CN102071348B - Preparation method of superfine grain nano-structure oxide dispersion strengthened steel - Google Patents
Preparation method of superfine grain nano-structure oxide dispersion strengthened steel Download PDFInfo
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- CN102071348B CN102071348B CN2010105941639A CN201010594163A CN102071348B CN 102071348 B CN102071348 B CN 102071348B CN 2010105941639 A CN2010105941639 A CN 2010105941639A CN 201010594163 A CN201010594163 A CN 201010594163A CN 102071348 B CN102071348 B CN 102071348B
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Abstract
The invention discloses a preparation method of superfine grain nano-structure oxide dispersion strengthened steel. The preparation method comprises the following steps of: performing ball-milling mechanical alloying on alloy powder which is prepared by an atomization method or pure metal element powder in a corresponding constituent element ratio, metal Ti powder and Y2O3 powder in a nanometer scale in vacuum or under Ar gas protection so as to form solid solution alloy powder which is rich in supersaturated Y, Ti and O; and putting the supersaturated solid solution alloy powder into a mould, and performing solidification sintering in spark plasma sintering equipment so as to obtain the superfine grain nano-structure oxide dispersion strengthened steel, wherein sintering environment can be vacuum or inert gas; a sintering temperature is between 800 and 1,200 DEG C; heat preserving time is between 1 and 15min; and pressure is between 10 and 200MPa. The grain size of the alloy is refined from a micron level to a level which is equal to or less than 500 nanometers by the method, the characteristic microstructure and the irradiation resistance performance of the nano-structure oxide dispersion strengthened steel are maintained, and the alloy strength and the high temperature creep strength are greatly improved, so that the using requirement of core parts of an advanced nuclear reactor on the high temperature resistance and the irradiation resistance of materials are met.
Description
Technical field
The preparation method of a kind of superfine crystal particle nanostructured oxide of the present invention dispersion-strengthened steel relates to the technology of preparing of nuclear reactor core component with high temperature resistant, HS, anti-irradiation alloy.
Background technology
The nuclear power developing direction is thermal reactor (pressurized-water reactor)-fast neutron reactor (the 4th generation heap)-fusion reactor at present.But the working temperature of advanced nuclear reactor (comprised four generations heap and fusion reactor) and irradiation intensity are far above existing two generations/three generations's fission-type reactor; Therefore the performance to advanced core heart block construction material has proposed very harsh requirement; Build consensus in the world: though there are many high-leveled and difficult technical problems to need to solve; But the development of advanced heap will be depended on the development of high performance new structural material, and promptly material is the main bottleneck of the advanced heap development of restriction.Have only the nanostructured oxide dispersion-strengthened steel might satisfy the anti-irradiation requirement of advanced heap at present, excellent anti-radiation performance is from its distinctive microtexture, particularly nanostructured oxide disperse precipitated phase.But its hot strength is still not enough with have the performance anisotropic problem.
Metallurgical ABC shows that the refinement of crystal grain can obviously improve alloy strength; After American scholar adopts hot extrusion to obtain the nanostructured oxide dispersion-strengthened steel of micro-meter scale crystal grain as solidification technology in preparation nanostructured oxide dispersion-strengthened steel process; Obtain the nanostructured oxide dispersion-strengthened steel of grain fineness number～200nm in the laboratory through the hot repeatedly treat mechanically of complicacy; Its performance data confirms that the refinement of crystal grain promotes intensity and strength that the nanostructured oxide fringing-type is strengthened steel significantly, but still has the anisotropic problem of structure and performance.
