CN111411352B - Die-casting aluminum frame containing nickel plating layer and preparation method thereof - Google Patents

Die-casting aluminum frame containing nickel plating layer and preparation method thereof Download PDF

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Publication number
CN111411352B
CN111411352B CN202010293203.XA CN202010293203A CN111411352B CN 111411352 B CN111411352 B CN 111411352B CN 202010293203 A CN202010293203 A CN 202010293203A CN 111411352 B CN111411352 B CN 111411352B
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nickel
die
aluminum frame
nickel plating
acid
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CN111411352A (en
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王小锋
刘秋华
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Shenzhen City Xin Maoxin Industrial Co ltd
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Shenzhen City Xin Maoxin Industrial Co ltd
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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
    • C23C18/48—Coating with alloys
    • C23C18/50—Coating with alloys with alloys based on iron, cobalt or nickel
    • 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
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1689—After-treatment
    • 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
    • C23C18/1844—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
    • 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
    • C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
    • C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites

Abstract

The invention relates to the technical field of die-casting aluminum materials, and particularly provides a die-casting aluminum frame containing a nickel plating layer and a preparation method thereof. The invention provides a die-casting aluminum frame containing a nickel-plated layer, which comprises the nickel layer and the die-casting aluminum frame from top to bottom, wherein the thickness of the nickel layer is 3-10 pm; the preparation raw materials of the nickel layer comprise a first deposition zinc-nickel solution, a second deposition zinc-nickel solution, an acid nickel plating solution and an alkaline nickel plating solution which are acted together, so that the obtained nickel layer is compact, the problems of easy oxidation and instability of the surface of the die-casting aluminum frame are solved, the adhesion force of the nickel layer is high, the nickel layer is not easy to fall off, meanwhile, the hardness of the obtained material is high, the corrosion resistance is good, the magnetic conductivity is low, and the preparation method has potential application in the field of mobile phone camera frames.

Description

Die-casting aluminum frame containing nickel plating layer and preparation method thereof
Technical Field
The invention relates to the technical field of die-casting aluminum materials, and particularly provides a die-casting aluminum frame containing a nickel plating layer and a preparation method thereof.
Background
The aluminum alloy has low density, good corrosion resistance, higher fatigue resistance, higher specific strength and specific stiffness, is equivalent to structural steel and even ultra-high strength steel, is widely applied to the preparation of mobile phone components so as to reduce the weight of the mobile phone structure, and the support material of the mobile phone lens is molded by the aluminum alloy at present; the die-casting aluminum frame has some defects, such as that the die-casting material is not compact, the hardness of the aluminum alloy is low in the actual use process, and the wear resistance is poor.
The coating can be coated in the practical application process of die-casting aluminum, and the surface hardness and the wear resistance can be greatly improved after chemical nickel plating. Chemical nickel plating is a new surface treatment technology, and is widely applied to the industries because of good plating quality, excellent corrosion resistance and wear resistance and convenient operation; however, most of the existing chemical nickel plating has some defects, for example, the nickel deposition speed and the stability of the plating solution are not efficiently balanced, the plating speed is faster 20 minutes before plating, the plating speed is rapidly reduced 20 minutes after plating, the average plating speed is slower, the bonding force of the plating layer is poor, the plating solution is easy to fall off, the plating solution is unstable, and autocatalytic decomposition is easy to occur during high-temperature chemical nickel plating; some nickel deposition rates are too slow, one plating period is too long, and the efficiency is not high; more importantly, the prepared die-cast aluminum surface nickel-plated workpiece has high magnetic conductivity, and is easy to generate adverse effects on mobile phone signals and the like in the use process of the mobile phone lens support.
Disclosure of Invention
In order to solve the technical problems, the invention provides a die-casting aluminum frame containing a nickel-plated layer, which comprises the nickel layer and the die-casting aluminum frame from top to bottom, wherein the thickness of the nickel layer is 3-10 pm; the preparation raw materials of the nickel layer comprise a first zinc-nickel deposition solution, a second zinc-nickel deposition solution, an acidic nickel plating solution and an alkaline nickel plating solution.
As a preferred technical scheme of the invention, the magnetic conductivity of the nickel layer is less than or equal to 1.01; the remanence is less than 0.8 Gs.
As a preferred technical scheme of the invention, the acidic nickel plating solution solvent comprises the following components in concentration: 18-42 g/L nickel salt, 33-146 g/L organic acid and salt thereof, 17-35 g/L hypophosphite and 5-17 mg/L stabilizer.
As a preferred technical scheme of the invention, the pH value of the acidic nickel plating solution is 4.2-4.8.
In a preferred embodiment of the present invention, the stabilizer is a metal-based stabilizer including at least one of a metal element, a metal salt of the metal element, and a metal oxide of the metal element.
As a preferred technical scheme of the invention, the organic acid and the salt thereof are carboxylic acid and the derivatives thereof and/or alpha-hydroxy acid and the derivatives thereof; preferably, the alpha-hydroxy acid and its derivatives are selected from any one or a combination of glycolic acid, lactic acid, citric acid, sodium citrate, mandelic acid, malic acid, salicylic acid.
As a preferred technical scheme of the invention, the acidic nickel plating solution also comprises 20-100 mg/L of penetrant; preferably, the infiltrant includes at least one of ruthenium, rhodium, palladium, osmium, iridium, platinum, and metal salts or metal oxides thereof.
