CN114293038A - Preparation method of corrosion-resistant cerium-containing Zn-Cu-Ti coating - Google Patents
Preparation method of corrosion-resistant cerium-containing Zn-Cu-Ti coating Download PDFInfo
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Abstract
The invention discloses a preparation method of a corrosion-resistant cerium-containing Zn-Cu-Ti coating, which comprises the following steps: (1) selecting high-quality sponge titanium and pure copper particles as raw materials in a ratio of 1:1, and smelting the raw materials by using a vacuum arc melting furnace with electromagnetic stirring conditions to prepare the Cu-50Ti intermediate alloy. (2) Weighing pure zinc blocks and pure cerium blocks according to the mass ratio of 50:1, and smelting by using a common resistance furnace to prepare the zinc-cerium intermediate alloy. (3) During hot dip coating, the components Zn-0.75Cu-0.15Ti-Ce are smelted, a Zn block is smelted firstly, and a Cu-50Ti intermediate alloy and a zinc-cerium intermediate alloy are put into the Zn block. (4) Before hot dipping, plating assistant treatment is carried out on the surface of Q235; (5) setting the hot dipping temperature at 700 ℃, taking out after dipping for 20-30s, pulling at the speed of 1.5cm/s, taking out, and putting into ultrapure water for cooling. The invention has the advantages that: on one hand, the Zn-Cu-Ti coating containing Ce is used for further improving the corrosion resistance of the hot dip plating Zn-Cu-Ti alloy coating; on the other hand, the problem of optimizing the hot dip coating process of the cerium-containing Zn-Cu-Ti coating is determined.
Description
Technical Field
The invention relates to the technical field of alloy and hot dip coating materials, in particular to a preparation method of a corrosion-resistant cerium-containing Zn-Cu-Ti coating.
Background
In the practical application process, Q235 steel material is easy to corrode in high-temperature oxidation and strong acid medium, and if a metal matrix is exposed to marine environment for a long time, surface lattices can be moved, chemical corrosion can be caused, and serious consumption and breakage phenomena can be generated, so that great waste of material can be caused, and serious economic loss can be generated. In recent years, with the development of industrial production, new requirements for corrosion resistance of workpieces are made, and the limitations of conventional materials are exposed, and there is a necessary trend in developing new hot dip coating materials. At present, Zn-Al is still used as a main material in hot dip coating, and the corrosion resistance and the mechanical property of the coating are improved to the top. However, no application report exists for the Zn-Cu-Ti alloy coating at present, not to mention the hot dip coating with Zn-Cu-Ti-Ce. The rare earth element cerium (Ce) is prone to be enriched on the surface layer, and a dense Ce2O3 oxide film is easily formed on the surface of the coating. Research shows that 0.05-0.2% of Ce is added into zinc bath to delay the expansion of brittle alloy layer obviously, while the Sandelin effect of active steel is effectively inhibited after 0.04% of Ti and 0.02% of Ce are added into zinc solution simultaneously, the micro-hardness and tensile strength of Zn alloy can be increased by Cu compound phase, and the toughness of alloy can be improved by Ti compound phase.
The hot dip plating Zn-Cu-Ti-Ce alloy plating layer not only has high corrosion resistance and mechanical property, but also has the cathode electrochemical protection effect of the zinc-aluminum plating layer, and has important application prospect in the aspect of engineering structure corrosion prevention. However, related research work is hardly carried out, the appearance of the hot dip coating Zn-Cu-Ti-Ce coating is not clear, and the influence of the Ce content on the performance of the Zn-Cu-Ti coating is not clear.
Disclosure of Invention
The invention provides a preparation method of a corrosion-resistant cerium-containing Zn-Cu-Ti coating in order to solve the various problems, and on one hand, the Ce-containing Zn-Cu-Ti coating is used for further improving the corrosion resistance of the hot-dip Zn-Cu-Ti alloy coating; on the other hand, the problem of optimizing the hot dip coating process of the cerium-containing Zn-Cu-Ti coating is determined.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a preparation method of a corrosion-resistant cerium-containing Zn-Cu-Ti coating comprises the following steps:
the method comprises the following steps: selecting high-quality sponge titanium and pure copper particles as raw materials in a ratio of 1:1, and smelting the raw materials by using a vacuum arc melting furnace with electromagnetic stirring conditions to prepare the Cu-50Ti intermediate alloy.
