CN102277525B - Method for preparing oxide dispersion reinforced stainless steel powder and stainless steel - Google Patents
Method for preparing oxide dispersion reinforced stainless steel powder and stainless steel Download PDFInfo
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- CN102277525B CN102277525B CN 201110242173 CN201110242173A CN102277525B CN 102277525 B CN102277525 B CN 102277525B CN 201110242173 CN201110242173 CN 201110242173 CN 201110242173 A CN201110242173 A CN 201110242173A CN 102277525 B CN102277525 B CN 102277525B
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- 239000000843 powder Substances 0.000 title claims abstract description 45
- 239000006185 dispersion Substances 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title claims description 13
- 239000010935 stainless steel Substances 0.000 title claims description 10
- 229910001220 stainless steel Inorganic materials 0.000 title claims description 10
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 14
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 9
- 239000000956 alloy Substances 0.000 claims abstract description 9
- 229910052786 argon Inorganic materials 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 5
- 230000006698 induction Effects 0.000 claims abstract description 3
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 3
- 238000005984 hydrogenation reaction Methods 0.000 claims description 12
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 12
- 238000005551 mechanical alloying Methods 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 10
- 238000000498 ball milling Methods 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 5
- 238000003701 mechanical milling Methods 0.000 claims description 4
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 3
- 238000009689 gas atomisation Methods 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 238000007670 refining Methods 0.000 claims description 2
- -1 wherein Substances 0.000 claims description 2
- 229910000831 Steel Inorganic materials 0.000 abstract description 15
- 239000010959 steel Substances 0.000 abstract description 15
- 238000005275 alloying Methods 0.000 abstract description 3
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract 3
- 229910052804 chromium Inorganic materials 0.000 abstract 2
- 239000011651 chromium Substances 0.000 abstract 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 abstract 1
- 238000003723 Smelting Methods 0.000 abstract 1
- 238000000889 atomisation Methods 0.000 abstract 1
- 230000000779 depleting effect Effects 0.000 abstract 1
- 238000001513 hot isostatic pressing Methods 0.000 abstract 1
- 238000007731 hot pressing Methods 0.000 abstract 1
- 229910052742 iron Inorganic materials 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 229910000859 α-Fe Inorganic materials 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 5
- 238000000713 high-energy ball milling Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000011824 nuclear material Substances 0.000 description 1
- 229910001175 oxide dispersion-strengthened alloy Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention belongs to the technical field of preparation of nano oxide dispersion reinforced ferrite steel for use in thermal power stations and advanced nuclear reactors and particularly provides a method for producing sintered body of ozone depleting substance (ODS) steel by mechanically alloying iron and chromium pre-alloy powder and a nano oxide by a high-performance ball mill and by means of hot pressing sintering and hot isostatic pressing treatment. In the invention, a mother alloy is smelted in a vacuum induction smelting furnace and Fe-Cr-W-Si-Zr-Ti-Y pre-alloy powder is obtained by argon atomization, wherein the pre-ally contains 12 to 19 percent of Cr, 1 to 2 percent of W, 0.1 to 0.2 percent of Si, 0.1 to 0.2 percent of Zr, 0.2 to 0.4 percent of Ti, 0.05 to 0.1 percent of Y and the balance of Fe. The addition of a proper amount of Si, Zr, Ti and Y into the pre-alloy powder is to ensure the precipitation of ultrafine complex oxide nano particles from the ODS steel.
Description
Technical field:
The invention belongs to the nano oxide dispersion that is applied to fuel-burning power plant, advanced nuclear reactor and strengthen (Oxide Dispersion Strengthened; ODS) ferritic steel preparing technical field; A kind of mechanical alloying through high-energy ball milling realization siderochrome pre-alloyed powder and nano-oxide particularly is provided, and then has obtained the sintered compact of ODS steel through the method for hot pressed sintering and hip treatment.
