CN101538674A - Method for preparing oxide dispersion strengthened austenitic stainless steel - Google Patents
Method for preparing oxide dispersion strengthened austenitic stainless steel Download PDFInfo
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- CN101538674A CN101538674A CN200910083638A CN200910083638A CN101538674A CN 101538674 A CN101538674 A CN 101538674A CN 200910083638 A CN200910083638 A CN 200910083638A CN 200910083638 A CN200910083638 A CN 200910083638A CN 101538674 A CN101538674 A CN 101538674A
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Abstract
The invention provides a method for preparing nitrogen-containing oxide dispersion strengthened austenitic stainless steel by using a mechanical alloying method. The method is characterized in that: pure metal element powder of Fe, Cr, Ni, W and Ti and nano Y2O3 powder are mixed according to a certain proportion, wherein the Cr is 17 to 19 percent, the Ni is 7 to 9 percent, the W is 1.5 to 2.5 percent, the Ti is 0.5 to 1.0 percent, the Y2O3 is 0.3 to 0.6 percent, and the balance is Fe; and the mixed powder is filled in a mill pot, high-purity nitrogen is filled into the mill pot after vacuumizing, and the mixed powder is milled for 30 to 120 hours which does not comprise stopping time in a planetary high-energy ball mill. The ball mill is stopped for 1 hour in every milling of 5 hours so as to prevent the temperature of the mill pot over-high. By controlling the intensity of the pressure of the ball milling atmosphere nitrogen and the ball milling time, the ODS austenitic stainless steel powder with different nitrogen contents can be obtained; and after the austenitic stainless steel powder is sintered, the nitrogen-containing ODS austenitic stainless steel can be formed. The austenitic stainless steel prepared by the method can realize solid solution strengthening and oxide dispersion strengthening of the nitrogen at the same time, and the service capability of the austenitic stainless steel under high-temperature environment can be improved to a great extent.
Description
Technical field:
The invention belongs to oxide dispersion intensifying (Oxide Dispersion Strengthened, ODS) powdered alloy preparing technical field, a kind of mechanical alloying by high-energy ball milling realization oxide compound, nitrogen element, pure metal powder particularly is provided, has obtained the method for subsphaeroidal nitrogenous ODS powder of stainless steel.
Background technology:
Austenitic stainless steel with its good comprehensive mechanical properties, good etch resistant properties, antioxidant property, easily advantage such as machine-shaping become the 4th generation nuclear power reactor, as one of candidate material of supercritical water cold dome fuel sheath.But the mechanical behavior under high temperature of austenitic stainless steel, high temperature creep-resisting ability can not satisfy its service requirements.The oxide particle dispersion-strengthened is the effective means that improves steel alloy mechanical behavior under high temperature, anti-irradiation ability, the ferrite/martensite steel of oxide dispersion intensifying becomes the research focus (to be seen: L.K.Mansur, A.F.Rowcliffe, R.K.Nanstad, S.J.Zinkle, W.R.Corwin, R.E.Stoller.Journal ofNuclear Materials 329-333 (2004) 166-172).But the application in austenitic stainless steel is also at the early-stage.Compare with strengthening phase in the conventional alloys such as carbide, intergranular, what dispersed oxide particle performance at high temperature will be stable is many; These disperses are distributed in oxide particle in the matrix can effectively improve alloy as the resistance of dislocation moving creep resisting ability and hot strength, in addition, disperse is distributed in the carrying out that oxide particle in the matrix can hinder recrystallization process, obtains stable grain-size easily.Dispersed oxide in the stainless steel communicates and often introduces by the method for mechanical alloying.Mechanical alloying mainly realizes by the mode of high-energy ball milling.Compare with other alloyage process, mechanical alloying has that cost is low, easy to operate, can realize advantages such as alloying under the normal temperature, and in ball grinder, can charge into different atmosphere, except that rare gas element, in mechanical milling process, can make the atom of gas participate in the solid state reaction that is taken place by the ball milling material; In addition, in raw material powder, add oxide particle, in mechanical milling process, the raw materials mixed powder in the high speed between ball and ball, ball and wall, ball and the powder, withstand shocks, shear, rub under the bump repeatedly and compress the effect of multiple power, experience extruding, cold welding and crushing process and then realization alloying repeatedly makes the disperse of fine oxide particulate be distributed in the matrix alloy.