The second aspect of the invention provides a preparation method of the die-casting aluminum frame containing the nickel-plated layer, wherein the surface of the die-casting aluminum frame is subjected to oil removal and silicon removal; and then sequentially carrying out first zinc nickel deposition, second zinc nickel deposition, alkaline nickel plating, acid nickel plating, hole sealing and drying treatment.
As a preferred technical scheme of the invention, the reagent used for the acidic nickel plating treatment is the acidic nickel plating solution, and the plating temperature is 76-93 ℃.
The third aspect of the invention provides a die-casting aluminum frame containing a nickel plating layer applied to a mobile phone camera.
Compared with the prior art, the invention has the following beneficial effects:
(1) the preparation raw materials of the nickel layer in the die-casting aluminum frame containing the nickel plating layer provided by the invention comprise a first zinc-nickel deposition solution, a second zinc-nickel deposition solution, an acidic nickel plating solution and an alkaline nickel plating solution which are acted together, so that the obtained nickel layer is compact, and the problems of easy oxidation and instability of the surface of the die-casting aluminum frame are solved;
(2) the preparation raw materials of the nickel layer in the die-casting aluminum frame containing the nickel-plated layer have synergistic effect, so that the nickel layer is high in adhesive force and not easy to fall off, and meanwhile, the obtained material is high in hardness, good in corrosion resistance and low in magnetic permeability, and has potential application in the field of mobile phone camera frames.
Detailed Description
In order to further understand the structure, characteristics and other objects of the present invention, the following detailed description is given with reference to the accompanying preferred embodiments, which are only used for illustrating the technical solutions of the present invention and are not limited to the present invention. The invention will be further understood by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. To the extent that a definition of a particular term disclosed in the prior art is inconsistent with any definitions provided herein, the definition of the term provided herein controls.
As used herein, a feature that does not define a singular or plural form is also intended to include a plural form of the feature unless the context clearly indicates otherwise. It will be further understood that the term "prepared from …," as used herein, is synonymous with "comprising," including, "comprising," "having," "including," and/or "containing," when used in this specification means that the recited composition, step, method, article, or device is present, but does not preclude the presence or addition of one or more other compositions, steps, methods, articles, or devices. Furthermore, the use of "preferred," "preferably," "more preferred," etc., when describing embodiments of the present application, is meant to refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. In addition, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
The invention provides a die-casting aluminum frame containing a nickel-plated layer, which comprises the nickel layer and the die-casting aluminum frame from top to bottom, wherein the thickness of the nickel layer is 3-10 pm; the preparation raw materials of the nickel layer comprise first deposition zinc nickel solution, second deposition zinc nickel solution, acidic nickel plating solution and alkaline nickel plating solution.
Preferably, the magnetic permeability of the nickel layer is less than or equal to 1.01; the remanence is less than 0.8 Gs.
The source of the die-cast aluminum frame is not particularly limited in the present invention, and in one embodiment, the die-cast aluminum frame is available from Dongguan and magnesium hardware, Inc.
The first-time zinc-nickel deposition solution is a mixed aqueous solution containing nickel ions and comprises the following components in concentration: 30-50 g/L nickel sulfate, 50-130 g/L nickel chloride, 20-60 g/L sodium hydroxide and 20-30 g/L zinc sulfate; preferably, the following concentrations of components are included: 36-43 g/L nickel sulfate, 70-95 g/L nickel chloride, 36-53 g/L sodium hydroxide and 23-26 g/L zinc sulfate; more preferably, the following concentrations of the components are included: 38g/L nickel sulfate, 86g/L nickel chloride, 48g/L sodium hydroxide and 25g/L zinc sulfate.
The second zinc-nickel deposition solution is a mixed aqueous solution containing nickel ions, and comprises the following components in concentration: 30-50 g/L nickel sulfate, 50-130 g/L nickel chloride, 20-60 g/L sodium hydroxide and 20-30 g/L zinc sulfate; preferably, the following concentrations of components are included: 38-45 g/L nickel sulfate, 68-97 g/L nickel chloride, 35-51 g/L sodium hydroxide and 23-28 g/L zinc sulfate; more preferably, the following concentrations of the components are included: 42g/L nickel sulfate, 83g/L nickel chloride, 43g/L sodium hydroxide and 28g/L zinc sulfate.
The alkaline nickel plating solution is a mixed aqueous solution and comprises the following components in concentration: 30-50 g/L nickel sulfamate, 10-40 g/L sodium hypophosphite and 10-30 g/L ammonia water; preferably, the following concentrations of components are included: 35-45 g/L of nickel sulfamate, 15-30 g/L of sodium hypophosphite and 15-25 g/L of ammonia water; more preferably, the following concentrations of the components are included: 39g/L of nickel sulfamate, 26g/L of sodium hypophosphite and 22g/L of ammonia water.
The acidic nickel plating solution comprises a solvent and the following components in concentration: 20-45 g/L nickel salt, 35-140 g/L organic acid and salt thereof, 17-35 g/L hypophosphite and 5-20 mg/L stabilizer.
