CN109652788A - A kind of preparation method of nickel-plated mild steel line - Google Patents

A kind of preparation method of nickel-plated mild steel line Download PDF

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Publication number
CN109652788A
CN109652788A CN201910035123.1A CN201910035123A CN109652788A CN 109652788 A CN109652788 A CN 109652788A CN 201910035123 A CN201910035123 A CN 201910035123A CN 109652788 A CN109652788 A CN 109652788A
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nickel
plating
dosage
mild steel
preparation
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CN109652788B (en
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朱向阳
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JIANGYIN SIX-CIRQUE ALLOY WIRE Co Ltd
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JIANGYIN SIX-CIRQUE ALLOY WIRE Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/16Chemical 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
    • C23C18/18Pretreatment of the material to be coated
    • C23C18/1803Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
    • C23C18/1824Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
    • C23C18/1837Multistep pretreatment
    • C23C18/1844Multistep pretreatment with use of organic or inorganic compounds other than metals, first
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/06Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of rods or wires
    • C21D8/065Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of rods or wires of ferrous alloys
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/16Chemical 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
    • C23C18/1601Process or apparatus
    • C23C18/1633Process of electroless plating
    • C23C18/1635Composition of the substrate
    • C23C18/1637Composition of the substrate metallic substrate
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/16Chemical 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
    • C23C18/1601Process or apparatus
    • C23C18/1633Process of electroless plating
    • C23C18/1646Characteristics of the product obtained
    • C23C18/165Multilayered product
    • C23C18/1651Two or more layers only obtained by electroless plating
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/16Chemical 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
    • C23C18/31Coating with metals
    • C23C18/32Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
    • C23C18/34Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
    • C23C18/36Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/16Chemical 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
    • C23C18/52Chemical 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
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23FNON-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
    • C23F17/00Multi-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

Abstract

The invention discloses a kind of preparation methods of nickel-plated mild steel line, including alkali cleaning activation, pickling, wire drawing and annealing, leaching zinc, nickel preplating, nickel plating, drying, heat treatment, take-up.The present invention is designed by optimization preparation process using dip galvanizing technique, and the oxidation film layer of removal product surface may be implemented, and can form the zinc film of even compact, is improved the associativity of subsequent nickel plating and is improved the compactness of coating;Using alkaline chemical nickel-plating pre-plating process; it can be poisoned to avoid because of zinc film layer by acid chemical plating nickel liquid; lead to the use for shortening chemical nickel-plating liquid; effectively inhibit the dissolution of zinc film layer; thin and careful, uniform nickel coating can be obtained to protect zinc film layer; it is also convenient for subsequent chemistry nickel plating processing simultaneously, is conducive to improve nickel plating associativity;Optimize nickel plating technology, reduces plating layer porosity, improve coating quality;Heat treatment process is added, to refine coating crystal grain, improves coating uniformity, it is ensured that increase binding force while coating hardness.

Description

A kind of preparation method of nickel-plated mild steel line
Technical field
The present invention relates to tin plated materials technical fields, and in particular to a kind of preparation method of nickel-plated mild steel line.
Background technique
Currently, existing iron wire does not have good corrosion resistance in the leads such as electron tube, because its phosphorus content is too high, It is easy to be corroded, so that service life is short, and the cost of nickel-coated wire is too high, is not suitable for large-scale production.
For this purpose, using more tin plating low-carbon steel wire now, the service performance of material can be increased with this, increase resistance to height Warm nature, corrosion resistance etc..If notification number is CN107564624A, a kind of hard state CP wire processing technology is disclosed, is wrapped Include following steps: step 1: softening low-carbon steel wire, alignment processing;Step 2: pickling;Step 3: the first nickel plating of plating Layer;Step 4: copper plate;Step 5: the second nickel coating of plating;Step 6: tin coating;Step 7: cleaning;Step 8: drying;Step Rapid nine: winding.By using processing technology described herein, copper facing and it is tin plating before, first nickel plating, can be enhanced coating with The binding force of substrate;Meanwhile the workability of copper is combined with the toughness of steel, plays its excellent toughness and resistance to torsion.So And more now is all to carry out processing wire using tin plating process for copper, the technique in order to enable with good performance, It needs thicker copper plate, leads to that process time is longer, production cost is relatively high, and the compactness of its coating exist it is opposite Poor problem.