The typical preparation technology of nanostructured oxide dispersion-strengthened steel is: the 1. pure metal powder of mother alloy powder by atomization or alloy composition element; With rare earth oxide and the common ball milling of metal Ti (mechanical alloying) with the alloy that obtains predetermined ingredients and realize rare earth oxide and the solid solution of Ti, about tens nanometers of the grain fineness number of the powder alloy that obtains; 2. hot extrusion/hot isostatic pressing realizes the solidification moulding of powder alloy, during the rare earth oxide and the Ti of solid solution separate out again with the oxide form of nanoscale.But since the temperature that solidification processings needs high (～1100 ℃), time grow (～120min), the grain fineness number of alloy is grown up to micron order after the solidification; 3. recrystallize thermal treatment/subsequent disposal such as hot treat mechanically.The solidification technology that adopts at present is hot isostatic pressing or hot extrusion, and the former needs the time of high-temp solidization long, and crystal grain is thicker; Latter's solidification time is shorter, and crystal grain is more tiny than the former, but has significant structure and the anisotropic problem of performance, needs complicated hot machinery of later stage/recrystallize to handle.
Summary of the invention
To the problems referred to above; The preparation method of a kind of superfine crystal particle nanostructured oxide of the present invention dispersion-strengthened steel; Adopt the discharge plasma sintering to replace the solidification technology of hot extrusion/hot isostatic pressing, the grain fineness number of alloy is reduced to≤500 nanometers by micron order as nanostructure ODS steel.
The preparation method of a kind of superfine crystal particle nanostructured oxide of the present invention dispersion-strengthened steel, with Fe base, basic, the basic alloy powder of Fe-Cr-W of Fe-Cr of atomization preparation, or the pure metal element powder of respective components ratio, with the Y of metal Ti powder and nanoscale
2O
3Powder carries out ball milling (mechanical alloying) under vacuum or Ar gas shiled, form the solid solution alloy powder that is rich in supersaturation Y, Ti, O; Then Y, Ti, the oversaturated solid solution alloy powder of O are inserted in the mould; In the discharge plasma agglomerating plant, carry out the solidification sintering; The sintering environment can be vacuum or rare gas element, and sintering temperature is 800 ~ 1200 ℃, and soaking time is 1 ~ 15min; Sintering pressure is 10 ~ 200MPa, obtains superfine crystal particle nanostructured oxide dispersion-strengthened steel.
In above-mentioned alloy powder or the metallic element powder each element by mass percentage Cr be 8 ~ 16%, W is 1 ~ 4%; Mn is 0 ~ 1%, Ta is 0 ~ 1%, and V is 0 ~ 1%, and surplus is Fe.
Above-mentioned adding Ti powder and Y
2O
3The mass percent of powder is Y
2O
3Be 0.1 ~ 3%, Ti is 0.1 ~ 3%.
Above-mentioned superfine crystal particle nanostructured oxide dispersion-strengthened steel is observed its microtexture through transmission electron microscope (TEM), the grain fineness number of alloy≤500 nanometers.
The crystalline structure of the superfine crystal particle nanostructured oxide dispersion-strengthened steel of above-mentioned preparation is ferritic, martensite or ferrite/martensite double structure.
Above-mentioned through behind the discharge plasma solidification sintering, 98% of alloy density>=theoretical density, crystal particle scale≤500 nanometers, containing that highly dispersed distributes, yardstick in the alloy substrate is the non-equilibrium oxide compound precipitated phase of several nanometers.
The present invention adopts the discharge plasma sintering to replace the solidification technology of hot extrusion/hot isostatic pressing as the nanostructured oxide dispersion-strengthened steel; Because sintering temperature can obviously reduce with sintering time and can significantly shorten; Suppressed powder alloy grain degree growing up in the solidification process; Make the grain fineness number of alloy be refined to ￡ 500nm by micron order; Construct superfine crystal particle nanostructured oxide dispersion-strengthened steel, when keeping nanostructured oxide dispersion-strengthened steel characteristic microtexture and anti-radiation performance, can realize the significantly lifting of alloy strength and high temperature creep strength; Advanced core heart parts are high temperature resistant to material to satisfy, the request for utilization of anti-irradiation, and higher use temperature means has higher reactor efficient.
Description of drawings
Fig. 1 utilizes transmission electron microscope (TEM) photo of discharge plasma sintering as the superfine crystal particle nanostructured oxide dispersion-strengthened steel microtexture of solidification prepared.
Fig. 2 utilizes the diffraction spectra photo of discharge plasma sintering as the superfine crystal particle nanostructured oxide dispersion-strengthened steel microtexture of solidification prepared.
