CN102127713B - Oxide dispersion-strengthening ferrite steel with bicrystal structure and production method thereof - Google Patents
Oxide dispersion-strengthening ferrite steel with bicrystal structure and production method thereof Download PDFInfo
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- CN102127713B CN102127713B CN2011100424518A CN201110042451A CN102127713B CN 102127713 B CN102127713 B CN 102127713B CN 2011100424518 A CN2011100424518 A CN 2011100424518A CN 201110042451 A CN201110042451 A CN 201110042451A CN 102127713 B CN102127713 B CN 102127713B
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- oxide dispersion
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- ferrite steel
- strengthening ferrite
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Abstract
The invention relates to oxide dispersion-strengthening ferrite steel with a bicrystal structure, compirisng the following components of Cr, W, Ti, Y2O3 and the balance of Fe. A preparation method of the oxide dispersion-strengthening ferrite steel with the bicrystal structure comprises the following steps of: uniformly mixing Fe-Cr-W prealloy powder and ball milled powder according to a certain proportion; placing the mixed powder into a steel capsule for degassing and seal welding; then thermally canned-forging, solidifying and molding; and carrying out thermal treatment. The ferrite steel with excellent mechanical property at room temperature and high temperature can be produced through mixing powders in different proportions and controlling on solidifying and molding as well as the following thermal treatment. Oxide dispersion-strengthening alloy produced by the invention has the characteristic of the bicrystal structure, and the structure can simultaneously give the alloy higher strength and excellent toughness. The efficiency for producing the oxide dispersion-strengthening ferrite steel can be increased effectively, the process cost can be greatly saved, and the oxide dispersion-strengthening ferrite steel is beneficial to industrial production.
Description
Technical field
The present invention relates to the excellent oxide dispersion strengthening ferrite steel of high-temperature behavior and be equipped with technical field.A kind of twin crystal structure oxide dispersion strengthening ferrite steel and preparation method particularly are provided, have belonged to technical field of metal material preparation.
Background technology
The oxide dispersion strengthening ferrite steel can be used as the fb cage walls and uses material, fusion reactor first wall material, thermal power generation material and engine chamber material because its superior anti-irradiation hangs down swelling and high temperature creep property.Its microstructure characteristic is mainly the Y-Ti-O group bunch of 2-3nm in ultra-fine crystalline substance and the matrix of nanoscale and the Y of several to dozens of nanometers
2Ti
2O
7, Y
2TiO
5Reach other oxide compounds as dispersion-strengthened particle pinning crystal boundary and dislocation, higher intensity of alloy and creep property are given in refined crystalline strengthening and dispersion-strengthened acting in conjunction.Through the prepared by mechanical alloy powder; The oxide dispersion strengthening ferrite steel that the fixed moulding of hot extrusion or hot isostatic pressing obtains, toughness is lower usually, room temperature uniform elongation less than 5%; Can have influence on the properties for follow of alloy thus, and the unexpected fracture failure in the military service process.
There is the researchist to attempt, nanocrystal regional area generation crystal grain is grown up unusually, thereby obtain the crystal grain of bomodal size distribution, improve the toughness of alloy through controlling heat treated condition.Eiselt is through [the Eiselt Ch Ch of the vacuum annealing after cold rolling; Klimenkov M; Lindau R, et al.Journal ofNuclear Materials, 2009; 385 (2): 231～235.], 20-500nm and 1-8 μ m low-activity oxide dispersion strengthening ferrite/martensitic steel (RAFM ODS-Eurofer) have been obtained having simultaneously.But the twin crystal structure that this method obtains is extremely inhomogeneous, and the abnormal grain growth process is wayward.
Summary of the invention
The object of the present invention is to provide a kind of preparation not only to possess HS but also possess the method for superior flexible oxide dispersion strengthening ferrite steel; The alloy that this method is prepared has the twin crystal grain size distribution, and has the strengthening phase particle that disperse distributes in the matrix.
A kind of twin crystal structure oxide dispersion strengthening ferrite of the present invention steel, by weight percentage, form by following component:
Cr?14-16％，
W?1％-3％，
Ti?0.3-1.0％，
Y
2O
30.3-1.0%, surplus is Fe.
