CN106834883B - A kind of method of residual ferrite and martensite lath structure in control 9Cr-ODS steel - Google Patents
A kind of method of residual ferrite and martensite lath structure in control 9Cr-ODS steel Download PDFInfo
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 73
- 239000010959 steel Substances 0.000 title claims abstract description 73
- 229910000734 martensite Inorganic materials 0.000 title claims abstract description 66
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 47
- 238000005245 sintering Methods 0.000 claims abstract description 31
- 238000005275 alloying Methods 0.000 claims abstract description 30
- 238000010792 warming Methods 0.000 claims abstract description 25
- 238000007493 shaping process Methods 0.000 claims abstract description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 11
- 238000000498 ball milling Methods 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 9
- 238000009413 insulation Methods 0.000 claims description 7
- 238000005054 agglomeration Methods 0.000 claims 1
- 230000002776 aggregation Effects 0.000 claims 1
- 238000001816 cooling Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 26
- 229910001566 austenite Inorganic materials 0.000 description 19
- 230000009466 transformation Effects 0.000 description 17
- 230000008569 process Effects 0.000 description 11
- 238000011068 loading method Methods 0.000 description 6
- 238000000465 moulding Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 239000004575 stone Substances 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000003701 mechanical milling Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 210000001519 tissue Anatomy 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000001192 hot extrusion Methods 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 229910001338 liquidmetal Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005551 mechanical alloying Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910001175 oxide dispersion-strengthened alloy Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 210000004872 soft tissue Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0207—Using a mixture of prealloyed powders or a master alloy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/002—Heat treatment of ferrous alloys containing Cr
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/22—Ferrous alloys, e.g. steel alloys containing chromium with molybdenum or tungsten
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/24—Ferrous alloys, e.g. steel alloys containing chromium with vanadium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/26—Ferrous alloys, e.g. steel alloys containing chromium with niobium or tantalum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D2211/00—Microstructure comprising significant phases
- C21D2211/005—Ferrite
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D2211/00—Microstructure comprising significant phases
- C21D2211/008—Martensite
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The present invention relates to a kind of method of residual ferrite and martensite lath structure in control 9Cr ODS steel, by pre-alloying powder and nanoscale Y2O3By 99.65:0.35 mass ratio is mixed, and pre-alloying powder mass component is Fe 9Cr 1.5W 0.2V 0.07Ta 0.1C；Mechanical ball mill is carried out in the ball mill, 800 DEG C is heated to using discharge plasma sintering, keeps the temperature 5~10min, is further continued for being warming up to 1100 DEG C, keeps the temperature 10~15min, obtains 9Cr ODS martensite steel of the shaping consistency more than 99%；The 9Cr ODS martensite steels of sintered state are heat-treated, 1100 DEG C is warming up to the rate of heat addition of 10 DEG C/min~40 DEG C/min, keeps the temperature, is then cooled to room temperature.It control effectively to the content of residual ferrite in 9Cr ODS martensite steels, while can also obtains ultrafine nanometer martensite lath in cooling procedure.
Description
Technical field
The invention belongs to oxide dispersion intensifying martensite steel preparing technical field, and it is strong to be related to a kind of control oxide disperse
Change the preparation of residual ferrite content and martensite lath width and heat treatment process in martensite steel.
Background technology
The construction of nuclear power station needs a large amount of high-quality steels and high-end core level steel.Low activation martensite/ferritic steel is because of it
With relatively low void swelling and thermal coefficient of expansion, high heat conductance, preferably resistance to liquid metal corrosion ability become fast neutron reactor and
The leading candidate structural material of fusion reactor, it is notable that such material still suffer from elevated temperature strength deficiency, service temperature it is low (<
600 DEG C), the problems such as helium is crisp.Nuclear reactor service temperature and the thermal efficiency further improve, and there is an urgent need to develop dispersed oxide
Strengthen (Oxide Dispersion-Strengthened, ODS) martensite/ferritic steel.By in martensite/ferrite base
The high heat stability nano-oxide of introducing Dispersed precipitate can realize the effectively pin to dislocation and crystal boundary in body, greatly improve material
High temperature and creep resistance intensity, it is ensured that its service temperature is improved to more than 700 DEG C.
