CN105238986B - A kind of preparation method of Cr Y O nanocluster oxide dispersion intensifying steel - Google Patents
A kind of preparation method of Cr Y O nanocluster oxide dispersion intensifying steel Download PDFInfo
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Abstract
It is an object of the invention to provide a kind of preparation method of the Cr Y O nanocluster oxide dispersion intensifying low activation steels suitable for following fusion reactor：To Cr Y ball milling mixing powder is added in low activation steel matrix powder, make the Cr Y produced in mechanical milling process dissolve each other metal and not molten simple metal Y powder respectively with the oxygen atom generation oxidation reaction of powder adsorption, in-situ preparation Cr Y O nanoclusters and Y2O3Inertia particle, its technological process is：Cr Y ball milling mixing powder is prepared first, then the mixed-powder of low activation steel master alloy powder and Cr Y ball-milled powders is prepared, hot setting forming processes are carried out to mixed powder for alloy again, is finally heat-treated, obtain Cr Y O nanocluster oxide dispersion intensifying low activation steels.The method can effectively reduce the free oxygen content and impurity content of oxide dispersion strengthening low activity martensitic steel, obtain Cr Y O nanocluster Dispersed precipitates, and microscopic structure is uniform, the oxide dispersion intensifying low activation steel of excellent in mechanical performance.
Description
Technical field
The invention belongs to Flouride-resistani acid phesphatase field of metal preparation, and in particular to a kind of dispersed oxide for fusion reactor is strong
Change the preparation method of low activation steel, the oxygen for possessing anti-strong neutron irradiation and excellent mechanical property can be obtained using the preparation method
Compound dispersion-strengthened steel.
Background technology
With the aggravation of energy crisis, development nuclear energy turns into the main trend of Future New Energy Source.At present, fission-type reactor
Have been able to successfully operate, the main disintegration energy using uranium atom generates electricity.In China Zhejiang and the province's nuclear power use ratio of Guangdong two
Reach 13%.Refine and enriched uranium complex process, it is relatively costly.Comparatively, deuterium and tritium fuel needed for fusion reactor
It is more easy to obtain, deuterium and tritium can be refined from seawater and obtained, and the nuke rubbish produced after nuclear fuel use is less.Even so, core
It is only that can be realized in theoretical calculation that fusion energy generates electricity, actual not to be applied also.Because nuclear fusion reaction is difficult to
Controlled when long, fusion pile structure is increasingly complex, and in fusion reactor structural material service condition it is more severe.For example, fission-type reactor
The neutron energy that middle fission of uranium atom is produced is about 1MeV, and material undergoes the lower spoke for producing of low energy neutron irradiation of 200dpa dosage
It is about 0.1appm He/dpa and 0.1appm H/dpa according to damaging.By comparison, in fusion reactor there is nuclear fusion reaction in tritium atom
The neutron energy of generation is up to 14.1MeV.The first wall construction material and tritium in fusion reactor breed coating at 320~700 DEG C
It is on active service under hot conditions, and can be irradiated more than 50dpa high-energy neutrons by dosage during military service, the irradiation damage of generation reaches
To 12appm He/dpa and 45appm H/dpa.Consider from the harsh Service Environment of fusion reactor structural material, at present suitable for core
Far from the use requirement for meeting following fusion reactor, this requires that following fusion reactor structural material possesses more to the structural material of fission-type reactor
Plus excellent mechanical performance, creep rupture performance, pyro-oxidation resistance and anti-neutron irradiation performance.Therefore, exploitation is applied to
The novel high-performance Flouride-resistani acid phesphatase structural material of following fusion reactor seems further important.
At present, with low activation steel as matrix, indifferent oxide nano particle is directly added into, using Mechanical Alloying system
Standby oxide dispersion intensifying low activation steel can improve the creep rupture performance and anti-neutron irradiation performance of material.In general,
The nano-scale particle being artificially introduced is divided into two classes.The first kind is directly to add Y2O3Nanometer inert particle (20~30nm).Equations of The Second Kind
It is addition Ti and Y2O3, Ti and Y2O3React the smaller Y of generation in the hot setting forming process in later stage2Ti2O7
(<20nm).These indifferent oxide particles (Y2O3And Y2Ti2O7) will not be roughened or melt with the rising of temperature, and i.e.