Summary of the invention
To solve the above problems, the present invention provides a kind of preparation method of nickel-plated mild steel line, plating good with uniformity The layer feature that compactness is strong, binding force is strong.
To achieve the above object, the technical scheme adopted by the invention is as follows:
A kind of preparation method of nickel-plated mild steel line, including nickel-plated mild steel line, comprising the following steps:
S1, alkali cleaning activation, by process specification selection low-carbon steel wire, be put into soda-wash solution and carry out alkali cleaning, however with clear water into Row cleaning, detects low-carbon steel wire;
Low-carbon steel wire is put into pickling solution and carries out pickling, however cleaned with clear water by S2, pickling, detects mild steel Line;
S3, wire drawing and annealing complete wire drawing and annealing process using continuous annealing wire drawing machine;
S4, leaching zinc, low-carbon steel wire is immersed in zincate solution, first-stage semi-finished product is obtained;
S41, zinc once being soaked, zincate solution is made of the mixed liquor of zinc sulfate, hydrofluoric acid and distilled water, and the time is 150s ~ 200s, Temperature is room temperature;
S42, secondary soaking zinc, zincate solution are made of the mixed liquor of zinc sulfate, hydrofluoric acid and distilled water, and the time is 300s ~ 360s, Temperature is room temperature;
First-stage semi-finished product is completed nickel preplating processing by alkaline chemical nickel-plating liquid, uses clear water after completing nickel preplating by S5, nickel preplating It rinses, second level semi-finished product;
S6, nickel plating, by second level semi-finished product by completing Nickel Plating Treatment in nickel-plating liquid, nickel-plating liquid includes nickel sulfamic acid solution, chlorine Change nickel, boric acid, captax, nickel plating wetting agent, nickel plate is placed in nickel-plating liquid, uses pure water rinsing after completing nickel plating, obtain three-level Semi-finished product;
Three-level semi-finished product are air-dried processing by cold wind by S7, drying;
S8, heat treatment, will three-level semi-finished product import temperature control pipeline in be heat-treated, 320 ~ 380 DEG C of temperature, the time be 45min ~ 75min is air-cooled to room temperature after export;
S9, take-up after finished product is passed through cooling, utilize admission machine to complete take-up and are packaged.
In step S4, zinc sulfate dosage is 8 ~ 12g/L, and hydrofluoric acid dosage is 70 ~ 80ml/L, and surplus is distilled water.
In step S4, zinc sulfate dosage is 10g/L, and hydrofluoric acid dosage is 75ml/L, and surplus is distilled water.
In step S41, galvanizing time is 180s, and in step S42, a galvanizing time is 320s.
In step S5, alkaline chemical nickel-plating liquid uses nickel sulfate, sodium hypophosphite, ammonium citrate and ammonium chloride mixed liquor, PH is 8 ~ 10, and temperature is 40 ~ 50 DEG C, and the time is 4 ~ 8min.
In step S5, alkaline chemical nickel-plating liquid uses nickel sulfate, sodium hypophosphite, ammonium citrate and ammonium chloride mixed liquor, PH is 9, and temperature is 45 DEG C, time 5min.
In step S6, nickel sulfamic acid solution dosage is 650 ~ 750g/L, nickel chloride dosage is 0 ~ 5g/L, boric acid dosage is 35 ~ 45g/L, captax dosage are 6 ~ 9ml/L, nickel plating wetting agent dosage is 0.2 ~ 0.5ml/L.
In step S6, nickel sulfamic acid solution dosage is 700g/L, nickel chloride dosage is 2g/L, boric acid dosage be 40g/L, Captax dosage is 7ml/L, nickel plating wetting agent dosage is 0.3ml/L.
In step S6, current density is 1 ~ 4A/dm2
In step S6, current density is 2 ~ 4A/dm2
The invention has the following advantages: the present invention is designed, Ke Yishi by optimization preparation process using dip galvanizing technique The oxidation film layer of product surface is now removed, and the zinc film of even compact can be formed, improves the associativity and raising of subsequent nickel plating The compactness of coating;Using alkaline chemical nickel-plating pre-plating process, can be poisoned to avoid because of zinc film layer by acid chemical plating nickel liquid, Lead to the use for shortening chemical nickel-plating liquid, effectively inhibit the dissolution of zinc film layer, thin and careful, uniform nickel coating can be obtained and used To protect zinc film layer, while it being also convenient for subsequent chemistry nickel plating processing, is conducive to improve nickel plating associativity;Optimize nickel plating technology, drop Low plating layer porosity, improves coating quality;Heat treatment process is added, refining coating crystal grain, improves coating uniformity, Ensure to increase binding force while coating hardness.
