CN104630639A - Nano yttrium nitride dispersed reinforced iron-based alloy and preparation method - Google Patents
Nano yttrium nitride dispersed reinforced iron-based alloy and preparation method Download PDFInfo
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Abstract
The invention relates to a nano yttrium nitride dispersed reinforced iron-based alloy and a preparation method, and belongs to the field of powder metallurgy materials. The iron-based alloy comprises a substrate and reinforced phase, wherein the substrate is prepared from the following components in percentage by mass: 12-17% of Cr, 1-4% of W and the balance of Fe; the reinforced phase comprises yttrium nitride. The preparation method comprises the following steps: ball-milling the substrate pre-alloy powder with yttrium nitride, crushing yttrium nitride into nanoparticles, uniformly dispersing the nanoparticles into the iron-based pre-alloy powder substrate, curing to form the powder, and preparing, thereby obtaining the nano yttrium nitride dispersed reinforced iron-based alloy. A great amount of nanoparticles which are fine and small and are distributed in a dispersion manner can be effectively obtained in the alloy substrate, so that the iron-based alloy is excellent in temperature and high-temperature mechanical property, and beneficial for large-scale preparation of a dispersed reinforced iron-based alloy with stable property, and the technical difficulty of preparation can be reduced.
Description
Technical field
The present invention relates to a kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy and preparation method; Belong to mmaterial field.
Background technology
Oxide dispersion intensifying (ODS) is the nano-oxide particles adding high thermal stability and chemical stability in alloy substrate, makes it in the base dispersed, produces strengthening effect by obstruction dislocation and grain boundary.Size and the distribution of disperse phase have remarkably influenced to strengthening effect, and the size of diffusing particle is more tiny, and distribute more even, strengthening effect is more remarkable.Therefore, obtaining tiny, equally distributed enhanced particles is improve the key of oxide-dispersed alloy performance.
ODS ferrous alloy has excellent high temperature creep-resisting, high temperature fatigue, radioprotective swelling and corrosion resistance nature, has wide application prospect in fields such as the energy and hot-work industry.In ferrous alloy matrix, introduce disperse even, tiny and there is good thermostability and the oxide particle of chemical stability, can significantly put forward heavy alloyed room temperature and mechanical behavior under high temperature.Yttrium oxide has high hardness and thermostability, is typically used as dispersion-strengthened phase.Concrete grammar passes through mechanical alloying, yttria particles is broken and make its Dispersed precipitate in powdered alloy matrix, then by powder forming, obtain the dispersion-strengthened phase being of a size of 10-40nm, be evenly distributed in alloy substrate, produce dispersion-strengthened action [I S Kim, J D Hunn, N Hashimoto, D L Larson, P J Maziasz, K Miyahara, E H Lee.Journal of Nuclear Materials280 (2000) 264].
In ferrous alloy, add Ti element, react between Ti, Y, O in sintering process, form the strengthening phase being of a size of 2-5nm.This strengthening phase particle components is Y-Ti-O, and complex structure is at high temperature highly stable, but the acquisition of tiny Y-Ti-O nanoparticle is very difficult, the preparation technology of alloy, and the content requirement of Y, Ti and O atom is very harsh.Simultaneously, powder is in powder process, forming process, and adsorb oxygen is understood on surface, and this part oxygen is unnecessary excess oxygen, oxide compound strengthening phase can be caused to grow up, form large size (>50nm), low-alloyed mechanical property [S Ohtsuka, seriously falls in the even oxide compound of micro-meter scale, S Ukai, M Fujiwara, T Kaito, T Narita.Journal of Physics and Chemistry of Solids 2-4 (2005) 571].
But in powder preparation, forming process, powder adsorption oxygen is unavoidable, this to grow up contradiction with being avoided oxide compound.How effectively utilizing the excess oxygen of powder adsorption, is the key of dealing with problems.
The present invention proposes, and adopts yttrium nitride to be that primary strengthening phase prepares high-performance ferrous alloy, develops the high-performance ferrous alloy and preparation method that more easily obtain.Be that Fe-Cr-W-M (M is one or more in the metallic elements such as Ti, Zr, Al) alloy of wild phase have not been reported in the prior art with yttrium nitride.
