CN105274440B - The preparation method and a kind of martensite steel of a kind of oxide dispersion intensifying steel - Google Patents
The preparation method and a kind of martensite steel of a kind of oxide dispersion intensifying steel Download PDFInfo
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Abstract
The present invention provides the preparation method and a kind of martensite steel of a kind of oxide dispersion intensifying steel, the preparation method adds the oxide of iron in the mould, appropriate rare earth element is added into the molten steel after abundant deoxidation and is quickly cast in mold, oxide dispersion intensifying steel is obtained by the oxide reaction of rare earth element and iron（ODS steel）；A kind of martensite steel, the ODS steel hot forging as made from the above method, hot rolling, hot-working and heat treatment gained, ODS steel hardenabilities prepared by the present invention are high, and residual austenite content is very low, can obtain full martensitic structure.W, V and Ta are carbides, with notable invigoration effect, the steel that mechanical property is prepared apparently higher than traditional smelting technology, ductile-brittle transition temperature DBTT50 values are 80 DEG C and 90 DEG C simultaneously, also the excellent toughness of traditional smelting technology is inherited well while also there is excellent anti-radiation performance, it is possible to achieve the batch of ODS steel is drawn, stabilized, the preparation demand that flow is short, inexpensive.
Description
Technical field
The invention belongs to metal material field, and in particular to a kind of preparation method of oxide dispersion intensifying steel and a kind of horse
Family name's body steel, the martensite steel is a kind of ODS low activities martensite steel as made from this preparation method.
Background technology
It is tiny and be evenly distributed in oxide dispersion intensifying (Oxide dispersion strengthening, ODS) steel
Dispersed oxide mutually not only significantly improve the high temperature creep strength of steel, and the presence of disperse phase can also play irradiation generation and lack
Fall into the effect of lower reaches, hence it is evident that improve the Flouride-resistani acid phesphatase swelling ability of steel, therefore ODS steel is considered as most promising Flouride-resistani acid phesphatase
Midium-carbon steel, its preparation technology is even more study hotspot.The ODS steel reported at present is all prepared using powder metallurgical technique, is led to
The ma process of high-energy ball milling is crossed by the ceramic particles such as yittrium oxide and iron alloy powder ball milling mixing, realizes that ceramic powder exists
Dispersed precipitate in steel；Powder after ball milling obtains steel billet by hip moulding sintering.Mechanical alloying prepares ODS steel most
The MA957 ferritic steels that early work is prepared from Fisher et al., the steel shows high tensile strength, creep strength and not
With ordinary radioresistance injury reinforcing ability.Japan has continued the research of ODS steel, with metal alloy powder and Y2O3 powder through mechanical ball mill,
In 673K degasification after big envelope, then in 1423K hot extrusions, the nanostructured ODS steel 9Cr- for fast reactor fuel can is prepared
0.13C-0.2Ti-2W-0.35Y2O3 bars；By the thermomechanical processing and recrystallization during subsequent technique, make steel reach compared with
High isotropism.Patent (A of application publication number CN 102277525) provides one kind and realizes that siderochrome is closed in advance by high-energy ball milling
Bronze end and the mechanical alloying of nano-oxide, and obtain by hot pressed sintering and hip treatment the sintered body of ODS steel
Method.In this patent of invention, inventor is using vacuum induction melting furnace refining foundry alloy and argon gas atomization obtains Fe-Cr-
W-Si-Zr-Ti-Y pre-alloyed powders are super in ODS steel to ensure by adding appropriate Si, Zr, Ti, Y in pre-alloyed powder
The precipitation of thin complex oxide nano particle；Prealloy powder and yttrium powder by long-time ball milling carry out disperse mix,
ODS steel is obtained by HIP sintering densification.
ODS steel is prepared using mechanical alloying and there is following subject matter：One is limited by mechanical alloying technique, single
Batch output is small, stability is poor between batch；Two be technological process length, manufacturing cost height；Three be material anisotropic problem dash forward
Go out.In view of the batch stroke of steel, stabilisation, inexpensive preparation demand, applicant explores obtain ODS by smelting technology always
Steel.