ODS steels are standby mainly to include mechanical alloying powder, hot consolidation shaping, thermal deformation processing and subsequent heat treatment
Deng.By pre-alloying powder or metal mixed powder and the Y with high thermal stability and chemical stability2O3Powder carries out machinery
Alloying is one of most important process.According to the difference of Cr contents, the matrix of ODS steel mainly have 9%Cr systems martensite steel and
Whether 12~22%Cr systems ferritic steel, its main distinction can occur (complete) austenite phase transformation in heating process.It is right
In oxide dispersion intensifying martensite steel, the Y added in its preparation process2O3Can be to ferrite to during austenite phase transformation
The austenite grain boundary of generation plays pinning effect, hinders the movement of austenite grain boundary, so that ferrite turns to austenite
Change is obstructed, and forms a certain amount of residual ferrite.Research shows that the position difference of martensite-residual ferrite boundary is larger,
These high-angle boundaries being capable of Anticrack.The collocation of residual ferrite and this hard and soft tissue of martensite more can be effectively
Alleviate stress concentration and suppress to strain, so as to improve the creep-resistant property of steel.With increasing for residual ferrite content, 9Cr-
ODS steel is improved in 700 DEG C of creep strength.At present, from the angle of design of alloy, control C, W in 9Cr-ODS steel,
The content of the elements such as Al, Ti, O can realize the control to residual ferrite content in steel.But for certain alloying component
9Cr-ODS steel, how effective control to residual ferrite in 9Cr-ODS steel realized by simple heat treatment process there is not yet
All reports.The present invention, using certain preparation process and heat treatment process, passes through control from the generting machanism of residual ferrite
The size of austenite phase transformation driving force processed, realizes effective control of 9Cr-ODS steel residual ferrite contents.
The content of the invention
The present invention is by applying suitable powder metallurgy and heat treatment process parameter, in the 9Cr-ODS of certain alloying component
The controllable residual ferrite of volume fraction has been obtained in steel, has been conducive to improve the creep life of 9Cr-ODS steel.
Concrete technical scheme is as follows：
A kind of method of residual ferrite and martensite lath structure in control 9Cr-ODS steel, its step are as follows：
1) by pre-alloying powder and nanoscale Y2O3By 99.65:0.35 mass ratio is mixed, pre-alloying powder
Mass component is Fe-9Cr-1.5W-0.2V-0.07Ta-0.1C；Mechanical ball mill is carried out in the ball mill, is protected using argon gas；Profit
Ball-milled powder is heated to 800 DEG C with discharge plasma sintering, keeps the temperature 5~10min, is further continued for being warming up to 1100 DEG C, insulation 10
~15min, sintering pressure are 40~50MP, cool to room temperature with the furnace, obtain 9Cr-ODS horse of the shaping consistency more than 99%
Family name's body steel；
2) the 9Cr-ODS martensite steels of sintered state are heat-treated, with 10 DEG C/min~40 DEG C/min rate of heat addition liters
Temperature is kept the temperature 0~5min, is then cooled to room temperature with the speed of 30~1000 DEG C/min to 1100 DEG C.
It is preferred that ratio of grinding media to material is 15 in the ball mill:1.
It is preferred that rotational speed of ball-mill is 400r/min in the ball mill.
It is preferred that Ball-milling Time is 45h in the ball mill.
The generation of residual ferrite and austenite phase transformation driving force and oxide are between austenite grain boundary pinning resistance
Compete related.Austenite phase transformation driving force is bigger, and residual ferrite content is fewer；Austenite phase transformation driving force is smaller, remainder fe
Ferritic content is more.And alloying component is certain, austenite phase transformation driving force is certain.If introduce one in 9Cr-ODS martensite steels
Quantitative strain energy, strain energy will promote austenite phase transformation, and the release of controlled strain energy will influence austenite phase transformation driving force
Size, so as to influence residual ferrite content.The preparation process flow of 9Cr-ODS is made a general survey of, in the powder metallurgy stage, due to machinery
Ball milling, is introduced into substantial amounts of dislocation and strain energy in alloy powder.Traditional hot rolling or HIP sintering technique, due to insulation
Time is grown, and holding temperature is high, and the strain energy stored in sintering process in ball-milled powder will discharge, Austria to being molded 9Cr-ODS steel
The phase transformation of family name's body without be obviously promoted effect.If can be by 9Cr-ODS powder rapid shapings, being molded in 9Cr-ODS steel will store necessarily
The strain energy of amount, in subsequent heat treatment technique, the release of controlled strain energy can then control the phase of austenite phase transformation driving force
To size, so as to influence residual ferrite content.
