CN115418592B - Chloride molten salt corrosion resistant coating and preparation method thereof - Google Patents

Chloride molten salt corrosion resistant coating and preparation method thereof Download PDF

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CN115418592B
CN115418592B CN202210917601.3A CN202210917601A CN115418592B CN 115418592 B CN115418592 B CN 115418592B CN 202210917601 A CN202210917601 A CN 202210917601A CN 115418592 B CN115418592 B CN 115418592B
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molten salt
salt corrosion
corrosion resistant
chloride molten
resistant coating
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CN115418592A (en
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张先满
李星涛
季坤鹏
罗洪峰
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Hainan University
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Hainan University
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/04—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the coating material
    • C23C2/12—Aluminium or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/26—After-treatment
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00—Energy generation of nuclear origin
    • Y02E30/30—Nuclear fission reactors

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Coating With Molten Metal (AREA)

Abstract

The invention provides a chloride molten salt corrosion resistant coating and a preparation method thereof, comprising FeAl 3 And a lamellar structure composed of FeAl having Si dissolved therein 3 And Cr-Al-Si-B quaternary MAB alternately. The preparation method comprises the following steps: step one, hot dip coating Al-Si alloy: immersing Fe-Cr-B alloy into an Al-Si alloy melt for hot dip plating, then extracting a sample from the alloy melt, and performing air cooling to obtain the Fe-Cr-B alloy with a coating attached to the surface; step two, chloride molten salt corrosion: and (3) immersing the Fe-Cr-B alloy with the plating layer on the surface prepared in the step (I) into chloride molten salt for chloride molten salt corrosion. The preparation process is simple, and the prepared metal coating is compact, well combined with a matrix, has a self-growth special effect and excellent chloride molten salt corrosion resistance.