The features of the present invention sees this case or less preferably detailed description of embodiment and is well understood.
Specific embodiment
In order to which objects and advantages of the present invention are more clearly understood, the present invention is carried out with reference to embodiments further It is described in detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to limit this hair It is bright.
Embodiment 1
The invention discloses a kind of preparation methods of nickel-plated mild steel line, including nickel-plated mild steel line, comprising the following steps:
S1, alkali cleaning activation, by process specification selection low-carbon steel wire, be put into soda-wash solution and carry out alkali cleaning, however with clear water into Row cleaning, detects low-carbon steel wire.
Low-carbon steel wire is put into pickling solution and carries out pickling, however cleaned with clear water by S2, pickling, detects low Carbon steel line.
S3, wire drawing and annealing complete wire drawing and annealing process using continuous annealing wire drawing machine.
S4, leaching zinc, low-carbon steel wire is immersed in zincate solution, obtains first-stage semi-finished product, and zinc sulfate dosage is 8 ~ 12g/L, hydrogen Fluoric acid dosage is 70 ~ 80ml/L, and surplus is distilled water;It is designed using dip galvanizing technique, the oxidation of removal product surface may be implemented Film layer, and the zinc film of even compact can be formed, improve the associativity of subsequent nickel plating and improve the compactness of coating.
S41, once soak zinc, zincate solution is made of the mixed liquor of zinc sulfate, hydrofluoric acid and distilled water, the time be 150s ~ 200s, temperature are room temperature.
S42, secondary soaking zinc, zincate solution are made of the mixed liquor of zinc sulfate, hydrofluoric acid and distilled water, the time be 300s ~ 360s, temperature are room temperature.
First-stage semi-finished product is completed nickel preplating processing by alkaline chemical nickel-plating liquid, used after completing nickel preplating by S5, nickel preplating Clear water rinses, second level semi-finished product, and alkaline chemical nickel-plating liquid is using nickel sulfate, sodium hypophosphite, ammonium citrate and ammonium chloride mixing Liquid, PH are 8 ~ 10, and temperature is 40 ~ 50 DEG C, and the time is 4 ~ 8min, preferably;Using alkaline chemical nickel-plating pre-plating process, can keep away Exempt to be poisoned because of zinc film layer by acid chemical plating nickel liquid, leads to the use for shortening chemical nickel-plating liquid, effectively inhibit the molten of zinc film layer Solution, can obtain thin and careful, uniform nickel coating to protect zinc film layer, while be also convenient for subsequent chemistry nickel plating processing, have Conducive to raising nickel plating associativity.
S6, nickel plating, by second level semi-finished product by completing Nickel Plating Treatment in nickel-plating liquid, nickel-plating liquid includes that nickel sulfamic acid is molten Liquid, nickel chloride, boric acid, captax, nickel plating wetting agent are placed with nickel plate in nickel-plating liquid, use pure water rinsing after completing nickel plating, obtain Three-level semi-finished product, nickel sulfamic acid solution dosage is 650 ~ 750g/L, nickel chloride dosage is 0 ~ 5g/L, boric acid dosage be 35 ~ 45g/L, captax dosage are 6 ~ 9ml/L, nickel plating wetting agent dosage is 0.2 ~ 0.5ml/L, and current density is 1 ~ 4A/dm2;It is excellent Change nickel plating technology, reduces plating layer porosity, improve coating quality.
Three-level semi-finished product are air-dried processing by cold wind by S7, drying, it is preferred to use cold wind processing, it can be to avoid because of blowing Temperature is excessively high, influences coating quality.
S8, heat treatment, will three-level semi-finished product import temperature control pipeline in be heat-treated, 320 ~ 380 DEG C of temperature, the time be 45min ~ 75min is air-cooled to room temperature after export, adds heat treatment process, to refine coating crystal grain, improves coating uniformity, it is ensured that plating Binding force is increased while layer hardness.
S9, take-up after finished product is passed through cooling, utilize admission machine to complete take-up and are packaged.
