CN104046954A - Method for improving liquid metal corrosion resistance of martensitic heat-resistant steel - Google Patents
Method for improving liquid metal corrosion resistance of martensitic heat-resistant steel Download PDFInfo
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Abstract
The invention aims to provide a method for carrying out liquid metal corrosion treatment on the surface of martensitic heat-resistant steel. The method comprises the following steps: after prearranging a layer of aluminum on a metal surface by virtue of electric arc ion plating, processing by using a laser cladding process, and controlling the surface aluminum activity to form compact and stable aluminum oxide. Therefore, the liquid metal corrosion resistance of metal is effectively improved, and the service life of the metal material is prolonged.
Description
Technical field
The invention belongs to field of metal surface treatment technology, a kind of processing method of metallic surface being carried out to coating, Laser Cladding Treatment is provided especially.
Background technology
Along with becoming increasingly conspicuous of environment and safety problem, and the petering out of traditional energy, the exploitation of novel energy is extremely urgent.ADS transmuting system (Accelerator Driven Transmutation System) is one of ideal chose of the above-mentioned challenge of reply, ADS transmuting system is efficiently utilized nuke rubbish and high security of system with it, having solved the nuclear waste disposal problem that is always restricting nuclear power sustainable development, is one of novel energy system of at present tool development prospect.Because having good thermophysical property and a chemical property, liquid lead, liquid lead bismuth eutectic (lead-bismuth eutectic) are regarded as the ADS transmuting system spallation target preferred material of refrigerant of holding concurrently.
9～12%Cr martensite heat-resistant steel has good mechanical behavior under high temperature, high thermal conductivity, low thermal expansivity and low void swelling rate, becomes covering and the involucrum candidate structure material of the advanced nuclear reaction system such as ADS.But the Working environment of ADS harshness (high temperature, irradiation, liquid metal corrosion), 9～12%Cr martensite heat-resistant steel structured material has been proposed to new challenge, and along with the raising of equipment service temperature and the more harsh corrosive atmosphere facing, need further to require the corrosion resistance nature of raising structured material.
By suitable surface modification technology, can further improve the corrosion resistance nature of 9～12%Cr martensite heat-resistant steel for ADS transmuting system.Research shows, the massfraction of aluminium is controlled at 5%～20% can form the aluminum oxide of one deck densification in liquid LBE, suppress iron ion to external diffusion and oxonium ion to internal diffusion, thereby protection matrix metal is avoided the corrosion of liquid metal.But because aluminium activity is high, if directly add more than 5% Al in matrix, easily generate the compound of complicated aluminium, worsen the mechanical property of metal etc.Therefore, urgently a kind of suitable surface treatment method, guarantees that in the mechanical property that does not affect metal the massfraction of aluminium is controlled at 5%～20%, to forming form compact and stable aluminum oxide, thereby reaches the object that protection metallic matrix is avoided LBE corrosion.
Summary of the invention
The object of the present invention is to provide a kind of method of carrying out resistance to liquid metal corrosion processing on martensite heat-resistant steel surface, by arc ions, be plated in after the preset one deck aluminium in metallic surface, adopt cladding laser surfaces technology controlling and process metallic surface aluminium activity, to form form compact and stable aluminum oxide, hinder iron and oxonium ion inwardly with to external diffusion, thereby effectively improve the resistance to liquid metal corrosion performance of metal, extend the work-ing life of metallic substance.
The present invention specifically provides a kind of method that improves the resistance to liquid metal corrosion of martensite heat-resistant steel; it is characterized in that: first at the preset aluminium lamination in martensite heat-resistant steel surface; then by laser melting and coating process, process and make preset aluminium lamination and metallic matrix metallurgical binding; and control the massfraction of aluminium between 5%～20%, the final aluminum oxide that forms densification continuously in liquid metal is protected metallic matrix.