Description

Chloride molten salt corrosion resistant coating and preparation method thereof
Technical Field
The invention relates to the field of novel materials, in particular to a chloride molten salt corrosion resistant coating and a preparation method thereof.
Background
The need for global carbon neutralization, various new energy technologies are rapidly developing. Among them, concentrating solar power generation technology has received a great deal of attention in recent years by combining with advanced energy storage systems. At present, the concentrating solar power generation technology mostly adopts chloride molten salt as a heat transfer and storage material, but high-temperature chloride molten salt, especially chloride ions in the chloride molten salt, can generate strong corrosion effect on contacted metal pipelines, thereby causing material failure and affecting the reliability of equipment. The Fe-based nickel-based alloy is a common metal material in the concentrating solar power generation device due to the high-temperature mechanical property and relatively good corrosion resistance. However, compared with nickel-based alloys, iron-based materials such as stainless steel have poorer resistance to molten salt corrosion, so that corrosion-resistant components of concentrating solar power generation devices often use nickel-based alloys with better resistance to molten salt corrosion, but the cost of the nickel-based alloys is higher.
The MAB phase (m=transition group metal element, a=al, B is B element) is a ternary layered intermetallic compound, the existing synthesis process is complex, the cost is high, and there are few reports of quaternary MAB phases, especially in which a is simultaneously Al and Si to form a solid solution.
Disclosure of Invention
The invention aims to solve the technical problem of providing a chloride molten salt corrosion resistant coating and a preparation method thereof, wherein the coating can be self-grown in molten salt corrosion, and further can realize long-term protection.
In order to solve the technical problems, the invention adopts the following technical scheme: a chloride molten salt corrosion resistant coating comprises FeAl 3 And a lamellar structure composed of FeAl having Si dissolved therein 3 And Cr-Al-Si-B quaternary MAB alternately.
The invention also provides a preparation method of the chloride molten salt corrosion resistant coating, which comprises the following steps:
step one, hot dip coating Al-Si alloy:
immersing Fe-Cr-B alloy into an Al-Si alloy melt for hot dip plating, then extracting a sample from the alloy melt, and performing air cooling to obtain the Fe-Cr-B alloy with a coating attached to the surface;
step two, chloride molten salt corrosion:
and (3) immersing the Fe-Cr-B alloy with the plating layer on the surface prepared in the step (I) into chloride molten salt for chloride molten salt corrosion.
In a preferred scheme, the plating layer obtained in the first step is sequentially formed by Fe-Al-Si ternary intermetallic compound and embedded FeAl from inside to outside 3 Lamellar structure and Al-Si alloy composition, inlaid FeAl 3 Is made of FeAl 3 And Cr-Al-Si-B quaternary MAB alternately.
In the preferred scheme, in the second step, the plating layer in the first step reacts with the substrate to generate the chloride molten salt corrosion resistant plating layer.
In a preferred embodiment, the mosaic FeAl 3 In the second step, the Cr-Al-Si-B quaternary MAB phase in the lamellar structure is first selectively separated out of Si and is then dissolved in adjacent FeAl 3 Is a kind of medium.
In a preferred embodiment, feAl in the lamellar structure of the chloride-resistant molten salt corrosion-resistant coating formed in the second step 3 The Si content of the solid solution is greater than that prepared in the first stepFeAl in lamellar structure of coating 3 Si content of solid solution.
In a preferred embodiment, the Cr-Al-Si-B quaternary MAB phase undergoes a flaky to particulate transformation in step two.
In a preferred scheme, the spacing of lamellar structures of the chloride molten salt corrosion resistant coating generated in the second step is larger than the spacing of lamellar structures of the coating prepared in the first step.
In a preferred scheme, the hot dip coating time in the first step is 30min, and the hot dip coating temperature is 750 ℃.
In a preferred scheme, in the second step, the temperature of the chloride molten salt is 700-800 ℃.
The chloride molten salt corrosion resistant coating and the preparation method thereof provided by the invention have the following beneficial effects:
1. the formed coating can grow automatically in the molten salt corrosion process, and the coating formed by hot dip plating can react with the matrix in the molten salt corrosion process, namely, the coating grows while being corroded by the molten salt, so that long-term protection can be realized.
2. Compared with the traditional hot dip aluminizing, the special coating obtained by adopting the Fe-Cr-B alloy hot dip Al-Si alloy has more excellent chloride molten salt corrosion resistance, simple preparation process, compact prepared metal coating, better combination with a matrix and self-growth special effect.