Embodiment 2
The invention discloses a kind of preparation methods of nickel-plated mild steel line, including nickel-plated mild steel line, comprising the following steps:
S1, alkali cleaning activation, by process specification selection low-carbon steel wire, be put into soda-wash solution and carry out alkali cleaning, however with clear water into Row cleaning, detects low-carbon steel wire.
Low-carbon steel wire is put into pickling solution and carries out pickling, however cleaned with clear water by S2, pickling, detects low Carbon steel line.
S3, wire drawing and annealing complete wire drawing and annealing process using continuous annealing wire drawing machine.
S4, leaching zinc, low-carbon steel wire is immersed in zincate solution, obtains first-stage semi-finished product, and zinc sulfate dosage is 10g/L, hydrogen fluorine Sour dosage is 75ml/L, and surplus is distilled water;It is designed using dip galvanizing technique, the oxidation film layer of removal product surface may be implemented, And the zinc film of even compact can be formed, the associativity of subsequent nickel plating is improved and improves the compactness of coating.
S41, zinc once being soaked, zincate solution is made of the mixed liquor of zinc sulfate, hydrofluoric acid and distilled water, and temperature is room temperature, Galvanizing time is 180s.
S42, secondary soaking zinc, zincate solution are made of the mixed liquor of zinc sulfate, hydrofluoric acid and distilled water, temperature is room temperature, Galvanizing time is 320s.
First-stage semi-finished product is completed nickel preplating processing by alkaline chemical nickel-plating liquid, used after completing nickel preplating by S5, nickel preplating Clear water rinses, second level semi-finished product, and alkaline chemical nickel-plating liquid is using nickel sulfate, sodium hypophosphite, ammonium citrate and ammonium chloride mixing Liquid, PH 9, temperature are 45 DEG C, time 5min;Using alkaline chemical nickel-plating pre-plating process, can to avoid because zinc film layer it is sour Property chemical nickel-plating liquid poisoned, cause shorten chemical nickel-plating liquid use, effectively inhibit zinc film layer dissolution, can obtain it is thin and Careful, uniform nickel coating is also convenient for subsequent chemistry nickel plating processing to protect zinc film layer, is conducive to improve nickel plating combination Property.
S6, nickel plating, by second level semi-finished product by completing Nickel Plating Treatment in nickel-plating liquid, nickel-plating liquid includes that nickel sulfamic acid is molten Liquid, nickel chloride, boric acid, captax, nickel plating wetting agent are placed with nickel plate in nickel-plating liquid, use pure water rinsing after completing nickel plating, obtain Three-level semi-finished product are obtained, nickel sulfamic acid solution dosage is 700g/L, nickel chloride dosage is 2g/L, boric acid dosage is 40g/L, promotes Agent M dosage is 7ml/L, nickel plating wetting agent dosage is 0.3ml/L, current density 2A/dm2;Optimize nickel plating technology, reduces plating Layer porosity improves coating quality;Heat treatment process is added, to refine coating crystal grain, improves coating uniformity, it is ensured that plating Binding force is increased while layer hardness.
Three-level semi-finished product are air-dried processing by cold wind by S7, drying, it is preferred to use cold wind processing, it can be to avoid because of blowing Temperature is excessively high, influences coating quality.
Three-level semi-finished product are imported in temperature control pipeline and are heat-treated by S8, heat treatment, and 350 DEG C of temperature, time 60min, export After be air-cooled to room temperature.
S9, take-up after finished product is passed through cooling, utilize admission machine to complete take-up and are packaged.
Embodiment 3
By in the step S6 in embodiment 2, current density is changed to 1A/dm2, remaining processing step and parameter are constant.
Embodiment 4
By in the step S6 in embodiment 2, current density is changed to 4A/dm2, remaining processing step and parameter are constant.
Reference examples 1
By in the step S6 in embodiment 2, current density is changed to 0.5A/dm2, remaining processing step and parameter are constant.
Reference examples 2
By in the step S6 in embodiment 2, current density is changed to 6A/dm2, remaining processing step and parameter are constant.
Reference examples 3
By in the step S8 in embodiment 2, heat treatment temperature is changed to 400 DEG C, remaining processing step and parameter are constant.
Reference examples 4
By in the step S8 in embodiment 2, heat treatment temperature is changed to 450 DEG C, remaining processing step and parameter are constant.