Embodiment
Below in conjunction with embodiment the preparation method of a kind of superfine crystal particle nanostructured oxide of the present invention dispersion-strengthened steel is described in detail.
Adopt high pure metal element powder, each component Cr by mass percentage is 9.0%, and W is 1.0%, and Mn is 0.4%, and V is 0.4%, and Ta is 0.4%, and surplus is Fe, with mass percent be 0.3% Ti powder, 0.3% Y
2O
3Powder mixes, and through high-energy ball milling, forms Y
2O
3With the supersaturation alloy powder of the complete solid solution of Ti, the powder granule degree is at micron order, and grain fineness number is in tens nanometer scale.Through discharge plasma sintering in vacuum environment, sintering temperature is 1000 ℃, and sintering time is 3min; Sintering pressure is 40MPa; The crystalline structure of alloy is a martensite after the solidification moulding, and density is 98.1% of theoretical density, and room temperature tensile intensity is 1204MPa; The yardstick of most crystal grain is seen Fig. 1, shown in Figure 2 between 100 ~ 300 nanometers.
Embodiment 2
Adopt high pure metal element powder, each component Cr by mass percentage is 16.0%, and W is 4.0%, and surplus is Fe, with mass percent be 3% Ti powder, 3% Y
2O
3Powder mixes, and through high-energy ball milling, forms Y
2O
3With the supersaturation alloy powder of the complete solid solution of Ti, the powder granule degree is at micron order, and grain fineness number is in tens nanometer scale.Through discharge plasma in Ar compression ring border sintering, 800 ℃ of sintering temperatures, sintering time 15min, sintering pressure 200MPa, the crystalline structure of alloy is a ferritic after the solidification moulding, density reaches 98.2% of theoretical density, room temperature tensile intensity reaches 1158MPa.The yardstick of most crystal grain is between 150-350nm.
Embodiment 3
Adopt the atomized alloy powder, each constituent element of alloy Cr by mass percentage is 12.0%, and W is 2.0%, and Mn is 1.0%, 1.0%V, 1.0%Ta,, surplus is Fe, with mass percent be 0.1% Ti, 0.1% Y
2O
3Mix,, form Y through high-energy ball milling
2O
3With the supersaturation alloy powder of the complete solid solution of Ti, the powder granule degree is at micron order, and grain fineness number is in tens nanometer scale.Through discharge plasma in Ar compression ring border sintering, 1200 ℃ of sintering temperatures, sintering time 1min; Sintering pressure 10MPa; The crystalline structure of alloy is the ferrite/martensite double structure after the solidification moulding, and density reaches 98.0% of theoretical density, and room temperature tensile intensity reaches 1047MPa.The yardstick of most crystal grain is between 200 ~ 500 nanometers.
Claims (5)
1. the preparation method of a superfine crystal particle nanostructured oxide dispersion-strengthened steel; It is characterized in that: with Fe base, basic, the basic mother alloy powder of Fe-Cr-W of Fe-Cr of atomization preparation; Or the pure metal element powder of respective components ratio, with the Y of metal Ti powder and nanoscale
2O
3Powder carries out high-energy ball milling machinery alloying under vacuum or Ar gas shiled; The solid solution alloy powder of supersaturation Y, Ti, O is rich in formation, and the supersaturated solid solution alloy powder is coated with carbon paper, inserts graphite jig; In the discharge plasma agglomerating plant, carry out the solidification sintering; The sintering environment can be vacuum or rare gas element, and sintering temperature is 800～1200 ℃, and soaking time is 1～15min; Sintering pressure is 10～200MPa, obtains the superfine crystal particle nanostructured oxide dispersion-strengthened steel of grain fineness number≤500 nanometers.
2. the preparation method of a kind of superfine crystal particle nanostructured oxide dispersion-strengthened steel according to claim 1; It is characterized in that said mother alloy powder; Or in the pure metal element powder of respective components ratio, each element Cr by mass percentage is 8～16%, and W is 1～4%; Mn is 0～1%, Ta is 0～1%, and V is 0～1%, and surplus is Fe.
