CN102828097A - Method for preparing nitrogen-contained ODS (oxide dispersion strengthened) nickel-free austenite alloy by mechanical alloying process - Google Patents
Method for preparing nitrogen-contained ODS (oxide dispersion strengthened) nickel-free austenite alloy by mechanical alloying process Download PDFInfo
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Abstract
本发明用机械合金化法制备含氮ODS无镍奥氏体合金的方法，以Fe、Cr、Mn、W、Ti、Al的纯金属元素粉末与纳米Y2O3粉末按Cr：17-20%，Mn：18-22%，W：1.5-2.5%，Al：2-4%，Ti：0.5-1.0%，Y2O3：0.3-0.6%，余量为Fe混合，装入卧式行星式高能球磨机的球磨罐中，抽真空后充入高纯氮气，控制压力0.1-1atm，球磨30-90h，每球磨5h，停机1h，获得含氮量为0.1-0.8%的ODS无镍奥氏体合金粉末，烧结后制得含氮ODS无镍奥氏体合金。该无镍奥氏体合金可同时实现氮的固溶强化和氧化物弥散强化，在很大程度上改善无镍奥氏体不锈钢在高温环境下的服役能力。The present invention uses mechanical alloying method to prepare nitrogen-containing ODS nickel-free austenitic alloy method, with pure metal element powder of Fe, Cr, Mn, W, Ti, Al and nanometer Y 2 O 3 powder according to Cr: 17-20 %, Mn: 18-22%, W: 1.5-2.5%, Al: 2-4%, Ti: 0.5-1.0%, Y 2 O 3 : 0.3-0.6%, the rest is mixed with Fe, put into horizontal In the ball mill tank of the planetary high-energy ball mill, after vacuuming, fill it with high-purity nitrogen, control the pressure 0.1-1 atm, mill for 30-90 hours, every 5 hours, stop for 1 hour, and obtain ODS nickel-free Austrian with a nitrogen content of 0.1-0.8% Nitrogen-containing ODS nickel-free austenitic alloy is obtained after sintering. The nickel-free austenitic alloy can realize nitrogen solid solution strengthening and oxide dispersion strengthening at the same time, and greatly improves the serviceability of the nickel-free austenitic stainless steel in a high-temperature environment.
Description
Technical field:
The invention belongs to oxide dispersion intensifying (Oxide Dispersion Strengthened; ODS) alloy preparing technical field; A kind of mechanical alloying that realizes oxide compound, nitrogen element, pure metal powder or pre-alloyed powder through high-energy ball milling particularly is provided; Obtaining subsphaeroidal nitrogenous ODS does not have Ni alloy powder, obtains its fine and close method for preparing nitrogenous ODS nickel-less austenitic alloy with mechanical alloying method through HIP sintering.
Background technology:
Austenitic stainless steel with its good comprehensive mechanical properties, good etch resistant properties, antioxidant property, be prone to advantage such as machine-shaping become the 4th generation nuclear power reactor, like 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 request for utilization.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 of Nuclear 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 through the method for mechanical alloying.Mechanical alloying mainly realizes through 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, the atom of gas is participated in by the solid state reaction of ball milling material generation; In addition; In raw material powder, add oxide particle; In mechanical milling process; The raw materials mixed powder is in the high speed between ball and ball, ball and wall, ball and the powder, bump down withstands shocks, shears, rubs and compresses the effect of multiple power repeatedly, and 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.
Common austenitic stainless steel contains more Ni, and Ni is common sensitization metal, causes easily when using as medical and biomaterial that organism is irritated, and using Mn is one of this type Development of Materials direction for Ni.Nickel still is the overactivity element simultaneously, makes it can not be used in the occasion that the activity of material component is had requirement for restriction, in the plasma structure material, at this moment can use low activating element Mn to replace Ni such as fusion reactor, replaces Mo with W.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 the raising corrosion resistance nature, particularly anti-local corrosion performance is like 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 complex equipments, technology controlling and process are difficult, cost is 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 that equipment is simple, cost is low, security is good, be prone to advantage such as realization.Wherein mechanical alloying is one of powder metallurgy process comparatively commonly used.