The method of the resistance to liquid metal corrosion of raising martensite heat-resistant steel of the present invention, is characterized in that: the method is applicable to 9～12%Cr martensite heat-resistant steel.
The method of the resistance to liquid metal corrosion of raising martensite heat-resistant steel of the present invention, it is characterized in that: the chemical composition of described martensite heat-resistant steel is: 0 < C < 0.5%, 0 < Si < 3%, 8.5% < Cr < 13%, 0≤Mo < 3%, 0≤W < 3%, 0% < Mn < 2.0%, 0 < Ta+Nb < 2.0%, 0% < V < 0.5%, surplus is iron.
The method of the resistance to liquid metal corrosion of raising martensite heat-resistant steel of the present invention, is characterized in that: adopt arc ions electroplating method at the preset aluminium lamination in martensite heat-resistant steel surface.
The method of the resistance to liquid metal corrosion of raising martensite heat-resistant steel of the present invention, is characterized in that, comprises the following steps:
(1), pre-treatment is carried out in metallic surface: with the abrasive paper for metallograph test button of polishing, and it is carried out to surperficial wet abrasive blasting, after metal detergent cleans, in deionized water for ultrasonic, clean, dry;
(2), adopt arc ions to be plated in the preset aluminium lamination in metallic surface, the purity of aluminium target is more than 99%: arc ion plating processing condition: vacuum degree in vacuum chamber is less than 8 * 10
-3pa, shielding gas air pressure remains on 0.1-0.3Pa, and furnace chamber temperature is 100-150 ℃, bias voltage-1000V-﹣ 800V, flame current is 50-60A, pre-sputtering is cleaned 3-5min, keep other parameter constant, bias voltage is adjusted into ﹣ 200-﹣ 250V, deposits one deck aluminium lamination on metallic matrix;
(3), laser melting and coating process: utilize the energy of laser beam by the aluminum coating raw material fusing being preset on metallic matrix, make metallic matrix top layer melt simultaneously, the cladding coating that formation and aluminium are metallurgical binding, and in cladding layer, the massfraction of aluminium is controlled between 5%～20%;
(4), thermal treatment: the metal after laser melting and coating process is processed is 400 ℃ ± 50 ℃ vacuum heat treatment, and soaking time is 2h ± 0.5h.
The method of the resistance to liquid metal corrosion of raising martensite heat-resistant steel of the present invention, is characterized in that: the aluminum layer thickness depositing on metallic matrix in step (2) is preferably 5～10 μ m.
Beneficial effect of the present invention:
The present invention adopts arc ions to be plated in the preset aluminium lamination in martensite heat-resistant steel surface; then by laser melting coating surface modification technology, make to be preset at the aluminium lamination of metallic matrix and the cladding layer that metallic matrix top layer forms metallurgical binding; and in cladding layer, the massfraction of aluminium is controlled within the specific limits; in LBE, form the aluminum oxide of continous-stable, thus protection metallic matrix.Because cladding layer is to be melted by preset aluminium lamination and metallic matrix simultaneously, and the extent of dilution forming after rapid solidification is extremely low, and become the top coat of metallurgical binding with matrix, greatly improve the clinging power between coating and metallic matrix, reduce the possibility that coating and metallic matrix peel off, significantly improve the performance such as corrosion-resistant, anti-oxidant of metallic substance.Meanwhile, thin cladding layer can not affect the mechanical property of metallic matrix, has stopped to add at metallic matrix the deterioration of the metallic substance performance that certain aluminium content brings.The resistance to liquid metal corrosion performance that effectively improves martensite heat-resistant steel, extends its work-ing life.
Accompanying drawing explanation
Fig. 1 be after the preset aluminium lamination of embodiment 1 and Laser Cladding Treatment after XRD.
Fig. 2 is the Cross Section Morphology after embodiment 1 laser melting coating thermal treatment.
Fig. 3 is that embodiment 1 corrodes the Cross Section Morphology of 500 hours in the plumbous bismuth eutectic of 600 ℃ of saturated oxygens.
