CN115161729A - Preparation method of coating tinplate and coating tinplate - Google Patents

Preparation method of coating tinplate and coating tinplate Download PDF

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Publication number
CN115161729A
CN115161729A CN202210828566.8A CN202210828566A CN115161729A CN 115161729 A CN115161729 A CN 115161729A CN 202210828566 A CN202210828566 A CN 202210828566A CN 115161729 A CN115161729 A CN 115161729A
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Prior art keywords
tin
substrate
coating
tinplate
passivation
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Chinese (zh)
Inventor
王振文
方圆
宋浩
徐海卫
于孟
吴明辉
孙宇
吴志国
周保欣
石云光
于兴旺
万一群
贾刘兵
齐智远
刘丽珍
缪军红
王凯
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Shougang Group Co Ltd
Shougang Jingtang United Iron and Steel Co Ltd
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Shougang Group Co Ltd
Shougang Jingtang United Iron and Steel Co Ltd
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Priority to CN202210828566.8A priority Critical patent/CN115161729A/en
Publication of CN115161729A publication Critical patent/CN115161729A/en
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10—Electroplating with more than one layer of the same or of different metals
    • C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34—Pretreatment of metallic surfaces to be electroplated
    • C25D5/36—Pretreatment of metallic surfaces to be electroplated of iron or steel
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C25D5/50—After-treatment of electroplated surfaces by heat-treatment
    • C25D5/505—After-treatment of electroplated surfaces by heat-treatment of electroplated tin coatings, e.g. by melting
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F1/00—Electrolytic cleaning, degreasing, pickling or descaling
    • C25F1/02—Pickling; Descaling
    • C25F1/04—Pickling; Descaling in solution
    • C25F1/06—Iron or steel

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating Methods And Accessories (AREA)

Abstract

The invention particularly relates to a preparation method of a plated tinplate and the plated tinplate, and belongs to the technical field of metal material treatment. A preparation method of a plated tinplate comprises the following steps: obtaining a steel plate substrate; carrying out alkali washing and acid washing on the steel plate substrate to obtain a pretreated substrate; electroplating nickel on the surface of the pretreated substrate to obtain a first plating layer substrate; electroplating tin on the surface of the first coating substrate to obtain a second coating substrate; and performing reflow and passivation on the second coating substrate to obtain the coating tinplate. The method has the advantages that the nickel layer is flash-plated on the surface of the steel plate substrate, so that the alloying degree between tin and iron on the surface of the tin plate is inhibited, the uniformity of the tin layer on the surface of the tin plate and the free tin content on the surface are improved, and the problem of poor complete alloying corrosion resistance of the low-tin-content tin plate is solved.

Description

Preparation method of plated tinplate and plated tinplate
Technical Field
The invention belongs to the technical field of metal material treatment, and particularly relates to a preparation method of a plated tinplate and the plated tinplate.
Background
The tin plate is a cold-rolled sheet plated with a pure tin layer on a substrate, is widely applied to packaging industries of food, chemical industry, pressure containers and the like, and the tin plating amount of the tin plate on the market is generally controlled to be 1.1-11.2g/m 2 In between. Due to the progress of coating printing technology and the increasing shortage of international tin resources, the low tin content is the key point of the subsequent development of the tin plating market, but in the actual production process, the tin coating is found to be less than 0.7g/m on the surface of the tin plate 2 In the process, the surface of the tinned plate is easy to be completely alloyed, the compactness of a tin layer on the surface is poor, and the welding and corrosion resistance of the low-tin-content tinned plate are sharply reduced.
Disclosure of Invention
The application aims to provide a preparation method of a plated tinplate, which aims to solve the technical problem that the corrosion resistance of a low-tin plated steel plate is sharply reduced in the prior art.
The embodiment of the invention provides a preparation method of a plated tinplate, which comprises the following steps:
obtaining a steel plate substrate;
carrying out alkali washing and acid washing on the steel plate substrate to obtain a pretreated substrate;
electroplating nickel on the surface of the pretreated substrate to obtain a first plating layer substrate;
electroplating tin on the surface of the first plating layer substrate to obtain a second plating layer substrate;
and performing reflow and passivation on the second coating substrate to obtain the coating tinplate.