3. The lamellar structure in the coating is composed of FeAl 3 The Cr-Al-Si-B quaternary MAB is alternately formed, so that molten salt corrosion can be obviously prevented, the corrosion time is further prolonged, and the steel matrix is further protected.
4. A Cr-Al-Si-B quaternary MAB phase is prepared by a simple method and shows excellent molten salt corrosion resistance.
Drawings
The invention is further illustrated by the following examples in conjunction with the accompanying drawings: (based on the pictures and numbers in this document)
FIG. 1 is a cross-sectional low-magnification microstructure of example 1 prior to chloride molten salt corrosion;
FIG. 2 is a graph showing the Si surface distribution before chloride molten salt corrosion in example 1; the method comprises the steps of carrying out a first treatment on the surface of the
FIG. 3 is a cross-sectional low-magnification microstructure of example 1 after molten chloride salt corrosion;
FIG. 4 is a cross-sectional high-power microstructure of example 1 after molten chloride salt corrosion;
FIG. 5 is a graph showing the Si surface distribution after corrosion with the molten chloride salt in example 1;
FIG. 6 is a graph showing the flaky to particulate transition of the Cr-Al-Si-B quaternary MAB phase in the examples;
FIG. 7 shows the cross-sectional high-power microstructure of example 2 after chloride molten salt corrosion.
Detailed Description
The Fe-Cr-Si-B alloy in the examples was prepared by the following method:
(1) and (3) batching: according to the designed alloy composition, calculating the weight of the required micro-carbon ferrochrome (Fe-58 wt.% Cr-0.06wt.% C), fe-18 wt wt.% B, fe-45 wt wt.% Si intermediate alloy and pig iron, and the total weight is 10kg;
(2) smelting: and (3) filling the weighed raw materials in the step (1) into a vacuum smelting furnace, and pouring the raw materials into a sand mould after the raw materials are completely melted to obtain the Fe-Cr-B alloy casting.
Example 1:
step one, hot dip Al-Si alloy
Immersing the prepared Fe-Cr-B cast steel into an Al-6 wt-content Si alloy melt for hot dip plating, wherein the hot dip plating temperature is 750 ℃, rapidly extracting a sample from an aluminum liquid after 30min, and air-cooling to obtain the Fe-Cr-B cast steel with a coating attached to the surface. The cross section structure is shown in figure 1, the thickness of the coating is about 600 mu m, and the coating is sequentially Fe-Al-Si ternary intermetallic compound and embedded FeAl from inside to outside 3 Is composed of lamellar structure and Al-Si alloy three-layer structure, wherein FeAl is inlaid 3 Is made of FeAl 3 And Cr-Al-Si-B quaternary MAB alternately. Si is mainly concentrated around the Cr-Al-Si-B quaternary MAB phase in the Fe-Al-Si ternary intermetallic compound and lamellar structure, and Si is higher in the latter than in the former, as shown in FIG. 2.
Step two, chloride molten salt corrosion
Immersing the Fe-Cr-B cast steel with the plating layer on the surface, which is prepared in the step one, into 45 wt percent NaCl-55 wt percent KCl fused salt with the temperature of 750 ℃ for 1h, taking out, and air cooling to be at the room temperature. The plating layer in the first step reacts with the substrate to generate a chloride molten salt corrosion resistant plating layer, and the thickness of the plating layer after corrosion for 1h is about 650 mu m, so that the self-growth effect is shown. The lamellar structure can block the corrosion of the chloride molten salt, as shown in FIGS. 3 and 4, wherein the Cr-Al-Si-B quaternary MAB phase has a blocking effect ratio FeAl 3 Stronger. Inlaid FeAl 3 In the second step, the Cr-Al-Si-B quaternary MAB phase in the lamellar structure is first selectively separated out of Si and is then dissolved in adjacent FeAl 3 And the spacing of the plies is significantly greater than when thermally dip coating the Al-Si alloy, as shown in fig. 5; the Cr-Al-Si-B quaternary MAB phase also undergoes a transition from platelet to particulate, as shown in FIG. 6.
Example 2:
step one, hot dip Al-Si alloy
And immersing the prepared Fe-Cr-B cast steel into an Al-6 wt-content Si alloy melt for 15 min, rapidly extracting a sample from the aluminum liquid, and air-cooling to obtain the Fe-Cr-B cast steel with a coating attached to the surface, wherein a regular lamellar structure is generated in the coating.
Step two, chloride molten salt corrosion
And (3) immersing the Fe-Cr-B alloy with the plating layer on the surface prepared in the step (I) into 45 wt percent NaCl-55 wt percent KCl fused salt with the temperature of 750 ℃ for 4h, taking out, and air cooling to be at the room temperature. The high-power microstructure of the cross section is shown in figure 7, and the lamellar structure can be seen to obviously block molten salt corrosion.
Example 3:
step one, hot dip Al-Si alloy
And immersing the prepared Fe-Cr-B cast steel into an Al-3wt.% Si alloy melt for 30min, rapidly extracting a sample from the aluminum liquid, and air-cooling to obtain the Fe-Cr-B cast steel with a coating attached to the surface, wherein a regular lamellar structure is generated in the coating.
Step two, chloride molten salt corrosion
And (2) immersing the Fe-Cr-B alloy with the Al-3wt.% Si alloy attached to the surface prepared in the step one into 45 wt% -NaCl-55-wt% -KCl molten salt at 750 ℃ for 24 hours, taking out, air cooling to the room temperature, and enabling the coating to have excellent molten salt corrosion resistance.