Summary of the invention:
In order to address the above problem, the object of the present invention is to provide a kind ofly to prepare the method for nitrogenous ODS nickel-less austenitic alloy with mechanical alloying method, mechanical alloying powder composition is even, under room temperature after 1100 ℃ of annealing, obtains complete austenite structure.This method can realize the reinforcement of nitrogen element solid solution and the oxide dispersion intensifying (ODS) of nickel-less austenitic stainless steel simultaneously.
Technical scheme of the present invention is: prepare the method for nitrogenous ODS nickel-less austenitic alloy with mechanical alloying method, specifically may further comprise the steps:
Prepare the method for nitrogenous ODS nickel-less austenitic alloy with mechanical alloying method, it is characterized in that, specifically may further comprise the steps: step 1: greater than 99.9 %, mean particle size is the nanometer Y of 30 nm with the pure metal element powder of Fe, Cr, Mn, W, Al, Ti and purity
2O
3Press massfraction Cr:17-20%, Mn:18-22%, W:1.5-2.5%, Al:2-4%, Ti:0.5-1.0%, Y
2O
3: 0.3-0.6%, surplus is that the proportioning of Fe is weighed and mixed, and according to ball-to-powder weight ratio is to charge into high pure nitrogen after vacuumizing in the ball grinder of 10: 1 horizontal planetary formula high energy ball mills of packing into after the proportioning; Control pressure is at 0.1-1atm; Rotational speed of ball-mill is 380r/min, ball milling 30-90h, and revolution 5h shuts down 1h in the mechanical milling process; Avoid in the mechanical milling process temperature too high, obtaining nitrogen content is the ODS nickel-less austenitic powdered alloy of 0.1-0.8%; Wherein, the granularity of Fe, Cr, Mn, Ti, Al 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 30 nm;
Step 2: the ODS nickel-less austenitic powdered alloy that above-mentioned steps is obtained is through HIP sintering, and sintering condition is 1100 ℃-1200 ℃, pressure 120MPa-180MPa, and insulation 3h makes nitrogenous ODS nickel-less austenitic alloy behind the sintering.
Further, another kind of the present invention prepares the method for nitrogenous ODS nickel-less austenitic stainless steel with mechanical alloying method, and concrete steps are following:
2. prepare the method for nitrogenous ODS nickel-less austenitic stainless steel with mechanical alloying method, it is characterized in that concrete steps are following:
Step 1: with pre-alloyed powder and Y
2O
3Weigh by the proportioning of massfraction 99.7-99.4:0.3-0.6% and to mix; Be to charge into high pure nitrogen after vacuumizing in the ball grinder of 10: 1 horizontal planetary formula high energy ball mills of packing into after the ratio according to ball-to-powder weight ratio, control pressure is at 0.1-1atm, and rotational speed of ball-mill is 380r/min; Ball milling 30-90h; Revolution 5h shuts down 1h in the mechanical milling process, avoids in the mechanical milling process temperature too high, and obtaining nitrogen content is the ODS nickel-less austenitic powdered alloy of 0.1-0.8%;
Step 2: the ODS nickel-less austenitic powdered alloy that above-mentioned steps is obtained is through HIP sintering, and sintering condition is 1100 ℃-1200 ℃, pressure 120MPa-180MPa, and insulation 3h makes nitrogenous ODS nickel-less austenitic alloy behind the sintering.
Wherein, the composition of said pre-alloyed powder is Fe, Cr, Mn, W, Al, Ti, and the mass percent of each component is Cr:17-20%, Mn:18-22%, and W:1.5-2.5%, Al:2-4%, Ti:0.5-1.0%, surplus is Fe; The granularity of pre-alloyed powder is-200 orders, Y
2O
3The mean particle size of powder is 30 nm.
Advantage of the present invention:
1. replace nickel with manganese, add an amount of W, Al, Ti and Y simultaneously
2O
3Adopt mechanical alloying and hot isostatic pressing method to prepare no nickel ODS austenitic alloy with higher mechanical property and antioxidant property.
