CN104278132A - Method for improving low-activation ferrite/martensitic steel high-temperature oxidation resistance - Google Patents
Method for improving low-activation ferrite/martensitic steel high-temperature oxidation resistance Download PDFInfo
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- CN104278132A CN104278132A CN201310287635.XA CN201310287635A CN104278132A CN 104278132 A CN104278132 A CN 104278132A CN 201310287635 A CN201310287635 A CN 201310287635A CN 104278132 A CN104278132 A CN 104278132A
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Abstract
The invention aims at providing a method for improving low-activation ferrite/martensitic steel high-temperature oxidation resistance, and the method enables the ferrite/martensitic steel to satisfy service conditions. The method helps to improve the high-temperature oxidation resistance of the material by forming a nanocrystal-composed surface layer on the low-activation steel surface. Especially, by performing surface mechanical grinding treatment (SMGT) on the low-activation ferrite/martensitic steel subjected to high-temperature tempering, the crystal grain is fined, the crystal boundary ratio is increased, and the element diffusion rate is improved, and thus a protective oxidation film is rapidly formed and anti-oxidation effect is finally given play. The method is capable of substantially improving the high-temperature oxidation resistance of the material, thereby solving the problem that the usage temperature is relatively low.
Description
Technical field
The present invention relates to metal protection technology, is a kind of method improving low activation ferrite/martensite steel high temperature oxidation resistance specifically.By surperficial cal rolling process (SMGT), introduce the gradient-structure changed to micron crystalline substance by nanocrystalline, sub-micron crystal at material surface, significantly improve the antioxidant property of low activation ferrite/martensite steel.
Background technology
Low activation ferrite/martensite steel due to high-performances such as low thermal expansivity, high thermal conductivity, excellent Flouride-resistani acid phesphatase swelling and Flouride-resistani acid phesphatase fragility, and is selected as the candidate structure material of following ADS spallation target.Such steel is formed with elements such as Mo, Nb, Ni in the low activating element replacement such as W, V, Ta ordinary steel, and primary alloy constituent is Fe-(8-12%) Cr.Low ferrite/martensite steel alive due to its Service Environment be hot environment, wherein Cr content is lower, and compactness and the Adhesion property of the oxide film therefore formed under high temperature are poor, causes the oxidation-resistance property of this material more weak, thus affects the use of material.The critical pumping rate of element needed for the outside oxidation transformation of internal oxidition, matrix alloy grain refining can increase the outside flux of alloying element, thus alloying element can be made under lower concentration can to form continuous print outer oxide layer, improve the antioxidant property of material.Making Nano surface technology is a kind of material surface deformation mechanism proposed recently, it utilizes the methods such as surperficial cal rolling process (SMGT) to make material surface metal that stream change occur, simultaneously form one deck at outside surface to be from outward appearance to inner essence followed successively by the gradient-structure of nanocrystalline, sub-micron crystal and micron crystalline substance and not destroy the integrity of material, therefore SMGT refiner material surface microstructure is utilized, be expected to make alloying element generation selective oxidation, quick formation outer oxide layer, improves the antioxidant property of material.
Summary of the invention
The object of this invention is to provide a kind of method improving low activation ferrite/martensite steel resistance to high temperature oxidation, make it meet the requirement of service condition.
The present invention specifically provides a kind of method improving low activation ferrite/martensite steel high temperature oxidation resistance, it is characterized in that: by forming on low activation steel surface the high temperature oxidation resistance being improved material by the nanocrystalline top layer formed.
The nanocrystalline size <100nm that low activation steel surface of the present invention is formed.
Present invention also offers the method preparing nanostructured surface laye on low activation ferrite/martensite steel surface; it is characterized in that: after low activation ferrite/martensite steel high tempering, carry out machining surface tool roll process (SMGT); can crystal grain thinning; increase the ratio of crystal boundary; improve Elements Diffusion speed; thus form protective oxide film fast, finally play oxidation resistant effect.
Surface cal rolling treatment process is that the spherical pressure head of wolfram varbide is along a certain amount of a of bar samples radial direction feeding
pafter along the length direction of sample with speed V
1motion, rod is with speed V simultaneously
2rotate.Processing parameter provided by the invention is: single amount of feed a
p=5-50 μm, pressure head rate of advance V
1=2-10mm/min, excellent velocity of rotation V
2=100-600rpm, repeating rolling layer is 1-10 time.Wherein optimizing technology parameters is: V
2/ V
1=20 ~ 100(is numeric ratio, wherein V herein
1unit is mm/min, V
2unit is rpm); a
p× repeat rolling layer≤80 μm.