Summary of the invention
The present invention is directed to the weak point that existing dispersed oxide ferrous alloy exists, providing a kind of take nano silicon nitride yttrium as ferrous alloy and the preparation method of main dispersion-strengthened phase.
A kind of nano silicon nitride yttrium of the present invention dispersion strengthening iron-base alloy, it comprises matrix and wild phase;
Described matrix comprises by percentage to the quality:
Cr:12-17%, is preferably 12-16%, more preferably 13-15%;
W:1-4%, is preferably 2-4%, more preferably 3-4%;
M：0-1％；
Surplus is Fe;
Described M is at least one in the metallic elements such as Ti, Zr, Al;
Described wild phase comprises yttrium nitride;
The quality of described yttrium nitride is the 0.3-1% of substrate quality, is preferably 0.3%-0.7%, more preferably 0.3%-0.5%.
A kind of nano silicon nitride yttrium of the present invention dispersion strengthening iron-base alloy, its room temperature tensile intensity >=1450MPa, the tensile strength >=1100MPa of 500 DEG C, the tensile strength >=800MPa of 600 DEG C.After component is preferred, its room temperature tensile intensity >=1450MPa, the tensile strength >=1140MPa of 500 DEG C, the tensile strength >=850MPa of 600 DEG C.
The preparation method of a kind of nano silicon nitride yttrium of the present invention dispersion strengthening iron-base alloy, comprises the steps:
Step one
Take yttrium nitride powder by the 0.3-1% of matrix alloy powder quality, under protective atmosphere, carry out with matrix alloy powder mixing, ball milling, obtain mechanical alloying powder;
Described matrix alloy powder comprises by percentage to the quality: Cr:12-17%, W:1-4%, M:0-1%, surplus are Fe; During ball milling, control rotating speed is 250-350rpm, Ball-milling Time is 30-60h; Described M is selected from a kind of at least one in the metallic elements such as Ti, Zr, Al;
Step 2
Jacket is loaded to step one gained mechanical alloying powder, vacuum stripping, soldering and sealing, then hot-pressed, carry out hot rolling or forge hot, high temperature annealing after shaping successively, obtain yttrium nitride dispersion strengthening iron-base alloy; Time hot-pressed, control temperature is 900-1000 DEG C; When hot rolling or forge hot, control temperature is 950-1150 DEG C; During high temperature annealing, control temperature is 1050-1200 DEG C.
The preparation method of a kind of nano silicon nitride yttrium of the present invention dispersion strengthening iron-base alloy, in step one, the granularity of yttrium nitride powder is less than or equal to 30 μm, is more preferably less than or equal to 10 μm; The granularity of iron(-)base powder is less than or equal to 150 μm (-100 orders), is preferably less than or equal to 106 μm (-150 orders), is more preferably less than or equal to 75 μm (-200 orders).
The preparation method of a kind of nano silicon nitride yttrium of the present invention dispersion strengthening iron-base alloy, in step one, the preparation method of described matrix alloy powder is:
Join by the matrix alloy component of design and get raw material, through vacuum induction melting, argon gas atomization, obtain the matrix alloy powder that granularity is less than or equal to 150 μm (-100 orders).
The preparation method of a kind of nano silicon nitride yttrium of the present invention dispersion strengthening iron-base alloy, in step one, described protective atmosphere is selected from the one in argon gas, helium.
The preparation method of a kind of nano silicon nitride yttrium of the present invention dispersion strengthening iron-base alloy, in step one, during ball milling, controlling ball material mass ratio is 8-12:1.
The preparation method of a kind of nano silicon nitride yttrium of the present invention dispersion strengthening iron-base alloy, in step 2, time hot-pressed, control extrusion ratio is 6-15:1; During hot rolling, control total deformation is 50-80%; During forge hot, control total deformation is 30-60%; During high temperature annealing, control annealing time is 1-2h.
Advantage of the present invention and positively effect:
The present invention adopts non-oxide system high stability yttrium nitride particle as dispersion-strengthened phase, fragility yttrium nitride is in Process During High Energy Ball Milling, very easily be broken into the fine particle that size is less than 10nm, be dispersed among alloy substrate, in powder forming subsequently, heat treatment process, high stability yttrium nitride not with alloy constituent element generation chemical reaction, avoid particle growth, ensure that dispersion-strengthened effect, put forward heavy alloyed mechanical property.
