CN109652788B - Preparation method of nickel-plated low-carbon steel wire - Google Patents
Preparation method of nickel-plated low-carbon steel wire Download PDFInfo
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- 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
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- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
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- C21D8/06—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of rods or wires
- C21D8/065—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of rods or wires of ferrous alloys
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- 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
- C23C18/1635—Composition of the substrate
- C23C18/1637—Composition of the substrate metallic substrate
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- 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
- C23C18/1646—Characteristics of the product obtained
- C23C18/165—Multilayered product
- C23C18/1651—Two or more layers only obtained by electroless plating
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- 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
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- 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
- C23C18/52—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 using reducing agents for coating with metallic material not provided for in a single one of groups C23C18/32 - C23C18/50
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- 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F17/00—Multi-step processes for surface treatment of metallic material involving at least one process provided for in class C23 and at least one process covered by subclass C21D or C22F or class C25
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Abstract
The invention discloses a preparation method of a nickel-plated low-carbon steel wire, which comprises alkali washing activation, acid washing, wire drawing annealing, zinc dipping, nickel preplating, nickel plating, drying, heat treatment and wire rewinding. According to the invention, by optimizing the preparation process and adopting the zinc dipping process design, the oxide film layer on the surface of the product can be removed, a uniform and compact zinc film can be formed, the binding property of subsequent nickel plating is improved, and the compactness of a plating layer is improved; by adopting the alkaline chemical nickel plating pre-plating process, the use of the chemical nickel plating solution can be avoided being shortened due to the fact that the zinc film layer is poisoned by the acidic chemical nickel plating solution, the dissolution of the zinc film layer is effectively inhibited, a thin, fine and uniform nickel plating layer can be obtained to protect the zinc film layer, meanwhile, the subsequent chemical nickel plating processing is facilitated, and the nickel plating binding property is improved; the nickel plating process is optimized, the porosity of the plated layer is reduced, and the quality of the plated layer is improved; and a heat treatment process is added for refining the crystal grains of the coating, improving the uniformity of the coating, ensuring the hardness of the coating and simultaneously increasing the binding force.
Description
Technical Field
The invention relates to the technical field of tinning materials, in particular to a preparation method of a nickel-plated low-carbon steel wire.
Background
At present, in a lead wire of an electronic tube and the like, the existing iron wire has no good corrosion resistance, and the service life is short because the carbon content of the iron wire is too high and the iron wire is easy to corrode, and the nickel-plated wire is too high in cost and is not suitable for large-scale production.
Therefore, a lot of tin-plated low-carbon steel wires are adopted nowadays, so that the service performance of the material can be increased, and the high-temperature resistance, the corrosion resistance and the like are increased. If the publication number is CN107564624A, a hard tinned copper clad steel wire processing technology is disclosed, which comprises the following steps: the method comprises the following steps: softening and straightening the low-carbon steel wire; step two: acid washing; step three: plating a first nickel plating layer; step four: plating a copper layer; step five: plating a second nickel plating layer; step six: plating a tin layer; step seven: cleaning; step eight: drying; step nine: and (6) rolling. By using the processing technology, nickel is plated before copper plating and tin plating, so that the bonding force between a plating layer and a base material can be enhanced; meanwhile, the workability of copper is combined with the toughness of steel, so that the excellent toughness and torsion resistance of the copper are exerted. However, nowadays, the steel wire is mostly processed by using a tin-copper plating process, and in order to have good performance, the process needs a thicker copper plating layer, which results in longer processing time, relatively higher production cost, and relatively poorer compactness of the plating layer.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a nickel-plated low-carbon steel wire, which has the characteristics of good uniformity, strong coating compactness and strong binding force.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a nickel-plated low-carbon steel wire comprises the following steps:
s1, performing alkali washing and activation, selecting a low-carbon steel wire according to the process specification, putting the low-carbon steel wire into an alkali washing solution for alkali washing, then washing the low-carbon steel wire with clear water, and detecting the low-carbon steel wire;
s2, acid washing, namely, putting the low-carbon steel wire into an acid washing solution for acid washing, then washing with clear water, and detecting the low-carbon steel wire;
s3, wire drawing and annealing, wherein a continuous annealing wire drawing machine is adopted to finish the wire drawing and annealing process;
s4, zinc dipping, namely dipping the low-carbon steel wire into a zinc dipping solution to obtain a first-grade semi-finished product;
s41, primary zinc dipping, wherein the zinc dipping solution is prepared from a mixed solution of zinc sulfate, hydrofluoric acid and distilled water, the time is 150-200S, and the temperature is normal temperature;
s42, secondary zinc dipping, wherein the zinc dipping liquid is prepared from a mixed solution of zinc sulfate, hydrofluoric acid and distilled water, the time is 300-360S, and the temperature is normal temperature;
s5, pre-plating nickel, namely, completing the pre-plating nickel treatment of the primary semi-finished product through alkaline chemical nickel plating solution, and washing the primary semi-finished product with clear water after completing the pre-plating nickel to obtain a secondary semi-finished product;
s6, nickel plating, namely, completing the nickel plating treatment of the secondary semi-finished product in a nickel plating solution, wherein the nickel plating solution comprises a nickel sulfamate solution, nickel chloride, boric acid, an accelerator M and a nickel plating wetting agent, a nickel plate is placed in the nickel plating solution, and the nickel plate is washed by pure water after the nickel plating is completed to obtain a tertiary semi-finished product;
s7, drying, and air-drying the third-level semi-finished product through cold air;
s7, performing heat treatment, namely introducing the three-stage semi-finished product into a temperature control pipeline for heat treatment at 320-380 ℃ for 45-75 min, and air-cooling to normal temperature after being led out;
and S8, taking up, cooling the finished product, and finishing taking up and packaging by using a take-up machine.
In step S4, the usage amount of zinc sulfate is 8-12 g/L, the usage amount of hydrofluoric acid is 70-80 mL/L, and the balance is distilled water.
In step S4, the usage amount of zinc sulfate is 10g/L, the usage amount of hydrofluoric acid is 75mL/L, and the balance is distilled water.
In step S41, the primary zincing time is 180S, and in step S42, the secondary zincing time is 320S.
In step S5, the alkaline chemical nickel plating solution is a mixture of nickel sulfate, sodium hypophosphite, ammonium citrate and ammonium chloride, the pH value is 8-10, the temperature is 40-50 ℃, and the time is 4-8 min.
In step S5, the alkaline chemical nickel plating solution is mixed solution of nickel sulfate, sodium hypophosphite, ammonium citrate and ammonium chloride, the pH value is 9, the temperature is 45 ℃, and the time is 5 min.
In step S6, the dosage of the nickel sulfamate solution is 650-750 g/L, the dosage of the nickel chloride is 0-5 g/L, the dosage of the boric acid is 35-45 g/L, the dosage of the accelerator M is 6-9 mL/L, and the dosage of the nickel plating wetting agent is 0.2-0.5 mL/L.
In step S6, the dosage of the nickel sulfamate solution is 700g/L, the dosage of the nickel chloride is 2g/L, the dosage of the boric acid is 40g/L, the dosage of the accelerator M is 7mL/L, and the dosage of the nickel plating wetting agent is 0.3 mL/L.
In step S6, the current density is 1-4A/dm2。
In step S6, the current density is 2-4A/dm2。
The invention has the following beneficial effects: according to the invention, by optimizing the preparation process and adopting the zinc dipping process design, the oxide film layer on the surface of the product can be removed, a uniform and compact zinc film can be formed, the binding property of subsequent nickel plating is improved, and the compactness of a plating layer is improved; by adopting the alkaline chemical nickel plating pre-plating process, the use of the chemical nickel plating solution can be avoided being shortened due to the fact that the zinc film layer is poisoned by the acidic chemical nickel plating solution, the dissolution of the zinc film layer is effectively inhibited, a thin, fine and uniform nickel plating layer can be obtained to protect the zinc film layer, meanwhile, the subsequent chemical nickel plating processing is facilitated, and the nickel plating binding property is improved; the nickel plating process is optimized, the porosity of the plated layer is reduced, and the quality of the plated layer is improved; and a heat treatment process is added for refining the crystal grains of the coating, improving the uniformity of the coating, ensuring the hardness of the coating and simultaneously increasing the binding force.