Step two: weighing pure zinc blocks and pure cerium blocks according to the mass ratio of 50:1, smelting by using a common muffle furnace, and stirring for multiple times to prepare the zinc-cerium intermediate alloy.
Step three: during hot dip coating, firstly smelting the components Zn-0.75Cu-0.15Ti-XCe, firstly melting a Zn block, selecting the temperature to be about 650 ℃, putting a Cu-50Ti intermediate alloy and a zinc-cerium intermediate alloy into the molten Zn block after the Zn block is completely molten, and preserving heat for at least 4 hours at the temperature.
Step four: before hot dipping, plating assistant treatment is carried out on the surface of Q235, and the plating assistant solvent is ZnCl2300g/L, NaCl 30g/L, NaF 5g/L, plating assistant temperature (75 ℃, 30s), and then drying (70 ℃, 5 min).
Step five: before immersing in the zinc bath, the dross and zinc ash on the surface of the zinc bath should be scraped clean, and then the temperature is set to 700 ℃ +/-5 ℃, and the sample is immersed from a fresh liquid surface. And (3) preheating the steel wire to be plated during hot dipping, carrying out dipping for 20-30s, then drawing out at the drawing speed of 1.5cm/s, and putting the drawn steel wire into ultrapure water for cooling.
Preferably, the heat preservation time of the Zn-Cu-Ti-Ce alloy in the step three is not less than 4 h.
Preferably, the components of the hot dip Zn-Cu-Ti-Ce alloy coating in the second step are Zn-0.75Cu-0.15Ti-0.1Ce, Zn-0.75Cu-0.15Ti-0.2Ce and Zn-0.75Cu-0.15Ti-0.3Ce respectively.
Preferably, the dip plating temperature of the hot dip Zn-Cu-Ti-Ce alloy coating in the third step is maintained at 700 ℃ ± 5 ℃.
Preferably, the immersion plating time of the hot dip Zn-Cu-Ti-Ce alloy coating in the step five is 20-30 s.
Preferably, the drawing speed of the hot dip Zn-Cu-Ti-Ce alloy coating in the step five is 1.5 cm/s.
Compared with the prior art, the invention has the advantages that: the preparation method comprises the steps of preparing Cu-50Ti intermediate alloy by vacuum arc melting, preparing zinc-cerium intermediate alloy by a muffle furnace, preparing and melting hot-dip plating solution, carrying out plating assisting temperature treatment on Q235 steel before hot-dip plating, and finally carrying out dip plating according to the process. The Zn-Cu-Ti-Ce coating is used for replacing the traditional Zn-Al coating, the hot dip coating process is adopted to prepare the Zn-Cu-Ti-Ce coating, and the problem of optimizing the hot dip coating process of the Zn-Cu-Ti coating containing Ce is determined, so that the popularization and the application of the Zn-Cu-Ti-Ce coating can be facilitated.
Drawings
FIG. 1 shows the morphology of a Zn-0.75Cu-0.15Ti-0.2Ce coating prepared by the invention with the immersion plating time of 20s at 700 ℃.
FIG. 2 shows the morphology of a Zn-0.75Cu-0.15Ti-0.2Ce coating prepared by the invention with the immersion plating time of 25s at 700 ℃.
FIG. 3 shows the morphology of a Zn-0.75Cu-0.15Ti-0.2Ce coating prepared by the invention with the immersion plating time of 30s at 700 ℃.
FIG. 4 is a polarization curve of Zn-0.75Cu-0.15Ti- (0.1-0.3) Ce coating in 3.5% NaCl solution prepared at 700 deg.C/25 s.