The pH value of the acidic nickel plating solution is 4.2-4.8, and the pH range and the components of the nickel plating solution act together, so that the stability of nickel plating in a system, the forming speed of a plating layer, and the flatness, the brightness, the hardness and the magnetic conductivity of the obtained plating layer are all better.
The solvent constitutes a large part of the nickel plating solution, and the solvent may be of a type well known to those skilled in the art, and is not particularly limited, such as water and the like.
The nickel salt may be dissolved in the solvent, and the nickel salt may supply nickel ions for plating to a plating object to form a nickel plating layer on a surface of the plating object. The nickel salt is well known to those skilled in the art, and is any one or combination of nickel salts for nickel plating, such as nickel sulfamate, nickel sulfate, nickel chloride, nickel nitrate, nickel oxide and nickel carbonate, and is preferably nickel sulfate.
The concentration of the nickel salt in the nickel plating solution is 20-45 g/L; preferably 25-35 g/L; the application adopts higher sulfate concentration, which is different from the prior art that the concentration is generally lower, and generally, when the concentration of nickel sulfate is higher than 15g/L, because the stability of nickel plating solution is reduced, self-decomposition can occur, the plating time is longer, a plating layer has defects, the hardness is poorer, and the flatness and the brightness are also poorer; the applicant also finds that in the overall technical scheme of the application, when the content of nickel sulfate is 18-42 g/L, the magnetic conductivity of the obtained coating is low, the hardness of the coating is high, and the plating efficiency is high, and when the content of nickel sulfate is low or nickel chloride is adopted, the performance of the coating is deteriorated, and the self-decomposition of the nickel plating solution at high concentration and the reduction of the content of impurities containing nickel are avoided and the formation of a uniform coating on the surface of a plated object are promoted probably due to the combined action of nickel sulfate and the specific organic acid and the salt thereof, the stabilizer and the penetrating agent in the scheme of the application, while when the concentration is low, the formation of a nickel layer on the surface of the plated object is influenced, and meanwhile, the tensile stress of the coating is prevented from being increased due to the accumulation of Cl-ions and the corrosion resistance of the coating is reduced.
The organic acid and its salt can be dissolved in a solution, and the organic acid and its salt are carboxylic acid and its derivatives and/or alpha-hydroxy acid and its derivatives.
As the carboxylic acid and its derivative, for example, but not limited to: acetic acid, adipic acid, formic acid, propionic acid, butyric acid, valeric acid, caproic acid, enanthic acid, caprylic acid, pelargonic acid, capric acid, undecanoic acid, lauric acid, tridecanoic acid, myristic acid, pentadecanoic acid, palmitic acid, margaric acid, stearic acid, arachidic acid, oxalic acid, malonic acid, tartaric acid, succinic acid, glutaric acid, pimelic acid, suberic acid, azelaic acid, sebacic acid, maleic acid, adipic acid, and the like.
The alpha-hydroxy acid and its derivatives are selected from glycolic acid, lactic acid, citric acid, sodium citrate, mandelic acid, malic acid, salicylic acid.
Preferably, the organic acid and salts thereof are alpha-hydroxy acids; further preferably, the organic acid and its salt include sodium citrate, malic acid and lactic acid.
The organic acid and the salt thereof can be chemically combined with the nickel ions to form a nickel complex, and the type and the content of the organic acid and the salt thereof have a large relationship with the stability of the nickel plating solution, the hardness and the magnetic permeability of a plating layer or the plating efficiency and the like in the actual use process, so that the selection of the appropriate organic acid and the salt thereof according to the actual needs and the actually solved problems or purposes is very important in the use process; in the technical scheme of the application, the applicant unexpectedly finds that when sodium citrate, malic acid, lactic acid and 20-45 g/L nickel sulfate are adopted to act together and act together with a stabilizer and a penetrating agent, the magnetic conductivity of the plating layer is low, the hardness of the plating layer is high, and the plating efficiency is high; probably because the malic acid is a hydroxycarboxylic acid substance containing 4 carbon atoms and two carboxyl groups, the malic acid is ionized under neutral conditions and is not ionized under acidic conditions, and the malic acid and the citric acid and the lactic acid containing 3 carbon atoms and one carboxyl group have the combined action of two organic acids with better complexing action, so that the generation content and speed of hydrogen ions are reduced, and the pH of the nickel plating solution is prevented from changing sharply.
Preferably, the concentration of the organic acid and the salt thereof is 35-140 g/L; more preferably, the concentration of the organic acid and the salt thereof is 90-125 g/L; more preferably the concentration of the organic acid and salts thereof is 110 g/L.
Preferably, the weight ratio of the sodium citrate, the malic acid and the lactic acid is 1: (1.5-5): (4-20); further preferably, the weight ratio of the sodium citrate, the malic acid and the lactic acid is 1: (1.5-2.5): (6.3-9.4); more preferably, the weight ratio of the sodium citrate, the malic acid and the lactic acid is 1: 2.2: 8.8.
as described above, the content of the organic acid or the salt thereof has a large relationship with respect to the stability of the nickel plating solution, the hardness and the magnetic permeability of the plating layer, the plating efficiency, and the like, and the applicant found that when the weight ratio of the sodium citrate, the malic acid, and the lactic acid is 1: (1.5-5): (4-20); particularly, when the weight ratio of the sodium citrate to the malic acid to the lactic acid is 1: (1.5-2.5): (6.3-9.4), the performance of the obtained coating is good, and probably because a stable network structure is formed between the organic acid and the salt thereof and the nickel ions under the condition that the pH of the system is controlled to be stable under the condition, the generation of a complexing agent, an impurity simple substance and the like in the plating process is avoided, and the deposition at the concave part of the aluminum alloy is promoted.