The content of the invention
In order to solve the above problems, the present invention provides the preparation method and a kind of martensite of a kind of oxide dispersion intensifying steel
Steel, the principle of the preparation method is that, based on combination energy strong between rare earth elements RE and O, its standard molar formation enthalpy is higher than
The oxide enthalpy of formation of other alloying elements, be easily created stable rare earth oxide, by the addition of rare earth element when
The incorporation way of machine and oxygen, makes rare earth element be combined generation fine oxide particle with oxygen, and the preparation method adds in the mould
Enter the oxide of iron, appropriate rare earth element is added into the molten steel after abundant deoxidation and is quickly cast in mold, passes through rare earth
The oxide reaction of element and iron obtains oxide dispersion intensifying steel (ODS steel)；
Further, the preparation method is specifically included：
S1：The oxide of iron is added in the mould；
S2：Ingot iron is added into crucible for smelting, power transmission when being evacuated down to 10Pa；
S3：It is evacuated down to vacuum<Refined after 7Pa, control to take off by deoxidant element Al scaling loss in refining process
Oxygen depth, as oxygen concentration [O]<10-5When add alloying element carry out alloying；
S4：Rare earth element is added into the molten steel for completing alloying, quickly molten steel is cast in mold after stirring, is obtained
ODS steel；
Further, it is Fe that the oxide that rare earth element is addition iron in yttrium, the S1 is added in the S42O3, the Y
And Fe2O3The ratio between the amount of material be 1:1-1.2:1.
Further, melting and vacuumized in the S2 using vacuum induction/magnetic agitation technique, smelting temperature is molten in iron
Cast temperature is reduced as far as possible depending on molten steel flow while mobility is ensured in 100-200 DEG C of the above of point, the S4
Molten steel temperature；
Further, a kind of martensite steel, the ODS steel hot forging as made from the above method, hot rolling, hot-working and heat treatment institute
, the ODS steel various composition accounts for the percentage of gross mass：C：0.08~0.15%, Cr：8.0~9.9%, Mn：0.45~
0.6%th, W：2.0~2.5%, N：0.05~0.07%, Ta：0.10~0.20%, Ti:0.4~0.55%, Si：0.10~
0.15%th, V：0.04~0.05%, Y：0.01~0.5%, B<0.001%th, S<0.003%th, P<0.005%th, Fe surpluses；
Further, the specific steps that prepared by the martensite steel include：
(a) progress first time thermal deformation is made or rolled to ODS steel forgings made from S4, obtain semi-finished product；
(b) semi-finished product are heated to 1150 DEG C -1200 DEG C of scope, are again deformed by hot rolling until obtaining institute
It is required that shape and size product；
(c) treat that part cooling is to room temperature described in (b), then be heated to 950-1050 DEG C of temperature range to keep 15-
25min, carries out austenitation heat treatment；
(d) then product is heated to 750- by the part cooling after the austenitation heat treatment again to less than 50 DEG C
790 DEG C of temperature ranges keep 90-130min, carry out tempering heat treatment and obtain martensite steel；
Further, ODS steel is in preparation process in the step (a), and rare earth element yttrium is added after deoxidation completion,
It is also the alloying element that last in alloying process is added, while on-line checking alloying element and according to test result supplement
Alloying element and oxygen activity；
Further, in the step (b) forging or the temperature range of rolling are at 1150 DEG C -1000 DEG C；
Further, the step (c) is cooling controlling and rolling controlling process, starts rolling temperature in 1100 DEG C, finishing temperature control
At 850-900 DEG C, online misting cooling is used after rolling；
Further, the heat treating regime of the austenitizing of the step (d) is：950-1050 DEG C/15-25min is quenched；
750-780 DEG C/90-120min is tempered, and the cooling operations after austenitation heat treatment are carried out in water, the step (e)
Cooling operations after tempering heat treatment are carried out in atmosphere；
Beneficial effects of the present invention are as follows：
1) ODS steel hardenabilities made from the preparation method are high, and residual austenite content is very low, can obtain full martensite
Tissue.W, V and Ta are carbides, with notable invigoration effect, and the ODS steel mechanical properties of preparation are apparently higher than biography
Steel prepared by smelting technology of uniting, while ductile-brittle transition temperature DBTT50 values are -80 DEG C and -90 DEG C, also inherits tradition well
The excellent toughness of smelting technology；
2) dissolving and agglomeration do not occur under the Y2O3 high temperature of Dispersed precipitate, and captures the vacancy cluster that irradiation is produced, shows
The void swelling for suppressing steel is write, the ODS steel of preparation has excellent anti-radiation performance；
3) martensite steel is single-phase martensite steel, is dispersed with substantial amounts of tiny precipitated phase to even dispersion in matrix,
By electronic microscope photos it can be found that these precipitated phases have a series of complex oxide and carbonitride to constitute, mechanical performance is excellent
More, its room temperature tensile intensity exceedes more than 880MPa, elongation percentage 20% or so, DBTT for tensile strength at -90 DEG C, 600 DEG C
390MPa, elongation percentage more than 20%；
4) preparation method can realize ODS steel batch draw, stabilize, low cost preparation demand, technological process
Short, manufacturing cost is relatively low.