Background technology:
Oxide particle dispersion-strengthened (Oxide dispersion strengthen; ODS) be the effective means that improves steel alloy mechanical behavior under high temperature, anti-irradiation ability; 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.The ODS ferritic steel 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).Ferritic steel can effectively improve its service temperature after ODSization, increase substantially its mechanical behavior under high temperature and anti-irradiation ability.Dispersed oxide in the 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, experience repeatedly extruding, cold welding and crushing process so that realize alloying, make fine oxide particle solid solution decomposition in matrix alloy.
Summary of the invention:
The object of the present invention is to provide a kind of method for preparing the ODS ferritic steel with mechanical alloying method.ODS ferritic steel powder composition with the mechanical alloying method preparation is even, through the good sintered compact of obtained performance after hot pressed sintering and the hip treatment.
The preparation method of a kind of oxide dispersion intensifying type of the present invention powder of stainless steel is characterized in that said method is following:
Adopt vacuum induction melting furnace refining mother alloy and argon gas atomizing to obtain the Fe-Cr-W-Si-Zr-Ti-Y pre-alloyed powder, wherein, Cr:12-19%, W:1-2%, Si:0.1-0.2%, Zr:0.1-0.2%, Ti:0.2-0.4%, Y:0.05-0.1%, surplus is Fe; With hydrogenation yttrium and nanometer Y
2O
3Powder is by following mixed, YH:0.1-0.2%, Y
2O
3: 0.2-0.3%, surplus is a pre-alloyed powder; Pack into after the mixing in the ball grinder, charge into high-purity argon gas after vacuumizing, ball milling 30 ~ 60 h do not comprise stop time in comprehensive planetary high-energy ball mill, and every ball milling 5h shuts down 1h, prevents that the ball grinder temperature is too high; Simultaneously add hydrogenation yttrium and yttrium oxide again in the mechanical milling process, add-on is controlled at YH:0.1-0.2%,, Y
2O
3: 0.2-0.3%.
The stainless preparation method of a kind of oxide dispersion intensifying type is characterized in that said method is following: the mechanical alloying powder that claim 1 is obtained is through 1050-1100 ℃; 2h, 50MPa and 1150-1200 degree, 1h; 50 MPa vacuum heating-press sinterings, then at 1100-1150 ℃, 3h; The 200MPa hip treatment is prepared oxide dispersion intensifying type stainless steel behind the sintering.
A kind of oxide dispersion intensifying type stainless steel is characterized in that, is made by aforesaid method.
The invention has the advantages that: can the uniform ODS ferritic steel of prepared composition powder through comprehensive high-energy ball milling, in pre-alloyed powder, add an amount of Si, Zr, Ti, Y to guarantee separating out of ultra-fine complex oxide nano particle in the ODS steel.In mechanical milling process, add hydrogenation yttrium and nano yttrium oxide simultaneously to reduce the residual oxygen of prepared powder.Adopt two step hot pressed sinterings and hip treatment to combine, simplify preparation technology.
Embodiment
Embodiment 1:
Test raw materials used be pre-alloyed powder (composition is Fe-12Cr-1.5W-0.15Si-0.15Zr-0.2Ti-0.1Y) and hydrogenation yttrium and nanometer Y
2O
3Powder, the purity of used powder are all greater than 99.9 %.Wherein, the granularity of pre-alloyed powder and hydrogenation yttrium is-200 orders, Y
2O
3The mean particle size of powder is 30 nm.Above-mentioned powder is prealloy powder-0.1YH-0.2Y by composition proportion
2O
3Weighing is put into ball grinder after mixing respectively, charges into high-purity argon gas after vacuumizing, and rotational speed of ball-mill is 300rpm, and the ball milling time is controlled to be 40h.With the powder of mechanical alloying at 1050 ℃, hot pressed sintering 2h and 1200 ℃ under the 50 MPa conditions, hot pressed sintering 1h under the 50 MPa conditions, (1150 ℃, 200 MPa obtain 12 Cr ODS ferritic steels after 3h) to carry out hip treatment again.The tensile strength of its room temperature and 700 ℃ is respectively 1350 MPa and 405MPa, and elongation after fracture is respectively 0.5% and 7%.