Optionally, the surface roughness Sa of the steel plate substrate is less than or equal to 0.5 μm.
Optionally, the surface roughness Sa of the steel plate substrate is 0.15 to 0.35 μm.
Optionally, the alkali washing is electrolytic alkali washing, the washing liquid of the alkali washing is potassium hydroxide solution, the concentration of the potassium hydroxide solution is 40-50g/L, the temperature of the potassium hydroxide solution is 70-80 ℃, and the alkali is usedThe current density of washing is 20-25A/dm 2 。
Optionally, the acid washing is electrochemical acid washing, the acid washing liquid is a sulfuric acid aqueous solution, the concentration of the sulfuric acid aqueous solution is 40-50g/L, the temperature of the sulfuric acid aqueous solution is 40-50 ℃, and the current density of the acid washing is 10-22A/dm 2 。
Optionally, the plating solution for the electroplating nickel has solutes including: nickel sulfamate, boric acid and potassium bromide, wherein the solvent of the plating solution adopted by the nickel electroplating is water;
the temperature of the electroplated nickel is 30-35 ℃;
the mass of the nickel coating of the first coating substrate is 50-150mg/m 2 ；
Wherein:
the concentration of the nickel sulfamate is 100-400g/L;
the concentration of the boric acid is 20-50g/L;
the concentration of the potassium bromide is 15-30g/L.
Optionally, the electrolytic tin plating is carried out by adopting an MSA high-speed tin plating system, and the current density of the electrolytic tin plating is 1-3A/dm 2 The tin ion concentration of the electroplated tin is 10-15g/L, and the mass of the tin coating of the second coating substrate is 0.4-0.7g/m 2 。
Optionally, the reflow is resistance reflow, the temperature of the reflow is not less than 265 ℃, and the end point of the reflow is as follows: the free tin content of the surface of the galvanized tinplate is 0.05-0.25g/m 2 。
Optionally, the passivation solution used for passivation is a sodium dichromate aqueous solution, the concentration of the passivation solution is 22-28g/L, the temperature of passivation is 40-44 ℃, the pH value of passivation is 4.2-4.6, and the current density of passivation is 0.5-3A/dm 2 。
Based on the same invention concept, the embodiment of the invention also provides the plated tinplate which is prepared by adopting any one of the preparation methods of the plated tinplate.
One or more technical solutions in the embodiments of the present invention at least have the following technical effects or advantages:
according to the preparation method of the galvanized tinplate provided by the embodiment of the invention, the nickel layer is flash-plated on the surface of the steel plate substrate, so that the alloying degree of tin and iron on the surface of the tin plate is inhibited, the uniformity of a tin layer on the surface of the tin plate and the free tin content on the surface are improved, and the problems that the surface of the tin plate is easy to be completely alloyed, the compactness of the tin layer on the surface is poor, and the corrosion resistance of the low-tin-content tin plate is rapidly reduced at the moment are solved.
The foregoing description is only an overview of the technical solutions of the present invention, and the embodiments of the present invention are described below in order to make the technical means of the present invention more clearly understood and to make the above and other objects, features, and advantages of the present invention more clearly understandable.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
Fig. 1 is a flow chart of a method provided by an embodiment of the invention.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are for the purpose of illustrating the invention and are not to be construed as limiting the invention.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings as commonly used in the art. Accordingly, 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 invention belongs. If there is a conflict, the present specification will control. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention. For example, room temperature may refer to a temperature in the interval 10 to 35 ℃.
Unless otherwise specifically indicated, various raw materials, reagents, instruments, equipment and the like used in the present invention may be commercially available or may be prepared by existing methods.