Fig. 4 is that comparative example 1 is corroded the Cross Section Morphology of 500 hours in the plumbous bismuth eutectic of 600 ℃ of saturated oxygens.
Fig. 5 is that comparative example 2 is corroded the Cross Section Morphology of 500 hours in the plumbous bismuth eutectic of 600 ℃ of saturated oxygens.
Embodiment
Following examples will be described further the present invention.
Embodiment 1
(1) pre-treatment is carried out in metallic surface: the test button of 15mm * 10mm * 2mm size is polished to No. 800 step by step with abrasive paper for metallograph, and all corner angle limit is changed into fillet, with 200 order glass balls, carry out surperficial wet abrasive blasting, after metal detergent cleans, in deionized water for ultrasonic, clean, dry.
(2), adopt arc ions to be plated in the preset aluminium lamination in metallic surface, the purity of aluminium target is more than 99%: arc ion plating processing condition: vacuum degree in vacuum chamber 9.5 * 10
-3pa, shielding gas air pressure remains at 2Pa, and furnace chamber temperature is 130 ℃, bias voltage ﹣ 800V, flame current is 55A, and pre-sputtering is cleaned 3min, keeps other parameter constant, and bias voltage is adjusted into ﹣ 225V, and on metallic matrix, deposit thickness is the aluminium lamination of 8 μ m;
(3), laser melting and coating process: utilize the energy of laser beam by the aluminum coating raw material fusing being preset on metallic matrix, make metallic matrix top layer melt simultaneously, the cladding coating that formation and aluminium are metallurgical binding, and in cladding layer, the massfraction of aluminium is 10～12%, laser beam mainly supplies processing parameter: electric current 100A, pulsewidth: 10ms, frequency: 4Hz;
(4), postheat treatment: the metal after laser melting and coating process is processed is 400 ℃ of vacuum heat treatment, and soaking time is 2h.
Above-mentioned metallic substance is martensite heat-resistant steel, and specific chemical composition is: C:0.25wt.%, Cr:10.8wt.%, Si:1.43wt.%, Mn:0.54wt.%, W:1.2wt.%, Ta:0.11wt.%, V:0.19wt.%, Nb:0.014wt.%, surplus is iron.
XRD after aluminizing and after laser melting coating thermal treatment is shown in Fig. 1, and Fig. 2 is the Cross Section Morphology after laser melting coating thermal treatment, and Fig. 3 is that embodiment 1 corrodes the Cross Section Morphology of 500 hours in 600 ℃ of liquid lead bismuth eutectics, and its its mechanical properties does not change.
Embodiment 2
The chemical composition of 9～12%Cr martensite heat-resistant steel is: C:0.1wt.%, and Cr:9.04wt.%, Si:0.26wt.%, Mn:0.46wt.%, Mo:0.92wt.%, Ni:0.17wt.%, V:0.2wt.%, Nb:0.04wt.%, surplus is iron.This metallic surface treatment process is identical with embodiment 1.Corrode 500 hours in 600 ℃ of liquid lead bismuth eutectics after, Cross Section Morphology and embodiment 1 are more or less the same, and its its mechanical properties does not change.
Embodiment 3
The chemical composition of 9～12%Cr martensite heat-resistant steel is: C:0.22wt.%, and Cr:10.73wt.%, Si:1.56wt.%, Mn:0.67wt.%, W:1.41wt.%, Ta:0.19wt.%, V:0.21wt.%, Nb:0.01wt.%, surplus is iron.This metallic surface treatment process is identical with embodiment 1.Corrode 500 hours in 600 ℃ of liquid lead bismuth eutectics after, Cross Section Morphology and embodiment 1 are more or less the same, and its its mechanical properties does not change.