The method preparing nanostructured surface laye on low activation ferrite/martensite steel surface of the present invention, it is characterized in that, low activation steel is 950 ~ 1050 DEG C of insulations shrend in 0.5 ~ 1.5 hour in surperficial cal rolling heat treating regime before treatment, 600 ~ 800 DEG C of insulations, 1 ~ 2 hour air cooling.
After surperficial cal rolling process, low activation steel is formed gradient-structure top layer, be followed successively by nanocrystalline, sub-micron crystal with the increase microtexture apart from treat surface distance and micron brilliant, this gradient-structure skin depth is 10-300 μm.
The invention has the advantages that:
1, the method for the invention significantly improves the high temperature oxidation resistance of material, make through SMGT than without SMGT material oxide film evenly, finer and close, therefore have more protectiveness.
2, can to solve low activation ferrite/martensite steel antioxidant property undesirable for the method for the invention, the problem that use temperature is lower.
3, the method for the invention can generate in club-shaped material surface working the gradient-structure that from outward appearance to inner essence microtexture is followed successively by nanocrystalline, sub-micron crystal and micron crystalline substance efficiently and stably.
Accompanying drawing explanation
Fig. 1 is surperficial cal rolling process (SMGT) Cross Section Morphology afterwards;
Fig. 2 is without SMGT sample (CG) and the XRD result through SMGT sample;
Fig. 3 be without SMGT sample (CG) and through SMGT sample through 600 DEG C oxidation 40h time weightening finish curve;
Fig. 4 is oxidized the surface topography after 510h without 600 DEG C, SMGT sample;
Fig. 5 is the surface topography after 600 DEG C, SMGT sample oxidation 510h;
Fig. 6 is oxidized the Cross Section Morphology after 510h without 600 DEG C, SMGT sample;
Fig. 7 is the Cross Section Morphology after 600 DEG C, SMGT sample oxidation 510h.
Embodiment
Embodiment 1
With 9CrWVTa low activation ferrite/martensite steel for research material illustrates the impact of the present invention on low activation steel high temperature oxidation resistance, its composition is as shown in table 1.The heat treating regime of material before SMGT is: 1050 DEG C of insulations shrend in 1 hour, 750 DEG C of insulations, 2 hours air coolings; Material after thermal treatment being cut into diameter is 20mm, and length is greater than the bar samples of 100mm, and to prepare a diameter at center, sample one end be the center hole of 4mm; Ready sample is fixed on lathe, first utilizes lathe tool by rod-like samples car to coaxial, then carry out SMGT with wolfram varbide pressure head; Treatment process is: single amount of feed a
p=20 μm, pressure head rate of advance V
1=6mm/min, excellent velocity of rotation V
2=300rpm, repeating rolling layer is 3 times; Finally make sample surfaces grain refining, thus significantly improve the antioxidant property of material.
Fig. 1 obtains one deck about 50 μm of thick gradient-structures after SMGT process; Fig. 2 is the XRD result of material before and after SMGT process, utilizes the broadening of diffraction peak to calculate and is about 20nm through SMGT process rear surface grain-size; Weightening finish curve when Fig. 3 is 600 DEG C of oxidation 40h, as seen from the figure, after SMGT process, the oxidation weight gain of material is starkly lower than non-SMGT process sample, and visible SMGT can significantly improve the antioxidant property of material.Fig. 4 is after 600 DEG C of oxidation 510h, without the surperficial macro morphology of SMGT process sample, Fig. 5 is after 600 DEG C of oxidation 510h, through the surperficial macro morphology of SMGT process sample, more known, SMGT process rear surface oxide film is complete, and there is crackle without SMGT treat surface oxide film, known, the oxide film formed after SMGT process has good mechanical property, thus keeps the integrity of oxide film.Fig. 6 is the sample Cross Section Morphology after 600 DEG C of oxidation 510h without SMGT process, and its oxidated layer thickness is about 40 μm as seen from the figure, and zone of oxidation is more loose, and local there occurs internal oxidition.Fig. 7 is the sample Cross Section Morphology after 600 DEG C of oxidation 510h through SMGT process, and as seen from the figure, oxidated layer thickness is about 500nm, and zone of oxidation is compact and complete.Significantly improve high temperature oxidation resistance as seen.
The composition (mass percent %) of table 1 9CrWVTa low activation ferrite/martensite steel
Embodiment 2
The thermal treatment process of starting materials with embodiment 1, SMGT treatment process is: single amount of feed a
p=20 μm, pressure head rate of advance V
1=2mm/min, excellent velocity of rotation V
2=300rpm, repeating rolling layer is 3 times; After nanometer, the crystal particle scale of sample surfaces is 30nm, but bits appear falling in sample surfaces, and namely surface is destroyed; Through 600 DEG C of oxidation 500h, increase compared to the weightening finish of experimental example 1, SMGT sample, and oxidated layer thickness increases, zone of oxidation is more loose, and therefore under this technique, SMGT is less on antioxidant property impact.