The concentration of the hypophosphite is 17-35 g/L; the nickel plating solution system is a nickel plating solution system with high phosphorus content, and the concentration is preferably 21-29 g/L; more preferably 23 to 26 g/L. In the technical scheme of the application, when the concentration of hypophosphite is low, the uniformity of the plating layer is damaged, and the magnetic permeability of the plating layer is also reduced.
The stabilizer is a metal stabilizer and comprises at least one of a metal element, a metal salt of the metal element and a metal oxide of the metal element; preferably, the metal element includes at least one of tin, zinc, magnesium, lead, cadmium, selenium, tellurium, molybdenum, arsenic, bismuth, zirconium; further preferably, the stabilizer comprises zinc sulfate and zirconium nitrate; further preferably, the weight ratio of zinc sulfate to zirconium nitrate is 1: (0.25-0.45); more preferably, the weight ratio of zinc sulfate to zirconium nitrate is 1: 0.33.
the concentration of the stabilizer is 5-20 mg/L; preferably 5-10 mg/L; further preferably 7.5 to 9.5 mg/L. The zinc sulfate and the zirconium nitrate are added into the system to inhibit the speed of reduction reaction, the rate of phosphate precipitation is controlled, and black precipitates in the system are prevented from being formed, so that the quality of a coating is influenced.
The nickel plating solution also comprises 20-100 mg/L of penetrating agent, wherein the penetrating agent comprises at least one of ruthenium, rhodium, palladium, osmium, iridium, platinum and metal salts or metal oxides thereof, such as palladium salt and palladium chloride; preferably, the concentration of the penetrating agent is 40-60 mg/L; further preferably 43 to 55 mg/L. The application adopts a specific metal substance as a penetrating agent, can act together with the stabilizer, nickel salt, organic acid and salt thereof, improves the stability of the plating solution and the stability of the deposition speed, avoids the instability of the system caused by high nickel sulfate concentration, and simultaneously, the applicant finds that the content of the components exists in a certain proportion, thereby being beneficial to rapidly seeping into tiny gaps on the surface of the aluminum alloy while depositing nickel, being beneficial to the smooth proceeding of the die casting process of the aluminum alloy in the process of a mobile phone lens frame and being beneficial to the reduction of the magnetic conductivity of the material.
The second aspect of the invention provides a preparation method of the die-casting aluminum frame containing the nickel-plated layer, wherein the surface of the die-casting aluminum frame is subjected to oil removal and silicon removal; and then sequentially carrying out first zinc nickel deposition, second zinc nickel deposition, alkaline nickel plating, acid nickel plating, hole sealing and drying treatment.
The reagents used for the first zinc nickel deposition, the second zinc nickel deposition, the alkaline nickel plating and the acidic nickel plating are respectively a first zinc nickel deposition solution, a second zinc nickel deposition solution, an alkaline nickel plating solution and an acidic nickel plating solution.
Preferably, the preparation method of the die-casting aluminum frame containing the nickel-plated layer comprises the following steps:
(1) oil removal: placing the die-casting aluminum frame in an oil removing tank containing an alkaline reagent, and treating for 5-10 min at 45-55 ℃; wherein the alkaline agent is at least one of sodium hydroxide aqueous solution, sodium carbonate aqueous solution or saponified alkali solution; the concentration of the sodium hydroxide is 50-75 wt%;
(2) silicon removal: then, continuously placing the die-cast aluminum frame obtained in the step (1) in a silicon removal tank containing a strong oxidant and/or a fluorine-containing reagent, and treating for 30-90 s at 10-30 ℃; preferably 50-70 s;
the kind of the strong oxidizing agent is not particularly limited in the present invention, and is an oxide well known to those skilled in the art, such as an aqueous hydrogen peroxide solution; further preferably, the concentration of the hydrogen peroxide is 50-70 mL/L;
the kind of the fluorine-containing agent is not particularly limited in the present invention, and is a fluorine-containing compound for removing silicon, such as ammonium bifluoride;
(3) depositing zinc and nickel for the first time: soaking the die-cast aluminum frame obtained in the step (2) in a first deposition zinc-nickel solution at the temperature of 20-40 ℃;
(4) and (3) depositing zinc and nickel for the second time: soaking the die-cast aluminum frame obtained in the step (3) in a secondary zinc-nickel deposition solution at the temperature of 20-40 ℃ for 10-50 s;
(5) alkaline nickel plating: soaking the die-cast aluminum frame obtained in the step (4) in an alkaline nickel plating solution at the temperature of 20-45 ℃ for 3-8 min;
(6) acid nickel plating: soaking the die-cast aluminum frame obtained in the step (5) in an acidic nickel plating solution at 76-93 ℃ for 25-100 min;
(7) hole sealing: placing the die-cast aluminum frame obtained in the step (6) at 60-80 ℃ for 3-10 min, and treating by using a hole sealing agent;
(8) and (3) drying: and (5) placing the die-cast aluminum frame obtained in the step (7) in a drying oven at the temperature of 150-260 ℃ for 1-3 h.