When being on active service under high-temperature alternate ambient stress when making long, indifferent oxide particle remain able to stabilization be present in matrix and
Being capable of pinning dislocation, the sliding of obstruction dislocation, reinforced alloys, so as to improve the mechanical behavior under high temperature and high-temperature stability of material；
Meanwhile, the helium atom that nanoscale composition granule is produced when can catch a small amount of active element in matrix through neutron irradiation, resistance
Only helium atom aggregation is as helium bubble.
But, there is a fatal weakness in the oxide dispersion intensifying steel that above-mentioned preparation method is obtained, i.e., raw in matrix
Into extra oxide, material property is deteriorated.Because metal powder granulates are smaller, surface-active is larger, easily adsorption of oxygen,
Therefore oxygenation is inevitable, the oxygen in the oxide dispersion intensifying steel matrix that above-mentioned preparation method is obtained in preparation process
Content is higher, and oxygen content higher generates detrimental oxide Fe in eventually resulting in steel matrix2O3、FeCr2O4Etc., force steel
Elevated temperature strength reduction, the anti-radiation performance of material deteriorates.The extra oxide produced in these preparation process is to pass through
What the Technology for Heating Processing in later stage was eliminated.
The content of the invention
It is strong it is an object of the invention to provide a kind of Cr-Y-O nanocluster dispersed oxides suitable for following fusion reactor
Change the preparation method of low activation steel, the method can effectively reduce the free oxygen content of oxide dispersion strengthening low activity martensitic steel
And impurity content, Cr-Y-O nanocluster Dispersed precipitates are obtained, microscopic structure is uniform, and the oxide of excellent in mechanical performance is more
Reinforcing low activation steel is dissipated, the elevated temperature strength and anti-neutron irradiation performance of the oxide dispersion intensifying low activation steel is further improved.
For the control oxygen problem of oxide dispersion intensifying steel, the present invention is creatively proposed using high-energy-milling twice
Prepare Cr-Y-O nanocluster oxide dispersion intensifying low activation steels.By first ball milling Cr-Y mixed-powders, obtain Cr-Y and dissolve each other
The mixed-powder of metal and the not molten simple metal Y in part, makes it generate Cr- in the high-temperature molding processing procedure situ in later stage respectively
Y-O nanoclusters and Y2O3Nano particle.The preparation method can not only obtain the nanocluster of complexity, and can be effectively
The free oxygen content and impurity content in matrix are reduced, the elevated temperature strength and anti-neutron irradiation performance of material is increased substantially, is
The design of following fusion reactor structural material provides new approaches.Document patent 1 (application number 201010513441.3) and document are special
The preparation method of oxide-dispersed alloy is refer in sharp 2 (application numbers 200810021329.0), i.e., to different matrix
In directly add indifferent oxide particle.But patent document 1,2 does not mention mentality of designing of the present invention, that is, carry out two
Secondary ball-milling technology obtains generated in-situ Cr-Y-O nanoclusters and Y2O3Inertia particle.Additionally, preparation method of the present invention
The control oxygen problem in current oxide dispersion intensifying steel production process is solved, is the industrialization of following oxide dispersion intensifying steel
Production provides experiment basis.
The present invention adopts the following technical scheme that realization：
A kind of preparation method of Cr-Y-O nanoclusters oxide dispersion intensifying steel, it is characterised in that to low activation steel base
Cr-Y ball milling mixing powder is added in body powder, makes that the Cr-Y produced in mechanical milling process dissolves each other metal and not molten simple metal Y powder divides
There is oxidation reaction, in-situ preparation Cr-Y-O nanoclusters and Y in the oxygen atom not with powder adsorption2O3Inertia particle, is reduced
The generation of detrimental oxide, while the free oxygen content in controlling oxide dispersion intensifying steel matrix, its technological process is：It is first
Cr-Y ball milling mixing powder is first prepared, low activation steel Fe-C-Cr-W-V-Ta-Mn-Si master alloy powders is then prepared (i.e. female to close
The mass fraction of Cr is 8-10% in bronze end) and Cr-Y ball-milled powders mixed-powder, then height is carried out to mixed powder for alloy
Warm curing molding treatment, is finally heat-treated, and obtains Cr-Y-O nanocluster oxide dispersion intensifying low activation steels.
The low activation steel matrix powder composition range is 8.0-10.0%Cr, 1-3%W, 0.1-0.3%V, 0.01-
0.25%Ta, 0.2-1.0%Mn, 0.05-1.50%Si, balance of Fe.In fact, Cr-Y-O nanometers of acquisition of the present invention
The preparation method of cluster is applied to the low activation ferrito-martensite steel of following fusion reactor all kinds.