In order to solve the technical problems, the general idea of the embodiment of the application is as follows:
according to an exemplary embodiment of the present invention, there is provided a method for preparing a plated tinplate, including the steps of:
s1, obtaining a steel plate substrate;
s2, carrying out alkali washing and acid washing on the steel plate substrate to obtain a pretreated substrate;
s3, electroplating nickel on the surface of the pretreated substrate to obtain a first plated substrate;
s4, electroplating tin on the surface of the first plating base plate to obtain a second plating base plate;
and S5, performing reflow and passivation on the second coating substrate to obtain the coating tinplate.
The preparation method of the galvanized tinplate can effectively solve the problem of rapid reduction of corrosion resistance caused by low tin content, inhibits the alloying degree between tin and iron on the surface of the tin plate by flash plating a layer of nickel on the surface of a steel plate substrate, improves the uniformity of a tin layer on the surface of the tin plate and the free tin content on the surface of the tin plate, and solves the problems of poor complete alloying corrosion resistance and poor weldability of the tin plate with low tin content.
In the present invention, it is noted that:
the effect of the alkali washing is as follows: the method is characterized in that the oil stain on the surface of the strip steel is removed through the saponification reaction of alkali liquor, and meanwhile, the residue on the surface of the strip steel is physically removed through the electrolysis to generate tiny bubbles of oxygen and hydrogen on the surface of the strip steel.
The pickling has the following functions: in the solution of dilute sulphuric acid, impurities such as iron scale and the like on the surface of the strip steel are removed through electrochemical action, so that a thin oxide film which is invisible to naked eyes is eliminated. The surface of the strip steel after pickling presents an activated state of a metal crystalline structure so as to ensure that a good junction is formed between the strip steel and a tin coating.
The reflow function is as follows: an appropriate iron-nickel-tin alloy layer is generated between the tin coating and the substrate through a combined heating mode of induction reflow, so that the corrosion resistance of the tin plate is improved, and the binding force and compactness of the tin coating and the substrate are improved.
The passivation function is as follows: a stable conversion coating is formed on the surface of the tin plate, so that the surface of the tin plate is prevented from being oxidized and yellowed, and the corrosion resistance of the low-tin-content tin plate is improved.
As an alternative embodiment, the surface roughness Sa of the steel plate substrate is less than or equal to 0.5 μm.
The reason why the surface roughness of the steel plate substrate is controlled is that: because the weight of the surface coating is only 0.4-0.7g/m < 2 >, the theoretical thickness is 0.055 mu m-0.096 mu m, and when Sa is higher than 0.5 mu m, the compactness of the surface coating is reduced, and the corrosion resistance of the coating is reduced.
Preferably, the surface roughness Sa of the steel plate substrate is 0.15-0.35 μm.
As an alternative embodiment, the alkali washing is electrolytic alkali washing, the washing liquid of the alkali washing is potassium hydroxide solution, the concentration of the potassium hydroxide solution is 40-50g/L, the temperature of the potassium hydroxide solution is 70-80 ℃, and the current density of the alkali washing is 20-25A/dm 2 。
The reason for controlling the concentration of the potassium hydroxide solution is that: when the concentration is higher than 50g/L, alkali liquor is wasted, the surface cleaning difficulty is increased during subsequent rinsing, and white spots and other defects are easily generated in the electroplating process; when the concentration is lower than 40g/L, the alkali washing concentration is too low, the surface grease cannot be cleaned cleanly, and plating leakage is easy to generate.
As an optional embodiment, the acid washing is electrochemical acid washing, the washing liquid of the acid washing is sulfuric acid aqueous solution, the concentration of the sulfuric acid aqueous solution is 40-50g/L, the temperature of the sulfuric acid aqueous solution is 40-50 ℃, and the current density of the acid washing is 10-22A/dm 2 。
The reason why the concentration of the aqueous sulfuric acid solution is controlled is that: when the pickling concentration is too high, the surface is easy to generate over pickling phenomenon, the surface is flowered during electroplating, when the concentration is too low, the surface is not pickled, the surface oxide film is not completely cleaned, and plating leakage is easy to generate.