The preparation method of a kind of twin crystal structure oxide dispersion strengthening ferrite of the present invention steel comprises the steps:
The first step: the preparation of ball-milled powder
The equal granularity of making even is that-200 purpose Fe-Cr-W powder and mean particle size are-325 purpose TiH
2, YH
2Powder and mean particle size are the Fe of 30nm
2O
3, prepare burden by following weight percent:
YH
2：0.3-0.6wt.％，
TiH
2：0.3-1.0wt.％，
Fe
2O
30.2-0.5wt.%, surplus is Fe-Cr-W;
Resulting mixed powder is carried out ball milling under protection of inert gas atmosphere, obtain ball-milled powder;
Second step: the preparation of ferritic steel
The equal granularity of making even for the ball-milled powder of-200 purpose Fe-Cr-W powder and the first step gained by mass ratio (2-4): 1 mix after, the Steel Capsule of packing into, the degassing, soldering and sealing are carried out the jacket heat forged, deflection 70%-90% in 900 ℃-1100 ℃; Sample after the forging is at 1000 ℃-1200 ℃ insulation 1-3h, and air cooling promptly makes twin crystal structure oxide dispersion strengthening ferrite steel then.
Among the preparation method of a kind of twin crystal structure oxide dispersion strengthening ferrite of the present invention steel, said Fe-Cr-W powder is prepared through inert gas atomizer by the Fe-14Cr-3W mother alloy; Said Fe-14Cr-3W mother alloy is processed for twice by the melting in the high frequency vacuum induction furnace of Fe, Cr, W master alloy.
Among the preparation method of a kind of twin crystal structure oxide dispersion strengthening ferrite of the present invention steel, said ball milling adopts mechanical ball milling, ball-to-powder weight ratio (6-8): 1, and rotating speed (250-350) r/min, ball milling time (24-48) h.
Among the preparation method of a kind of twin crystal structure oxide dispersion strengthening ferrite of the present invention steel, said rare gas element is selected from a kind of in argon gas, the nitrogen.
The preparation method of a kind of twin crystal structure oxide dispersion strengthening ferrite of the present invention steel, the twin crystal structure oxide dispersion strengthening ferrite steel of preparation, fine grained region average grain size scope is 200-500nm, coarse grain zone average grain size scope is 10-15 μ m.
The preparation method of a kind of twin crystal structure oxide dispersion strengthening ferrite of the present invention steel, the second phase particle that exists disperse to distribute in the twin crystal structure oxide dispersion strengthening ferrite steel of preparation, and the fine grained texture that produces by ball-milled powder.
The present invention is owing to adopt said components proportioning and process method; Utilize powder metallurgy process; Through mixing prealloy and ball-milled powder, hot consolidation moulding and thermal treatment are that the interpolation grain-size is micron-sized pre-alloyed powder in the nano level ball-milled powder in grain-size; Then carry out powder curing, directly obtain material with grain-size bomodal size distribution.The twin crystal structure oxide dispersion strengthening ferrite steel that obtains by this method, nanoscale crystal grain and micro-meter scale crystal grain are evenly distributed, thereby have improved the toughness of alloy significantly, and effectively balance the intensity and the toughness of alloy.In addition, can effectively reduce the amount of finish of ball-milled powder in the alloy course of processing, increase the turnout of alloy unit time, improve production efficiency; Fixed moulding has simultaneously replaced technologies such as traditional powder jacket hot extrusion or powder jacket hot isostatic pressing with the powder canned forging, thereby has practiced thrift production cost, effectively improves alloy toughness.Compared with prior art, the present invention has following advantage.
1, the oxide-dispersed alloy of the present invention's preparation has the twin crystal structure characteristic, and this structure can be given higher intensity of alloy and superior toughness simultaneously.
2, the present invention has greatly improved the efficient of preparation oxide dispersion strengthening ferrite steel, has practiced thrift the technology cost greatly.
Description of drawings
Accompanying drawing 1 is macrostructure's pattern of the alloy with twin crystal structure of the embodiment of the invention 1 preparation.
