CN101774012A - Preparation method for forming Ti2O3 nano particles in molten steel - Google Patents
Preparation method for forming Ti2O3 nano particles in molten steel Download PDFInfo
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- CN101774012A CN101774012A CN201010034185A CN201010034185A CN101774012A CN 101774012 A CN101774012 A CN 101774012A CN 201010034185 A CN201010034185 A CN 201010034185A CN 201010034185 A CN201010034185 A CN 201010034185A CN 101774012 A CN101774012 A CN 101774012A
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Abstract
The invention belongs to the field of steel material, in particular to a preparation method for forming Ti2O3 nano particles in molten steel. The method has the following characteristics that: Fe-Ti alloy wires are added in molten low-carbon steel or low-carbon alloy steel with the oxygen concentration of less than 100PPm, so that molten steel containing O and Ti is obtained; since the alloying elements Ti and O of precipitated phase Ti2O3 higher than the melting point of matrix alloy are contained, the solubility of Ti and O reduces with the decrease of the temperature, the high cooling speed can form high supercooling degree, meanwhile, the melt can form the high linear rate of flow in the process of solidification, and thereby solidified alloy strengthened by dispersed and precipitated nano Ti2O3 is obtained. The invention has the following advantages that: nano Ti2O3 dispersed phase can be directly formed in the solidified alloy, and thereby the strength of the alloy is enhanced under the premise that the plasticity and toughness of the alloy are nearly kept unchanged.
Description
Technical field
The invention belongs to field of iron and steel, relate to a kind of nanometer Ti that in molten steel, forms
2O
3The preparation method of particle.
Background technology
Compare with nanometer reguline metal material, nano particle dispersion-strengthened metal material can keep the alloy percentage elongation, intensity with alloy increases substantially simultaneously, and strengthening effect be better than employed micron order and submicron order on traditional steel and iron industry second mutually particle dispersion strengthen, the research that nano-diffusion is strengthened iron and steel mutually becomes focus in recent years.Nano reinforcement not only can increase substantially the intensity of structural steel, can also improve the high temperature creep property of alloy.The nano reinforcement technology has important use for wide spectrums such as automobile industry, shipbuilding industry, power industries with steel and is worth.
Form nano reinforcement in iron and steel, reported method mainly contains in recent years: MA/ODS or MA/CDS method, distortion heat treating process.MA/ODS or MA/CDS method are that the several metal powder is mixed in high energy ball mill, carry out pressing and fragmentation repeatedly, and processes such as application machine alloying realize that the even dispersion of alloying and oxide or carbide particle distributes.This method is to release first the sixties from eighties of last century, because the material that this method is produced has good high-temperature behavior, is still the focus of research at present.Utilize MA/ODS or MA/CDS preparation, generally believe process complexity, cost height.Another kind method is distortion heat treatment, and distortion comprises thermal deformation and cold deformation, and the deformation process by pressure processing has formed a large amount of dislocations and room in steel, helps separating out of nano-diffusion phase in the follow-up heat treatment process.For containing the Ti steel by follow-up distortion heat treatment, can obtain nitride, carbide or the carbonitride disperse precipitated phase of Ti, different with the distortion Technology for Heating Processing according to alloying component, the precipitated phase kind has difference, mean particle size is also different, does not wait to the hundreds of nanometer from 10 nanometers.For example composition (wt.%) is the C that contains of Fe-1.5Mn-(0.1-0.2) Mo-(0.065-0.085) Ti-(0.07-0.09) Nb-(0.0005-0.0010) B-0.06C, the steel of N is by being heated to 1200 ℃ with steel with the rate of heat addition of 1.5-2 ℃/s in vacuum drying oven, then through 870 ℃ of-970 ℃ of deformation processing, last air cooling is to room temperature, can form carbide and nitride [the R D K Misra of several nanometers to 500 nanometer titaniums, H Nathani, J E Hartmann, FSiciliano.Microstructural evolution in a new 770MPa hot rolled Nb-Timicroalloyed steel, Materials Science and Engineering A 394 (2005) 339-352].Article [S W Ooi, G Fourlaris.A comparative study of precipitationeffects in Ti only and Ti-V Ultra Low Carbon (ULC) strip steels.MaterialsCharacterization 56 (2006) 214-226] in point out: composition is 0.0025wt%C, 0.0038wt%N, 0.0030wt%N, 0.0200wt%Al, 0.1600wt%Mn, 0.0120wt%P, 0.0260wt%Ti, 0.0030wt%Nb, the ultra-low carbon steel of 0.0010wt%V after the cold rolling and annealing, has formed the nitride and the carbide of nano grade titanium through 80% distortion.
The Ti nanoscale hardening constituent that contains that the present method of using alloy melting obtains in steel mainly is nitride or carbonitride, and generally needing to be out of shape heat treatment to solidified superalloy could obtain; And directly solidify way by alloy melting, in iron and steel, obtain nano-strengthening phase Ti
2O
3The also rarely seen report of particle.