Embodiment 4
The chemical composition of 9～12%Cr martensite heat-resistant steel is: C:0.23wt.%, and Cr:9.93wt.%, Si:1.3wt.%, Mn:1.09wt.%, W:1.16wt.%, Ta:0.1wt.%, V:0.2wt.%, Nb:0.01wt.%, surplus is iron.This metallic surface treatment process is identical with embodiment 1.Corrode 500 hours in 600 ℃ of liquid lead bismuth eutectics after, Cross Section Morphology and embodiment 1 are more or less the same, and its its mechanical properties does not change.
Embodiment 5
The chemical composition of 9～12%Cr martensite heat-resistant steel is: C:0.32wt.%, and Si:1.4wt.%, Cr:11.2wt.%, Mn:0.53wt.%, W:1.43wt.%, Ta:0.15wt.%, V:0.2wt.%, Ni:0.09wt.%, surplus is iron.This metallic surface treatment process is identical with embodiment 1.Corrode 500 hours in 600 ℃ of liquid lead bismuth eutectics after, Cross Section Morphology and embodiment 1 are more or less the same, and its its mechanical properties does not change.
Comparative example 1
The test button of 15mm * 10mm * 2mm size is polished to No. 2000 step by step with abrasive paper for metallograph, and all corner angle limit is changed into fillet, after metal detergent cleans, in deionized water for ultrasonic, clean, dry, the chemical composition of metallic substance is identical with embodiment 1.Fig. 4 is that comparative example 1 is corroded the Cross Section Morphology of 500 hours in 600 ℃ of liquid lead bismuth eutectics.
Comparative example 2
The test button of 15mm * 10mm * 2mm size is polished to No. 2000 step by step with abrasive paper for metallograph, and all corner angle limit is changed into fillet, after metal detergent cleans, in deionized water for ultrasonic, clean, dry, the chemical composition of metallic substance is identical with embodiment 2.Fig. 5 is that comparative example 2 is corroded the Cross Section Morphology of 500 hours in 600 ℃ of liquid lead bismuth eutectics.
Comparative example 3
The test button of 15mm * 10mm * 2mm size is polished to No. 2000 step by step with abrasive paper for metallograph, and all corner angle limit is changed into fillet, after metal detergent cleans, in deionized water for ultrasonic, clean, dry, the chemical composition of metallic substance is identical with embodiment 3.In 600 ℃ of liquid lead bismuth eutectics, corroding 500 hours Cross Section Morphologies and comparative example 1 is more or less the same.
Comparative example 4
The test button of 15mm * 10mm * 2mm size is polished to No. 2000 step by step with abrasive paper for metallograph, and all corner angle limit is changed into fillet, after metal detergent cleans, in deionized water for ultrasonic, clean, dry, the chemical composition of metallic substance is identical with embodiment 4.In 600 ℃ of liquid lead bismuth eutectics, corroding 500 hours Cross Section Morphologies and comparative example 1 is more or less the same.
Comparative example 5
The test button of 15mm * 10mm * 2mm size is polished to No. 2000 step by step with abrasive paper for metallograph, and all corner angle limit is changed into fillet, after metal detergent cleans, in deionized water for ultrasonic, clean, dry, the chemical composition of metallic substance is identical with embodiment 5.In 600 ℃ of liquid lead bismuth eutectics, corroding 500 hours Cross Section Morphologies and comparative example 1 is more or less the same.
Above-described embodiment is only explanation technical conceive of the present invention and feature, and its object is to allow person skilled in the art can understand content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences that spirit is done according to the present invention change or modify, within all should being encompassed in protection scope of the present invention.
Claims (6)
1. a method that improves the resistance to liquid metal corrosion of martensite heat-resistant steel, it is characterized in that: first at the preset aluminium lamination in martensite heat-resistant steel surface, then adopt laser melting and coating process to make the cladding layer that martensite heat-resistant steel surface forms and aluminium is metallurgical binding, and in cladding layer, the massfraction of aluminium is controlled between 5%～20%.