Claims (10)

1. The preparation method of the chloride molten salt corrosion resistant coating is characterized by comprising the following steps of:
step one, hot dip coating Al-Si alloy:
immersing Fe-Cr-B alloy into an Al-Si alloy melt for hot dip plating, then extracting a sample from the alloy melt, and performing air cooling to obtain the Fe-Cr-B alloy with a coating attached to the surface;
step two, chloride molten salt corrosion:
and (3) immersing the Fe-Cr-B alloy with the plating layer on the surface prepared in the step (I) into chloride molten salt for chloride molten salt corrosion.
2. The method for preparing a chloride molten salt corrosion resistant coating according to claim 1, wherein the coating obtained in the first step is a ternary intermetallic compound of Fe-Al-Si and inlaid FeAl from inside to outside in sequence 3 Lamellar structure and Al-Si alloy composition, inlaid FeAl 3 Is made of FeAl 3 And Cr-Al-Si-B quaternary MAB alternately, si is mainly distributed around the Cr-Al-Si-B quaternary MAB phase in the Fe-Al-Si ternary intermetallic compound and lamellar structure in a concentrated manner.
3. The method for preparing a molten salt corrosion resistant coating according to claim 1, wherein in the second step, the coating in the first step reacts with the substrate to form the molten salt corrosion resistant coating.
4. The method for preparing a chloride molten salt corrosion resistant coating according to claim 2, wherein the inlaid FeAl 3 In the second step, the Cr-Al-Si-B quaternary MAB phase in the lamellar structure is first selectively separated out of Si and is then dissolved in adjacent FeAl 3 Is a kind of medium.
5. According to claimThe method for preparing a chloride molten salt corrosion resistant coating according to claim 1, wherein FeAl in lamellar structure of the chloride molten salt corrosion resistant coating generated in the second step 3 The Si content of the solid solution is greater than that of FeAl in the lamellar structure of the coating layer prepared in the first step 3 Si content of solid solution.
6. The method for producing a chloride molten salt corrosion resistant coating according to claim 2, wherein the Cr-Al-Si-B quaternary MAB phase undergoes a flaky to particulate transformation in step two.
7. The method for preparing a chloride molten salt corrosion resistant coating according to claim 1, wherein the spacing of lamellar structures of the chloride molten salt corrosion resistant coating formed in the second step is larger than the spacing of lamellar structures of the coating prepared in the first step.
8. The method for preparing a molten salt corrosion resistant coating according to claim 1, wherein the hot dip coating time in the first step is 30min and the hot dip coating temperature is 750 ℃.
9. The method for preparing a chloride molten salt corrosion resistant coating according to claim 1, wherein in the second step, the temperature of the chloride molten salt is 700-800 ℃.
10. The chloride molten salt corrosion resistant coating prepared by the preparation method according to any one of claims 1 to 9, which is characterized by comprising FeAl 3 And a lamellar structure composed of FeAl having Si dissolved therein 3 And Cr-Al-Si-B quaternary MAB alternately.
CN202210917601.3A 2022-08-01 2022-08-01 Chloride molten salt corrosion resistant coating and preparation method thereof Active CN115418592B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104745846A (en) * 2015-03-23 2015-07-01 常州大学 Alloy having periodic lamellar microstructure characteristic and preparation method thereof
CN113969381A (en) * 2021-10-27 2022-01-25 海南大学 Chloride ion corrosion resistant coating and preparation method and application thereof
CN114276148A (en) * 2022-01-03 2022-04-05 西北工业大学 Hexagonal layered boride ceramic h-MAB material and preparation method thereof

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102017006658A1 (en) * 2017-07-13 2019-01-17 Forschungszentrum Jülich GmbH Process for the preparation of non-oxide, ceramic powders

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104745846A (en) * 2015-03-23 2015-07-01 常州大学 Alloy having periodic lamellar microstructure characteristic and preparation method thereof
CN113969381A (en) * 2021-10-27 2022-01-25 海南大学 Chloride ion corrosion resistant coating and preparation method and application thereof
CN114276148A (en) * 2022-01-03 2022-04-05 西北工业大学 Hexagonal layered boride ceramic h-MAB material and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Influence of Cr on the interfacial boride reaction between Fe-Cr-B cast steel and molten aluminium;xianman zhang.et.al;《Corrosion Science》;page108098 *

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