using an organic solvent, wherein the workpiece size is 100x50x5, and the treatment area is 1dm 2 Removing greasy dirt on the surface of the workpiece and drying; the organic solvent is carbon tetrachloride as a commercial oil removing agent;
step two: stress relief annealing
Placing the workpiece with the surface oil stain removed into a constant temperature oven for stress removal 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 completed;
step three: chemical degreasing
Degreasing the workpiece treated in the second step in an aluminum piece degreasing agent solution, wherein the aluminum piece degreasing agent is a degreasing agent special for PA30-IM commercial steel pieces, the mass fraction of the aluminum piece degreasing agent is 100%, the solution temperature is 30 ℃, the degreasing time is 20min, and the aluminum piece degreasing agent is sequentially washed clean by hot water at 60 ℃ and running tap water at room temperature after degreasing; the surface of the washed workpiece is in a soaking state, a continuous water film is formed, and the water film is not broken within 30 seconds;
step four: electrolytic passivation treatment
Placing the workpiece treated in the third step into electrolytic passivation tank liquor for electrolytic passivation treatment, wherein in the electrolytic passivation tank liquor, the storage battery contains 160g/L sulfuric acid, 20g/L industrial oxalic acid, 4ml/L lactic acid and the balance deionized water with the conductivity less than 30 us/cm; adopting a voltage stabilization power supply mode, wherein 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 completed;
step five: activation treatment
The workpiece treated in the fourth step is placed in an activation tank liquid for activation treatment, wherein the content of industrial grade nitric acid in the activation tank liquid is 500g/L, and the balance is tap water; the treatment temperature is room temperature, the treatment time is 2min, tap water and deionized water are sequentially used for washing after the activation treatment is finished, and the activated water and deionized water are immediately transferred into an electroless nickel plating tank for plating treatment.
After pretreatment in this example, the surface of the workpiece is darker than the original metallic luster; after electroless plating with nickel and phosphorus, the plating layer is bright, flat, uniform and compact, and the thickness of the plating layer is 40 mu m (electroless plating for 2 hours). The plating layer has no phenomena of bubbling, flaking and cracking when observed by an optical microscope; and (3) carrying out a thermal shock test on the plated workpiece, taking out the workpiece after heat preservation for 1.5 hours at 200 ℃, putting the workpiece into tap water for cooling, and reciprocating for 5 times, wherein the plating layer has no bubbling, peeling and cracking phenomena.
Example 3: a pretreatment method for chemical nickel-phosphorus plating of aluminum and aluminum alloy comprises the following steps:
step one: deoiling with organic solvents
Brushing and degreasing the surface of the aluminum alloy workpiece at room temperature by using an organic solvent, wherein the workpiece size is 100x50x5, and the treatment area is 1dm 2 Removing greasy dirt on the surface of the workpiece and drying; the organic solvent is a commercial general quick-drying diluent;
step two: stress relief annealing
Placing the workpiece with the surface oil stain removed into a constant temperature oven for stress removal 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 completed;
step three: chemical degreasing
Degreasing the workpiece treated in the second step in an aluminum piece degreasing agent solution, wherein the aluminum piece degreasing agent is a degreasing agent special for PA30-IM commercial steel pieces, the mass fraction of the aluminum piece degreasing agent is 100%, the solution temperature is 30 ℃, the degreasing time is 30min, and the aluminum piece degreasing agent is sequentially washed clean by hot water at 60 ℃ and running tap water at room temperature after degreasing; the surface of the washed workpiece is in a soaking state, a continuous water film is formed, and the water film is not broken within 30 seconds;
step four: electrolytic passivation treatment
Placing the workpiece treated in the third step into electrolytic passivation tank liquor for electrolytic passivation treatment, wherein in the electrolytic passivation tank liquor, the storage battery contains 200g/L sulfuric acid, 25g/L industrial oxalic acid, 5ml/L lactic acid and the balance deionized water with the conductivity less than 30 us/cm; adopting a voltage stabilization power supply mode, wherein 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 completed;
step five: activation treatment
The workpiece treated in the fourth step is placed in an activation tank liquid for activation treatment, wherein the content of industrial grade nitric acid in the activation tank liquid 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 activated water and deionized water are immediately transferred into an electroless nickel plating tank for plating treatment.