2. can prepare the ODS nickel-less austenitic stainless steel powder of different nitrogen contents through protective atmosphere nitrogen gas pressure in the control ma process, its composition is even, and nitrogen content can change between 0.1-0.8 %.Through this process of mechanical alloying, can in nickel-less 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 nickel-less austenitic stainless steel.
3. the nitrogenous ODS nickel-less austenitic stainless steel powder size tiny (5-25 μ m) for preparing, particle size distribution is narrow, and the gained powder particle has higher sphericity, is beneficial to and when sintering, obtains higher density.
4. the nitrogenous ODS nickel-less austenitic stainless steel that adopts HIP sintering to prepare has submicron fine grained texture, and the intragranular disperse distributes and takes measurements greatly less than the dispersed oxide particle of 100nm, has higher mechanical behavior under high temperature.
Embodiment
Below in conjunction with specific embodiment technical scheme of the present invention is further specified.
Embodiment 1
Testing raw materials used is pure metal powder and the nanometer Y of Fe, Cr, Mn, W, Ti, Al
2O
3Powder, the purity of used powder are all greater than 99.9 %.Wherein, the granularity of Fe, Cr, Mn, Ti, Al 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 30 nm.Above-mentioned powder is by composition proportion (Cr:18%, Mn:20%, W:1.5%, Al:2.5%, Ti:0.5%, Y
2O
3: 0.4%, surplus is Fe) put into ball grinder after the weighing mixing respectively, charge into nitrogen after vacuumizing, charging into nitrogen gas pressure is 0.5atm.The ball milling time is controlled to be 60h.The employing actual nitrogen content that the infrared heat conduction method of gas pulse (ASTME1019-2003) records powder of falling is 0.52%; Obtain nitrogenous ODS nickel-less austenitic stainless steel behind the powder HIP sintering with mechanical alloying.Sintering condition is 1150 ℃, 150MPa, insulation 3h.Gained non-nickel nitrogen ODS austenitic stainless steel specific density is 97.5%, and its room temperature tensile strength is 730MPa, and unit elongation is 6%; Tensile strength is 230MPa in the time of 700 ℃, and unit elongation is 9%.
Embodiment 2
Testing raw materials used is pure metal powder and the nanometer Y of Fe, Cr, Mn, W, Ti, Al
2O
3Powder, the purity of used powder are all greater than 99.9 %.Wherein, the granularity of Fe, Cr, Mn, Ti, Al 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 30 nm.Above-mentioned powder is by composition proportion (Cr:17%, Mn:22%, W:2%, Al:4%, Ti:0.75%, Y
2O
3: 0.6%, surplus is Fe) put into ball grinder after the weighing mixing respectively, charge into nitrogen after vacuumizing, charging into nitrogen gas pressure is 1atm.The ball milling time is controlled to be 30h.The employing actual nitrogen content that the infrared heat conduction method of gas pulse (ASTME1019-2003) records powder of falling is 0.35%; Obtain nitrogenous ODS nickel-less austenitic stainless steel behind the powder HIP sintering with mechanical alloying.Sintering condition is 1200 ℃, 120MPa, insulation 3h.Gained non-nickel nitrogen ODS austenitic stainless steel specific density is 98%, and its room temperature tensile strength is 750MPa, and unit elongation is 5%; Tensile strength is 260MPa in the time of 700 ℃, and unit elongation is 9%.