Summary of the invention
The present invention seeks to when alloy melting, to add nano-strengthening phase Ti
2O
3Forming element Ti, O, in molten steel, form stabilized nano Ti
2O
3Particle is solidifying back acquisition nano particle Ti
2O
3The steel alloy of dispersion-strengtherning.
The inventor in the last few years, to separating out of nanophase in the alloy graining process, carried out deep basic research, part Study the results are shown in [Zidong Wang, Xuewen Wang, QiangsongWang, I Shih and J J Xu.Fabrication of a nanocomposite from situ ironnanoparticle reinforced copper alloy, Nanotechnology, 2009,20:075605].The preliminary conclusion that we obtain is: 1) high-melting-point precipitated phase atom is dissolved in the alloy melt that forms in the low-melting-point metal, its solubility reduces and reduces along with temperature, from the pouring temperature to the setting temperature, the fusing point of relative precipitated phase, precipitated phase has obtained very big supercooling degree, the forming core radius is minimum, can form the nano level particle of separating out; 2) the high-melting-point precipitated phase atomic concentration in the melt can not be too high, avoids nano particle to grow up.These two is to obtain nanometer Ti
2O
3The theoretical foundation of dispersed particle-strengthened steel alloy; 3) in the process of setting, under the melt flow field effect of big flow velocity, help obtaining the stabilized nano precipitated phase, reduce and avoid the formation of thick precipitated phase in the alloy structure.
A kind of nanometer Ti that in molten steel, forms
2O
3The preparation method of particle at first is the steel alloy melt that preparation contains nanometer precipitated phase element ti, O, it is characterized in that adding in containing the molten steel that O concentration is 5～100PPm
Fe～(1～15) wt.%Ti alloy silk, solidify (greater than 500K/min) with cooling velocity faster then.In the process of setting, contain the precipitated phase Ti that is higher than the matrix alloy fusing point in the melt
2O
3Element ti, O, along with temperature decline Ti, O solubility descend, form nanometer Ti
2O
3The casting alloy of precipitated phase.
Alloy composition (mass percent): 0.01～0.25wt.%C, 0～0.55wt.%Si, 0.2～1wt.%Mn, 0～0.04wt.%P, 0～0.05wt.%S, 0～5wt.%Cr, 0～5wt.%Ni, 0～1wt.%Mo, 0.01～1wt.%Ti, 0.0005～0.01wt.% (are equivalent to 5～100PPm) O, surplus Fe.
Technical process of the present invention:
1) alloy melting under air atmosphere;
2) steel is all after the fusing, after 50～100 ℃ of heat, treat liquid level stabilizing after, after oxygen content reaches 0～100PPm in measuring molten steel, add Ti with the form of Fe-Ti alloy silk, should be 0.01～1wt.%Ti through measuring and calculating Ti addition;
3) treat the dissolving of Fe-Ti alloy, cast behind the insulation 5-20min;
4) adopt centrifugal casting or cast under the electromagnetic agitation situation, the linear velocity that molten metal flows in the casting solidification process is not less than 1.7/s;
5) cooling velocity in the control process of setting is not less than 500 ℃/min;
6) heterogeneous microstructure of solidified superalloy is analyzed.
Advantage of the present invention is:
Obtain nanometer Ti
2O
3Dispersed particle-strengthened solidified steel alloy structure helps keeping improving the intensity of alloy under the constant substantially prerequisite of alloy plasticity and toughness.
The specific embodiment
Embodiment 1
Carry out melting under argon shield atmosphere, after steel all melted, after 1600 ℃ of heat, the chemical composition of steel alloy and mass percent are: C was 0.08%, and Si is 0.36%, and Mn is 0.9%, and P is 0.0078%, and S is 0.0004%, and surplus is Fe; After treating the alloy liquid level stabilizing, oxygen content reaches 10PPm in measuring molten steel, choosing Ti content and be by percentage to the quality 5% Fe-Ti alloy silk, is that the Fe-Al alloy silk of 3mm joins and makes in the molten steel that the mass percent of Ti reaches 0.06% in the molten steel with wire feeder with diameter.After treating the dissolving of Fe-Ti alloy, beginning cast behind the 10-15min behind the insulation 1-2min under 1580～1600 ℃.Be coated with cast iron steel ingot mould casting, the centrifugal casting of ceramic coating in the employing, centrifugal rotational speed is 250 commentaries on classics/min, and the metal liquid stream linear rate of flow is about 3m/s～8m/s; In process of setting,, guarantee that molten steel is not less than 500 ℃/min by the cooling velocity that liquid state becomes in the solid-state process at cast iron mold outer surface water spray.The temperature of unpacking that arrives to be cooled is opened metal pattern, takes out foundry goods, obtains nanometer Ti
2O
3The solidified superalloy of particle strengthening.Use a transmission electron microscopy and an emission microscopic analysis technology, the microscopic structure of solidified superalloy is carried out quality analysis, can find a large amount of 10～200 nanometer Ti
2O
3Particle dispersion is distributed on the alloy substrate.