The features of the present invention will be clearly understood by reference to the following detailed description of the preferred embodiments of the present invention.
Detailed Description
In order that the objects and advantages of the invention will be more clearly understood, the invention is further described in detail below with reference to examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The invention discloses a preparation method of a nickel-plated low-carbon steel wire, which comprises the following steps:
and S1, performing alkali washing and activation, selecting a low-carbon steel wire according to the process specification, putting the low-carbon steel wire into an alkali washing solution for alkali washing, then washing the low-carbon steel wire with clear water, and detecting the low-carbon steel wire.
And S2, acid washing, namely, putting the low-carbon steel wire into an acid washing solution for acid washing, then washing with clear water, and detecting the low-carbon steel wire.
And S3, wire drawing and annealing, wherein a continuous annealing wire drawing machine is adopted to finish the wire drawing and annealing process.
S4, zinc dipping, namely dipping the low-carbon steel wire into a zinc dipping solution to obtain a first-grade semi-finished product, wherein the dosage of zinc sulfate is 8-12 g/L, the dosage of hydrofluoric acid is 70-80 mL/L, and the balance is distilled water; by adopting the zinc dipping process design, the oxide film on the surface of the product can be removed, a uniform and compact zinc film can be formed, the bonding property of subsequent nickel plating is improved, and the compactness of a plating layer is improved.
S41, primary zinc dipping, wherein the zinc dipping liquid is prepared from a mixed solution of zinc sulfate, hydrofluoric acid and distilled water, the time is 150-200S, and the temperature is normal temperature.
S42, secondary zinc dipping, wherein the zinc dipping liquid is prepared from a mixed liquid of zinc sulfate, hydrofluoric acid and distilled water, the time is 300-360S, and the temperature is normal temperature.
S5, pre-plating nickel, namely, completing the pre-plating nickel treatment of the primary semi-finished product through an alkaline chemical nickel plating solution, washing the primary semi-finished product with clear water after the pre-plating nickel is completed, and preparing a secondary semi-finished product, wherein the alkaline chemical nickel plating solution is a mixed solution of nickel sulfate, sodium hypophosphite, ammonium citrate and ammonium chloride, the pH value is 8-10, the temperature is 40-50 ℃, the time is 4-8 min, and the preference is given; by adopting the alkaline chemical nickel plating pre-plating process, the use of the chemical nickel plating solution can be prevented from being shortened due to the fact that the zinc film layer is poisoned by the acidic chemical nickel plating solution, the dissolution of the zinc film layer is effectively inhibited, a thin, fine and uniform nickel plating layer can be obtained to protect the zinc film layer, meanwhile, the subsequent chemical nickel plating processing is facilitated, and the nickel plating binding property is favorably improved.
S6, nickel plating, namely, completing the nickel plating treatment on the secondary semi-finished product in a nickel plating solution, wherein the nickel plating solution comprises a nickel sulfamate solution, nickel chloride, boric acid, an accelerator M and a nickel plating wetting agent, a nickel plate is placed in the nickel plating solution, and the nickel plate is washed by pure water after the nickel plating is completed to obtain a tertiary semi-finished product, the dosage of the nickel sulfamate solution is 650-750 g/L, the dosage of the nickel chloride is 0-5 g/L, the dosage of the boric acid is 35-45 g/L, the dosage of the accelerator M is 6-9 mL/L, the dosage of the nickel plating wetting agent is 0.2-0.5 mL/L, and the current density is 1-4A/dm2(ii) a The nickel plating process is optimized, the porosity of the plating layer is reduced, and the quality of the plating layer is improved.
S7, drying, and air-drying the three-stage semi-finished product by cold air, preferably by cold air, so that the influence on the quality of the plating layer due to too high air temperature can be avoided.
And S7, performing heat treatment, namely introducing the three-stage semi-finished product into a temperature control pipeline for heat treatment at 320-380 ℃ for 45-75 min, cooling the product to normal temperature after the product is led out, and adding a heat treatment process for refining coating grains, improving coating uniformity, ensuring coating hardness and simultaneously increasing bonding force.
And S8, taking up, cooling the finished product, and finishing taking up and packaging by using a take-up machine.