As an alternative embodiment, the plating solution for the electroplating of nickel has a solute comprising: nickel sulfamate, boric acid and potassium bromide, wherein the solvent of the plating solution adopted by the nickel electroplating is water;
the temperature of the electroplated nickel is 30-35 ℃;
the mass of the nickel coating of the first coating substrate is 50-150mg/m 2 ；
Wherein:
the concentration of the nickel sulfamate is 100-400g/L;
the concentration of the boric acid is 20-50g/L;
the concentration of the potassium bromide is 15-30g/L.
The reason for controlling the quality (thickness) of the nickel plating layer is that: when the thickness of the plating layer is too high, the surface brightness of the plating layer is reduced, the surface is faint yellow, and the requirement of a bright tin plate cannot be met; when the plating layer is too low, the nickel layer on the surface is not uniformly covered, the part of the plated layer after tin plating and reflow has a complete alloying phenomenon, and the corrosion resistance of the plated layer is reduced.
Preferably, the mass of the nickel coating of the first coating substrate is 50-100mg/m 2 。
As an alternative embodiment, the electrotinning is carried out by using an MSA high-speed tinning system, and the electrotinning has a current density of 1-3A/dm 2 The tin ion concentration of the electroplating tin is 10-15g/L, and the mass of the tin coating of the second coating substrate is 0.4-0.7g/m 2 。
The reason for controlling the quality (thickness) of the tin plating layer is: when the tin plating amount is less than 0.4g/m 2 When the content of the surface coating is too low, the coating coverage uniformity is poor, the corrosion resistance of the coating is reduced, and when the weight of the coating is higher than 0.7g/m 2 The amount of tin plating is 1.1g/m as compared with the conventional one 2 The plating range is close, the purpose of saving tin resources can not be achieved, so the tin layer range is required to be controlled between 0.4 and 0.7g/m 2 。
Preferably, the mass of the tin coating of the second coating substrate is 0.5-0.7g/m 2 。
As an optional implementation manner, the reflow is resistance reflow, the temperature of the reflow is not less than 265 ℃, and the end point of the reflow is as follows: the free tin content of the surface of the galvanized tinplateThe amount is 0.05-0.25g/m 2 。
Preferably, the end points of the reflow are: the free tin content of the surface of the galvanized tinplate is 0.05-0.15g/m 2 。
As an optional implementation mode, the passivation solution adopted by the passivation is a sodium dichromate water solution, the concentration of the passivation solution is 22-28g/L, the temperature of the passivation is 40-44 ℃, the pH value of the passivation is 4.2-4.6, and the current density of the passivation is 0.5A/dm 2 。
According to another exemplary embodiment of the present invention, there is provided a coated tinplate, which is prepared by any one of the above-mentioned methods for preparing a coated tinplate.
The present application will be described in detail below with reference to examples, comparative examples, and experimental data.
Example 1
The embodiment provides a preparation method of a plated tinplate, which comprises the following steps:
and S1, obtaining a steel plate substrate.
Wherein: the surface roughness of the steel plate substrate was 0.28. Mu.m.
S2, carrying out alkali washing and acid washing on the steel plate substrate to obtain a pretreated substrate.
Wherein:
the alkaline washing is electrolytic alkaline washing, the washing liquid of the alkaline washing is potassium hydroxide solution, the concentration of the potassium hydroxide solution is 45g/L, the temperature of the potassium hydroxide solution is 70 ℃, and the current density of the alkaline washing is 20A/dm 2 ；
The pickling is electrochemical pickling, the pickling solution is sulfuric acid aqueous solution, the concentration of the sulfuric acid aqueous solution is 45g/L, the temperature of the sulfuric acid aqueous solution is 45 ℃, and the current density of the pickling is 20A/dm 2 。
And S3, electroplating nickel on the surface of the pretreated substrate to obtain a first plating layer substrate.
Wherein:
the plating solution adopted by the nickel electroplating has the following solutes: nickel sulfamate, boric acid and potassium bromide, wherein the solvent of the plating solution adopted by the nickel electroplating is water;
the temperature of the electroplated nickel is 30 ℃;
the mass of the nickel coating of the first coating substrate is 50mg/m 2 ；
The concentration of the nickel sulfamate is 150g/L;
the concentration of the boric acid is 25g/L;
the concentration of potassium bromide was 15g/L.