Brief description of the drawings
Fig. 1 is the metallograph of the embodiment of the present invention 1；
The metallograph that Fig. 2 is example 950-1 in the embodiment of the present invention 1；
The ESEM macrograph that Fig. 3 is example 950-2 in the embodiment of the present invention 1；
The transmission electron microscope photo that Fig. 4 is example 950-4 in the embodiment of the present invention 1；
Fig. 5 is the energy spectrum analysis at Fig. 4 arrows in description of the invention accompanying drawing；
The metallographic structure that Fig. 6 is example 1050-7 in the embodiment of the present invention 2；
The ESEM macrograph that Fig. 7 is example 1050-8 in the embodiment of the present invention 2；
The precipitate for having identical power spectrum that Fig. 8 points to for precipitate energy spectrum analysis in circle in Fig. 7 and arrow；
Fig. 9 is example 1050-8 in the embodiment of the present invention 2 in 475 DEG C, 200dpa, the transmission electron microscope photograph of iron ion predose
Piece；
Figure 10 is transmission electron microscopes of the example 1050-8 after 475 DEG C, 200dpa, iron ion irradiation in the embodiment of the present invention 2
Photo.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is explained in further detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, and
It is not used in the restriction present invention.On the contrary, the present invention cover it is any be defined by the claims the present invention spirit and scope on do
Replacement, modification, equivalent method and scheme.Further, in order that the public has a better understanding to the present invention, below to this
It is detailed to describe some specific detail sections in the detailed description of invention.It is thin without these for a person skilled in the art
The description of section part can also understand the present invention completely.
The invention will be further described with specific embodiment below in conjunction with the accompanying drawings, but not as a limitation of the invention.
Below most preferred embodiment is enumerated for the present invention：
The present invention is a kind of preparation method of ODS steel, and general principle is based on combination strong between rare earth elements RE and O
Can, its standard molar formation enthalpy is higher than the oxide enthalpy of formation of other alloying elements, is easily created stable rare-earth oxidation
Thing, the incorporation way for adding opportunity and oxygen by rare earth element, make rare earth element be combined generation fine oxide particle with oxygen.
Appropriate iron oxide is for example added in the mould, and appropriate rare earth element yttrium is added into the molten steel after abundant deoxidation and is quickly cast,
Yttrium in molten steel captures the oxygen formation yittrium oxide in iron oxide, and Dispersed precipitate is in molten steel.By controlling the oxygen content in molten steel
With the addition of rare earth element, the melting ODS steel of rare earth oxide even dispersion is obtained.Rare earth element in the present invention is metal
Yttrium.Specific preparation method step is as follows：
Using the steel-making of vacuum induction/magnetic agitation technique, smelting temperature is in 100-200 DEG C of the iron fusing point above；
1. adding the oxide of iron in the mould, the oxide of the iron is Fe2O3
2nd, ingot iron etc. is added in crucible, power transmission when being first evacuated down to 10Pa；Start essence after vacuum ＜ 7Pa
Refining；
3rd, deoxidation depth is controlled by deoxidant element Al scaling loss in fusion process, as oxygen concentration [O]<10-5Shi Jia
Enter alloying element and carry out alloying；
4th, after alloying process terminates, rare earth element yttrium, the Y and Fe are added in the molten steel of melting2O3Material amount
The ratio between be 1:1-1.2:1, quickly molten steel is cast in mold after stirring, cast temperature is ensureing depending on molten steel flow
Molten steel temperature is reduced while mobility as far as possible；
5th, hot forging, hot rolling are carried out to pouring ingot casting (ODS steel)；
6th, the slab after hot-working is heat-treated, obtains single-phase martensite tissue, i.e. martensite steel.