Embodiment 3
Testing raw materials used is pure metal powder and the nanometer Y of Fe, Cr, Mn, W, Ti, Al
2O
3Powder, the purity of used powder are all greater than 99.9 %.Wherein, the granularity of Fe, Cr, Mn, Ti, Al 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 30 nm.Above-mentioned powder is by composition proportion (Cr:19%, Mn:21%, W:1.75%, Al:3%, Ti:1.0%, Y
2O
3: 0.0.35%, surplus is Fe) put into ball grinder after the weighing mixing respectively, charge into nitrogen after vacuumizing, charging into nitrogen gas pressure is 0.75atm.The ball milling time is controlled to be 90h.The employing actual nitrogen content that the infrared heat conduction method of gas pulse (ASTME1019-2003) records powder of falling is 0.78%; Obtain nitrogenous ODS nickel-less austenitic stainless steel behind the powder HIP sintering with mechanical alloying.Sintering condition is 1100 ℃, 120MPa, insulation 3h.Gained non-nickel nitrogen ODS austenitic stainless steel specific density is 97%, and its room temperature tensile strength is 710MPa, and unit elongation is 5%; Tensile strength is 215MPa in the time of 700 ℃, and unit elongation is 7%.
Embodiment 4
Test raw materials used be pre-alloyed powder (composition proportion is Cr:19 %, Mn:21%, W:2.2%, Al:3.5%, Ti:0.55%, surplus is Fe) and nanometer Y
2O
3Powder (purity is greater than 99.9 %, and mean particle size is 30 nm) is by composition proportion (pre-alloyed powder 99.5%, Y
2O
3: 0.5%) weighing is put into ball grinder after mixing respectively, charges into nitrogen after vacuumizing, and charging into nitrogen gas pressure is 0.2 atm.The ball milling time is controlled to be 40h.The employing actual nitrogen content that the infrared heat conduction method of gas pulse (ASTME1019-2003) records powder of falling is 0.21%; Obtain nitrogenous ODS nickel-less austenitic alloy behind the powder HIP sintering with mechanical alloying.Sintering condition is 1200 ℃, 180MPa, insulation 3h.Gained non-nickel nitrogen ODS austenitic alloy specific density is 98.5%, and its room temperature tensile strength is 850MPa, and unit elongation is 11 %; Tensile strength is 325MPa in the time of 700 ℃, and unit elongation is 14.5%.
Embodiment 5
Test raw materials used be pre-alloyed powder (composition proportion is Cr:17 %, Mn:18%, W:1.5%, Al:2%, Ti:0.5%, surplus is Fe) and nanometer Y
2O
3Powder (purity is greater than 99.9 %, and mean particle size is 30 nm) is by composition proportion (pre-alloyed powder 99.6%, Y
2O
3: 0.4%) weighing is put into ball grinder after mixing respectively, charges into nitrogen after vacuumizing, and charging into nitrogen gas pressure is 0.9 atm.The ball milling time is controlled to be 70h.The employing actual nitrogen content that the infrared heat conduction method of gas pulse (ASTME1019-2003) records powder of falling is 0.75 %; Obtain nitrogenous ODS nickel-less austenitic alloy behind the powder HIP sintering with mechanical alloying.Sintering condition is 1200 ℃, 180MPa, insulation 3h.Gained non-nickel nitrogen ODS austenitic alloy specific density is 98.5%, and its room temperature tensile strength is 860MPa, and unit elongation is 12 %; Tensile strength is 330MPa in the time of 700 ℃, and unit elongation is 15%.
Claims (2)
1. the method for preparing nitrogenous ODS nickel-less austenitic alloy with mechanical alloying method; It is characterized in that; Specifically may further comprise the steps: step 1: greater than 99.9 %, mean particle size is the nanometer Y of 30 nm with the pure metal element powder of Fe, Cr, Mn, W, Al, Ti and purity
2O
3Press massfraction Cr:17-20%, Mn:18-22%, W:1.5-2.5%, Al:2-4%, Ti:0.5-1.0%, Y
2O
3: 0.3-0.6%, surplus is that the proportioning of Fe is weighed and mixed, and according to ball-to-powder weight ratio is to charge into high pure nitrogen after vacuumizing in the ball grinder of 10: 1 horizontal planetary formula high energy ball mills of packing into after the proportioning; Control pressure is at 0.1-1atm; Rotational speed of ball-mill is 380r/min, ball milling 30-90h, and revolution 5h shuts down 1h in the mechanical milling process; Avoid in the mechanical milling process temperature too high, obtaining nitrogen content is the ODS nickel-less austenitic powdered alloy of 0.1-0.8%; Wherein, the granularity of Fe, Cr, Mn, Ti, Al 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 30 nm;
Step 2: the ODS nickel-less austenitic powdered alloy that above-mentioned steps is obtained adopts isostatic sintering, and sintering condition is 1100 ℃-1200 ℃, pressure 120MPa-180MPa, and insulation 3h makes nitrogenous ODS nickel-less austenitic alloy behind the sintering.