The preparation method of Cr-Y-O nanoclusters oxide dispersion intensifying steel of the present invention, it is characterised in that Cr-Y balls
Grind mixed-powder preparation method be：Mass ratio is taken for Cr：Y=2.3~9:1 Cr powder, Y powder, high energy is carried out after being mixed
Ball milling, design parameter is：Ball-milling medium be the hardened steel balls of Φ 6, milling atmosphere be 99.99% argon gas, ball material mass ratio be 8~
10：1, Ball-milling Time 0.5-4h, rotating speed are more than or equal to 800r/min.
The preparation method of Cr-Y-O nanoclusters oxide dispersion intensifying steel of the present invention, it is characterised in that using high
Energy ball grinding method prepares the mixed-powder of low activation steel Fe-C-Cr-W-V-Ta-Mn-Si foundry alloys and Cr-Y ball-milled powders：Ball milling
Medium is Φ 6 and Φ 10 mixing hardened steel balls, and milling atmosphere is 99.99% argon gas, and ball material mass ratio is 8~10:1, during ball milling
Between 40-70h, rotating speed is 350-450r/min.
The preparation method of Cr-Y-O nanoclusters oxide dispersion intensifying steel of the present invention, it is characterised in that alloy is mixed
Closing powder metallurgy cure process is：Mixed-powder first fills jacket pumping, and vacuum is not less than 10-1Pa, temperature 400-550
DEG C, the time is 4-5h, by high temperature insostatic pressing (HIP) curing molding, pressure 120-150MPa, 1050-1200 DEG C of temperature, during heat-insulation pressure keeping
Between 3-5h；Or use spark plasma sintering method curing molding, pressure 35-50MPa, 1050-1100 DEG C of temperature, heat-insulation pressure keeping
Time 20-30min.
The preparation method of Cr-Y-O nanoclusters oxide dispersion intensifying steel of the present invention, it is characterised in that specific system
Standby technological process and parameter are as follows：
It is prepared by a, Cr-Y ball-milled powder：Mass ratio is taken for Cr：Y=2.3~9:1 Cr powder, Y powder, ball-milling medium is that Φ 6 is hard
Matter steel ball, milling atmosphere is 99.99% argon gas, and ball material mass ratio is 8~10：1, Ball-milling Time 0.5-4h, rotating speed is more than or equal to
800r/min；
It is prepared by the mixed-powder of b, low activation steel Fe-C-Cr-W-V-Ta-Mn-Si matrix powders and Cr-Y ball-milled powders：Ball
Grinding media is Φ 6 and Φ 10 mixing hardened steel balls, and milling atmosphere is 99.99% argon gas, and ball material mass ratio is 8~10：1, ball milling
Time 40-70h, rotating speed is 350-450r/min；
C, mixed powder for alloy cure process：Mixed-powder first fills jacket pumping, and vacuum is not less than 10-1Pa, temperature
400-550 DEG C of degree, the time is 4-5h, and by high temperature insostatic pressing (HIP) curing molding, pressure 120-150MPa, 1050-1200 DEG C of temperature is protected
Warm dwell time 3-5h；Or use spark plasma sintering method curing molding, pressure 35-50MPa, 1050-1100 DEG C of temperature,
Heat-insulation pressure keeping time 20-30min.
Preparation method of the present invention seems simple, but the preparation process of secondary high-energy ball milling is carried out to mixed-powder
It is the Cr-Y-O nanoclusters and Y to form Dispersed precipitate2O3The prerequisite of nano-oxide particles, and the later stage curing molding
Treatment is to form Cr-Y-O nanoclusters and Y2O3The necessary condition of oxide particle.Below will be to Cr-Y-O of the present invention
The step of preparation process of nanocluster oxide dispersion intensifying low activation steel is illustrated one by one.