Vacuum induction melting, teeming are carried out according to above-mentioned preparation method.To obtain the mechanical property of steel, steel ingot is entered
Row controlled rolling and controlled cooling is simultaneously optimized to Technology for Heating Processing, is controlled cold technique and is：Start rolling temperature in 1100-1050 DEG C, finish to gauge temperature
Degree control uses online misting cooling at 850-950 DEG C or so after rolling, Technology for Heating Processing is：Quenching and high tempering, wherein quenching
Fiery temperature is 850-1100 DEG C, and temperature is 710-800 DEG C, and tempering time is 90min-120min.
Embodiment 1：
One kind prepares ODS martensite steels based on the above method, and its various composition accounts for the percentage of gross mass：
C：0.09%th, Cr：8.9%th, Mn：0.51%th, W：2.09%th, N：0.055%th, Ta：0.12%th, Ti:0.45%th,
Si：0.13%th, V：0.045%th, Y：0.07%th, B<0.001%th, S<0.003%th, P<0.005%th, in Fe surpluses, mold
Fe2O3：0.14%；Finished product is made by following steps：
(a) according to the S1-S4 in preparation method of the present invention, vacuum melting prepares steel ingot or direct casting rod iron, has
Following various composition accounts for the percentage of gross mass：
C：0.09%th, Cr：8.9%th, Mn：0.51%th, W：2.09%th, N：0.055%th, Ta：0.12%th, Ti:0.45%th,
Si：0.13%th, V：0.045%th, Y：0.07%th, B<0.001%th, S<0.003%th, P<0.005%th, Fe surpluses；In mold
Fe2O3：0.14%.
(b) first time thermal deformation is carried out by the forging of steel ingot or direct casting rod iron or rolling so as to obtain half into
Product；
(c) semi-finished product are heated to 1150 DEG C of austenitizings, be again deformed by hot rolling until obtaining required
Shape and size；
(d) then product is made sample by part cooling again to less than 50 DEG C.And it is 950-1 to 950-6 to number；
(e) and by all samples while heated to 950 DEG C of temperature ranges are kept for 15min time cycle carry out austenitizing
Heat treatment；
(f) sample is cooled to less than 50 DEG C in water, the sample of different numberings is then heated separately to 720 DEG C again,
750 DEG C, 780 DEG C of temperature ranges simultaneously accordingly keep 20 and 120min time cycle to carry out tempering heat treatment.It is specific to compile
Number and its correspondence technique list in the following table.
The heat treatment process and its feature of the present invention is embodied in example set in following table.Its its composition accounts for gross mass
Percentage be：
C：0.09%th, Cr：8.9%th, Mn：0.51%th, W：2.09%th, N：0.055%th, Ta：0.12%th, Ti:0.45%th,
Si：0.13%th, V：0.045%th, Y：0.07%th, B<0.001%th, S<0.003%th, P<0.005%th, in Fe surpluses, mold
Fe2O3：0.14%；
Embodiment 2：
One kind prepares ODS martensite steels based on the above method, and its various composition accounts for the percentage of gross mass：
C：0.09%th, Cr：9.3%th, Mn：0.55%th, W：2.5%th, N：0.06%th, Ta：0.19%th, Ti:0.53%th, Si：
0.13%th, V：0.045%th, Y：0.2%th, B<0.001%th, S<0.003%th, P<0.005%th, the Fe in Fe surpluses, mold2O3：
0.4%；Finished product is made by following steps：
(a) according to the S1-S4 in preparation method of the present invention, vacuum melting prepares steel ingot or direct casting rod iron, has
Following various composition accounts for the percentage of gross mass：
C：0.09%th, Cr：9.3%th, Mn：0.55%th, W：2.5%th, N：0.06%th, Ta：0.19%th, Ti:0.53%th, Si：
0.13%th, V：0.045%th, Y：0.2%th, B<0.001%th, S<0.003%th, P<0.005%th, the Fe in Fe surpluses, mold2O3：
0.4%.