The kind of the sealing agent is not particularly limited in the present invention, and is a material of the sealing agent well known to those skilled in the art, and preferably, the sealing agent includes water and the following components in concentration: 5-10 g/L siloxane, 300-600 mL/L polyethylene glycol and 25-30 g/L octadecanethiol.
The siloxane is selected from any one of isobutyl triethoxysilane, gamma-aminopropyl triethoxysilane, 3-aminopropyl trimethoxysilane, gamma-mercaptopropyl triethoxysilane and gamma-glycidoxypropyl trimethoxysilane; preferably, the siloxane comprises isobutyl triethoxysilane and gamma-aminopropyl triethoxysilane; further preferably, the weight ratio of the isobutyl triethoxysilane to the gamma-aminopropyltriethoxysilane is (0.2-0.4): 1; more preferably, the weight ratio of isobutyltriethoxysilane to gamma-aminopropyltriethoxysilane is from 0.3: 1.
the polyethylene glycol is selected from any one or combination of polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 600, polyethylene glycol 800, polyethylene glycol 1000 and polyethylene glycol 2000; preferably, the polyethylene glycol is polyethylene glycol 200, polyethylene glycol 400, and polyethylene glycol 800; further preferably, the weight ratio of polyethylene glycol 200, polyethylene glycol 400 and polyethylene glycol 800 is 1: (2.5-3): (0.3 to 0.6); more preferably, the weight ratio of polyethylene glycol 200, polyethylene glycol 400 and polyethylene glycol 800 is 1: 2.7: 0.5.
in the plating process, the final plating layer is finally protected by adopting a hole sealing agent, and the experimental process shows that the corrosion resistance effect can be effectively improved by adopting the combined action of isobutyl triethoxysilane and gamma-aminopropyltriethoxysilane and polyethylene glycol, particularly when the polyethylene glycol is polyethylene glycol 200, polyethylene glycol 400 and polyethylene glycol 800, and the weight ratio of the polyethylene glycol 200 to the polyethylene glycol 400 to the polyethylene glycol 800 is 1: (2.5-3): (0.3-0.6), polyethylene glycol with different molecular weights and different viscosities can act together, so that the system uniformity of the hole sealing agent is facilitated, the dispersion of siloxane is facilitated, a protective film with water resistance and corrosion resistance is formed on the surface of a workpiece under the combined action of the hole sealing agent and the siloxane, the residual metal reactivity on the surface of a coating can be eliminated, the corrosion resistance effect of the film material is enhanced, and the coating is prevented from falling off.
The third aspect of the invention provides a die-casting aluminum frame containing a nickel plating layer applied to a mobile phone camera.
Example 1
Embodiment 1 of the invention provides a die-casting aluminum frame containing a nickel plating layer, which comprises the nickel layer and the die-casting aluminum frame from top to bottom, wherein the preparation raw material of the nickel layer comprises a first zinc-nickel deposition solution, a second zinc-nickel deposition solution, an acidic nickel plating solution and an alkaline nickel plating solution;
the first-time zinc-nickel deposition solution is a mixed aqueous solution containing nickel ions and comprises the following components in concentration: 38g/L nickel sulfate, 86g/L nickel chloride, 48g/L sodium hydroxide and 25g/L zinc sulfate;
the second zinc-nickel deposition solution is a mixed aqueous solution containing nickel ions, and comprises the following components in concentration: 42g/L nickel sulfate, 83g/L nickel chloride, 43g/L sodium hydroxide and 28g/L zinc sulfate;
the alkaline nickel plating solution comprises the following components in concentration: 39g/L of nickel sulfamate, 26g/L of sodium hypophosphite and 22g/L of ammonia water;
the acidic nickel plating solution comprises a solvent and the following components in concentration: 31g/L of nickel salt, 110g/L of organic acid and salt thereof, 26g/L of hypophosphite, 8.6mg/L of stabilizer and 51mg/L of penetrant;
the solvent is water; the nickel salt is nickel sulfate; the organic acid and the salt thereof comprise sodium citrate, malic acid and lactic acid, and the weight ratio of the sodium citrate to the malic acid to the lactic acid is 1: 2.2: 8.8 of; the hypophosphite is sodium hypophosphite; the stabilizer comprises zinc sulfate and zirconium nitrate, wherein the weight ratio of the zinc sulfate to the zirconium nitrate is 1: 0.33; the penetrating agent is palladium chloride;
the preparation method of the die-casting aluminum frame containing the nickel-plated layer comprises the following steps:
(1) oil removal: placing the die-casting aluminum frame in an oil removing tank containing an alkaline reagent, and treating for 8min at 50-55 ℃; wherein the alkaline reagent is sodium hydroxide aqueous solution; the concentration of sodium hydroxide was 65 wt%;
(2) silicon removal: then, continuously placing the die-cast aluminum frame obtained in the step (1) in a silicon removal tank containing a strong oxidant, and treating for 60s at 25-30 ℃;
the strong oxidant is aqueous hydrogen peroxide; the concentration of the hydrogen peroxide is 62 mL/L;
(3) depositing zinc and nickel for the first time: soaking the die-cast aluminum frame obtained in the step (2) in a first deposition zinc-nickel solution at 35-40 ℃;
(4) and (3) depositing zinc and nickel for the second time: soaking the die-cast aluminum frame obtained in the step (3) in a secondary zinc-nickel deposition solution at 35-40 ℃ for 30 s;
(5) alkaline nickel plating: soaking the die-cast aluminum frame obtained in the step (4) in an alkaline nickel plating solution at 35-40 ℃ for 6 min;
(6) acid nickel plating: soaking the die-cast aluminum frame obtained in the step (5) in an acidic nickel plating solution at 85-90 ℃ for 85 min;
(7) hole sealing: placing the die-cast aluminum frame obtained in the step (6) at 70-80 ℃ for 6min, and treating by using a hole sealing agent;
the sealant comprises water and the following components in concentration: 8g/L siloxane, 550mL/L polyethylene glycol and 28g/L octadecanethiol;
the siloxane comprises isobutyl triethoxysilane and gamma-aminopropyl triethoxysilane; the weight ratio of isobutyl triethoxysilane to gamma-aminopropyl triethoxysilane is 0.3: 1; the polyethylene glycol is polyethylene glycol 200, polyethylene glycol 400 and polyethylene glycol 800; the weight ratio of polyethylene glycol 200, polyethylene glycol 400 and polyethylene glycol 800 is 1: 2.7: 0.5;
(8) and (3) drying: and (5) placing the die-cast aluminum frame obtained in the step (7) in a drying oven at 220-230 ℃ for 2h to obtain the aluminum frame.