The first step, prepares Cr-Y ball-milled powders.This process is dissolved each other metal dust and few to obtain the Cr-Y of stabilization
The mixed-powder of the not molten simple metal Y powder of amount.In high-energy mechanical milling process in short-term, the alloying element in Cr-Y systems can appoint
Meaning proportioning, and the soldering repeatedly of powder and the broken defect that increased in reaction interface area and powder particle are close in ball milling
Degree so that the reaction that could only occur under the high temperature conditions can be rapidly completed at ambient temperature, promote two kinds of metals fast
Speed is dissolved each other；Meanwhile, hardened steel ball is mutually collided and rolls powder, and metal dust is smashed and is well mixed, and reduces mixed-powder
In element segregation.Therefore, when preparing Cr-Y ball-milled powders, rotational speed of ball-mill and ratio of grinding media to material are improved and is promoted with providing more energy
Cr-Y dissolves each other；Ensure the degree of purity of milling atmosphere, reduce oxidation of the simple metal Y powder in mechanical milling process.Therefore, it is of the present invention
Cr-Y powder rotational speed of ball-mill is more than or equal to 800r/ in the preparation method of Cr-Y-O nanocluster oxide dispersion intensifying low activation steels
Min, Ball-milling Time is 0.5~4h, and ratio of grinding media to material is (8~10):1, milling atmosphere is 99.99% argon gas atmosphere, and ball-milling medium is
The hardened steel balls of Φ 6.
Second step, prepares the mixed powder of low activation steel Fe-C-Cr-W-V-Ta-Mn-Si matrix powders and Cr-Y ball-milled powders
End.Cr-Y ball-milled powders are sufficiently mixed uniformly with matrix comminuted steel shot, just can guarantee that Cr-Y-O nanoclusters and Y2O3Nano particle disperse
Distribution is in the base.During mixed-powder ball milling, the Cr-Y that the first step is prepared dissolve each other powder and not molten simple metal Y powder will with it is low
There is the process of the cold welding of cold welding-broken-again-broken again in activation steel Fe-C-Cr-W-V-Ta-Mn-Si matrix powders, compel again
Cr-Y powder is set to be well mixed with matrix powder, while introduce more vacancy defects, in being later stage hot setting forming process
Cr-Y-O nanoclusters and Y2O3The forming core of nano particle provides advantage.Therefore, Cr-Y-O nanoclusters of the present invention
Low activation steel Fe-C-Cr-W-V-Ta-Mn-Si matrix powders and Cr-Y in the preparation method of oxide dispersion intensifying low activation steel
The mixed-powder milling parameters of ball-milled powder are：Ball-milling medium is Φ 6 and Φ 10 mixing hardened steel balls, and milling atmosphere is
99.99% argon gas, ball material mass ratio is (8~10):1, Ball-milling Time 40-70h, rotating speed is 350-450r/min.
3rd step, hot setting forming processes are carried out to mixed powder for alloy.Two step ball-milling technologies of early stage are in powder
Substantial amounts of vacancy defect is introduced in last particle, is Cr-Y-O nanoclusters and Y2O3Nano particle forming core provides advantage.But
Be forming core also need to it is extraneous energy is provided, the only energy barrier needed for energy crosses forming core could complete Cr-Y-O nanometers
Cluster and Y2O3The forming core of nano particle.Additionally, in second step ball milling, phase between Cr-Y ball-milled powders and matrix steel powder particle
Mutual cold welding adhesion, Cr-Y elements a small amount of in crystal defect high energy region can with matrix comminuted steel shot alloying element phase counterdiffusion, but
It is that most of Cr-Y powder is to be wrapped by matrix alloy powder.2 points of considerations based on more than, during hot setting forming processes
The energy of offer is extremely important to nanocluster forming core and diffusion of alloy elements.Temperature should reach single phase austenite during curing molding
Phase region, promotes the diffusion of alloying element, and alloy powder to soften, it is easy to which pressing reaches Physical Metallurgy combination degree；Additionally, as far as possible
The gas molecule of powder adsorption is dispelled, the generation of detrimental oxide is reduced.Therefore, Cr-Y-O nanoclusters of the present invention
The high temperature insostatic pressing (HIP) curing molding before processing of the alloy powder in the preparation method of oxide dispersion intensifying low activation steel, mixed-powder
First dress jacket pumping, vacuum is not less than 10-1Pa, 400-550 DEG C of temperature, the time is 4-5h, by high temperature insostatic pressing (HIP) curing molding,
Pressure 120-150MPa, 1050-1200 DEG C of temperature, heat-insulation pressure keeping time 3-5h；Or using the solidification of spark plasma sintering method
Shaping, pressure 35-50MPa, 1050-1100 DEG C of temperature, heat-insulation pressure keeping time 20-30min.