The present invention key be the composition design of pre-alloying powder, mechanical ball mill technological parameter, using electric discharge etc. from
The rate of heat addition is selected in sub- sintering technology progress rapid shaping, sintering process parameter, subsequent heat treatment.Pre-alloying powder
Alloying component is Fe-9Cr-1.5W-0.2V-0.07Ta-0.1C (wt.%), determines 9Cr-ODS martensite steel austenite phase transformations
Intrinsic driving force；A large amount of dislocations are produced in mechanical milling process, in powder, store certain strain energy；In order to retain mechanical milling process
The high dislocation density and strain energy of middle generation, rapid shaping, rather than conventional heat are carried out using discharge plasma sintering process
Isostatic pressed or hot extrusion technique；In sintered state 9Cr-ODS martensite steels, Y2O3Distribution it is certain, in subsequent heat treatment technique
The pinning effect of austenite grain boundary is certain；But by controlling the rate of heat addition (10 DEG C/min~40 DEG C/min), it can control and add
In thermal process in sintered state martensite steel residual strain can release, and then influence promotion of the strain energy to austenite phase transformation and make
With so as to fulfill the control to residual ferrite content in 9Cr-ODS martensite steels；It can obtain under the slow rate of heat addition substantial amounts of
Residual ferrite, and a small amount of residual ferrite is obtained under the fast rate of heat addition；In austenitization, dislocation is not complete
Reply, high density dislocation region will promote the forming core of martensite in Martensitic Transformation, cause nanoscale martensite lath
Generation, improves the grain boundary structure of 9Cr-ODS martensite steels.
Advantage of the present invention：
Certain composition design is carried out to 9Cr-ODS martensite steels by early period and preparation process adjusts, at subsequent thermal
The rate of heat addition only need to be simply controlled to be carried out to the content of residual ferrite in 9Cr-ODS martensite steels during reason effective
Control, while ultrafine nanometer martensite lath can be also obtained in cooling procedure, nanometer martensite lath size is about 15nm
Left and right, technique is simple, and purpose is strong, is of great significance to the elevated temperature strength for improving ODS- martensite steels.
Brief description of the drawings
Fig. 1 (a) is scanning electron microscope (SEM) photo of sintered state 9Cr-ODS martensite steels in embodiment 1；
Fig. 1 (b) is transmission electron microscope (TEM) photo of sintered state 9Cr-ODS martensite steels in embodiment 1；
Fig. 2 (a) is that sintered state 9Cr-ODS martensite steels are heated to 1100 DEG C with 10 DEG C/min in embodiment 1, insulation
5min, the scanning electron microscope being then cooled to room temperature with the speed of 30 DEG C/min (SEM) photo；
Fig. 2 (b) is that sintered state 9Cr-ODS martensite steels are heated to 1100 DEG C with 10 DEG C/min in embodiment 1, insulation
5min, the transmission electron microscope being then cooled to room temperature with the speed of 30 DEG C/min (TEM) photo；
Fig. 3 is that sintered state 9Cr-ODS martensite steels are heated to 1100 DEG C with 20 DEG C/min in embodiment 2, keeps the temperature 5min,
Scanning electron microscope (SEM) photo being then cooled to room temperature with the speed of 30 DEG C/min；
Fig. 4 is that sintered state 9Cr-ODS martensite steels are heated to 1100 DEG C with 30 DEG C/min in embodiment 3, keeps the temperature 5min,
Scanning electron microscope (SEM) photo being then cooled to room temperature with the speed of 30 DEG C/min；
Fig. 5 (a) is that sintered state 9Cr-ODS martensite steels are heated to 1100 DEG C with 40 DEG C/min in embodiment 4, insulation
5min, light microscopic scanning electron microscope (SEM) photo being then cooled to room temperature with the speed of 30 DEG C/min；
Fig. 5 (b) is that sintered state 9Cr-ODS martensite steels are heated to 1100 DEG C with 40 DEG C/min in embodiment 4, insulation
5min, the transmission electron microscope being then cooled to room temperature with the speed of 30 DEG C/min (TEM) photo；
Fig. 6 is the song that residual ferrite content changes with the rate of heat addition in sintered state 9Cr-ODS martensite steels in embodiment
Line chart.