After pretreatment in this example, the surface of the workpiece is darker than the original metallic luster; after electroless plating with nickel and phosphorus, the plating layer is bright, flat, uniform and compact, and the thickness of the plating layer is 70 mu m (4 hours of electroless plating). The plating layer has no phenomena of bubbling, flaking and cracking when observed by an optical microscope; and (3) carrying out a thermal shock test on the plated workpiece, taking out the workpiece after heat preservation for 1.5 hours at 200 ℃, putting the workpiece into tap water for cooling, and reciprocating for 5 times, wherein the plating layer has no bubbling, peeling and cracking phenomena.
The foregoing is merely exemplary of the present invention and is not intended to limit the present invention. Various modifications and variations of the present invention will be apparent to those skilled in the art. Any modification, replacement, etc. 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 (6)
1. The pretreatment method of the chemical nickel-phosphorus plating of the aluminum and the aluminum alloy is characterized by comprising the following steps:
step one: deoiling with organic solvents
Soaking or brushing the surface of an aluminum or aluminum alloy workpiece with an organic solvent at room temperature to remove oil, degreasing the surface of the workpiece, and drying;
step two: stress relief annealing
Placing the workpiece with the surface oil stain removed into a constant temperature oven for stress removal 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 completed;
step three: chemical degreasing
Degreasing the workpiece treated in the second step in aluminum piece degreasing agent solution at 30-60 ℃ for 10-30min, and washing the workpiece with 40-80 ℃ hot water and room-temperature flowing tap water in sequence after degreasing, wherein the surface of the washed workpiece is in a wetting state, and a continuous water film is formed and is not broken for at least 30 seconds;
step four: electrolytic passivation treatment
Placing the workpiece treated in the third step into electrolytic passivation tank liquor for electrolytic passivation treatment, adopting a voltage stabilizing and power supplying mode, controlling the voltage range to be 15-20V, the electrolysis temperature to be less than or equal to 20 ℃ and the electrolysis time to be 5-15min, and washing the workpiece cleanly by tap water and deionized water in sequence after the treatment is finished;
wherein the electrolytic passivation tank solution consists of sulfuric acid, industrial oxalic acid, lactic acid and deionized water with the conductivity of less than 30us/cm for a storage battery; in the electrolytic passivation tank solution, the storage battery uses deionized water with the sulfuric acid content of 140-200g/L, the industrial oxalic acid content of 15-25g/L, the lactic acid content of 3-10ml/L and the rest of conductivity less than 30 us/cm;
step five: activation treatment
Placing the workpiece subjected to the treatment in an activation tank liquid for activation treatment, wherein the treatment temperature is room temperature, the treatment time is 1-3min, and after the activation treatment is finished, the workpiece is sequentially washed by tap water and deionized water and immediately transferred into a chemical nickel plating tank for plating treatment;
wherein the activation tank liquor consists of industrial grade nitric acid and tap water; in the activation tank liquid, the content of industrial grade nitric acid is 300-650g/L, and the balance is tap water.
2. The method according to claim 1, wherein the organic solvent in the first step is any one or a mixture of several of the following organic solvents: gasoline, kerosene, ethanol, acetone, trichloroethylene, carbon tetrachloride and a universal quick-drying diluent.
3. The method of claim 1, wherein the electrolytic passivation tank solution contains 140g/L sulfuric acid, 15g/L technical oxalic acid, 3ml/L lactic acid and deionized water with conductivity less than 30 us/cm.
4. The method of claim 1, wherein the electrolytic passivation tank solution contains 160g/L sulfuric acid, 20g/L technical oxalic acid, 4ml/L lactic acid and deionized water with conductivity less than 30 us/cm.
5. The method of claim 1, wherein the electrolytic passivation tank solution contains 200g/L sulfuric acid, 25g/L technical oxalic acid, 5ml/L lactic acid and deionized water with conductivity less than 30 us/cm.
6. Use of the pretreatment method of electroless nickel phosphorus plating of aluminum and aluminum alloy according to any one of claims 1 to 5 in the field of surface protection treatment of metal materials.
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| 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 |
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| 铝及铝合金直接化学镀镍前处理工艺研究;范建凤等;《忻州师范学院学报》;第23卷(第2期);第7-9页 * |
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