The oxygen of the present invention's powder adsorption in powder preparation, forming process, when hot forming, can react with the active element in alloy and form steady oxide, become the second strengthening phase, make the oxygen of inevitable absorption in technological process, be utilized effectively.Because matrix interalloy Elemental redistribution is even, the be evenly distributed disperse of the oxide compound formed in alloy substrate.
Compared with oxide-dispersed alloy, added Oxides strengthening phase is not had to grow up core as oxide compound in alloy substrate of the present invention, the oxygen adsorbed in powder preparation, forming process directly forms dispersed oxide distribution in the base, effectively overcomes the defect that adsorb oxygen in oxide-dispersed alloy causes oxide compound strengthening phase to be grown up.
In a word, the present invention with fragility yttrium nitride for raw material, with Fe-Cr (12-17wt%)-W (1-4wt%)-M (0-1%, M are one or more in the metallic elements such as Ti, Zr, Al) as matrix; By the broken yttrium nitride particle of high-energy ball milling, obtain the fine particle that particle size is less than 10nm, even dispersion is distributed in matrix and produces dispersion-strengthened effect, prepares high performance ferrous alloy material.Due to tiny yttrium nitride particle not with alloy constituent element generation chemical reaction, effectively can avoid particle growth, ensure that the acquisition of nanoparticle tiny in alloy substrate, and then ensure that the high-performance of alloy, reduce difficulty prepared by dispersion strengthening iron-base alloy; Meanwhile, the oxygen that technological process is introduced, being utilized effectively by forming oxide dispersion intensifying phase, effectively can reducing the difficulty of powder preparation, storage, transport, reduces powder preparation cost.Present invention process is simple, prepares high performance material difficulty low, efficiently solves a difficult problem for this puzzlement field of powder metallurgy of oxygen of technological process absorption, is conducive to the high-performance dispersion strengthening iron-base alloy that processability in enormous quantities is stable.
Accompanying drawing explanation
Accompanying drawing 1 is Fe-13.6Cr-3.3W-0.3YN (massfraction) the alloy microscopic structure transmission photo prepared by embodiment 1.
As can be seen from Figure 1, the strengthening phase particle that diameter is less than 6nm is uniform-distribution with in matrix.
Embodiment
The present invention adopts high-energy ball milling, and prepare nano silicon nitride yttrium dispersion strengthening iron-base alloy, below in conjunction with example, the present invention will be further described.
Comparative example 1:
Design alloying constituent, described alloy comprises following component by percentage to the quality:
Cr:13.6%; W:3.3%; Y
2o
3: 0.3; Surplus is Fe;
Testing raw materials used is atomization pre-alloyed powder (composition is Fe-13.6Cr-3.3W, massfraction) and Y
2o
3powder.Wherein, the granularity of pre-alloyed powder is less than or equal to 75 μm (-200 orders), Y
2o
3the median size of powder is for being less than or equal to 30nm.The Y that massfraction is 0.3% is added in pre-alloyed powder
2o
3powder, mix rearmounted enter in ball grinder, be filled with high-purity argon gas after vacuumizing, ball milling, rotational speed of ball-mill is 350rpm, and Ball-milling Time controls, for 48h, to obtain the mechanical alloying powder that granularity is less than or equal to 13 μm.By the powder of mechanical alloying load Steel Capsule, vacuumize degasification, soldering and sealing, then at 950 DEG C of extrusion moldings, then extruded bars carried out at 950 DEG C the rolling that total reduction is 70%, finally by alloy 1050 DEG C annealing 1h.The alloy of preparation, matrix grain size is about 600nm, even dispersion distribution nanometer Y in matrix
2o
3particle (10-20nm), its average particle size particle size is 14nm, and be respectively 1135MPa, 898MPa and 654MPa in the tensile strength of room temperature, 500 DEG C and 600 DEG C, elongation after fracture is respectively 15.7%, 15% and 17.5%.