FIG. 5 is an AC impedance curve of Zn-0.75Cu-0.15Ti- (0.1-0.3) Ce coating in 3.5% NaCl solution prepared at 700 deg.C/25 s.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Example 1
A preparation method of a corrosion-resistant cerium-containing Zn-Cu-Ti coating comprises the following steps:
(1) selecting high-quality sponge titanium and pure copper particles as raw materials in a ratio of 1:1, and smelting the raw materials by using a vacuum arc melting furnace with electromagnetic stirring conditions to prepare the Cu-50Ti intermediate alloy.
(2) Pure copper particles, pure zinc and pure cerium are used as raw materials, a resistance furnace is utilized to prepare Zn-10Cu and Zn-3Ce intermediate alloy, the smelting temperature is 650 ℃, the heat preservation time is not less than 5 hours, and multiple times of stirring are carried out in the heat preservation process.
(3) Pure Zn, Cu-50Ti, Zn-10Cu and Zn-3Ce intermediate alloy are used as raw materials, a resistance furnace is used for preparing a Zn-0.75Cu-0.15Ti-0.1Ce immersion plating solution, a Zn block is firstly melted during smelting, the selected temperature is about 650 ℃, the intermediate alloy is added after the Zn block is completely melted, and the temperature is kept at 650 ℃ for at least 4 hours.
(4) Before the hot dipping experiment, the plating assistant treatment is carried out on the surface of Q235, and the plating assistant solvent comprises ZnCl2300g/L, 30g/L NaCl, 5g/L NaF, 75 ℃ of plating assisting temperature and 30s of time; and finally drying at 70 deg.C for 5 min. .
(5) Before immersing in Zn-Cu-Ti-Ce bath, the dross and zinc ash on the surface of zinc bath are scraped clean, and then the temperature is set at 700 ℃ +/-5 ℃. And (3) preheating a Q235 sample to be plated during hot dipping, carrying out dipping for 25s, then pulling out at the pulling speed of 1.5cm/s, and putting the pulled out into ultrapure water for cooling.
Example 2
A preparation method of a corrosion-resistant cerium-containing Zn-Cu-Ti coating comprises the following steps:
(1) selecting high-quality sponge titanium and pure copper particles as raw materials in a ratio of 1:1, and smelting the raw materials by using a vacuum arc melting furnace with electromagnetic stirring conditions to prepare the Cu-50Ti intermediate alloy.
(2) Pure copper particles, pure zinc and pure cerium are used as raw materials, a resistance furnace is utilized to prepare Zn-10Cu and Zn-3Ce intermediate alloy, the smelting temperature is 650 ℃, the heat preservation time is not less than 5 hours, and multiple times of stirring are carried out in the heat preservation process.
(3) Pure Zn, Cu-50Ti, Zn-10Cu and Zn-3Ce intermediate alloy are used as raw materials, a resistance furnace is used for preparing a Zn-0.75Cu-0.15Ti-0.2Ce immersion plating solution, a Zn block is firstly melted during smelting, the selected temperature is about 650 ℃, the intermediate alloy is added after the Zn block is completely melted, and the temperature is kept at 650 ℃ for at least 4 hours.
(4) Before the hot dipping experiment, the plating assistant treatment is carried out on the surface of Q235, and the plating assistant solvent comprises ZnCl2300g/L, 30g/L NaCl, 5g/L NaF, 75 ℃ of plating assisting temperature and 30s of time; and finally drying at 70 deg.C for 5 min. .
(5) Before immersing in Zn-Cu-Ti-Ce bath, the dross and zinc ash on the surface of zinc bath are scraped clean, and then the temperature is set at 700 ℃ +/-5 ℃. And (3) preheating a Q235 sample to be plated during hot dipping, carrying out dipping for 25s, then pulling out at the pulling speed of 1.5cm/s, and putting the pulled out into ultrapure water for cooling.
Example 3
A preparation method of a corrosion-resistant cerium-containing Zn-Cu-Ti coating comprises the following steps:
(1) selecting high-quality sponge titanium and pure copper particles as raw materials in a ratio of 1:1, and smelting the raw materials by using a vacuum arc melting furnace with electromagnetic stirring conditions to prepare the Cu-50Ti intermediate alloy.