Reference examples 5
Heat treatment procedure will be removed in embodiment 2, remaining processing step and parameter are constant.
Process flow of the invention are as follows: alkali cleaning activation, pickling, wire drawing and annealing, leaching zinc, nickel preplating, nickel plating, drying, heat at Reason, take-up;Wherein alkali cleaning activation, pickling, wire drawing and annealing, drying, take-up are conventional process in the prior art.
In conjunction with the embodiments 2, the reference of embodiment 3, embodiment 4 and reference examples 1 and reference examples 2 utilizes SEW electron scanning electricity Observe Deposit appearance under 1000 times of mirror, wherein 4 coating surface uniform color of embodiment 2, embodiment 3 and embodiment, have matt Metallochrome, no pin-hole defect and burr phenomena;1 coating surface color brightness of reference examples is poor;2 coating surface gloss of reference examples Degree is high, part has circinate needle pore defect.
In conjunction with each embodiment, after Overheating Treatment, layer cross section is plated using observation under 5000 times of SEW electron scanning Electronic Speculum, Thickness of coating uniformly, between coating and matrix (mild steel wire) has uniform more coating, while cladding grain size after 350 DEG C of heat treatments It is tiny, uniform;Coating planarization is relatively preferable after 3,400 DEG C of reference examples heat treatments, the thickness uniformity is relatively preferable, thickness of coating It is relatively thin;There are bubbles, de- there are uneven phenomenon, in uneven thickness, coating for coating after 4,450 DEG C of reference examples heat treatments Fall phenomenon;Reference examples 5, are not heat-treated, and the boundary of coating and matrix is obvious, and profile pattern is poor, there are graininess.
The present invention is designed by optimization preparation process using dip galvanizing technique, and the oxidation film of removal product surface may be implemented Layer, and the zinc film of even compact can be formed, improve the associativity of subsequent nickel plating and improve the compactness of coating, utilize leaching zinc Zinc-iron principle,displacement, to realize above structure.
The present invention use alkaline chemical nickel-plating pre-plating process, can to avoid because zinc film layer it is malicious by acid chemical plating nickel liquid Change, leads to the use for shortening chemical nickel-plating liquid, effectively inhibit the dissolution of zinc film layer, thin and careful, uniform nickel plating can be obtained Layer is also convenient for subsequent chemistry nickel plating processing to protect zinc film layer, is conducive to improve nickel plating associativity;It is preferred that using alkali cleaning Chemical nickel plating avoids increasing the progress of subsequent nickel plating process because zinc film in acid condition little Yi because being dissolved as pre-plating process.
The present invention optimizes nickel plating technology, reduces plating layer porosity, improves coating quality;Optimize current density, improves Coating quality.
Heat treatment process is added in present invention optimization, to refine coating crystal grain, improves coating uniformity, it is ensured that coating hardness While increase binding force;Using heat treatment process, coating is allowed to continue to complete diffusion, the combination of increase and matrix Property, and reasonable temperature range is selected, it avoids that coating is caused bubble, obscission occur because temperature is excessively high.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, without departing from the principle of the present invention, it can also make several improvements and retouch, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims (10)

1. a kind of preparation method of nickel-plated mild steel line, including nickel-plated mild steel line, which comprises the following steps:
S1, alkali cleaning activation, by process specification selection low-carbon steel wire, be put into soda-wash solution and carry out alkali cleaning, however with clear water into Row cleaning, detects low-carbon steel wire;
Low-carbon steel wire is put into pickling solution and carries out pickling, however cleaned with clear water by S2, pickling, detects mild steel Line;
S3, wire drawing and annealing complete wire drawing and annealing process using continuous annealing wire drawing machine;
S4, leaching zinc, low-carbon steel wire is immersed in zincate solution, first-stage semi-finished product is obtained;
S41, zinc once being soaked, zincate solution is made of the mixed liquor of zinc sulfate, hydrofluoric acid and distilled water, and the time is 150s ~ 200s, Temperature is room temperature;
S42, secondary soaking zinc, zincate solution are made of the mixed liquor of zinc sulfate, hydrofluoric acid and distilled water, and the time is 300s ~ 360s, Temperature is room temperature;
First-stage semi-finished product is completed nickel preplating processing by alkaline chemical nickel-plating liquid, uses clear water after completing nickel preplating by S5, nickel preplating It rinses, second level semi-finished product;
S6, nickel plating, by second level semi-finished product by completing Nickel Plating Treatment in nickel-plating liquid, nickel-plating liquid includes nickel sulfamic acid solution, chlorine Change nickel, boric acid, captax, nickel plating wetting agent, nickel plate is placed in nickel-plating liquid, uses pure water rinsing after completing nickel plating, obtain three-level Semi-finished product;
Three-level semi-finished product are air-dried processing by cold wind by S7, drying;
S8, heat treatment, will three-level semi-finished product import temperature control pipeline in be heat-treated, 320 ~ 380 DEG C of temperature, the time be 45min ~ 75min is air-cooled to room temperature after export;
S9, take-up after finished product is passed through cooling, utilize admission machine to complete take-up and are packaged.