Embodiment 2:
Testing raw materials used is pre-alloyed powder (composition Fe-14.5Cr-1W-0.10Si-0.15Zr-0.3Ti-0.05Y) and hydrogenation yttrium and nanometer Y
2O
3Powder, the purity of used powder are all greater than 99.9 %.Wherein, the granularity of pre-alloyed powder and hydrogenation yttrium is-200 orders, Y
2O
3The mean particle size of powder is 30 nm.Above-mentioned powder is pre-alloyed powder-0.15Y-0.25Y by composition proportion
2O
3Weighing is put into ball grinder after mixing respectively, charges into high-purity argon gas after vacuumizing, and rotational speed of ball-mill is 280rpm, and the ball milling time is controlled to be 50h.With the powder of mechanical alloying at 1100 ℃, hot pressed sintering 2h under the 50 MPa conditions, 1200 ℃, hot pressed sintering 1h under the 50 MPa conditions, (1150 ℃, 200 MPa obtain 14 Cr ODS ferritic steels after 3h) to carry out hip treatment again.The tensile strength of its room temperature and 700 ℃ is respectively 1250 MPa and 315MPa, and elongation after fracture is respectively 1% and 17%.
Embodiment 3
Test raw materials used be pre-alloyed powder (composition is Fe-18Cr-1.2W-0.15Si-0.2Zr-0.2Ti-0.1Y) and hydrogenation yttrium and nanometer Y
2O
3Powder, the purity of used powder are all greater than 99.9 %.Wherein, the granularity of pre-alloyed powder and hydrogenation yttrium is-200 orders, Y
2O
3The mean particle size of powder is 30 nm.Above-mentioned powder is pre-alloyed powder-0.1Y-0.3Y by composition proportion
2O
3Weighing is put into ball grinder after mixing respectively, charges into high-purity argon gas after vacuumizing, and rotational speed of ball-mill is 330rpm, and the ball milling time is controlled to be 30h.At 1100 ℃, hot pressed sintering 2h is 1200 ℃ under the 50 MPa conditions with the powder of mechanical alloying, hot pressed sintering 1h under the 50 MPa conditions, and (1100 ℃, 200 MPa obtain 18 Cr ODS ferritic steels after 3h) to carry out hip treatment again.The tensile strength of its room temperature and 700 ℃ is respectively 950 MPa and 285MPa, and elongation after fracture is respectively 13% and 40%.
Claims (3)
1. the preparation method of an oxide dispersion intensifying type powder of stainless steel is characterized in that, said method is following:
Adopt vacuum induction melting furnace refining mother alloy and argon gas atomizing to obtain the Fe-Cr-W-Si-Zr-Ti-Y pre-alloyed powder, wherein, Cr:12-19%, W:1-2%, Si:0.1-0.2%, Zr:0.1-0.2%, Ti:0.2-0.4%, Y:0.05-0.1%, surplus is Fe; With hydrogenation yttrium and nanometer Y
2O
3Powder is by following mixed, YH:0.1-0.2%, Y
2O
3: 0.2-0.3%, surplus is a pre-alloyed powder; Pack into after the mixing in the ball grinder, charge into high-purity argon gas after vacuumizing, ball milling 30～60h in comprehensive planetary high-energy ball mill does not comprise stop time, and every ball milling 5h shuts down 1h, prevents that the ball grinder temperature is too high; Simultaneously add hydrogenation yttrium and yttrium oxide again in the mechanical milling process, add-on is controlled at YH:0.1-0.2%, Y
2O
3: 0.2-0.3%; Wherein, the granularity of pre-alloyed powder and hydrogenation yttrium is-200 orders, Y
2O
3The mean particle size of powder is 30nm.
2. stainless preparation method of oxide dispersion intensifying type is characterized in that said method is following: the mechanical alloying powder that claim 1 is obtained is through 1050-1100 ℃; 2h, 50MPa and 1150-1200 ℃, 1h; The 50MPa vacuum heating-press sintering, then at 1100-1150 ℃, 3h; The 200MPa hip treatment is prepared oxide dispersion intensifying type stainless steel behind the sintering.
3. an oxide dispersion intensifying type stainless steel is characterized in that, is made by the said method of claim 2.