Example 2
The invention discloses a preparation method of a nickel-plated low-carbon steel wire, which comprises the following steps:
and S1, performing alkali washing and activation, selecting a low-carbon steel wire according to the process specification, putting the low-carbon steel wire into an alkali washing solution for alkali washing, then washing the low-carbon steel wire with clear water, and detecting the low-carbon steel wire.
And S2, acid washing, namely, putting the low-carbon steel wire into an acid washing solution for acid washing, then washing with clear water, and detecting the low-carbon steel wire.
And S3, wire drawing and annealing, wherein a continuous annealing wire drawing machine is adopted to finish the wire drawing and annealing process.
S4, zinc dipping, namely dipping the low-carbon steel wire into a zinc dipping solution to obtain a first-grade semi-finished product, wherein the dosage of zinc sulfate is 10g/L, the dosage of hydrofluoric acid is 75mL/L, and the balance is distilled water; by adopting the zinc dipping process design, the oxide film on the surface of the product can be removed, a uniform and compact zinc film can be formed, the bonding property of subsequent nickel plating is improved, and the compactness of a plating layer is improved.
S41, primary zinc dipping, wherein the zinc dipping solution is prepared from a mixed solution of zinc sulfate, hydrofluoric acid and distilled water, the temperature is normal temperature, and the primary zinc dipping time is 180S.
S42, secondary zinc dipping, wherein the zinc dipping liquid is prepared by a mixed liquid of zinc sulfate, hydrofluoric acid and distilled water, the temperature is normal temperature, and the secondary zinc dipping time is 320S.
S5, pre-plating nickel, namely, completing the pre-plating nickel treatment of the primary semi-finished product through alkaline chemical nickel plating solution, washing the primary semi-finished product with clear water after the pre-plating nickel is completed, and preparing a secondary semi-finished product, wherein the alkaline chemical nickel plating solution is a mixed solution of nickel sulfate, sodium hypophosphite, ammonium citrate and ammonium chloride, the pH value is 9, the temperature is 45 ℃, and the time is 5 min; by adopting the alkaline chemical nickel plating pre-plating process, the use of the chemical nickel plating solution can be prevented from being shortened due to the fact that the zinc film layer is poisoned by the acidic chemical nickel plating solution, the dissolution of the zinc film layer is effectively inhibited, a thin, fine and uniform nickel plating layer can be obtained to protect the zinc film layer, meanwhile, the subsequent chemical nickel plating processing is facilitated, and the nickel plating binding property is favorably improved.
S6, nickel plating, namely, completing the nickel plating treatment of the secondary semi-finished product in a nickel plating solution, wherein the nickel plating solution comprises 700g/L of nickel sulfamate solution, 2g/L of nickel chloride, 40g/L of boric acid, 7mL/L of accelerator M, 0.3mL/L of nickel plating wetting agent and 2g/L of current density, the nickel chloride, the boric acid, the accelerator M and the nickel plating wetting agent are placed in the nickel plating solution, and the nickel plate is placed in the nickel plating solution and washed with pure water after the nickel plating is completed to obtain the tertiary semi-finished productA/dm2(ii) a The nickel plating process is optimized, the porosity of the plated layer is reduced, and the quality of the plated layer is improved; and a heat treatment process is added for refining the crystal grains of the coating, improving the uniformity of the coating, ensuring the hardness of the coating and simultaneously increasing the binding force.
S7, drying, and air-drying the three-stage semi-finished product by cold air, preferably by cold air, so that the influence on the quality of the plating layer due to too high air temperature can be avoided.
And S7, heat treatment, namely introducing the three-stage semi-finished product into a temperature control pipeline for heat treatment at 350 ℃ for 60min, and air cooling to normal temperature after being led out.
And S8, taking up, cooling the finished product, and finishing taking up and packaging by using a take-up machine.
Example 3
The current density was changed to 1A/dm in step S6 in example 22The rest of the process steps and parameters are unchanged.
Example 4
The current density was changed to 4A/dm in step S6 in example 22The rest of the process steps and parameters are unchanged.
Comparative example 1
The current density was changed to 0.5A/dm in step S6 in example 22The rest of the process steps and parameters are unchanged.