The advantage of the invention is that using Cr-Y powder and low activation steel Fe-C-Cr-W-V-Ta-Mn-Si matrixes comminuted steel shot with
The high-energy-milling twice of Cr-Y ball-milled powders prepares Cr-Y-O nanocluster oxide dispersion intensifying low activation steels, prepares
Generated in-situ small yardstick Cr-Y-O complexity nanoclusters and Y can be not only obtained in journey2O3Nano particle, and can be effective
Ground reduces free oxygen content and impurity content in matrix, increases substantially the elevated temperature strength and anti-neutron irradiation performance of material.
The preparation method of Cr-Y-O nanoclusters oxide dispersion intensifying steel of the present invention is setting for following fusion reactor structural material
Meter provides new approaches, while solving the control oxygen problem in current oxide dispersion intensifying steel production process.
Brief description of the drawings
Fig. 1 is the displaing micro tissue topography of pure Cr powder, and simple metal Cr powder structure in the form of sheets, particle size reaches 10~30 μ
m。
Fig. 2 is the displaing micro tissue topography of pure Y powder, because the electric conductivity of simple metal Y powder is bad, therefore its stereoscan photograph
White dichromatism is presented, particle size is suitable with simple metal Cr powder, about 10~30 μm.
Fig. 3 is 9 for the quality proportioning of simple metal Cr and Y:1, the displaing micro tissue topography after ball milling 4h, Cr-Y is mixed as seen from the figure
Close powder particle uniform particle sizes (about 1.8 μm).
Fig. 4 is 9 for the quality proportioning of simple metal Cr and Y:1 and 2.3:After 1 mixed-powder difference ball milling 0.5h and 4h
XRD spectrum；Compared with the pre- ball-milled powder of ball milling 0.5h, with the diffraction maximum peak width of the 4h that increases to, Cr and Y of Ball-milling Time
Become big, diffraction peak intensity diminishes, and diffraction maximum peak position is not moved significantly.This shows with the increase of Ball-milling Time,
Powder average particle size is gradually reduced.Additionally, the diffraction peak intensity of Y understands that the Y diffraction peak intensities after ball milling 4h are bright in Comparative map
It is aobvious to be weaker than the Y diffraction peak intensities after ball milling 0.5h, and Cr-Y ratios are 9:Y diffraction peak intensities when 1 are significantly less than Cr-Y ratios
It is 2.3:Y diffraction peak intensities when 1.After this shows Cr-Y mixed-powder ball millings 4h, most of simple metal Y has been solid-solution in Cr bases
In body, the final Cr-Y for obtaining stabilization dissolves each other the mixed-powder of metal and a small amount of not molten simple metal Y.
Fig. 5 is that simple metal Cr and Y quality proportioning are 9:The mixed-powder of 1 ball milling 4h is incubated 4h under 1150 DEG C of argon gas atmospheres
XRD spectrum afterwards；As seen from the figure, after carrying out soak treatment to Cr-Y ball-milled powders under protective atmosphere, Cr-Y dissolves each other gold
There is oxidation reaction generation Cr-Y-O nanoclusters, Cr respectively in category and simple metal Cr and Y2O3And Y2O3Nano particle.
Fig. 6 be by composition proportion be 9:Cr-Y ball-milled powders after 1 ball milling 4h are added to low activation steel Fe-C-Cr-W-V-
Displaing micro tissue topography after ball milling 70h, the mixed powder for alloy uniform particle sizes after ball milling in Ta-Mn-Si matrix comminuted steel shots, size is 10
~20 μm.
Fig. 7 is the displaing micro tissue topography of the steel of embodiment 1, and as seen from the figure, Dispersed precipitate tiny in low activation steel matrix
Cr-Y-O and Y2O3Particle.
Specific embodiment
The present invention is described in detail below by way of embodiments and comparative examples.
Embodiment steel and comparative example steel system are prepared from powder metallurgy process, are all heat-treated (normalizing by identical
980-1100 DEG C/50-70min/ air coolings+760-800 DEG C of tempering/90-120min/ air coolings) after, test at room temperature embodiment steel and
The tensile property of comparative example steel.