Embodiment 1:
Design alloying constituent is: Fe-13.6Cr-3.3W-0.3YN (massfraction)
Testing raw materials used is atomization pre-alloyed powder (composition is Fe-13.6Cr-3.3W, massfraction) and YN powder.Wherein, the granularity of pre-alloyed powder is less than or equal to 75 μm (-200 orders), and the median size of YN powder is for being less than or equal to 10 μm.In pre-alloyed powder, add the YN powder that massfraction is 0.3%, mix rearmounted enter in ball grinder, be filled with high-purity argon gas after vacuumizing, ball milling, rotational speed of ball-mill is 350rpm, and Ball-milling Time controls, for 48h, to obtain the mechanical alloying powder that granularity is less than or equal to 12 μm.By the powder of mechanical alloying load Steel Capsule, vacuumize degasification, soldering and sealing, then 950 DEG C of extrusion moldings, then extruded bars carried out at 950 DEG C the rolling that total reduction is 70%, finally by alloy 1050 DEG C annealing 1h.The alloy of preparation, matrix grain size is about 500nm, in matrix, even dispersion is distributed with nanoparticle tiny in a large number, its particle size is less than 6nm (see accompanying drawing 1), 1461MPa, 1127MPa and 825MPa is respectively in the tensile strength of room temperature, 500 DEG C and 600 DEG C, elongation after fracture is respectively 14.7%, 16.6% and 19.2%.
Embodiment 2:
Fe-13.9Cr-4.0W-1YN (massfraction)
Testing raw materials used is atomization pre-alloyed powder (composition is Fe-13.9Cr-4.0W, massfraction) and YN powder.Wherein, it is 75 μm (-200 orders) that the granularity of pre-alloyed powder is less than or equal to, and the median size of YN powder is for being less than or equal to 10 μm.In pre-alloyed powder, add the YN powder that massfraction is 1%, mix rearmounted enter in ball grinder, be filled with high-purity argon gas after vacuumizing, ball milling, rotational speed of ball-mill is 300rpm, and Ball-milling Time controls, for 60h, to obtain the mechanical alloying powder that granularity is less than or equal to 10 μm.By the powder of mechanical alloying load Steel Capsule, vacuumize degasification, soldering and sealing, then 1000 DEG C of extrusion moldings, then extruded bars carried out at 1000 DEG C the rolling that total reduction is 60%, finally by alloy 1050 DEG C annealing 1h.The alloy of preparation, matrix grain size is about 500nm, in matrix, even dispersion is distributed with nanoparticle tiny in a large number, its average particle size particle size is 8nm, 1590MPa, 1307MPa and 895MPa is respectively in the tensile strength of room temperature, 500 DEG C and 600 DEG C, elongation after fracture is respectively 12.5%, 14.1% and 16.7%.
Embodiment 3:
Fe-15.2Cr-3.7W-0.5YN (massfraction)
Testing raw materials used is atomization pre-alloyed powder (composition is Fe-15.2Cr-3.7W, massfraction) and YN powder.Wherein, the granularity of pre-alloyed powder is less than or equal to 75 μm (-200 orders), and the median size of YN powder is less than or equal to 10 μm.In pre-alloyed powder, add the YN powder that massfraction is 0.5%, mix rearmounted enter in ball grinder, be filled with high-purity argon gas after vacuumizing, ball milling, rotational speed of ball-mill is 300rpm, and Ball-milling Time controls, for 60h, to obtain the mechanical alloying powder that granularity is less than or equal to 9.5 μm.By the powder of mechanical alloying load Steel Capsule, vacuumize degasification, soldering and sealing, then 1000 DEG C of extrusion moldings, then extruded bars carried out at 1050 DEG C the forging that total reduction is 40%, finally by alloy 1050 DEG C annealing 1h.The alloy of preparation, matrix grain size is about 500nm, in matrix, even dispersion is distributed with nanoparticle tiny in a large number, its average particle size particle size is 7nm, 1506MPa, 1164MPa and 879MPa is respectively in the tensile strength of room temperature, 500 DEG C and 600 DEG C, elongation after fracture is respectively 13.5%, 14.2% and 15.3%.