Embodiment
The present invention is described in further detail with reference to embodiment.
Pre-alloying powder of the present invention, forms according to mass percent with following components：C=0.1%, Cr=
9%, W=1.5%, V=0.2%, Ta=0.07%, remaining is Fe.Y of the present invention2O3Powder size is distributed as 30~
50nm。
To controlling residual ferrite content in 9Cr-ODS martensite steels in the present invention and obtaining ultrafine nanometer martensite plate
The preparation of bar and heat treatment process, its step are：
1. it is Fe-9Cr-1.5W-0.2V-0.07Ta-0.1C's (wt.%) to obtain alloying component by powder by atomization technique
Pre-alloying powder, by pre-alloying powder and nanoscale Y2O3By 99.65:0.35 mass ratio is mixed, in planetary ball
Mechanical ball mill, ratio of grinding media to material 15 are carried out in grinding machine:1, rotational speed of ball-mill 400r/min, Ball-milling Time 45h, is protected using argon gas
Shield；Ball-milled powder is heated to 800 DEG C using discharge plasma sintering process, 5~10min is kept the temperature, is further continued for being warming up to 1100
DEG C, 10~15min is kept the temperature, sintering pressure is 40~50MP, cools to room temperature with the furnace, obtains shaping consistency more than 99%
9Cr-ODS martensite steels.
2. the 9Cr-ODS martensite steels that pair sintering obtains carry out subsequent heat treatment, with adding for 10 DEG C/min~40 DEG C/min
Hot speed is warming up to 1100 DEG C, keeps the temperature 0~5min, is then cooled to room temperature with the speed of 30~1000 DEG C/min.
It is the specific embodiment of the present invention below, but the invention is not restricted to following embodiments.
Embodiment 1：
It is Fe-9Cr-1.5W-0.2V-0.07Ta-0.1C that the component of 1 pre-alloying powder of embodiment, which is shown in Table as component,
(wt.%).By pre-alloying powder and Y2O3Powder presses 99.65：0.35 mass ratio is mixed, in planetary ball mill
Carry out mechanical ball mill, ratio of grinding media to material 15:1, rotational speed of ball-mill 400r/min, Ball-milling Time 45h, is protected using argon gas；In stone
After loading suitable ball-milled powder in black mould, it is put into discharge plasma sintering stove and carries out curing molding, with 100 DEG C/min's
The rate of heat addition is warming up to 800 DEG C, keeps the temperature 5min, then is warming up to 1100 DEG C at the same rate, keeps the temperature 10min, and sintering pressure is
40MP, cools to room temperature with the furnace.
Subsequent heat treatment is carried out to the 9Cr-ODS martensite steels that sintering obtains, is warming up to the rate of heat addition of 10 DEG C/min
1100 DEG C, 5min is kept the temperature, is then cooled to room temperature with the speed of 30 DEG C/min.
Fig. 1 (a) is scanning electron microscope (SEM) photo of sintered state 9Cr-ODS martensite steels in embodiment 1, can be with from figure
The microstructure even tissue of the 9Cr-ODS martensite steels obtained through discharge plasma sintering is found out, mainly by martensite and less
The residual ferrite composition of amount.Fig. 1 (b) is the TEM photos of sintered state 9Cr-ODS martensite steels in embodiment 1, after sintering,
Still contain highdensity dislocation in tissue, the strain energy introduced in mechanical milling process is not completely eliminated.Sintered state 9Cr-ODS geneva
When body steel is heated to 1100 DEG C with 10 DEG C/min, the rate of heat addition is slower, and strain energy release is more in heating process, and strain energy is to Austria
The facilitation of family name's body phase transformation weakens, and austenite phase transformation driving force reduces, and residual ferrite content increases, residual ferrite content
For 13.05%, as shown in Fig. 2 (a).Fig. 2 (b) is that the TEM photos of 9Cr-ODS martensite steels, can see after subsequent heat treatment
Ultra-fine nanoscale martensite lath can be obtained while residual ferrite content by going out above-mentioned subsequent heat treatment.