The low activation steel matrix used in the present invention is 8-10%Cr low activation martensitic steel powder, the content of each alloying element
(mass percent wt.%) is as shown in table 1.In order to ensure the accuracy of mentality of designing of the present invention, Cr-Y ball milling powders are developed first
End, and being detected to its oxygen content, can probe into simple metal Y and be solid-solution in Cr protect simple metal Y not oxidized.Y is chemically
Matter is more active, it is easy to oxidation reaction occurs with the oxygen in air, generates Y2O3Oxide.The purpose for adding Y is for Y
Oxygen can be taken by force during cured later is molded, the generation of detrimental oxide is reduced.Theoretical according to high-temperature oxydation, Cr has very
Good oxidation-resistance property, therefore, pre- ball milling is carried out to Y and Cr mixed-powders, Y can be protected not oxidized, and rear
During phase curing molding, being capable of in-situ preparation Cr-Y-O nano-oxides in the base.
Fig. 1,2 are seen by the displaing micro tissue topography of pure Cr powder and pure Y powder, prepare Cr-Y ball milling mixing powder：The matter of Cr powder and Y powder
Amount is than being 2.3:Isosorbide-5-Nitrae:1 and 9:1, ratio of grinding media to material is 10:1, milling atmosphere is inert gas Ar, respectively ball milling 0.5h, 1.0h,
2.0h、4.0h.The particle diameter of Cr-Y powder after measurement ball milling, as a result as shown in table 2, its displaing micro tissue topography and XRD spectrum are shown in figure
3-6.With the extension of Ball-milling Time, the particle diameter of powder is less and less, because with the growth of Ball-milling Time, energy is continuous
, constantly there is the cold welding process of cold welding-broken-again in accumulation, powder diameter is substantially refined between powder.It is prepared by different ball-milling technologies
The Cr-Y mixed-powders for going out carry out oxygen content detection, as a result as shown in table 3.The powder of heterogeneity, different ball-milling technologies is existed
The oxygen content in powder is measured after being exposed 24 hours in air, it is possible to find Cr-Y ratios are 9:1 and 2.3:When 1, mixed-powder ball
Oxygen content after mill 0.5h is significantly greater than the oxygen content of ball milling 4h.The Cr-Y mixed-powders of ball milling 0.5h expose 24h in atmosphere
Oxygen content has increased slightly after oxygen content does not change afterwards, but the Cr-Y mixed-powders of ball milling 4h expose 24h in atmosphere, this
Because the Cr-Y mixed-powder particle diameters of ball milling 4h are too small, particle surface easily adsorbs air, causes oxygen content to be increased slightly.To sum up
Described, Cr-Y ball-milled powders are relatively stablized, and antioxygenic property is preferable.
Mass percent in the low activation martensitic steel powder of table 1. shared by each alloying element
Cr-Y mixed-powder particle diameters after the ball milling different time of table 2.
Table 3.Cr-Y ball-milled powders expose the oxygen content before and after 24h in atmosphere
Embodiment 1
The addition 7.0wt.%Cr- in low activation steel matrix powder (i.e. Fe-C-Cr-W-V-Ta-Mn-Si master alloy powders)
Y ball-milled powders (Y contents are 0.7% in matrix after conversion, in actual matrix Y contents for 0.74%), wherein Cr-Y ball-milled powders
Material quality ratio is Cr：Y=9:1, the ball milling 4h under the conditions of rotating speed is 1425r/min；Gained mixed-powder is through high-energy ball milling (ball
Grinding media is Φ 6 and Φ 10 mixing hardened steel balls, and milling atmosphere is 99.99% argon gas, and ball material mass ratio is 10:1, Ball-milling Time
70h, rotating speed is 450r/min) and the treatment of spark plasma sintering method curing molding (pressure 50MPa, 1090 DEG C of temperature, insulation
Dwell time 20min) after, Cr-Y-O nanocluster oxide dispersion intensifying low activation steels are obtained, its microscopic structure is shown in Fig. 7.
Embodiment 2
The addition 7.0wt.%Cr- in low activation steel matrix powder (i.e. Fe-C-Cr-W-V-Ta-Mn-Si master alloy powders)
Y ball-milled powders (Y contents are 0.7% in matrix after conversion, in actual matrix Y contents for 0.74%), wherein Cr-Y ball-milled powders
Material quality ratio is Cr：Y=9:1, the ball milling 4h under the conditions of rotating speed is 1425r/min；Gained mixed-powder is through high-energy ball milling (ball
Grinding media is Φ 6 and Φ 10 mixing hardened steel balls, and milling atmosphere is 99.99% argon gas, and ball material mass ratio is 10:1, Ball-milling Time
70h, rotating speed is 450r/min) and high temperature insostatic pressing (HIP) curing molding treatment (powder jacket be evacuated, vacuum be less than 10-1Pa, temperature
450 DEG C, the time is 4h, by hip moulding, pressure 130MPa, 1050 DEG C of temperature, heat-insulation pressure keeping time 3h) after, obtain
Cr-Y-O nanocluster oxide dispersion intensifying low activation steels.