Embodiment 2
Under air atmosphere, carry out melting, maximum temperature can be superheated to 1600 ℃, after steel all melts, after 50～100 ℃ of heat, the chemical composition and the mass percent of steel alloy choosing are: C:0.01%, Si:0.16%, Mn:0.47%, P:0.01%, S:0.01%, Cr:0.5%, Ni:0.5%, Mo:0.6%, surplus Fe; After treating the alloy liquid level stabilizing, oxygen content reaches 90PPm in measuring molten steel, choosing Ti content and be by percentage to the quality 10% Fe-Ti alloy silk, is that the Fe-Ti alloy silk of 2mm joins and makes in the molten steel that the mass percent of Ti reaches 0.3% in the molten steel with wire feeder with diameter.After treating the dissolving of Fe-Ti alloy, after being incubated 10-15min under 1570～1590 ℃, use the continuous cast method block, pour about 1550 ℃ of the temperature of molten steel in the crystallizer into, the molten steel surface is added with covering slag, and the solidification front molten metal is added with electromagnetic mixing apparatus, impel flowing of melt, about 10m/s～the 20m/s of linear velocity that flows, the about 500 ℃/min of continuous casting and solidifying cooling velocity, continuous casting steel billet thickness 70mm; Obtain nanometer Ti
2O
3The slab of particle strengthening.Use a transmission electron microscopy and an emission microscopic analysis technology, the microscopic structure of slab is carried out quality analysis, can find a large amount of 10～200 nanometer Ti
2O
3Particle dispersion is distributed on the alloy substrate.
Claims (2)
1. one kind forms nanometer Ti in molten steel
2O
3The preparation method of particle, it is characterized in that being no more than in the molten steel of the mild steel of 100PPm or low-carbon alloy steel at oxygen concentration, add Fe-1～15wt.%Ti alloy silk, acquisition contains the molten steel of O, Ti, and in the casting cycle, melt forms mobile, and melt is to be not less than the mobile type that fills of 1.7m/s linear velocity; The cooling velocity that is not less than 500K/min in process of setting is become solid-state by liquid state, form nanometer Ti
2O
3Dispersed particle-strengthened steel alloy.
2. a kind of nanometer Ti that in molten steel, forms as claimed in claim 1
2O
3The preparation method of particle, it is characterized in that mild steel or low-carbon alloy steel chemical analysis are: 0.01～0.25wt.%C, 0～0.55wt.%Si, 0.2～1wt.%Mn, 0～0.04wt.%P, 0～0.05wt.%S, 0～5wt.%Cr, 0～5wt.%Ni, 0～1wt.%Mo, 0.01～1wt.%Ti, 0.0005～0.01wt.%O, surplus Fe.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103484762A (en) * | 2013-09-10 | 2014-01-01 | 北京科技大学 | Preparation method of Ti5O9 nanoparticles formed in plain carbon steel |
| CN103495720A (en) * | 2013-09-10 | 2014-01-08 | 北京科技大学 | Method for manufacturing in-situ nano-particle strengthening Q195 steel |
| CN107824771A (en) * | 2017-11-13 | 2018-03-23 | 北京科技大学 | A kind of method that melt casting process prepares oxide dispersion intensifying F/M steel |
| CN108998729A (en) * | 2018-08-06 | 2018-12-14 | 北京科技大学 | A kind of high strength steel and preparation method thereof |
| CN113249654A (en) * | 2021-06-11 | 2021-08-13 | 北京科技大学 | In-situ nanoparticle reinforced ultrahigh-strength steel for ocean engineering and preparation method thereof |
-
2010
- 2010-01-15 CN CN201010034185A patent/CN101774012A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103484762A (en) * | 2013-09-10 | 2014-01-01 | 北京科技大学 | Preparation method of Ti5O9 nanoparticles formed in plain carbon steel |
| CN103495720A (en) * | 2013-09-10 | 2014-01-08 | 北京科技大学 | Method for manufacturing in-situ nano-particle strengthening Q195 steel |
| CN103495720B (en) * | 2013-09-10 | 2016-04-27 | 北京科技大学 | A kind of method preparing in-situ nano particle strengthening Q195 steel |
| CN107824771A (en) * | 2017-11-13 | 2018-03-23 | 北京科技大学 | A kind of method that melt casting process prepares oxide dispersion intensifying F/M steel |
| CN107824771B (en) * | 2017-11-13 | 2019-01-15 | 北京科技大学 | A kind of method that melt casting process prepares oxide dispersion intensifying F/M steel |
| US11203792B2 (en) | 2017-11-13 | 2021-12-21 | University Of Science And Technology Beijing | Method for preparing oxide dispersion strengthening F/M steel using smelting and casting process |
| CN108998729A (en) * | 2018-08-06 | 2018-12-14 | 北京科技大学 | A kind of high strength steel and preparation method thereof |
| CN113249654A (en) * | 2021-06-11 | 2021-08-13 | 北京科技大学 | In-situ nanoparticle reinforced ultrahigh-strength steel for ocean engineering and preparation method thereof |
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Open date: 20100714 |