Embodiment 2：
It is Fe-9Cr-1.5W-0.2V-0.07Ta-0.1C that the component of 2 pre-alloying powder of embodiment, which is shown in Table as component,
(wt.%).By pre-alloying powder and Y2O3Powder presses 99.65：0.35 mass ratio is mixed, in planetary ball mill
Carry out mechanical ball mill, ratio of grinding media to material 15:1, rotational speed of ball-mill 400r/min, Ball-milling Time 45h, is protected using argon gas；In stone
After loading suitable ball-milled powder in black mould, it is put into discharge plasma sintering stove and carries out curing molding, with 100 DEG C/min's
The rate of heat addition is warming up to 800 DEG C, keeps the temperature 5min, then is warming up to 1100 DEG C at the same rate, keeps the temperature 10min, and sintering pressure is
40MP, cools to room temperature with the furnace.
Subsequent heat treatment is carried out to the 9Cr-ODS martensite steels that sintering obtains, is warming up to the rate of heat addition of 20 DEG C/min
1100 DEG C, 5min is kept the temperature, is then cooled to room temperature with the speed of 30 DEG C/min.
Fig. 3 is the rate of heat addition of sintered state 9Cr-ODS martensite steel subsequent heat treatment techniques when being 20 DEG C/min, 9Cr-
Scanning electron microscope (SEM) photo of ODS martensite steels, residual ferrite content are 11.48%.
Embodiment 3：
It is Fe-9Cr-1.5W-0.2V-0.07Ta-0.1C that the component of 3 pre-alloying powder of embodiment, which is shown in Table as component,
(wt.%).By pre-alloying powder and Y2O3Powder presses 99.65：0.35 mass ratio is mixed, in planetary ball mill
Carry out mechanical ball mill, ratio of grinding media to material 15:1, rotational speed of ball-mill 400r/min, Ball-milling Time 45h, is protected using argon gas；In stone
After loading suitable ball-milled powder in black mould, it is put into discharge plasma sintering stove and carries out curing molding, with 100 DEG C/min's
The rate of heat addition is warming up to 800 DEG C, keeps the temperature 5min, then is warming up to 1100 DEG C at the same rate, keeps the temperature 10min, and sintering pressure is
40MP, cools to room temperature with the furnace.
Subsequent heat treatment is carried out to the 9Cr-ODS martensite steels that sintering obtains, is warming up to the rate of heat addition of 30 DEG C/min
1100 DEG C, 5min is kept the temperature, is then cooled to room temperature with the speed of 30 DEG C/min.
Fig. 4 is the rate of heat addition of sintered state 9Cr-ODS martensite steel subsequent heat treatment techniques when being 30 DEG C/min, 9Cr-
Scanning electron microscope (SEM) photo of ODS martensite steels, residual ferrite content are 7.08%.
Embodiment 4：
It is Fe-9Cr-1.5W-0.2V-0.07Ta-0.1C that the component of 2 pre-alloying powder of embodiment, which is shown in Table as component,
(wt.%).By pre-alloying powder and Y2O3Powder presses 99.65：0.35 mass ratio is mixed, in planetary ball mill
Carry out mechanical ball mill, ratio of grinding media to material 15:1, rotational speed of ball-mill 400r/min, Ball-milling Time 45h, is protected using argon gas；In stone
After loading suitable ball-milled powder in black mould, it is put into discharge plasma sintering stove and carries out curing molding, with 100 DEG C/min's
The rate of heat addition is warming up to 800 DEG C, keeps the temperature 5min, then is warming up to 1100 DEG C at the same rate, keeps the temperature 10min, and sintering pressure is
40MP, cools to room temperature with the furnace.
Subsequent heat treatment is carried out to the 9Cr-ODS martensite steels that sintering obtains, is warming up to the rate of heat addition of 40 DEG C/min
1100 DEG C, 5min is kept the temperature, is then cooled to room temperature with the speed of 30 DEG C/min.
When sintered state 9Cr-ODS martensite steels are heated to 1100 DEG C with 40 DEG C/min, the rate of heat addition is very fast, in heating process
Strain energy release is less, and strain energy is obvious to the facilitation of austenite phase transformation, and residual ferrite content reduces, residual ferrite
Content is 4.12%, as shown in Fig. 5 (a).Fig. 5 (b) is that the TEM photos of 9Cr-ODS martensite steels can after subsequent heat treatment
To find out that above-mentioned subsequent heat treatment can also obtain ultra-fine nanoscale martensite lath while residual ferrite content.