Embodiment 3
The addition 1.5wt.%Cr- in low activation steel matrix powder (i.e. Fe-C-Cr-W-V-Ta-Mn-Si master alloy powders)
Y ball-milled powders (Y contents are 0.35% in matrix after conversion, in actual matrix Y contents for 0.33%), wherein Cr-Y ball-milled powders
Material quality ratio is Cr：Y=2.3:1, the ball milling 2h under the conditions of rotating speed is 1425r/min；Gained mixed-powder is through high-energy ball milling
(ball-milling medium is Φ 6 and Φ 10 mixing hardened steel balls, and milling atmosphere is 99.99% argon gas, and ball material mass ratio is 10:1, ball milling
Time 50h, rotating speed is 450r/min) and the treatment of spark plasma sintering method curing molding (pressure 40MPa, 1100 DEG C of temperature,
Heat-insulation pressure keeping time 30min) after, obtain Cr-Y-O nanocluster oxide dispersion intensifying low activation steels.
Embodiment 4
The addition 2.5wt.%Cr- in low activation steel matrix powder (i.e. Fe-C-Cr-W-V-Ta-Mn-Si master alloy powders)
Y ball-milled powders (Y contents are 0.35% in matrix after conversion, in actual matrix Y contents for 0.33%), wherein Cr-Y ball-milled powders
Material quality ratio is Cr：Y=4:1, the ball milling 0.5h under the conditions of rotating speed is 1425r/min；Gained mixed-powder is through high-energy ball milling
(ball-milling medium is Φ 6 and Φ 10 mixing hardened steel balls, and milling atmosphere is 99.99% argon gas, and ball material mass ratio is 10:1, ball milling
Time 40h, rotating speed is 450r/min) and the treatment of spark plasma sintering method curing molding (pressure 35MPa, 1100 DEG C of temperature,
Heat-insulation pressure keeping time 25min) after, obtain Cr-Y-O nanocluster oxide dispersion intensifying low activation steels.
Comparative example 1
0.5wt.% simple metal Y powder is added in low activation steel matrix powder, (ball-milling medium is Φ 6 through high-energy ball milling
Mix hardened steel ball with Φ 10, milling atmosphere is 99.99% argon gas, and ball material mass ratio is 10:1, Ball-milling Time 70h, rotating speed is
450r/min) (pressure 50MPa, 1090 DEG C of temperature, heat-insulation pressure keeping time are processed with spark plasma sintering method curing molding
After 20min), oxide dispersion intensifying low activation steel is obtained.
Comparative example 2
0.3wt.%Y is added in low activation steel matrix powder2O3Powder, through high-energy ball milling, (ball-milling medium is Φ 6 and Φ
10 mixing hardened steel balls, milling atmosphere is 99.99% argon gas, and ball material mass ratio is 10:1, Ball-milling Time 50h, rotating speed is 450r/
Min), powder jacket pumping (vacuum 10-1Pa, 450 DEG C of temperature, time 4h) and high temperature insostatic pressing (HIP), curing molding (temperature 1200
DEG C, pressure 150MPa, heat-insulation pressure keeping time 4h) after, obtain final oxide dispersion intensifying low activation steel.
The intensity of table 4. each embodiment steel and comparative example steel at room temperature
By above-mentioned tensile property test result, the intensity for adding the steel of embodiment 1~4 of Cr-Y ball-milled powders is obvious
Higher than addition simple metal Y and Y2O3The comparative example 1 of nano particle, 2 steel.Wherein (adding ingredient proportioning is 9 to the steel of embodiment 1:1 ball milling
The Cr-Y mixed-powders of 4h) intensity highest, tensile strength is up to 1260MPa, respectively beyond comparative example 1, the tensile strength of 2 steel
About 285MPa and 345MPa.This shows that Cr-Y-O nanoclusters serve dispersion-strengthened action in low activation steel matrix, hinders
The motion of matrix Dislocations.
The above embodiments merely illustrate the technical concept and features of the present invention, its object is to allow person skilled in the art
Scholar will appreciate that present disclosure and implement according to this that it is not intended to limit the scope of the present invention.It is all according to the present invention
The equivalent change or modification that Spirit Essence is made, should all be included within the scope of the present invention.