Embodiment 4:
Fe-14.2Cr-3.7W-1.0Ti-0.5YN (massfraction)
Testing raw materials used is atomization pre-alloyed powder (composition is Fe-15.2Cr-3.7W, massfraction) and YN powder.Wherein, the granularity of pre-alloyed powder is less than or equal to 75 μm (-200 orders), and the median size of YN powder is less than or equal to 10 μm.In pre-alloyed powder, add the YN powder that massfraction is 0.5%, mix rearmounted enter in ball grinder, be filled with high-purity argon gas after vacuumizing, ball milling, rotational speed of ball-mill is 300rpm, and Ball-milling Time controls, for 60h, to obtain the mechanical alloying powder that granularity is less than or equal to 9 μm.By the powder of mechanical alloying load Steel Capsule, vacuumize degasification, soldering and sealing, then 900 DEG C of extrusion moldings, then extruded bars carried out at 1150 DEG C the forging that total reduction is 40%, finally by alloy 1100 DEG C annealing 2h.The alloy of preparation, matrix grain size is about 500nm, in matrix, even dispersion is distributed with nanoparticle tiny in a large number, its average particle size particle size is 7nm, 1595MPa, 1435MPa and 910MPa is respectively in the tensile strength of room temperature, 500 DEG C and 600 DEG C, elongation after fracture is respectively 10.5%, 13.2% and 14.3%.
Claims (9)
1. a nano silicon nitride yttrium dispersion strengthening iron-base alloy, comprises matrix and wild phase; It is characterized in that:
Described matrix comprises by percentage to the quality:
Cr:12-17%; W:1-4%; Surplus is Fe;
Described wild phase comprises yttrium nitride;
The quality of described yttrium nitride is the 0.3-1% of substrate quality.
2. a kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy according to claim 1; It is characterized in that:
Described matrix comprises by percentage to the quality:
Cr:12-16%; W:2-4%; M:0-1%; Surplus is Fe;
Described M is at least one in Ti, Zr, Al;
Described wild phase comprises yttrium nitride;
The quality of described yttrium nitride is the 0.3%-0.7% of substrate quality.
3. a kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy according to claim 2; It is characterized in that:
Described matrix comprises by percentage to the quality:
Cr:13-15%; W:3-4%; M:0-1%; Surplus is Fe;
Described M is at least one in Ti, Zr, Al;
Described wild phase comprises yttrium nitride;
The quality of described yttrium nitride is the 0.3%-0.5% of substrate quality.
4. a kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy according to claim 1-3 any one, is characterized in that: the room temperature tensile intensity of described yttrium nitride dispersion strengthening iron-base alloy is >=1450MPa, the tensile strength of 500 DEG C is >=1100MPa, the tensile strength of 600 DEG C is >=800MPa.
5. prepare the method for nano silicon nitride yttrium dispersion strengthening iron-base alloy as claimed in claim 4 for one kind; It is characterized in that, comprise the steps:
Step one
Take yttrium nitride powder by the 0.3-1% of matrix alloy powder quality, under protective atmosphere, carry out with matrix alloy powder mixing, ball milling, obtain mechanical alloying powder;
Described matrix alloy powder comprises by percentage to the quality: Cr:12-17%, W:1-4%, M:0-1%, surplus are Fe; During ball milling, control rotating speed is 250-350rpm, Ball-milling Time is 30-60h; Described M is at least one in Ti, Zr, Al;
Step 2
Jacket, vacuum stripping, soldering and sealing are loaded to step one gained mechanical alloying powder, then hot-pressed, carry out hot rolling or forge hot, high temperature annealing after shaping successively, obtain yttrium nitride dispersion strengthening iron-base alloy; Hot-pressed temperature is 900-1000 DEG C; Hot rolling or hot forging temperature are 950-1150 DEG C; High temperature anneal temperature is 1050-1200 DEG C.
6. the preparation method of a kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy according to claim 5, it is characterized in that: in step one, the granularity of yttrium nitride powder is less than or equal to 10 μm; The granularity of matrix alloy powder is less than or equal to 150 μm.
7. the preparation method of a kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy according to claim 5, it is characterized in that: in step one, described protective atmosphere is selected from the one in argon gas, helium.
8. the preparation method of a kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy according to claim 5, is characterized in that: in step one, and during ball milling, controlling ball material mass ratio is 8-12:1.
9. the preparation method of a kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy according to claim 5, is characterized in that: in step 2, and time hot-pressed, control extrusion ratio is 6-15:1; During hot rolling, control total deformation is 50-80%; During forge hot, control total deformation is 30-60%; During high temperature annealing, control annealing time is 1-2h.
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