Embodiment 3
The thermal treatment process of starting materials with embodiment 1, SMGT treatment process is: single amount of feed a
p=2 μm of pressure head rate of advance V
1=15mm/min, excellent velocity of rotation V
2=300rpm, repeating rolling layer is 1 time; After process, sample surfaces does not form nanometer gradient structure; Through 600 DEG C of oxidation 500h, increase weight compared to experimental example 1, SMGT sample and CG sample, oxidated layer thickness is close, therefore under this technique, SMGT cannot improve the antioxidant property of material.
Above-described embodiment, only for technical conceive of the present invention and feature are described, its object is to person skilled in the art can be understood content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences done according to spirit of the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (7)
1. improve a method for low activation ferrite/martensite steel high temperature oxidation resistance, it is characterized in that: by forming on low activation steel surface the high temperature oxidation resistance being improved material by the nanocrystalline top layer formed.
2. according to the method improving low activation ferrite/martensite steel high temperature oxidation resistance described in claim 1, it is characterized in that: the nanocrystalline size <100nm that described low activation steel surface is formed.
3. prepare a method for nanostructured surface laye on low activation ferrite/martensite steel surface, it is characterized in that: after low activation ferrite/martensite steel high tempering, carry out machining surface tool roll process (SMGT).
4., according to the method preparing nanostructured surface laye described in claim 3 on low activation ferrite/martensite steel surface, it is characterized in that: surperficial cal rolling treatment process is that the spherical pressure head of wolfram varbide is along a certain amount of a of bar samples radial direction feeding
pafter along the length direction of sample with speed V
1motion, rod is with speed V simultaneously
2rotate; Processing parameter is: single amount of feed a
p=5-50 μm, pressure head rate of advance V
1=2-10mm/min, excellent velocity of rotation V
2=100-600rpm, repeating rolling layer is 1-10 time.
5., according to the method preparing nanostructured surface laye described in claim 4 on low activation ferrite/martensite steel surface, it is characterized in that: V
2/ V
1=20 ~ 100; a
p× repeat rolling layer≤80 μm.
6. according to the method preparing nanostructured surface laye described in claim 4 or 5 on low activation ferrite/martensite steel surface, it is characterized in that, low activation steel in surperficial cal rolling heat treating regime before treatment is: 950 ~ 1050 DEG C of insulations shrend in 0.5 ~ 1.5 hour, 600 ~ 800 DEG C of insulations, 1 ~ 2 hour air cooling.
7. according to the method preparing nanostructured surface laye described in claim 4 or 5 on low activation ferrite/martensite steel surface, it is characterized in that: after surperficial cal rolling process, low activation steel is formed gradient-structure top layer, be followed successively by nanocrystalline, sub-micron crystal with the increase microtexture apart from treat surface distance and micron brilliant, this gradient-structure skin depth is 10-300 μm.
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Cited By (4)
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| CN105695904A (en) * | 2016-02-02 | 2016-06-22 | 西安建筑科技大学 | Super-refining method for low-melting-point metal ring-direction grinding surface and device realizing super-refining method |
| CN106148659A (en) * | 2015-04-17 | 2016-11-23 | 中国科学院金属研究所 | A kind of preparation technology of high-strength plasticity Ultra-fine Grained low activation ferrite/martensite steel |
| CN106367572A (en) * | 2016-09-08 | 2017-02-01 | 中国科学院金属研究所 | Method for improving lead bismuth alloy corrosion resistance of nuclear power structural material |
| CN111593265A (en) * | 2020-06-09 | 2020-08-28 | 西安建筑科技大学 | Nanostructured low-activation martensitic steel and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106148659A (en) * | 2015-04-17 | 2016-11-23 | 中国科学院金属研究所 | A kind of preparation technology of high-strength plasticity Ultra-fine Grained low activation ferrite/martensite steel |
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| CN105695904B (en) * | 2016-02-02 | 2018-01-23 | 西安建筑科技大学 | A kind of low-melting-point metal ring rolles over rub surface fine method and its device |
| CN106367572A (en) * | 2016-09-08 | 2017-02-01 | 中国科学院金属研究所 | Method for improving lead bismuth alloy corrosion resistance of nuclear power structural material |
| CN111593265A (en) * | 2020-06-09 | 2020-08-28 | 西安建筑科技大学 | Nanostructured low-activation martensitic steel and preparation method thereof |
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Application publication date: 20150114 |