Comparative example 2
The current density was changed to 6A/dm in step S6 in example 22The rest of the process steps and parameters are unchanged.
Comparative example 3
The heat treatment temperature in step S7 in example 2 was changed to 400 ℃, and the remaining process steps and parameters were not changed.
Comparative example 4
The heat treatment temperature in step S7 in example 2 was changed to 450 ℃, and the remaining process steps and parameters were not changed.
Comparative example 5
The heat treatment process was removed in example 2, and the remaining process steps and parameters were unchanged.
The process flow of the invention is as follows: alkali washing activation, acid washing, wire drawing annealing, zinc dipping, nickel preplating, nickel plating, drying, heat treatment and wire winding; wherein, the alkali washing activation, the acid washing, the wire drawing annealing, the drying and the wire winding are all common processes in the prior art.
The appearance of the coating is observed by using a SEW (scanning electron microscope) under 1000 times by combining the references of example 2, example 3, example 4 and comparative example 1 and comparative example 2, wherein the coating of example 2, example 3 and example 4 has uniform surface color, has matte metallic color, and has no pinhole defect and burr phenomenon; the surface of the plating layer of the comparative example 1 has poor color brightness; comparative example 2 the surface of the plating layer had a high gloss and had a vortex pinhole defect locally.
With the combination of each embodiment, after heat treatment, the cross section of the coating is observed by using an SEW electron scanning electron microscope at 5000 times, the thickness of the coating is uniform after heat treatment at 350 ℃, multiple uniform coatings are arranged between the coating and a substrate (low-carbon steel wire), and the particle size of the coating is fine and uniform; in comparison with example 3, the plating layer after heat treatment at 400 ℃ has relatively good flatness, relatively good thickness uniformity and relatively thin thickness; in comparative example 4, after the heat treatment at 450 ℃, the coating had unevenness and uneven thickness, and had bubbles and falling-off phenomena; in comparative example 5, no heat treatment was performed, the boundary between the plating layer and the substrate was significant, the surface smoothness was poor, and particles were present.
According to the invention, by optimizing the preparation process and adopting the zinc dipping process design, the oxide film on the surface of the product can be removed, a uniform and compact zinc film can be formed, the binding property of subsequent nickel plating and the compactness of a coating are improved, and the structure is realized by utilizing the zinc-iron displacement principle of zinc dipping.
The invention adopts the alkaline chemical nickel plating pre-plating process, can avoid shortening the use of the chemical nickel plating solution because the zinc film layer is poisoned by the acidic chemical nickel plating solution, effectively inhibit the dissolution of the zinc film layer, can obtain a thin, fine and uniform nickel plating layer for protecting the zinc film layer, is convenient for the subsequent chemical nickel plating processing, and is beneficial to improving the nickel plating associativity; preferably, alkaline washing chemical nickel plating is adopted as a pre-plating process, so that the phenomenon that a subsequent nickel plating process is increased because a zinc film is small and easy to dissolve under an acidic condition is avoided.
The invention optimizes the nickel plating process, reduces the porosity of the plating layer and improves the quality of the plating layer; the current density is optimized, and the quality of the plating layer is improved.
The invention optimizes and adds a heat treatment process for refining the crystal grains of the plating layer, improving the uniformity of the plating layer, ensuring the hardness of the plating layer and simultaneously increasing the binding force; by utilizing the heat treatment process, the coating can continuously complete diffusion, the bonding property with a substrate is increased, and a reasonable temperature interval is selected, so that the phenomena of bubbles and falling off of the coating caused by overhigh temperature are avoided.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be construed as the protection scope of the present invention.