(2) Pure copper particles, pure zinc and pure cerium are used as raw materials, a resistance furnace is utilized to prepare Zn-10Cu and Zn-3Ce intermediate alloy, the smelting temperature is 650 ℃, the heat preservation time is not less than 5 hours, and multiple times of stirring are carried out in the heat preservation process.
(3) Pure Zn, Cu-50Ti, Zn-10Cu and Zn-3Ce intermediate alloy are used as raw materials, a resistance furnace is used for preparing a Zn-0.75Cu-0.15Ti-0.3Ce immersion plating solution, a Zn block is firstly melted during smelting, the selected temperature is about 650 ℃, the intermediate alloy is added after the Zn block is completely melted, and the temperature is kept at 650 ℃ for at least 4 hours.
(4) Before the hot dipping experiment, the plating assistant treatment is carried out on the surface of Q235, and the plating assistant solvent comprises ZnCl2300g/L, 30g/L NaCl, 5g/L NaF, 75 ℃ of plating assisting temperature and 30s of time; and finally drying at 70 deg.C for 5 min. .
(5) Before immersing in Zn-Cu-Ti-Ce bath, the dross and zinc ash on the surface of zinc bath are scraped clean, and then the temperature is set at 700 ℃ +/-5 ℃. And (3) preheating a Q235 sample to be plated during hot dipping, carrying out dipping for 25s, then pulling out at the pulling speed of 1.5cm/s, and putting the pulled out into ultrapure water for cooling.
Example 4
A preparation method of a corrosion-resistant cerium-containing Zn-Cu-Ti coating comprises the following steps:
(1) selecting high-quality sponge titanium and pure copper particles as raw materials in a ratio of 1:1, and smelting the raw materials by using a vacuum arc melting furnace with electromagnetic stirring conditions to prepare the Cu-50Ti intermediate alloy.
(2) Pure copper particles, pure zinc and pure cerium are used as raw materials, a resistance furnace is utilized to prepare Zn-10Cu and Zn-3Ce intermediate alloy, the smelting temperature is 650 ℃, the heat preservation time is not less than 5 hours, and multiple times of stirring are carried out in the heat preservation process.
(3) Pure Zn, Cu-50Ti, Zn-10Cu and Zn-3Ce intermediate alloy are used as raw materials, a resistance furnace is used for preparing Zn-0.75Cu-0.15Ti- (0.1-0.3) Ce immersion plating solution, a Zn block is firstly melted during smelting, the selected temperature is about 650 ℃, the intermediate alloy is added after the Zn block is completely melted, and the temperature is kept at 650 ℃ for at least 4 hours.
(4) Before the hot dipping experiment, the plating assistant treatment is carried out on the surface of Q235, and the plating assistant solvent comprises ZnCl2300g/L, 30g/L NaCl, 5g/L NaF, 75 ℃ of plating assisting temperature and 30s of time; and finally drying at 70 deg.C for 5 min. .
(5) Before immersing in Zn-Cu-Ti-Ce bath, the dross and zinc ash on the surface of zinc bath are scraped clean, and then the temperature is set at 700 ℃ +/-5 ℃. During hot dipping, the Q235 sample to be plated is preheated, is pulled out after being dipped for 20s at the pulling speed of 1.5cm/s, and is put into ultrapure water for cooling.
Example 5
A preparation method of a corrosion-resistant cerium-containing Zn-Cu-Ti coating comprises the following steps:
(1) selecting high-quality sponge titanium and pure copper particles as raw materials in a ratio of 1:1, and smelting the raw materials by using a vacuum arc melting furnace with electromagnetic stirring conditions to prepare the Cu-50Ti intermediate alloy.
(2) Pure copper particles, pure zinc and pure cerium are used as raw materials, a resistance furnace is utilized to prepare Zn-10Cu and Zn-3Ce intermediate alloy, the smelting temperature is 650 ℃, the heat preservation time is not less than 5 hours, and multiple times of stirring are carried out in the heat preservation process.