Accompanying drawing 2 is a fine grained region tissue topography in the accompanying drawing 1
Accompanying drawing 3 is a dispersion-strengthened particulate TEM pattern in the accompanying drawing 1
In the accompanying drawing 1, obviously can find out in the alloy of embodiment 1 preparation to have the twin crystal grain size distribution, be respectively the fine grained region and the coarse grain zone that is of a size of 5～25 μ m that is of a size of 50～500nm, can effectively improve alloy toughness.
In the accompanying drawing 2, shown that tissue is amplified in the part of the fine grained region that is of a size of 50～500nm in the accompanying drawing 1.
The dispersion-strengthened particle of the second phase nanoscale can be obviously found out in the accompanying drawing 3, alloy strength can be effectively improved.
Embodiment
Embodiment 1
Master alloy induction melting in the high frequency vacuum induction furnace of Fe, Cr, W is processed the Fe-14Cr-3W mother alloy for twice, prepare the Fe-Cr-W pre-alloyed powder through inert gas atomizer.In the Fe-Cr-W pre-alloyed powder, add 0.3wt%TiH
2, 0.3wt%YH
2, 0.2wt%Fe
2O
3, Fe-Cr-W pre-alloyed powder granularity is-200 orders, TiH
2And YH
2Powder size is-325 orders, Fe
2O
3Mean particle size is 30nm, in planetary ball mill, carries out mechanical ball milling under the argon shield atmosphere, ball milling time 24h, and rotating speed 350r/min, ball-to-powder weight ratio 6: 1 obtains ball-milled powder.With Fe-Cr-W pre-alloyed powder and ball-milled powder ratio uniform mixing according to 3: 1, mixed powder is packed into after Steel Capsule, the degassing, soldering and sealing handle, carry out the fixed moulding of hot canned forging at 1000 ℃, at 1000 ℃ of annealing 1h, air coolings then.Can obtain fine grained region average grain size scope is 200-500nm, and coarse grain zone average grain size scope is the alloy of 10-15 μ m; Alloy at room temperature tensile strength can reach 1216.7MPa, and unit elongation is 12.3%.
Embodiment 2
Than embodiment 1, add 0.7wt%TiH
2, 0.5wt%YH
2, 0.4wt%Fe
2O
3, surplus is carried out ball milling for the Fe-Cr-W powder, ball milling time 48h, rotating speed 250r/min, ball-to-powder weight ratio 7: 1.With Fe-Cr-W pre-alloyed powder and ball-milled powder ratio uniform mixing according to 2: 1, mixed powder is packed into after Steel Capsule, the degassing, soldering and sealing handle, carry out the fixed moulding of hot canned forging at 900 ℃, at 1100 ℃ of annealing 1h, air coolings then.The microstructure characteristic of alloy is obviously difference not, and the fine grained region ratio increases, and the alloy grain size increases slightly.Alloy at room temperature tensile strength is 1172.6MPa, and unit elongation is 11.32%.
Embodiment 3
Than embodiment 1, add 1.0wt%TiH
2, 0.6wt%YH
2, 0.5wt%Fe
20
3, surplus is carried out ball milling for the Fe-Cr-W powder, ball milling time 36h, rotating speed 300r/min, ball-to-powder weight ratio 8: 1.With Fe-Cr-W pre-alloyed powder and ball-milled powder ratio uniform mixing according to 4: 1, mixed powder is packed into after Steel Capsule, the degassing, soldering and sealing handle, carry out the fixed moulding of hot canned forging at 1100 ℃, at 1200 ℃ of annealing 1h, air coolings then.。Alloy at room temperature tensile strength is 1103.3MPa, and unit elongation is 13.8%.
Claims (7)
1. twin crystal structure oxide dispersion strengthening ferrite steel, fine grained region average grain size scope is 200-500nm, coarse grain zone average grain size scope is 10-15 μ m, by weight percentage, is made up of following component:
Cr?14-16%，
W?1%-3%，
Ti?0.3-1.0%，
Y
2O
30.3-1.0%, surplus is Fe.