3. the preparation method of a kind of superfine crystal particle nanostructured oxide dispersion-strengthened steel according to claim 1 is characterized in that adding Ti powder and Y
2O
3The mass percent Y of powder
2O
3Be 0.1-3%, Ti is 0.1-3%.
4. the preparation method of a kind of superfine crystal particle nanostructured oxide dispersion-strengthened steel according to claim 1, the crystalline structure that it is characterized in that prepared superfine crystal particle nanostructured oxide dispersion-strengthened steel is ferritic, martensite or ferrite/martensite double structure.
5. the preparation method of a kind of superfine crystal particle nanostructured oxide dispersion-strengthened steel according to claim 1; It is characterized in that through behind the discharge plasma sintering; 98% of alloy density>=theoretical density; Crystal particle scale≤500 nanometers, containing that highly dispersed distributes, yardstick in the alloy substrate is the non-equilibrium oxide compound precipitated phase of several nanometers.
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| CN105039857B (en) * | 2015-06-15 | 2017-01-04 | 北京科技大学 | A kind of oxide dispersion strengthening ferrite/martensite steel and preparation method |
| CN106868383B (en) * | 2015-12-14 | 2019-01-18 | 东北大学 | The method for preparing nano-structure oxide dispersion strengthened steel workpiece with 3D printing technique |
| CN105906347A (en) * | 2016-04-22 | 2016-08-31 | 西南交通大学 | Method for preparing nanocrystal aluminum nitride ceramics |
| CN106399807A (en) * | 2016-09-28 | 2017-02-15 | 天津大学 | Preparation method of oxide dispersion strengthened steel with micro-nano-scale double-crystal-grain structure |
| CN107243639A (en) * | 2017-05-11 | 2017-10-13 | 广西大学 | A kind of preparation method of supersaturated Mg (Ti) metal solid solution powder |
| CN110016603B (en) * | 2019-05-20 | 2020-07-24 | 燕山大学 | Ultra-high-strength and high-thermal-stability nanocrystalline ODS steel, and preparation method and application thereof |
| CN110423876B (en) * | 2019-08-02 | 2021-09-10 | 清华大学深圳研究生院 | Method for improving radiation resistance of steel for nuclear power plant reactor |
| CN111020347B (en) * | 2019-12-30 | 2021-08-17 | 广州航海学院 | High-density complex phase alloy material and preparation method thereof |
| CN113231647B (en) * | 2021-04-29 | 2022-08-23 | 西安建筑科技大学 | Multi-scale rare earth oxide reinforced low-activation steel and preparation method thereof |
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|---|---|---|---|---|
| US4963200A (en) * | 1988-04-25 | 1990-10-16 | Doryokuro Kakunenryo Kaihatsu Jigyodan | Dispersion strengthened ferritic steel for high temperature structural use |
| EP0949346A1 (en) * | 1998-04-07 | 1999-10-13 | Commissariat A L'energie Atomique | Process of producing a dispersion strengthened ferritic-martensitic alloy |
| CN101328562A (en) * | 2008-07-17 | 2008-12-24 | 中国科学院等离子体物理研究所 | Oxide dispersion strengthening low activity martensitic steel material and preparation thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4963200A (en) * | 1988-04-25 | 1990-10-16 | Doryokuro Kakunenryo Kaihatsu Jigyodan | Dispersion strengthened ferritic steel for high temperature structural use |
| EP0949346A1 (en) * | 1998-04-07 | 1999-10-13 | Commissariat A L'energie Atomique | Process of producing a dispersion strengthened ferritic-martensitic alloy |
| CN101328562A (en) * | 2008-07-17 | 2008-12-24 | 中国科学院等离子体物理研究所 | Oxide dispersion strengthening low activity martensitic steel material and preparation thereof |
Non-Patent Citations (2)
| Title |
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| JP特开平11-343526A 1999.12.14 |
| 张鑫等.放电等离子烧结制备超细晶奥氏体不锈钢的研究.《钢铁钒钛》.2006,第27卷(第2期),17-20,47. * |
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