(b) first time thermal deformation is carried out by the forging of steel ingot or direct casting rod iron or rolling so as to obtain half into
Product；
(c) semi-finished product are heated to 1200 DEG C of austenitizings, be again deformed by hot rolling until obtaining required
Shape and size；
(d) then product is made sample by part cooling again to less than 50 DEG C.And respectively numbering be 1000-5 extremely
1000-6 and 1050-7 to 1050-8；
(e) sample is heated separately to 1000 DEG C again and 1050 DEG C of temperature ranges is kept for 20min time cycle carry out Austria
Family name's bodyization is heat-treated；
(f) sample is cooled to less than 50 DEG C in water, the sample of different numberings is then heated separately to 720 DEG C again,
780 DEG C of temperature ranges simultaneously accordingly keep 20 and 120min time cycle to carry out tempering heat treatment.Specific numbering and its
Correspondence technique is listed in upper table.
Following table gives the mechanical property contrast of the specific embodiment of the invention 1 and 2.
As seen from the table, what the ODS RAFM steel mechanical properties prepared by this technique were prepared apparently higher than traditional smelting technology
Steel.Ductile-brittle transition temperature DBTT50 values are -80 DEG C and -90 DEG C simultaneously, and the good tough of traditional smelting technology is also inherited well
Property.As can be seen that there is no helium bubble aggregation after 475 DEG C, 200dpa predoses from Fig. 9-Figure 10, illustrate that material has excellent
Anti-radiation performance.
One kind of embodiment described above, simply more preferably embodiment of the invention, those skilled in the art
The usual variations and alternatives that member is carried out in the range of technical solution of the present invention all should be comprising within the scope of the present invention.
Claims (9)
1. a kind of preparation method of oxide dispersion intensifying steel, it is characterised in that the preparation method adds iron in the mould
Oxide, appropriate rare earth element is added into the molten steel after abundant deoxidation and is quickly cast in mold, by rare earth element with
The oxide reaction of iron obtains oxide dispersion intensifying steel (ODS steel), and the preparation method is specifically included：
S1：The oxide of iron is added in the mould；
S2：Ingot iron is added into crucible for smelting, power transmission when being evacuated down to 10Pa；
S3：It is evacuated down to vacuum<Refined after 7Pa, control deoxidation deep by deoxidant element Al scaling loss in refining process
Degree, as oxygen concentration [O]<10-5When add alloying element carry out alloying；
S4：Rare earth element is added into the molten steel for completing alloying, quickly molten steel is cast in mold after stirring, ODS is obtained
Steel.
2. preparation method according to claim 1, it is characterised in that it is yttrium, the S1 that rare earth element is added in the S4
The middle oxide for adding iron is Fe2O3, the Y and Fe2O3The ratio between the amount of material be 1:1-1.2:1.
3. preparation method according to claim 2, it is characterised in that melting and vacuumized in the S2 using vacuum sense
Should/magnetic agitation technique, smelting temperature cast temperature in 100-200 DEG C of the iron fusing point above, the S4 regard molten steel flow and
It is fixed, molten steel temperature is reduced as far as possible while mobility is ensured.
4. a kind of martensite steel, based on the preparation method described in one of the claims 1-3, it is characterised in that the geneva
The ODS steel hot forging as made from the above method of body steel, hot rolling, hot-working and heat treatment gained, the ODS steel various composition account for total matter
The percentage of amount：C：0.08~0.15%, Cr：8.0~9.9%, Mn：0.45~0.6%, W：2.0~2.5%, N：0.05~
0.07%th, Ta：0.10~0.20%, Ti:0.4~0.55%, Si：0.10~0.15%, V：0.04~0.05%, Y：0.01~
0.5%th, B<0.001%th, S<0.003%th, P<0.005%th, Fe surpluses.