2. the preparation method of a twin crystal structure oxide dispersion strengthening ferrite steel according to claim 1 comprises the steps:
The first step: the preparation of ball-milled powder
The equal granularity of making even is that-200 purpose Fe-Cr-W powder and mean particle size are-325 purpose TiH
2, YH
2Powder and mean particle size are the Fe of 30nm
2O
3, prepare burden by following weight percent:
YH
2：0.3-0.6?wt.%，
TiH
2：0.3-1.0?wt.%，
Fe
2O
30.2-0.5 wt.%, surplus is Fe-Cr-W;
Resulting mixed powder is carried out ball milling under protection of inert gas atmosphere, obtain ball-milled powder;
Second step: the preparation of ferritic steel
The equal granularity of making even for the ball-milled powder of-200 purpose Fe-Cr-W powder and the first step gained by mass ratio (2-4): 1 mix after, the Steel Capsule of packing into, the degassing, soldering and sealing are carried out the jacket heat forged, deflection 70%-90% in 900 ℃-1100 ℃; Sample after the forging is at 1000 ℃-1200 ℃ insulation 1-3h, and air cooling promptly makes twin crystal structure oxide dispersion strengthening ferrite steel then.
3. the preparation method of twin crystal structure oxide dispersion strengthening ferrite steel according to claim 2 is characterized in that: said Fe-Cr-W powder is prepared through inert gas atomizer by the Fe-14Cr-3W mother alloy; Said Fe-14Cr-3W mother alloy is processed for twice by the melting in the high frequency vacuum induction furnace of Fe, Cr, W master alloy.
4. the preparation method of twin crystal structure oxide dispersion strengthening ferrite steel according to claim 3 is characterized in that: said ball milling adopts mechanical ball milling, ball-to-powder weight ratio (6-8): 1, and rotating speed (250-350) r/min, ball milling time (24-48) h.
5. the preparation method of twin crystal structure oxide dispersion strengthening ferrite steel according to claim 4 is characterized in that: said rare gas element is selected from a kind of in argon gas, the nitrogen.
6. the preparation method of twin crystal structure oxide dispersion strengthening ferrite steel according to claim 5; It is characterized in that: prepared twin crystal structure oxide dispersion strengthening ferrite steel fine grained region average grain size scope is 200-500nm, and coarse grain zone average grain size scope is 10-15 μ m.
7. the preparation method of twin crystal structure oxide dispersion strengthening ferrite steel according to claim 6; It is characterized in that: the second phase particle that exists disperse to distribute in the prepared twin crystal structure oxide dispersion strengthening ferrite steel, and the fine grained texture that produces by ball-milled powder.
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| RU2493282C2 (en) * | 2011-09-13 | 2013-09-20 | Государственная корпорация по атомной энергии "Росатом" | Method of steel production with strengthening nanoparticles |
| CN103374684A (en) * | 2012-04-16 | 2013-10-30 | 中国科学院合肥物质科学研究院 | Aluminum oxide containing dispersion strengthening ferrite steel and preparation method thereof |
| CN102994884B (en) * | 2012-12-03 | 2014-10-29 | 东北大学 | Efficient preparation method for nanostructure oxide dispersion strengthening steel |
| KR20150104348A (en) * | 2014-03-05 | 2015-09-15 | 한국원자력연구원 | Ferrite/martensitic oxide dispersion strengthened steel with excellent creep resistance and manufacturing method thereof |
| CN103966500B (en) * | 2014-05-22 | 2017-11-14 | 北京航空航天大学 | A kind of ODS high temperature alloys for adding composite oxides nano particle and preparation method thereof |
| CN104451225B (en) * | 2014-11-23 | 2016-08-10 | 北京科技大学 | A kind of method preparing double connectivity structure superalloy composite |
| CN106755729B (en) * | 2016-12-05 | 2018-08-28 | 东北大学 | A kind of RAFM steel nano reinforcement agent and its preparation and application |
| CN107541666B (en) * | 2017-09-08 | 2019-06-25 | 中国科学院合肥物质科学研究院 | A kind of preparation method of oxide dispersion intensifying steel |
| CN108950357B (en) * | 2018-07-27 | 2020-03-27 | 中南大学 | Multi-scale multiphase dispersion strengthening iron-based alloy and preparation and characterization method thereof |
| CN108907209B (en) * | 2018-07-27 | 2020-04-07 | 中南大学 | Oxide dispersion strengthening iron-based alloy powder and characterization method thereof |
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