Example 2
Embodiment 2 of the present invention provides a die-casting aluminum frame containing a nickel plating layer, which comprises a nickel layer and a die-casting aluminum frame from top to bottom, wherein the nickel layer is prepared from raw materials including a first zinc-nickel deposition solution, a second zinc-nickel deposition solution, an acidic nickel plating solution and an alkaline nickel plating solution;
the first-time zinc-nickel deposition solution is a mixed aqueous solution containing nickel ions and comprises the following components in concentration: 50/L nickel sulfate, 95g/L nickel chloride, 60g/L sodium hydroxide and 30g/L zinc sulfate;
the second zinc-nickel deposition solution is a mixed aqueous solution containing nickel ions, and comprises the following components in concentration: 50/L nickel sulfate, 95g/L nickel chloride, 60g/L sodium hydroxide and 30g/L zinc sulfate;
the alkaline nickel plating solution comprises the following components in concentration: 50g/L of nickel sulfamate, 40/L of sodium hypophosphite and 30g/L of ammonia water;
the acidic nickel plating solution comprises a solvent and the following components in concentration: 45g/L of nickel salt, 125g/L of organic acid and salt thereof, 35g/L of hypophosphite, 15mg/L of stabilizer and 60mg/L of penetrant;
the solvent is water; the nickel salt is nickel sulfate; the organic acid and the salt thereof comprise sodium citrate, malic acid and lactic acid, and the weight ratio of the sodium citrate to the malic acid to the lactic acid is 1: 5: 20; the hypophosphite is sodium hypophosphite; the stabilizer comprises zinc sulfate and zirconium nitrate, wherein the weight ratio of the zinc sulfate to the zirconium nitrate is 1: 0.45 of; the penetrating agent is palladium chloride;
the preparation method of the die-casting aluminum frame containing the nickel-plated layer comprises the following steps:
(1) oil removal: placing the die-casting aluminum frame in an oil removing tank containing an alkaline reagent, and treating for 8min at 50-55 ℃; wherein the alkaline reagent is sodium hydroxide aqueous solution; the concentration of sodium hydroxide was 65 wt%;
(2) silicon removal: then, continuously placing the die-cast aluminum frame obtained in the step (1) in a silicon removal tank containing a strong oxidant, and treating for 60s at 25-30 ℃;
the strong oxidant is hydrogen peroxide aqueous solution; the concentration of the hydrogen peroxide is 62 mL/L;
(3) depositing zinc and nickel for the first time: soaking the die-cast aluminum frame obtained in the step (2) in a first deposition zinc-nickel solution at 35-40 ℃;
(4) and (3) depositing zinc and nickel for the second time: soaking the die-cast aluminum frame obtained in the step (3) in a secondary zinc-nickel deposition solution at 35-40 ℃ for 30 s;
(5) alkaline nickel plating: soaking the die-cast aluminum frame obtained in the step (4) in an alkaline nickel plating solution at 35-40 ℃ for 6 min;
(6) acid nickel plating: soaking the die-cast aluminum frame obtained in the step (5) in an acidic nickel plating solution at 85-90 ℃ for 85 min;
(7) hole sealing: placing the die-cast aluminum frame obtained in the step (6) at 70-80 ℃ for 6min, and treating by using a hole sealing agent;
the sealant comprises water and the following components in concentration: 10g/L siloxane, 600mL/L polyethylene glycol and 30g/L octadecanethiol;
the siloxane comprises isobutyl triethoxysilane and gamma-aminopropyl triethoxysilane; the weight ratio of isobutyl triethoxysilane to gamma-aminopropyltriethoxysilane is 0.4: 1; the polyethylene glycol is polyethylene glycol 200, polyethylene glycol 400 and polyethylene glycol 800; the weight ratio of polyethylene glycol 200, polyethylene glycol 400 and polyethylene glycol 800 is 1: 3: 0.6;
(8) and (3) drying: and (5) placing the die-cast aluminum frame obtained in the step (7) in a drying oven at 220-230 ℃ for 2h to obtain the aluminum frame.