In austenitic stainless steel, introduce nitrogen, can the stable austenite tissue, effectively improve intensity, toughness, the work hardening capacity of steel, make steel reach good combination of strength and toughness, and raising corrosion resistance nature, particularly anti-local corrosion performance is as intergranular corrosion resistance, pitting attack and crevice corrosion etc.Nitrogenous austenitic stainless steel has obtained the favor of various countries' researchers with its superior mechanical property and corrosion resisting property.Since the eighties in 20th century, started the upsurge of research nitrogenous austenitic stainless steel.Nitrogenous austenitic stainless steel can be divided into control nitrogen type (N content is 0.05-0.10wt%), middle nitrogen type (N content is 0.10-0.40wt%) and high nitrogen type (N content is higher than 0.40wt%) according to nitrogen content.The main method of preparation nitrogenous austenitic stainless steel has pressurized Induction Melting, pressurization plasma melting, pressurization electroslag melting, back-pressure casting etc. both at home and abroad.The common disadvantage of these methods is that equipment complexity, technology controlling and process difficulty, cost are too high.Powder metallurgy process begins to be applied to the research of nitrogen-contained stainless steel in recent years.Prepare nitrogen-contained stainless steel with method with melting and compare, powder metallurgy process has advantages such as equipment is simple, cost is low, security is good, easy realization.Wherein mechanical alloying is one of powder metallurgy process comparatively commonly used.
Summary of the invention:
The object of the present invention is to provide a kind of method for preparing nitrogenous ODS austenitic stainless steel with mechanical alloying method.Nitrogenous ODS austenitic stainless steel power composition with the mechanical alloying method preparation is even, obtains complete austenite structure under room temperature after 1100 ℃ of annealing.This method can realize the reinforcement of nitrogen element solid solution and the oxide dispersion intensifying (ODS) of austenitic stainless steel simultaneously.
The preparation technology that the present invention prepares nitrogenous ODS austenitic stainless steel is: a kind of method for preparing oxide dispersion strengthened austenitic stainless steel, its feature is with pure metal element powders and the nanometer Y of Fe, Cr, Ni, W, Ti
2O
3Powder is mixed in proportion, Cr:17-19% wherein, Ni:7-9%, W:1.5-2.5%, Ti:0.5-1.0%, Y
2O
3: 0.3-0.6%, surplus is Fe, in the ball grinder of packing into then, charges into high pure nitrogen after vacuumizing, and ball milling 30～120h in planetary high-energy ball mill does not comprise stop time, and every ball milling 5h shuts down 1h, and rotational speed of ball-mill is 380r/min, ratio of grinding media to material is 10: 1.In the high-energy ball milling process, each mixed powder is along with the prolongation of ball milling time realizes mechanical alloying.By changing the nitrogen-contained stainless steel powder that the ball milling time can obtain different nitrogen contents, by promptly getting nitrogenous ODS austenitic stainless steel behind the method sintering such as hot pressing or hot isostatic pressing.
Another technical scheme of the present invention is that above-mentioned high pure nitrogen pressure is 0--1.0atm, by changing the powder of stainless steel that nitrogen pressure can obtain different nitrogen contents.
Advantage of the present invention:
1. Zhi Bei nitrogenous ODS austenitic stainless steel power composition is even, and nitrogen content can change between 0-1.05%.By this process of mechanical alloying, can in austenitic stainless steel, realize the solution strengthening and the oxide dispersion intensifying (ODS) of nitrogen simultaneously, improve the mechanical behavior under high temperature and the corrosion resisting property of austenitic stainless steel.
2. Zhi Bei nitrogenous ODS austenitic stainless steel power granularity tiny (5-25 μ m), particle size distribution is narrow, and the gained powder particle has higher sphericity, is beneficial to and obtains higher density when sintering.
3. present device is simple, cost is low, easy to operate.