And S4, electroplating tin on the surface of the first plating base plate to obtain a second plating base plate.
Wherein: the electrotinning is carried out by adopting an MSA high-speed tinning system, and the current density of the electrotinning is 2A/dm 2 The tin ion concentration of the electrolytic tin plating is 12g/L, and the mass of the tin plating layer of the second plating base plate is 0.58g/m 2 。
S5, performing reflow and passivation on the second coating substrate to obtain the coating tinplate.
Wherein:
the reflow adopts resistance reflow, the temperature of the reflow is 290 ℃, and the end point of the reflow is as follows: the free tin content of the surface of the galvanized tinplate is 0.09g/m 2 ；
The passivation solution adopted by the passivation is sodium dichromate water solution, the concentration of the passivation solution is 25g/L, the passivation temperature is 42 ℃, the passivation pH value is 4.4, and the passivation current density is 0.5A/dm 2 。
The embodiment also provides the galvanized tinplate prepared by the method.
Example 2
The embodiment provides a preparation method of a plated tinplate, which comprises the following steps:
and S1, obtaining a steel plate substrate.
Wherein: the surface roughness of the steel plate substrate was 0.28. Mu.m.
And S2, carrying out alkali washing and acid washing on the steel plate substrate to obtain a pretreated substrate.
Wherein:
the alkaline washing is electrolytic alkaline washing, the washing liquid of the alkaline washing is potassium hydroxide solution, the concentration of the potassium hydroxide solution is 45g/L, the temperature of the potassium hydroxide solution is 70 ℃, and the current density of the alkaline washing is 20A/dm 2 ；
The acid washing is electrochemical acid washing, and the washing liquid of the acid washing isThe concentration of the sulfuric acid aqueous solution is 45g/L, the temperature of the sulfuric acid aqueous solution is 45 ℃, and the current density of the acid washing is 20A/dm 2 。
And S3, electroplating nickel on the surface of the pretreated substrate to obtain a first plating layer substrate.
Wherein:
the plating solution adopted by the nickel electroplating has the following solutes: nickel sulfamate, boric acid and potassium bromide, wherein a solvent of a plating solution adopted by the nickel electroplating is an aqueous solution;
the temperature of the electroplated nickel is 30 ℃;
the mass of the nickel coating of the first coating substrate is 100mg/m 2 ；
The concentration of the nickel sulfamate is 150g/L;
the concentration of the boric acid is 25g/L;
the concentration of potassium bromide was 15g/L.
And S4, electroplating tin on the surface of the first plating base plate to obtain a second plating base plate.
Wherein: the electrotinning is carried out by adopting an MSA high-speed tinning system, and the current density of the electrotinning is 2A/dm 2 The tin ion concentration of the electroplated tin is 12g/L, and the mass of the tin coating of the second coating substrate is 0.50g/m 2 。
And S5, carrying out reflow and passivation on the second coating substrate to obtain the coating tinplate.
Wherein:
the reflow adopts resistance reflow, the temperature of the reflow is 290 ℃, and the end point of the reflow is as follows: the free tin content on the surface of the galvanized tinplate is 0.11g/m < 2 >;
the passivation solution adopted by the passivation is sodium dichromate water solution, the concentration of the passivation solution is 25g/L, the passivation temperature is 42 ℃, the passivation pH value is 4.4, and the passivation current density is 0.5A/dm < 2 >.
The embodiment also provides the galvanized tinplate prepared by the method.
Example 3
The embodiment provides a preparation method of a plated tinplate, which comprises the following steps:
and S1, obtaining a steel plate substrate.
Wherein: the surface roughness of the steel plate substrate was 0.32. Mu.m.
S2, carrying out alkali washing and acid washing on the steel plate substrate to obtain a pretreated substrate.