Fig. 6 is the residual ferrite content in 9Cr-ODS steel under different heating rates, it can be seen that with the rate of heat addition
Raising, the content of residual ferrite gradually reduces, when the rate of heat addition is improved to 40 DEG C/min by 10 DEG C/min, remainder fe element
Body content is down to 4.12% by 13.05%.
Embodiment 5：
It is Fe-9Cr-1.5W-0.2V-0.07Ta-0.1C that the component of 5 pre-alloying powder of embodiment, which is shown in Table as component,
(wt.%).By pre-alloying powder and Y2O3Powder presses 99.65：0.35 mass ratio is mixed, in planetary ball mill
Carry out mechanical ball mill, ratio of grinding media to material 15:1, rotational speed of ball-mill 400r/min, Ball-milling Time 45h, is protected using argon gas；In stone
After loading suitable ball-milled powder in black mould, it is put into discharge plasma sintering stove and carries out curing molding, with 100 DEG C/min's
The rate of heat addition is warming up to 800 DEG C, keeps the temperature 10min, then is warming up to 1100 DEG C at the same rate, keeps the temperature 15min, and sintering pressure is
50MP, cools to room temperature with the furnace.
Subsequent heat treatment is carried out to the 9Cr-ODS martensite steels that sintering obtains, is warming up to the rate of heat addition of 10 DEG C/min
1100 DEG C, 5min is kept the temperature, is then cooled to room temperature with the speed of 400 DEG C/min.
Embodiment 6：
It is Fe-9Cr-1.5W-0.2V-0.07Ta-0.1C that the component of 6 pre-alloying powder of embodiment, which is shown in Table as component,
(wt.%).By pre-alloying powder and Y2O3Powder presses 99.65：0.35 mass ratio is mixed, in the planetary balls of QM-3SP4
Mechanical ball mill, ratio of grinding media to material 15 are carried out in grinding machine:1, rotational speed of ball-mill 400r/min, Ball-milling Time 45h, is protected using argon gas
Shield；After loading suitable ball-milled powder in graphite jig, it is put into discharge plasma sintering stove and carries out curing molding, with 100
DEG C/rate of heat addition of min is warming up to 800 DEG C, 5min is kept the temperature, then 1100 DEG C are warming up at the same rate, 10min is kept the temperature, is burnt
Knot pressure power is 45MP, cools to room temperature with the furnace.
Subsequent heat treatment is carried out to the 9Cr-ODS martensite steels that sintering obtains, is warming up to the rate of heat addition of 10 DEG C/min
1100 DEG C, 3min is kept the temperature, is then cooled to room temperature with the speed of 1000 DEG C/min.
Although above in conjunction with figure, invention has been described, and the invention is not limited in above-mentioned specific embodiment party
Formula, above-mentioned embodiment is only schematical, rather than restricted, and those of ordinary skill in the art are in this hair
Under bright enlightenment, without deviating from the spirit of the invention, many variations can also be made, these belong to the guarantor of the present invention
Within shield.
Claims (4)
1. a kind of method of residual ferrite and martensite lath structure in control 9Cr-ODS steel, it is characterized in that step is as follows：
1) by pre-alloying powder and nanoscale Y2O3By 99.65:0.35 mass ratio is mixed, pre-alloying powder quality
Component is Fe-9Cr-1.5W-0.2V-0.07Ta-0.1C；Mechanical ball mill is carried out in the ball mill, is protected using argon gas；Using putting
Ball-milled powder is heated to 800 DEG C by electric plasma agglomeration, keeps the temperature 5~10min, is further continued for being warming up to 1100 DEG C, and insulation 10~
15min, sintering pressure are 40~50MP, cool to room temperature with the furnace, obtain 9Cr-ODS geneva of the shaping consistency more than 99%
Body steel；
2) the 9Cr-ODS martensite steels of sintered state are heat-treated, are warming up to 10 DEG C/min~40 DEG C/min rates of heat addition
1100 DEG C, 0~5min is kept the temperature, is then cooled to room temperature with the speed of 30~1000 DEG C/min.
2. the method as described in claim 1, it is characterized in that ratio of grinding media to material is 15 in the ball mill in step 1):1.
3. the method as described in claim 1, it is characterized in that rotational speed of ball-mill is 400r/min in the ball mill in step 1).
4. the method as described in claim 1, it is characterized in that Ball-milling Time is 45h in the ball mill in step 1).
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