2. prepare the method for nitrogenous ODS nickel-less austenitic stainless steel with mechanical alloying method, it is characterized in that concrete steps are following:
Step 1: with pre-alloyed powder and Y
2O
3Weigh by the proportioning of massfraction 99.7-99.4:0.3-0.6% and to mix; Be to charge into high pure nitrogen after vacuumizing in the ball grinder of 10: 1 horizontal planetary formula high energy ball mills of packing into after the ratio according to ball-to-powder weight ratio, control pressure is at 0.1-1atm, and rotational speed of ball-mill is 380r/min; Ball milling 30-90h; Revolution 5h shuts down 1h in the mechanical milling process, avoids in the mechanical milling process temperature too high, and obtaining nitrogen content is the ODS nickel-less austenitic powdered alloy of 0.1-0.8%;
Step 2: the ODS nickel-less austenitic powdered alloy that above-mentioned steps is obtained adopts isostatic sintering, and sintering condition is 1100 ℃-1200 ℃, pressure 120MPa-180MPa, and insulation 3h makes nitrogenous ODS nickel-less austenitic alloy behind the sintering; Wherein, the composition of said pre-alloyed powder is Fe, Cr, Mn, W, Al, Ti, and the mass percent of each component is Cr:17-20%, Mn:18-22%, and W:1.5-2.5%, Al:2-4%, Ti:0.5-1.0%, surplus is Fe; The granularity of pre-alloyed powder is-200 orders, Y
2O
3The mean particle size of powder is 30 nm.
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| CN108031851A (en) * | 2017-12-28 | 2018-05-15 | 西安交通大学 | A kind of preparation method of austenitic stainless steel alloy |
| CN108907209A (en) * | 2018-07-27 | 2018-11-30 | 中南大学 | A kind of oxide dispersion intensifying iron(-)base powder and its characterizing method |
| CN109014211A (en) * | 2018-08-09 | 2018-12-18 | 上海富驰高科技有限公司 | A kind of inexpensive MIM manufacturing process of the high nitrogen without magnetic high strength stainless steel part |
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| CN110343935A (en) * | 2019-07-11 | 2019-10-18 | 中国科学院金属研究所 | Oxide dispersion strengthening ferrite steel is prepared using surface oxidation+explosive compaction |
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| CN108031851A (en) * | 2017-12-28 | 2018-05-15 | 西安交通大学 | A kind of preparation method of austenitic stainless steel alloy |
| CN110193598A (en) * | 2018-02-27 | 2019-09-03 | 劳斯莱斯有限公司 | A method of manufacture austenitic iron alloy |
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| CN108907209A (en) * | 2018-07-27 | 2018-11-30 | 中南大学 | A kind of oxide dispersion intensifying iron(-)base powder and its characterizing method |
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| CN110343935A (en) * | 2019-07-11 | 2019-10-18 | 中国科学院金属研究所 | Oxide dispersion strengthening ferrite steel is prepared using surface oxidation+explosive compaction |
| CN110760760A (en) * | 2019-12-05 | 2020-02-07 | 中国核动力研究设计院 | Preparation method of FeCrAl-based alloy for nuclear reactor structural material |
| CN112475304A (en) * | 2020-12-09 | 2021-03-12 | 福州大学 | 12Cr stainless steel surface strengthening method based on spark plasma sintering |
| CN113834833A (en) * | 2021-03-31 | 2021-12-24 | 中国工程物理研究院材料研究所 | Characterization method of nanophase in ODS steel magnetic powder |
| CN113231648A (en) * | 2021-04-29 | 2021-08-10 | 西安建筑科技大学 | High-strength austenitic stainless steel and preparation method thereof |
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