Wherein:
the alkaline washing is electrolytic alkaline washing, the washing liquid of the alkaline washing is potassium hydroxide solution, the concentration of the potassium hydroxide solution is 45g/L, the temperature of the potassium hydroxide solution is 70 ℃, and the current density of the alkaline washing is 20A/dm 2 ；
The pickling is electrochemical pickling, the pickling solution is sulfuric acid aqueous solution, the concentration of the sulfuric acid aqueous solution is 45g/L, the temperature of the sulfuric acid aqueous solution is 45 ℃, and the current density of the pickling is 20A/dm 2 。
And S3, electroplating nickel on the surface of the pretreated substrate to obtain a first plating layer substrate.
Wherein:
the plating solution for electroplating nickel has the following solutes: nickel sulfamate, boric acid and potassium bromide, wherein a solvent of a plating solution adopted by the nickel electroplating is an aqueous solution;
the temperature of the electroplated nickel is 30 ℃;
the mass of the nickel coating of the first coating substrate is 150mg/m 2 ；
The concentration of the nickel sulfamate is 150g/L;
the concentration of the boric acid is 25g/L;
the concentration of potassium bromide was 15g/L.
And S4, electroplating tin on the surface of the first plating base plate to obtain a second plating base plate.
Wherein: the electrotinning is carried out by adopting an MSA high-speed tinning system, and the current density of the electrotinning is 2A/dm 2 The tin ion concentration of the electroplated tin is 12g/L, and the mass of the tin coating of the second coating substrate is 0.48g/m 2 。
And S5, carrying out reflow and passivation on the second coating substrate to obtain the coating tinplate.
Wherein:
the reflow adopts resistance reflow, the temperature of the reflow is 280 ℃, and the end point of the reflow is as follows: the free tin content of the surface of the galvanized tinplate is 0.20g/m 2 ；
The passivation solution adopted for passivation is sodium dichromate water solutionThe concentration of the passivation solution is 25g/L, the passivation temperature is 42 ℃, the passivation pH value is 4.4, and the passivation current density is 0.5A/dm 2 。
Comparative example 1
The preparation method of the galvanized tinplate comprises the following steps:
and S1, obtaining a steel plate substrate.
Wherein: the surface roughness of the steel plate substrate was 0.3. Mu.m.
And S2, carrying out alkali washing and acid washing on the steel plate substrate to obtain a pretreated substrate.
Wherein:
the alkaline washing is electrolytic alkaline washing, the washing liquid of the alkaline washing is potassium hydroxide solution, the concentration of the potassium hydroxide solution is 45g/L, the temperature of the potassium hydroxide solution is 70 ℃, and the current density of the alkaline washing is 20A/dm 2 ；
The pickling is electrochemical pickling, the pickling solution is sulfuric acid aqueous solution, the concentration of the sulfuric acid aqueous solution is 45g/L, the temperature of the sulfuric acid aqueous solution is 45 ℃, and the current density of the pickling is 20A/dm 2 。
And S3, electroplating tin on the surface of the substrate to obtain the low-tin-content tin-plated plate.
Wherein: the electrotinning is carried out by adopting an MSA high-speed tinning system, and the current density of the electrotinning is 2A/dm 2 The tin ion concentration of the electrolytic tin plating is 12g/L, and the mass of the tin plating layer of the second plating base plate is 0.51g/m 2 。
S5, performing reflow and passivation on the second coating substrate to obtain the coating tinplate.
The reflow adopts resistance reflow, the temperature of the reflow is 290 ℃, and the free tin content on the surface of the galvanized tinplate is 0g/m 2 ；
The passivation solution adopted by the passivation is sodium dichromate water solution, the concentration of the passivation solution is 25g/L, the passivation temperature is 42 ℃, the passivation pH value is 4.4, and the passivation current density is 0.5A/dm 2 。
Comparative example 2
Taking an industrially normally produced 1.1g/m2 tin plate, the roughness is 0.35 μm, and the thickness of the tin layer is 1.02g/m 2 Free tin thickness of 0.65g/m 2 Passivation solution for passivationThe passivation solution is sodium dichromate water solution, the concentration of the passivation solution is 25g/L, the passivation temperature is 42 ℃, the passivation pH value is 4.4, and the passivation current density is 0.5A/dm 2 。
Comparative example 3
The preparation method of the coated tinplate comprises the following steps:
and S1, obtaining a steel plate substrate.