Example 3
Embodiment 3 of the present invention provides a die-casting aluminum frame containing a nickel plating layer, which comprises a nickel layer and a die-casting aluminum frame from top to bottom, wherein the nickel layer is prepared from raw materials including a first zinc-nickel deposition solution, a second zinc-nickel deposition solution, an acidic nickel plating solution and an alkaline nickel plating solution;
the first-time zinc-nickel deposition solution is a mixed aqueous solution containing nickel ions and comprises the following components in concentration: 30g/L nickel sulfate, 50g/L nickel chloride, 40g/L sodium hydroxide and 20g/L zinc sulfate;
the second zinc-nickel deposition solution is a mixed aqueous solution containing nickel ions, and comprises the following components in concentration: 30g/L nickel sulfate, 50g/L nickel chloride, 40g/L sodium hydroxide and 20g/L zinc sulfate;
the alkaline nickel plating solution comprises the following components in concentration: 30g/L of nickel sulfamate, 15g/L of sodium hypophosphite and 15g/L of ammonia water;
the acidic nickel plating solution comprises a solvent and the following components in concentration: 25g/L of nickel salt, 90g/L of organic acid and salt thereof, 21g/L of hypophosphite, 5mg/L of stabilizer and 40mg/L of penetrant;
the solvent is water; the nickel salt is nickel sulfate; the organic acid and the salt thereof comprise sodium citrate, malic acid and lactic acid, and the weight ratio of the sodium citrate to the malic acid to the lactic acid is 1: 1.5: 5; the hypophosphite is sodium hypophosphite; the stabilizer comprises zinc sulfate and zirconium nitrate, wherein the weight ratio of the zinc sulfate to the zirconium nitrate is 1: 0.25; the penetrating agent is palladium chloride;
the preparation method of the die-casting aluminum frame containing the nickel-plated layer comprises the following steps:
(1) oil removal: placing the die-casting aluminum frame in an oil removing tank containing an alkaline reagent, and treating for 8min at 50-55 ℃; wherein the alkaline reagent is sodium hydroxide aqueous solution; the concentration of sodium hydroxide was 65 wt%;
(2) silicon removal: then, continuously placing the die-cast aluminum frame obtained in the step (1) in a silicon removal tank containing a strong oxidant, and treating for 60s at 25-30 ℃;
the strong oxidant is hydrogen peroxide aqueous solution; the concentration of the hydrogen peroxide is 62 mL/L;
(3) depositing zinc and nickel for the first time: soaking the die-cast aluminum frame obtained in the step (2) in a first deposition zinc-nickel solution at 35-40 ℃;
(4) and (3) depositing zinc and nickel for the second time: soaking the die-cast aluminum frame obtained in the step (3) in a secondary zinc-nickel deposition solution at 35-40 ℃ for 30 s;
(5) alkaline nickel plating: soaking the die-cast aluminum frame obtained in the step (4) in an alkaline nickel plating solution at 35-40 ℃ for 6 min;
(6) acid nickel plating: soaking the die-cast aluminum frame obtained in the step (5) in an acidic nickel plating solution at 85-90 ℃ for 85 min;
(7) hole sealing: placing the die-cast aluminum frame obtained in the step (6) at 70-80 ℃ for 6min, and treating by using a hole sealing agent;
the sealant comprises water and the following components in concentration: 5g/L siloxane, 450mL/L polyethylene glycol and 25g/L octadecanethiol;
the siloxane comprises isobutyl triethoxysilane and gamma-aminopropyl triethoxysilane; the weight ratio of isobutyl triethoxysilane to gamma-aminopropyl triethoxysilane is 0.2: 1; the polyethylene glycol is polyethylene glycol 200, polyethylene glycol 400 and polyethylene glycol 800; the weight ratio of polyethylene glycol 200, polyethylene glycol 400 and polyethylene glycol 800 is 1: 2.5: 0.3;
(8) and (3) drying: and (5) placing the die-cast aluminum frame obtained in the step (7) in a drying oven at 220-230 ℃ for 2h to obtain the aluminum frame.
Example 4
Example 4 of the present invention provides a die-cast aluminum frame comprising a nickel plating layer, and the specific embodiment thereof is the same as example 1 except that the content of the alkaline nickel plating solution is 0.
Example 5
Example 5 of the present invention provides a die-cast aluminum frame comprising a nickel plating layer, and the specific embodiment thereof is the same as example 1 except that the content of the acidic nickel plating solution is 0.
Example 6
Example 6 of the present invention provides a die-cast aluminum frame comprising a nickel-plated layer, and the specific embodiment thereof is the same as example 1, except that the content of malic acid in the acidic nickel plating solution is 0.
Example 7
Example 7 of the present invention provides a die-cast aluminum frame comprising a nickel-plated layer, and the specific embodiment thereof is the same as example 1, except that the content of citric acid in the acidic nickel plating solution is 0.
Example 8
Example 8 of the present invention provides a die-cast aluminum frame including a nickel-plated layer, and the specific embodiment thereof is the same as example 1, except that the contents of citric acid and malic acid in the acidic nickel plating solution are 0.