2. a kind of preparation method of nickel-plated mild steel line according to claim 1, it is characterised in that: in step S4, sulfuric acid Zinc dosage is 8 ~ 12g/L, and hydrofluoric acid dosage is 70 ~ 80ml/L, and surplus is distilled water.
3. a kind of preparation method of nickel-plated mild steel line according to claim 2, it is characterised in that: in step S4, sulfuric acid Zinc dosage is 10g/L, and hydrofluoric acid dosage is 75ml/L, and surplus is distilled water.
4. a kind of preparation method of nickel-plated mild steel line as claimed in any of claims 1 to 3, it is characterised in that: In step S41, galvanizing time is 180s, and in step S42, a galvanizing time is 320s.
5. a kind of preparation method of nickel-plated mild steel line according to claim 1, it is characterised in that: in step S5, alkalinity Chemical nickel-plating liquid uses nickel sulfate, sodium hypophosphite, ammonium citrate and ammonium chloride mixed liquor, and PH is 8 ~ 10, and temperature is 40 ~ 50 DEG C, the time is 4 ~ 8min.
6. a kind of preparation method of nickel-plated mild steel line according to claim 1 or 5, it is characterised in that: in step S5, alkali Property chemical nickel-plating liquid use nickel sulfate, sodium hypophosphite, ammonium citrate and ammonium chloride mixed liquor, PH 9, temperature be 45 DEG C, when Between be 5min.
7. a kind of preparation method of nickel-plated mild steel line according to claim 1, it is characterised in that: in step S6, amino Nickel sulphonic acid solution usage is 650 ~ 750g/L, nickel chloride dosage is 0 ~ 5g/L, boric acid dosage is 35 ~ 45g/L, captax dosage It is 0.2 ~ 0.5ml/L for 6 ~ 9ml/L, nickel plating wetting agent dosage.
8. a kind of preparation method of nickel-plated mild steel line according to claim 1 or claim 7, it is characterised in that: in step S6, ammonia Base nickel sulphonic acid solution usage is 700g/L, nickel chloride dosage is 2g/L, boric acid dosage is 40g/L, captax dosage be 7ml/L, Nickel plating wetting agent dosage is 0.3ml/L.
9. a kind of preparation method of nickel-plated mild steel line according to claim 1 or claim 7, it is characterised in that: in step S6, electricity Current density is 1 ~ 4A/dm2
10. a kind of preparation method of nickel-plated mild steel line according to claim 9, it is characterised in that: in step S6, electric current Density is 2 ~ 4A/dm2
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CN110468395A (en) * 2019-09-11 2019-11-19 泰州友润电子科技股份有限公司 A kind of second level nickel plating technology based on chemical nickel plating alloy plate
CN115161739A (en) * 2021-04-01 2022-10-11 泰州俊宇不锈钢材料有限公司 Special alloy microwire surface coating anticorrosion processing technology

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CN203637272U (en) * 2013-08-28 2014-06-11 朱向阳 Nickel-plated low-carbon steel wire
CN103911634A (en) * 2014-03-06 2014-07-09 中国电子科技集团公司第五十五研究所 Surface nickel plating method for molybdenum-based composite material
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CN203637272U (en) * 2013-08-28 2014-06-11 朱向阳 Nickel-plated low-carbon steel wire
CN103911634A (en) * 2014-03-06 2014-07-09 中国电子科技集团公司第五十五研究所 Surface nickel plating method for molybdenum-based composite material
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