2. according to the method that improves the resistance to liquid metal corrosion of martensite heat-resistant steel described in claim 1, it is characterized in that: described martensite heat-resistant steel is 9～12%Cr martensite heat-resistant steel.
3. according to the method that improves the resistance to liquid metal corrosion of martensite heat-resistant steel described in claim 1, it is characterized in that, the chemical composition of described martensite heat-resistant steel is: 0 < C < 0.5%, 0 < Si < 3%, 8.5% < Cr < 13%, 0≤Mo < 3%, 0≤W < 3%, 0% < Mn < 2.0%, 0 < Ta+Nb < 2.0%, 0% < V < 0.5%, surplus is iron.
4. according to the method that improves the resistance to liquid metal corrosion of martensite heat-resistant steel described in claim 1, it is characterized in that: adopt arc ions electroplating method at the preset aluminium lamination in martensite heat-resistant steel surface.
5. according to the method that improves the resistance to liquid metal corrosion of martensite heat-resistant steel described in claim 1, it is characterized in that, comprise the following steps:
(1), pre-treatment is carried out in metallic surface: with the abrasive paper for metallograph test button of polishing, and it is carried out to surperficial wet abrasive blasting, after metal detergent cleans, in deionized water for ultrasonic, clean, dry;
(2), adopt arc ions to be plated in the preset aluminium lamination in metallic surface, the purity of aluminium target is more than 99%: arc ion plating processing condition: vacuum degree in vacuum chamber is less than 8 * 10
-3pa, shielding gas air pressure remains on 0.1-0.3Pa, and furnace chamber temperature is 100-150 ℃, bias voltage-1000V-﹣ 800V, flame current is 50-60A, pre-sputtering is cleaned 3-5min, keep other parameter constant, bias voltage is adjusted into ﹣ 200-﹣ 250V, deposits one deck aluminium lamination on metallic matrix;
(3), laser melting and coating process: utilize laser by the aluminum coating raw material fusing being preset on metallic matrix, make metallic matrix top layer melt, the cladding coating that formation and aluminium are metallurgical binding simultaneously;
(4), thermal treatment: the metal after laser melting and coating process is processed is 400 ℃ ± 50 ℃ vacuum heat treatment, and soaking time is 2h ± 0.5h.
6. according to the method that improves the resistance to liquid metal corrosion of martensite heat-resistant steel described in claim 1, it is characterized in that: the aluminum layer thickness depositing on metallic matrix in step (2) is 5～10 μ m.
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Cited By (4)
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| CN108774729A (en) * | 2018-06-29 | 2018-11-09 | 南京先进激光技术研究院 | Duplex coating single pass forming method based on laser melting and coating technique |
| CN109161869A (en) * | 2018-09-12 | 2019-01-08 | 云南科威液态金属谷研发有限公司 | A method of corrosion-inhibiting coating is formed in metal part surface |
| CN112144008A (en) * | 2020-08-14 | 2020-12-29 | 中国科学院金属研究所 | Method for improving high-temperature-resistant liquid metal corrosion resistance of oxide dispersion strengthened steel through pre-oxidation |
| CN114717511A (en) * | 2022-03-30 | 2022-07-08 | 北矿磁材（阜阳）有限公司 | Preparation method of Al film on surface of sintered neodymium-iron-boron magnet |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108774729A (en) * | 2018-06-29 | 2018-11-09 | 南京先进激光技术研究院 | Duplex coating single pass forming method based on laser melting and coating technique |
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| CN112144008A (en) * | 2020-08-14 | 2020-12-29 | 中国科学院金属研究所 | Method for improving high-temperature-resistant liquid metal corrosion resistance of oxide dispersion strengthened steel through pre-oxidation |
| CN114717511A (en) * | 2022-03-30 | 2022-07-08 | 北矿磁材（阜阳）有限公司 | Preparation method of Al film on surface of sintered neodymium-iron-boron magnet |
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