Wherein: the surface roughness of the steel plate substrate was 0.3. Mu.m.
S2, carrying out alkali washing and acid washing on the steel plate substrate to obtain a pretreated substrate.
Wherein:
the alkaline washing is electrolytic alkaline washing, the washing liquid of the alkaline washing is potassium hydroxide solution, the concentration of the potassium hydroxide solution is 45g/L, the temperature of the potassium hydroxide solution is 70 ℃, and the current density of the alkaline washing is 20A/dm 2 ；
The acid washing is electrochemical acid washing, the washing solution of the acid washing is sulfuric acid aqueous solution, the concentration of the sulfuric acid aqueous solution is 45g/L, the temperature of the sulfuric acid aqueous solution is 45 ℃, and the current density of the acid washing is 20A/dm 2 。
And S3, electroplating nickel on the surface of the pretreated substrate to obtain a first plating layer substrate.
Wherein:
the plating solution for electroplating nickel has the following solutes: nickel sulfamate, boric acid and potassium bromide, wherein a solvent of a plating solution adopted by the nickel electroplating is an aqueous solution;
the temperature of the electroplated nickel is 30 ℃;
the mass of the nickel coating of the first coating substrate is 10mg/m 2 ；
The concentration of the nickel sulfamate is 150g/L;
the concentration of the boric acid is 25g/L;
the concentration of potassium bromide was 15g/L.
And S4, electroplating tin on the surface of the first plating base plate to obtain a second plating base plate.
Wherein: the electrotinning is carried out by adopting an MSA high-speed tinning system, and the current density of the electrotinning is 2A/dm 2 The tin ion concentration of the electroplated tin is 12g/L, and the mass of the tin coating of the second coating substrate is 0.51g/m 2 。
S5, performing reflow and passivation on the second coating substrate to obtain the coating tinplate.
Wherein:
the reflow adopts resistance reflow, the temperature of the reflow is 280 ℃, and the end point of the reflow is as follows: the free tin content of the surface of the galvanized tinplate is 0.04g/m 2 ；
The passivation solution adopted by the passivation is sodium dichromate water solution, the concentration of the passivation solution is 25g/L, the passivation temperature is 42 ℃, the passivation pH value is 4.4, and the passivation current density is 0.5A/dm 2 。
Also provides a galvanized tinplate prepared by the method.
Comparative examples, or changes in the procedures and parameters described herein, distinguish the protocol from that of the present application.
Examples of the experiments
The performance of the plated tinplate provided in examples 1-3 and comparative examples 1-3 was tested, and the specific results are shown in the following table.
The detection method comprises the following steps:
and (3) testing adhesive force: according to a corresponding test method in Standard QB/T2763-2006 coating tin (or chromium) plated thin steel plate, the surface of the tin plate is coated with epoxy phenolic paint, baked for 15min at 200 ℃, repeated for 2 times, cooled to form a film-coated tin plate, and adhesion tests are carried out for 3 times in each group.
Salt spray rating test: according to the salt spray test, the sample is inclined by 25 degrees and placed in a salt spray box according to GB/T10125-2012 salt spray test for artificial atmosphere corrosion test. The temperature in the box is (35 +/-2) DEG C, the mass fraction of the saline is 5 +/-0.5 percent, the pH is 6.5-7.2, and the pH is 80cm 2 The sedimentation rate of the horizontal area is 1.0-1.5mL/h. The neutral salt spray test is carried out for 2 hours after the same pretreatment (alcohol degreasing, 60 ℃ hot water cleaning) is carried out on different samples, and the performance of the neutral salt spray test is further rated according to the rating of a test sample and a test piece after corrosion tests of metal and other inorganic coatings on a GBT6461-2002 metal substrate.