(3) Pure Zn, Cu-50Ti, Zn-10Cu and Zn-3Ce intermediate alloy are used as raw materials, a resistance furnace is used for preparing Zn-0.75Cu-0.15Ti- (0.1-0.3) Ce immersion plating solution, a Zn block is firstly melted during smelting, the selected temperature is about 650 ℃, the intermediate alloy is added after the Zn block is completely melted, and the temperature is kept at 650 ℃ for at least 4 hours.
(4) Before the hot dipping experiment, the plating assistant treatment is carried out on the surface of Q235, and the plating assistant solvent comprises ZnCl2300g/L, 30g/L NaCl, 5g/L NaF, 75 ℃ of plating assisting temperature and 30s of time; and finally drying at 70 deg.C for 5 min. .
(5) Before immersing in the Zn-Cu-Ti-Ce bath, dross and zinc ash on the surface of the zinc bath were scraped clean, and then the temperature was set at 700 ℃. During hot dipping, the Q235 sample to be plated is preheated, is drawn out after being dipped for 30s at the drawing speed of 1.5cm/s, and is drawn out and put into ultrapure water for cooling.
The present invention and its embodiments have been described above, and the description is not intended to be limiting, and the drawings are only one embodiment of the present invention, and the actual structure is not limited thereto. In summary, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. The preparation method of the corrosion-resistant cerium-containing Zn-Cu-Ti coating is characterized by comprising the following preparation steps:
the method comprises the following steps: proportioning high-quality sponge titanium and pure copper particles in a ratio of 1:1, smelting in a vacuum arc melting furnace, and performing electromagnetic stirring to prepare a Cu-50Ti intermediate alloy;
step two: proportioning a pure zinc block and a pure cerium block according to the mass ratio of 50:1, smelting in a resistance furnace, and stirring for multiple times to prepare a zinc-cerium intermediate alloy;
step three: firstly, melting a Zn block, keeping the temperature at 650 ℃ for 1h, and respectively adding a Cu-50Ti intermediate alloy and a zinc-cerium intermediate alloy;
step four: before hot dipping, Q235 is subjected to plating assistant treatment, and the plating assistant solvent is ZnCl2300g/L, NaCl 30g/L and NaF 5 g/L; the plating assisting temperature is 75 ℃, and the time is 30 s; finally drying at 70 deg.CThe time is 5 min;
step five: and (3) carrying out heat preservation treatment on the hot dip Zn-Cu-Ti-Ce alloy coating, then slowly pulling out the hot dip Zn-Cu-Ti-Ce alloy coating at the pulling speed of 1.5cm/s, and then putting the hot dip Zn-Cu-Ti-Ce alloy coating into water for cooling.
2. The method for preparing a corrosion-resistant cerium-containing Zn-Cu-Ti coating according to claim 1, wherein: in the third step, the heat preservation time of the Zn-Cu-Ti-Ce alloy is not less than 4 h.
3. The method for preparing a corrosion-resistant cerium-containing Zn-Cu-Ti coating according to claim 1, wherein: in the third step, the components of the hot-dip galvanized copper-titanium alloy coating are Zn-0.75Cu-0.15Ti-0.1Ce, Zn-0.75Cu-0.15Ti-0.2Ce and Zn-0.75Cu-0.15Ti-0.3Ce respectively.
4. The method for preparing a corrosion-resistant cerium-containing Zn-Cu-Ti coating according to claim 1, wherein: in the fourth step, the hot dipping plating assistant solvent comprises ZnCl 2300 g/L, NaCl 30g/L and NaF 5 g/L.
5. The method for preparing a corrosion-resistant cerium-containing Zn-Cu-Ti coating according to claim 1, wherein: in the fifth step, the dip plating temperature of the hot dip plating Zn-Cu-Ti-Ce alloy coating is kept at 700 +/-5 ℃.
6. The method for preparing a corrosion-resistant cerium-containing Zn-Cu-Ti coating according to claim 1, wherein: in the fifth step, the dip plating time of the hot dip plating Zn-Cu-Ti-Ce alloy coating is 20-30 s.
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