Description of drawings
Nitrogen content is with the variation of ball milling time under Figure 11 .0atm nitrogen pressure
The surface topography of ball milling 90h powder under Figure 21 .0atm nitrogen pressure
Fig. 3 hot pressed sintering ODS austenitic stainless steel bloom
Embodiment
Embodiment 1
Testing raw materials used is pure metal powder and the nanometer Y of Fe, Cr, Ni, W, Ti
2O
3Powder, the purity of used powder is all greater than 99.9%.Wherein, the granularity of Fe, Cr, Ni, Ti powder is-200 orders, and the mean particle size of W powder is 2 μ m, Y
2O
3The mean particle size of powder is 30nm.Above-mentioned powder is Fe-18Cr-8Ni-2W-1Ti-0.35Y by composition proportion
2O
3Weighing is put into ball grinder after mixing respectively, charges into nitrogen after vacuumizing, and nitrogen gas pressure is respectively 0atm (be vacuum, vacuum tightness is 5Pa), 0.5atm and 1.0atm.Ratio of grinding media to material is that 10: 1, rotating speed are 380r/min, and the ball milling time is controlled to be 30h, 60h, 90h, 120h.The employing infrared heat conduction method of gas pulse (ASTME1019-2003) of falling is surveyed the actual nitrogen content of powder.When fixedly the ball milling time was 60h, under the 0atm nitrogen pressure, the nitrogen content of powder was 0%, did not promptly have nitrogen to participate in the alloying of powder; When the nitrogen pressure that charges in the ball grinder was 0.5atm, the nitrogen content of powder was 0.52%; When the nitrogen pressure in the ball grinder was 1atm, the nitrogen content of powder was up to 0.85%.Charge into nitrogen pressure when being 1.0atm, the ball milling time lengthening is during to 120h, and nitrogen content is up to 1.05%.Under the 1.0atm nitrogen pressure, the nitrogen content behind the ball milling different time as shown in Figure 1.According to specific requirement, press size and ball milling time can obtain the powder of stainless steel of different nitrogen contents by the nitrogen that adjusting charges in the ball grinder, gained powder particle particle size distribution is narrow, and particle has higher sphericity as shown in Figure 2.Can obtain nitrogenous ODS austenitic stainless steel behind the powder hot-pressing sintering with mechanical alloying.As shown in Figure 3, be that 0.85% powder is an example with nitrogen content, at 1200 ℃, 80MPa under the hot pressing condition of insulation 2h, can obtain the nitrogenous ODS austenite stainless steel sample of relative density 98.5%.
Testing raw materials used is pure metal powder and the nanometer Y of Fe, Cr, Ni, W, Ti
2O
3Powder, the purity of used powder is all greater than 99.9%.Wherein, the granularity of Fe, Cr, Ni, Ti powder is-200 orders, and the mean particle size of W powder is 2 μ m, Y
2O
3The mean particle size of powder is 30nm.Above-mentioned powder is Fe-17.5Cr-7.5Ni-1.5W-0.5Ti-0.35Y by composition proportion
2O
3Weighing is put into ball grinder after mixing respectively, charges into nitrogen after vacuumizing, and charging into nitrogen gas pressure is 1.0atm.Ratio of grinding media to material is that 10: 1, rotating speed are 380r/min, be controlled to be that nitrogen content is 0.85% behind the 60h ball milling ball milling time, with the powder of mechanical alloying at 1200 ℃, 80MPa, carry out sintering under the hot pressing condition of insulation 2h, can obtain the nitrogenous ODS austenite stainless steel sample of relative density 98.2%.
Embodiment 3
Testing raw materials used is pure metal powder and the nanometer Y of Fe, Cr, Ni, W, Ti
2O
3Powder, the purity of used powder is all greater than 99.9%.Wherein, the granularity of Fe, Cr, Ni, Ti powder is-200 orders, and the mean particle size of W powder is 2 μ m, Y
2O
3The mean particle size of powder is 30nm.Above-mentioned powder is Fe-19Cr-8.5Ni-2.5W-1Ti-0.60Y by composition proportion
2O
3Put into ball grinder after weighing mixes respectively, carry out ball milling after vacuumizing, ratio of grinding media to material is that 10: 1, rotating speed are 380r/min, and the ball milling time is controlled to be 60h.At 1100 ℃, 200MPa under the hot isostatic pressing condition of insulation 3h, can obtain the ODS austenite stainless steel sample of relative density 98.8% with the powder of mechanical alloying.
Claims (2)
1. method for preparing oxide dispersion strengthened austenitic stainless steel, its feature is with pure metal element powders and the nanometer Y of Fe, Cr, Ni, W, Ti
2O
3Powder is mixed in proportion, Cr:17-19% wherein, Ni:7-9%, W:1.5-2.5%, Ti:0.5-1.0%, Y
2O
3: 0.3-0.6%, surplus is Fe, in the ball grinder of packing into then, charges into high pure nitrogen after vacuumizing, and ball milling 30～120h in planetary high-energy ball mill does not comprise stop time, and every ball milling 5h shuts down 1h.