Claims (10)
1. The preparation method of the nickel-plated low-carbon steel wire comprises the following steps:
s1, performing alkali washing and activation, selecting a low-carbon steel wire according to the process specification, putting the low-carbon steel wire into an alkali washing solution for alkali washing, then washing the low-carbon steel wire with clear water, and detecting the low-carbon steel wire;
s2, acid washing, namely, putting the low-carbon steel wire into an acid washing solution for acid washing, then washing with clear water, and detecting the low-carbon steel wire;
s3, wire drawing and annealing, wherein a continuous annealing wire drawing machine is adopted to finish the wire drawing and annealing process;
s4, zinc dipping, namely dipping the low-carbon steel wire into a zinc dipping solution to obtain a first-grade semi-finished product;
s41, primary zinc dipping, wherein the zinc dipping solution is prepared from a mixed solution of zinc sulfate, hydrofluoric acid and distilled water, the time is 150-200S, and the temperature is normal temperature;
s42, secondary zinc dipping, wherein the zinc dipping liquid is prepared from a mixed solution of zinc sulfate, hydrofluoric acid and distilled water, the time is 300-360S, and the temperature is normal temperature;
s5, pre-plating nickel, namely, completing the pre-plating nickel treatment of the primary semi-finished product through alkaline chemical nickel plating solution, and washing the primary semi-finished product with clear water after completing the pre-plating nickel to obtain a secondary semi-finished product;
s6, nickel plating, namely, completing the nickel plating treatment of the secondary semi-finished product in a nickel plating solution, wherein the nickel plating solution comprises a nickel sulfamate solution, nickel chloride, boric acid, an accelerator M and a nickel plating wetting agent, a nickel plate is placed in the nickel plating solution, and the nickel plate is washed by pure water after the nickel plating is completed to obtain a tertiary semi-finished product;
s7, drying, and air-drying the third-level semi-finished product through cold air;
s7, performing heat treatment, namely introducing the three-stage semi-finished product into a temperature control pipeline for heat treatment at 320-380 ℃ for 45-75 min, and air-cooling to normal temperature after being led out;
and S8, taking up, cooling the finished product, and finishing taking up and packaging by using a take-up machine.
2. The method for preparing the nickel-plated low-carbon steel wire according to claim 1 is characterized by comprising the following steps of: in step S4, the usage amount of zinc sulfate is 8-12 g/L, the usage amount of hydrofluoric acid is 70-80 mL/L, and the balance is distilled water.
3. The method for preparing the nickel-plated low-carbon steel wire according to claim 2 is characterized by comprising the following steps of: in step S4, the usage amount of zinc sulfate is 10g/L, the usage amount of hydrofluoric acid is 75mL/L, and the balance is distilled water.
4. The method for preparing the nickel-plated low-carbon steel wire according to any one of claims 1 to 3, wherein the method comprises the following steps: in step S41, the primary zincing time is 180S, and in step S42, the secondary zincing time is 320S.
5. The method for preparing the nickel-plated low-carbon steel wire according to claim 1 is characterized by comprising the following steps of: in step S5, the alkaline chemical nickel plating solution is a mixture of nickel sulfate, sodium hypophosphite, ammonium citrate and ammonium chloride, the pH value is 8-10, the temperature is 40-50 ℃, and the time is 4-8 min.
6. The method for preparing the nickel-plated low-carbon steel wire according to claim 1 or 5, characterized by comprising the following steps: in step S5, the alkaline chemical nickel plating solution is mixed solution of nickel sulfate, sodium hypophosphite, ammonium citrate and ammonium chloride, the pH value is 9, the temperature is 45 ℃, and the time is 5 min.
7. The method for preparing the nickel-plated low-carbon steel wire according to claim 1 is characterized by comprising the following steps of: in step S6, the dosage of the nickel sulfamate solution is 650-750 g/L, the dosage of the nickel chloride is 0-5 g/L, the dosage of the boric acid is 35-45 g/L, the dosage of the accelerator M is 6-9 mL/L, and the dosage of the nickel plating wetting agent is 0.2-0.5 mL/L.
8. The method for preparing the nickel-plated low-carbon steel wire according to claim 1 or 7, is characterized by comprising the following steps of: in step S6, the dosage of the nickel sulfamate solution is 700g/L, the dosage of the nickel chloride is 2g/L, the dosage of the boric acid is 40g/L, the dosage of the accelerator M is 7mL/L, and the dosage of the nickel plating wetting agent is 0.3 mL/L.
9. The method for preparing the nickel-plated low-carbon steel wire according to claim 1 or 7, is characterized by comprising the following steps of: in step S6, the current density is 1-4A/dm2。
10. The method for preparing the nickel-plated low-carbon steel wire according to claim 9 is characterized by comprising the following steps of: in step S6, the current density is 2-4A/dm2。
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