5. martensite steel according to claim 4, it is characterised in that specific steps prepared by the martensite steel include：
(a) progress first time thermal deformation is made or rolled to ODS steel forgings made from S4, obtain semi-finished product；
(b) semi-finished product are heated to 1150 DEG C -1200 DEG C of scope, are again deformed by hot rolling until obtaining required
Shape and size product；
(c) treat that part cooling is to room temperature described in (b), then be heated to 950-1050 DEG C of temperature range to keep 15-25min,
Carry out austenitation heat treatment；
(d) then product is heated to 750-790 DEG C by the part cooling after the austenitation heat treatment again to less than 50 DEG C
Temperature range keeps 90-130min, carries out tempering heat treatment and obtains martensite steel.
6. martensite steel according to claim 5, it is characterised in that in the step (a) ODS steel in preparation process,
Rare earth element yttrium is added after deoxidation completion, is also the alloying element of last addition in alloying process, while online
Detect alloying element and augment alloying element and oxygen activity according to test result.
7. martensite steel according to claim 6, it is characterised in that the temperature of forging or rolling in the step (a)
Scope is spent at 1150 DEG C -1000 DEG C.
8. martensite steel according to claim 7, it is characterised in that the step (c) starts rolling temperature at 1100 DEG C,
Finishing temperature control uses online misting cooling at 900 DEG C after rolling.
9. martensite steel according to claim 8, it is characterised in that the heat treatment system of the austenitizing of the step (c)
Spend and be：950-1050 DEG C/15-25min is quenched；750-780 DEG C/90-120min is tempered, the cooling after austenitation heat treatment
Operation is carried out in water, and the cooling operations after the tempering heat treatment of the step (d) are carried out in atmosphere.
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| 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 |
| CN107881368A (en) * | 2017-11-23 | 2018-04-06 | 宁波升鸿机械设备有限公司 | A kind of blower fan |
| CN108342661A (en) * | 2018-01-22 | 2018-07-31 | 江苏理工学院 | A kind of fired power generating unit heat-resisting steel alloy material and its manufacturing process |
| CN108754079A (en) * | 2018-06-13 | 2018-11-06 | 武汉科技大学 | It is a kind of to promote the heat treatment method that nano-carbide is precipitated in steel containing W alloy |
| CN108893580B (en) * | 2018-07-10 | 2019-08-16 | 中国科学院金属研究所 | A kind of nitride strengthening ODS steel and preparation method thereof |
| CN110541122A (en) * | 2019-10-24 | 2019-12-06 | 东莞市中瑞金属材料有限公司 | novel alloy steel and manufacturing process thereof |
| CN111349842B (en) * | 2020-02-27 | 2021-05-18 | 北京科技大学 | Method for preparing oxide dispersion strengthened steel through high-flux continuous smelting |
| CN111979469B (en) * | 2020-07-31 | 2021-07-27 | 青岛理工大学 | Preparation method of oxide dispersion strengthened steel based on powder forging |
| CN112481544B (en) * | 2020-10-21 | 2021-09-17 | 上海大学 | Preparation method of high-density oxide dispersion strengthened steel |
| CN115491600A (en) * | 2022-09-19 | 2022-12-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Ferrite/martensite heat-resistant steel for lead-bismuth pile and preparation method thereof |
| CN115491612A (en) * | 2022-09-26 | 2022-12-20 | 中国科学院金属研究所 | High-strength low-activation steel and preparation method thereof |
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| FR2777020B1 (en) * | 1998-04-07 | 2000-05-05 | Commissariat Energie Atomique | PROCESS FOR MANUFACTURING A FERRITIC - MARTENSITIC ALLOY REINFORCED BY OXIDE DISPERSION |
| JP3359007B2 (en) * | 1999-08-04 | 2002-12-24 | 三菱重工業株式会社 | Oxide dispersion strengthened steel |
| CN101328562B (en) * | 2008-07-17 | 2011-01-26 | 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 |
| CN100552053C (en) * | 2008-07-17 | 2009-10-21 | 鞍钢股份有限公司 | The preparation method of fine oxide dispersion steel |
| CN102994884B (en) * | 2012-12-03 | 2014-10-29 | 东北大学 | Efficient preparation method for nanostructure oxide dispersion strengthening steel |
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