2. according to the described a kind of method for preparing oxide dispersion strengthened austenitic stainless steel of claim 1, it is characterized in that described high pure nitrogen pressure is 0--1.0atm.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101886213A (en) * | 2010-06-30 | 2010-11-17 | 北京航空航天大学 | Ultra-disperse structure complex phase alloy steel and preparation method thereof |
| CN102277525A (en) * | 2011-08-23 | 2011-12-14 | 北京科技大学 | Method for preparing oxide dispersion reinforced stainless steel powder and stainless steel |
| WO2012016649A1 (en) * | 2010-08-02 | 2012-02-09 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Process for producing components which are made close to final shape from a dispersion-reinforced iron- or nickel-based alloy |
| CN102828097A (en) * | 2012-09-16 | 2012-12-19 | 北京科技大学 | Method for preparing nitrogen-contained ODS (oxide dispersion strengthened) nickel-free austenite alloy by mechanical alloying process |
| CN103060586A (en) * | 2013-01-15 | 2013-04-24 | 北京科技大学 | Preparation method for complex-shape niobium-based ODS (oxide dispersion strengthening) alloy |
| CN105238986A (en) * | 2014-07-11 | 2016-01-13 | 中国科学院金属研究所 | Method for preparing Cr-Y-O nanocluster oxide dispersion strengthening steel |
| CN105274445A (en) * | 2014-06-06 | 2016-01-27 | 中国科学院金属研究所 | Oxide-dispersion-strengthened low-activation steel and preparation method thereof |
| CN108838388A (en) * | 2018-07-13 | 2018-11-20 | 山东大学 | A kind of powder metallurgy austenitic stainless steel and preparation method thereof |
| CN109570508A (en) * | 2018-12-13 | 2019-04-05 | 北京科技大学 | The preparation method of the oxide dispersion strengthening ferrite steel of double grain size distributions |
-
2009
- 2009-05-06 CN CN200910083638A patent/CN101538674A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101886213A (en) * | 2010-06-30 | 2010-11-17 | 北京航空航天大学 | Ultra-disperse structure complex phase alloy steel and preparation method thereof |
| WO2012016649A1 (en) * | 2010-08-02 | 2012-02-09 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Process for producing components which are made close to final shape from a dispersion-reinforced iron- or nickel-based alloy |
| CN102277525A (en) * | 2011-08-23 | 2011-12-14 | 北京科技大学 | Method for preparing oxide dispersion reinforced stainless steel powder and stainless steel |
| CN102277525B (en) * | 2011-08-23 | 2012-12-05 | 北京科技大学 | Method for preparing oxide dispersion reinforced stainless steel powder and stainless steel |
| CN102828097A (en) * | 2012-09-16 | 2012-12-19 | 北京科技大学 | Method for preparing nitrogen-contained ODS (oxide dispersion strengthened) nickel-free austenite alloy by mechanical alloying process |
| CN103060586B (en) * | 2013-01-15 | 2014-09-17 | 北京科技大学 | Preparation method for complex-shape niobium-based ODS (oxide dispersion strengthening) alloy |
| CN103060586A (en) * | 2013-01-15 | 2013-04-24 | 北京科技大学 | Preparation method for complex-shape niobium-based ODS (oxide dispersion strengthening) alloy |
| CN105274445A (en) * | 2014-06-06 | 2016-01-27 | 中国科学院金属研究所 | Oxide-dispersion-strengthened low-activation steel and preparation method thereof |
| CN105274445B (en) * | 2014-06-06 | 2017-06-13 | 中国科学院金属研究所 | A kind of oxide dispersion intensifying low activation steel and preparation method thereof |
| CN105238986A (en) * | 2014-07-11 | 2016-01-13 | 中国科学院金属研究所 | Method for preparing Cr-Y-O nanocluster oxide dispersion strengthening steel |
| CN108838388A (en) * | 2018-07-13 | 2018-11-20 | 山东大学 | A kind of powder metallurgy austenitic stainless steel and preparation method thereof |
| CN109570508A (en) * | 2018-12-13 | 2019-04-05 | 北京科技大学 | The preparation method of the oxide dispersion strengthening ferrite steel of double grain size distributions |
| CN109570508B (en) * | 2018-12-13 | 2022-03-29 | 北京科技大学 | Preparation method of oxide dispersion strengthened ferrite steel with double-grain size distribution |
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