Claims (5)
1. a kind of preparation method of Cr-Y-O nanoclusters oxide dispersion intensifying steel, it is characterised in that to low activation ferrite
Cr-Y ball-milled powders are added in martensite steel master alloy powder, the Cr-Y produced in mechanical milling process is dissolved each other metal and not molten proof gold
There is oxidation reaction, in-situ preparation Cr-Y-O nanoclusters and Y with the oxygen atom of powder adsorption respectively in category Y powder2O3Inertia matter
Point, its technological process is：Cr-Y ball-milled powders are prepared using high energy ball mill method first, Cr, Y mass ratio are Cr：Y=2.3~
9:1, low activation steel Fe-C-Cr-W-V-Ta-Mn-Si master alloy powders and Cr-Y ball millings are then prepared using high energy ball mill method
The mixed-powder of powder, then hot setting forming processes are carried out to mixed powder for alloy, finally it is heat-treated, obtain Cr-Y-O
Nanocluster oxide dispersion intensifying low activation steel.
2. according to the preparation method of Cr-Y-O nanoclusters oxide dispersion intensifying steel described in claim 1, it is characterised in that
The preparation method of Cr-Y ball-milled powders is：Mass ratio is taken for Cr：Y=2.3~9:1 Cr powder, Y powder, height is carried out after being mixed
Can ball milling, design parameter is：Ball-milling medium be the hardened steel balls of Φ 6, milling atmosphere be 99.99% argon gas, ball material mass ratio be 8~
10：1, Ball-milling Time 0.5-4h, rotating speed are more than or equal to 800r/min.
3., according to the preparation method of Cr-Y-O nanoclusters oxide dispersion intensifying steel described in claim 1 or 2, its feature exists
In preparing low activation steel Fe-C-Cr-W-V-Ta-Mn-Si master alloy powders and Cr-Y ball-milled powders using high energy ball mill method
Mixed-powder：Ball-milling medium is Φ 6 and Φ 10 mixing hardened steel balls, and milling atmosphere is 99.99% argon gas, and ball material mass ratio is 8
~10:1, Ball-milling Time 40-70h, rotating speed is 350-450r/min.
4., according to the preparation method of Cr-Y-O nanoclusters oxide dispersion intensifying steel described in claim 1 or 2, its feature exists
In mixed powder for alloy hot setting moulding process is：Mixed-powder first fills jacket pumping, and vacuum is not less than 10-1Pa, temperature
400-550 DEG C, the time is 4-5h, by high temperature insostatic pressing (HIP) curing molding, pressure 120-150MPa, 1050-1200 DEG C of temperature, insulation
Dwell time 3-5h；Or spark plasma sintering method curing molding is used, pressure 35-50MPa, 1050-1100 DEG C of temperature is protected
Warm dwell time 20-30min.
5. according to the preparation method of Cr-Y-O nanoclusters oxide dispersion intensifying steel described in claim 1, it is characterised in that tool
Preparation process flow and parameter are as follows：
It is prepared by a, Cr-Y ball-milled powder：Mass ratio is taken for Cr：Y=2.3~9:1 Cr powder, Y powder, ball-milling medium is the converted steels of Φ 6
Ball, milling atmosphere is 99.99% argon gas, and ball material mass ratio is 8~10：1, Ball-milling Time 0.5-4h, rotating speed is 1425r/min；
It is prepared by the mixed-powder of b, low activation steel Fe-C-Cr-W-V-Ta-Mn-Si master alloy powders and Cr-Y ball-milled powders：Ball milling
Medium is Φ 6 and Φ 10 mixing hardened steel balls, and milling atmosphere is 99.99% argon gas, and ball material mass ratio is 8~10：1, during ball milling
Between 40-70h, rotating speed is 350-450r/min；
C, mixed powder for alloy cure process：Mixed-powder first fills jacket pumping, and vacuum is not less than 10-1Pa, temperature
400-550 DEG C, the time is 4-5h, by high temperature insostatic pressing (HIP) curing molding, pressure 120-150MPa, 1050-1200 DEG C of temperature, insulation
Dwell time 3-5h；Or spark plasma sintering method curing molding is used, pressure 35-50MPa, 1050-1100 DEG C of temperature is protected
Warm dwell time 20-30min.
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