Salt spray rating Grade of adhesion
Example 1 6-8 ≤2
Example 2 6-8 ≤2
Example 3 6-8 ≤2
Comparative example 1 0-1 2-3
Comparative example 2 6-8 ≤2
Comparative example 3 0-2 ≤2
As can be seen from the above table, the plated tinplate of examples 1-3 of the present application has significant performance advantages compared with the materials of comparative examples 1 and 3, the surface corrosion resistance is significantly better than that of the comparative examples, and the salt spray grade of 2h neutral salt spray resistance test can reach 6-8 stages; conventional 1.1g/m compared to comparative example 2 2 As for the material of the coating, the 2h neutral salt spray resistance test salt spray level of the galvanized tinplate of the embodiment 1-3 of the application is comparable with that of the galvanized tinplate, and the adhesive force reaches the level of 2 and above 2.
Finally, it should be further noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.

Claims (10)

1. The preparation method of the coated tinplate is characterized by comprising the following steps of:
obtaining a steel plate substrate;
performing alkali washing and acid washing on the steel plate substrate to obtain a pretreated substrate;
electroplating nickel on the surface of the pretreated substrate to obtain a first coating substrate;
electroplating tin on the surface of the first plating layer substrate to obtain a second plating layer substrate;
and carrying out reflow and passivation on the second coating substrate to obtain the coating tinplate.
2. The method of claim 1, wherein the surface roughness Sa of the steel plate substrate is not more than 0.5 μm.
3. The method according to claim 2, wherein the surface roughness Sa of the steel sheet substrate is 0.15 to 0.35 μm.
4. The method for preparing coated tinplate as claimed in claim 1, wherein the alkaline washing is electrolytic alkaline washing, the alkaline washing is potassium hydroxide solution, the concentration of the potassium hydroxide solution is 40-50g/L, the temperature of the potassium hydroxide solution is 70-80 ℃, and the current density of the alkaline washing is 20-25A/dm 2 。
5. The method for preparing coated tinplate as claimed in claim 1, wherein the acid washing is electrochemical acid washing, the washing solution of the acid washing is aqueous solution of sulfuric acid, the concentration of the aqueous solution of sulfuric acid is 40-50g/L, the temperature of the aqueous solution of sulfuric acid is 40-50 ℃, and the current density of the acid washing is 10-22A/dm 2 。
6. The method of claim 1, wherein the step of forming the plated tinplate includes the steps of,
the electroplating solution adopted by the electroplating nickel has the following solutes: nickel sulfamate, boric acid and potassium bromide, wherein the solvent of the plating solution adopted by the nickel electroplating is water;
the temperature of the electroplated nickel is 30-35 ℃;
the mass of the nickel coating of the first coating substrate is 50-150mg/m 2 ；
Wherein:
the concentration of the nickel sulfamate is 100-400g/L;
the concentration of the boric acid is 20-50g/L;
the concentration of the potassium bromide is 15-30g/L.
7. The method for preparing coated tinplate as claimed in claim 1, wherein the electrolytic tinning is carried out using MSA high speed tinning system,the current density of the electrolytic tin plating is 1-3A/dm 2 The tin ion concentration of the electroplated tin is 10-15g/L, and the mass of the tin coating of the second coating substrate is 0.4-0.7g/m 2 。
8. The method for preparing the coated tinplate as claimed in claim 1, wherein the temperature of the reflow is not less than 265 ℃, and the end point of the reflow is as follows: the free tin content of the surface of the galvanized tinplate is 0.05-0.25g/m 2 。
9. The method for preparing coated tinplate as claimed in claim 1, wherein the passivation solution used in the passivation is an aqueous solution of sodium dichromate, the concentration of the passivation solution is 22-28g/L, the temperature of the passivation is 40-44 ℃, the pH value of the passivation is 4.2-4.6, and the current density of the passivation is 0.5-3A/dm 2 。
10. A coated tinplate, characterized in that it is produced by the process for the production of a coated tinplate according to any one of claims 1 to 9.
CN202210828566.8A 2022-07-13 2022-07-13 Preparation method of coating tinplate and coating tinplate Pending CN115161729A (en)

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