Example 9
Example 9 of the present invention provides a die-cast aluminum frame comprising a nickel-plated layer, the embodiment being the same as example 1 except that the stabilizer is lead nitrate.
Example 10
Example 10 of the present invention provides a die-cast aluminum frame comprising a nickel-plated layer, which is similar to example 1, except that the content of the penetrant is 0.
Example 11
Example 11 of the present invention provides a die-cast aluminum frame comprising a nickel-plated layer, which is the same as example 1 except that the content of siloxane in the sealing agent is 0.
Example 12
Example 12 of the present invention provides a die-cast aluminum frame comprising a nickel-plated layer, which is the same as example 1 except that the content of polyethylene glycol 400 in the sealing agent is 0.
Performance evaluation
1. Film thickness: the thickness of the plated layer obtained in example 1 was measured by a film thickness meter to be 7 pm.
2. And (3) corrosion resistance testing: the coating obtained in the embodiments 1 to 4 is subjected to a smoke experiment by using a smoke machine, and the experiment shows that the smoke experiment treatment under 24H has no influence on the coatings obtained in the embodiments 1 to 3, and has no corrosion problem; the surface of the plating layer obtained in example 4 had corroded portions;
3. and (3) testing high temperature and high humidity resistance: carrying out high temperature and high humidity resistance tests on the examples 1-3 and the examples 5, 11 and 12 by using a high temperature and high humidity box, wherein the humidity is 85-90%, and the temperature is 90 ℃; after 120H treatment, the plating layers obtained in the embodiments 1 to 3 have no obvious change, particularly have good high temperature and high humidity resistance, and the plating layers in the embodiments 5, 11 and 12 have the problem of falling off;
4. testing the residual magnetic rate: the remanence rate test is carried out on the gauss meter of the example 1, and the test result is that the gauss meter of the example 1 is 0.5 Gs;
5. and (3) magnetic permeability test: and the magnetic permeability tester is used for carrying out the magnetic permeability test on the embodiment 1 and the embodiment 5, and the test result shows that the magnetic permeability of the embodiment 1 is 1.006 ur; the magnetic permeability of example 4 was 1.095.
6. And (3) hardness testing: the hardness test was carried out for examples 1 to 12;
7. and (3) testing the plating layer formation time: measuring the deposition rate V when the coating is formed in the examples 1 to 12; grade A: when the deposition rate is 16< V <22 μm/h; grade B: when the deposition rate is 12< V <16 μm/h; grade C: when the deposition rate is V <12 mu m/h;
8. testing the flatness and smoothness of the plating layer: the flatness and smoothness of the plating layers of examples 1 to 12 were observed, that is, whether the formed plating layers had depressions or projections or black spots was observed, and the evaluation scale was as follows: each example corresponds to 45 samples, a: the number of the pits or projections or black spots is 0-3; b: the number of the pits or projections or black spots is 4-13; c: the number of the pits or projections or black spots is 14-28; d: the number of the concave or convex or black spots is 29-45.
TABLE 1
Hardness of 100g/f Flatness and smoothness Coating time
Example 1 579 A A
Example 2 576 A A
Example 3 571 A A
Example 6 535 \ B
Example 7 544 \ B
Example 8 475 \ C
Example 9 464 B B
Example 10 457 D C
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.

Claims (6)

1. A die-casting aluminum frame containing a nickel plating layer is characterized by comprising the nickel layer and the die-casting aluminum frame from top to bottom, wherein the preparation raw material of the nickel layer comprises a first zinc-nickel deposition solution, a second zinc-nickel deposition solution, an acidic nickel plating solution and an alkaline nickel plating solution;
the acidic nickel plating solution solvent comprises the following components in concentration: 25-35g/L of nickel salt, 33-146 g/L of organic acid and salt thereof, 17-35 g/L of hypophosphite and 7.5-9.5mg/L of stabilizer;
the stabilizer comprises zinc sulfate and zirconium nitrate;
the organic acid and the salt thereof are sodium citrate, malic acid and lactic acid, and the weight ratio is 1: (1.5-2.5): (6.3-9.4);
the acid nickel plating solution also comprises 43-55mg/L of penetrant; the penetrant is palladium chloride.
2. The die-cast aluminum frame with nickel plating layer as recited in claim 1, wherein the magnetic permeability of the nickel layer is 1.01 or less; the remanence is less than 0.8 Gs.
3. The die-cast aluminum frame with nickel plating layer according to claim 1, wherein the acidic nickel plating solution has a pH of 4.2 to 4.8.
4. A method for preparing the die-casting aluminum frame containing the nickel-plated layer according to any one of claims 1 to 3, wherein the surface of the die-casting aluminum frame is degreased and desilicated; and then sequentially carrying out first zinc nickel deposition, second zinc nickel deposition, alkaline nickel plating, acid nickel plating, hole sealing and drying treatment.
5. The method for manufacturing a die-cast aluminum frame with a nickel-plated layer according to claim 4, wherein the acidic nickel plating solution is used as a reagent for acidic nickel plating, and the plating temperature is 76 to 93 ℃.
6. A die-cast aluminum frame containing a nickel-plated layer according to any one of claims 1 to 4, which is applied to a camera for a cellular phone.
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