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| CN 201110242173 CN102277525B (en) | 2011-08-23 | 2011-08-23 | Method for preparing oxide dispersion reinforced stainless steel powder and stainless steel |
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| CN 201110242173 CN102277525B (en) | 2011-08-23 | 2011-08-23 | Method for preparing oxide dispersion reinforced stainless steel powder and stainless steel |
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| CN102277525B true CN102277525B (en) | 2012-12-05 |
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| CN104073725A (en) * | 2013-03-29 | 2014-10-01 | 韩国原子力研究院 | Ferritic oxide dispersion strengthened alloy with enhanced room temperature and high temperature strength and manufacturing method thereof |
| KR20150104348A (en) * | 2014-03-05 | 2015-09-15 | 한국원자력연구원 | Ferrite/martensitic oxide dispersion strengthened steel with excellent creep resistance and manufacturing method thereof |
| CN105880222A (en) * | 2014-11-15 | 2016-08-24 | 赵坚强 | Novel environmentally-friendly processor made from high-energy-state material and capable of scale inhibition, rust removal and catalysis |
| CN104476842B (en) * | 2014-11-18 | 2016-06-29 | 华中科技大学 | A kind of toughness reinforcing ODS steel of stratiform and preparation method thereof |
| CN104630639B (en) * | 2015-03-10 | 2016-11-30 | 中南大学 | A kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy and preparation method |
| CN106399806B (en) * | 2015-07-31 | 2018-04-17 | 东北大学 | A kind of batch preparation of nano-structure oxide dispersion strengthened steel |
| CN105401047B (en) * | 2016-01-05 | 2017-09-08 | 西南大学 | A kind of preparation method of ODS ferritic stainless steels |
| 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 |
| 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 |
| CN109097661A (en) * | 2018-08-10 | 2018-12-28 | 杭州电子科技大学 | The method that stainless steel micro constitutent homogenizes |
| CN111531173B (en) * | 2020-06-17 | 2021-09-07 | 中南大学 | Yttrium-containing powder metallurgy high-speed steel and preparation method thereof |
| CN112453413B (en) * | 2020-11-20 | 2023-05-12 | 中科南京绿色制造产业创新研究院 | Preparation method of oxide dispersion strengthening steel spherical powder for 3D printing |
| CN112548107A (en) * | 2020-11-20 | 2021-03-26 | 中科院过程工程研究所南京绿色制造产业创新研究院 | Preparation method of carbon nano tube coated oxide dispersion strengthened steel composite powder |
| CN112935265B (en) * | 2021-01-25 | 2022-07-08 | 北京科技大学 | Preparation method of high-strength powder austenitic stainless steel |
| CN112941407B (en) * | 2021-01-27 | 2022-07-01 | 中国核动力研究设计院 | Nano-oxide reinforced ferrite steel for reactor, pipe and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1480280A (en) * | 2003-07-02 | 2004-03-10 | 北京科技大学 | Method for preparing stainless steel powder containing nitrogen by using mechanical alloying |
| CN101538674A (en) * | 2009-05-06 | 2009-09-23 | 北京科技大学 | Method for preparing oxide dispersion strengthened austenitic stainless steel |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP3467740B2 (en) * | 1999-04-02 | 2003-11-17 | 北海道大学長 | Manufacturing method of oxide dispersion strengthened ferritic steel |
| JP4192249B2 (en) * | 2005-12-14 | 2008-12-10 | 独立行政法人 日本原子力研究開発機構 | Method for producing ferritic oxide dispersion strengthened steel with coarse grain structure and excellent high temperature creep strength |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1480280A (en) * | 2003-07-02 | 2004-03-10 | 北京科技大学 | Method for preparing stainless steel powder containing nitrogen by using mechanical alloying |
| CN101538674A (en) * | 2009-05-06 | 2009-09-23 | 北京科技大学 | Method for preparing oxide dispersion strengthened austenitic stainless steel |
Non-Patent Citations (2)
| Title |
|---|
| JP特开2000-282101A 2000.10.10 |
| JP特开2006-176878A 2006.07.06 |
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