CN104630639B - A kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy and preparation method - Google Patents
A kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy and preparation method Download PDFInfo
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Abstract
The present invention relates to a kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy and preparation method, belong to powdered metallurgical material field.Ferrous alloy of the present invention, including matrix and enhancing phase；Described matrix includes by percentage to the quality: Cr:12 17%, W:1 4%, and surplus is Fe；Described enhancing includes yttrium nitride mutually.Yttrium nitride, by matrix pre-alloyed powder and yttrium nitride mixing and ball milling, is broken into nano-particle by the present invention, evenly spreads to iron-based prealloyed powder matrix, then shapes powder consolidation, prepare nano yttrium oxide dispersion strengthening iron-base alloy.The present invention effectively obtains the most tiny, the nanoparticle of Dispersed precipitate in alloy substrate, it is ensured that ferrous alloy possesses the room temperature of excellence, mechanical behavior under high temperature, reduces difficulty of preparation technology, is conducive to being prepared on a large scale the dispersion strengthening iron-base alloy of stable performance.
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
Powdered metallurgical material field.
Background technology
Oxide dispersion intensifying (ODS) is to add high thermal stability and chemistry in alloy substrate
The nano-oxide particles of stability so that it is dispersed in the base, by hinder dislocation and
Grain boundary and produce invigoration effect.Strengthening effect is had significantly by size and the distribution of disperse phase
Impact, the size of diffusing particle is the most tiny, is distributed the most uniform, and strengthening effect is the most notable.Cause
This, it is thus achieved that enhanced particles tiny, equally distributed is to improve oxide-dispersed alloy performance
Key.
ODS ferrous alloy have excellence high temperature creep-resisting, fatigue at high temperature, radioprotective swelling and
Decay resistance, has wide application prospect in fields such as the energy and hot-working industry.At iron-based
In alloy substrate, introducing disperse is uniform, tiny and has good heat stability and chemical stability
Oxide particle, room temperature and the mechanical behavior under high temperature of alloy can be greatly improved.Yittrium oxide has
High hardness and heat stability, be typically used as dispersion-strengtherning phase.Concrete grammar is to be closed by machinery
Aurification, crushes yttria particles and makes its Dispersed precipitate in alloy powder matrix, then leading to
Cross powder forming, it is thus achieved that the dispersion-strengtherning phase of a size of 10-40nm, be evenly distributed on alloy-based
In body, generation 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 Materials
280(2000)264]。
In ferrous alloy, add Ti element, react between Ti, Y, O in sintering process,
Form the hardening constituent of a size of 2-5nm.This hardening constituent particle components is Y-Ti-O, and structure is multiple
Miscellaneous, the most highly stable, but the acquisition of tiny Y-Ti-O nanoparticle is extremely difficult,
Preparation technology to alloy, and the content requirement of Y, Ti and O atom is the harshest.Meanwhile,
Powder is in powder process, forming process, and oxygen can be adsorbed in surface, and this part oxygen is unnecessary surplus
Oxygen, can cause oxide hardening constituent to be grown up, and forms large scale (> 50nm), even micro-meter scale
Oxide, serious fall low-alloyed mechanical property [S Ohtsuka, S Ukai, M Fujiwara, T
Kaito,T Narita.Journal of Physics and Chemistry of Solids 2-4(2005)
571]。
But, to prepare at powder, in forming process, powder adsorption oxygen is unavoidable, this
Grow up contradiction with avoiding oxide.The most effectively utilize the excess oxygen of powder adsorption, be to solve to ask
The key of topic.
The present invention proposes, and using yttrium nitride is that primary strengthening phase prepares high-performance ferrous alloy, opens
Send out the high-performance ferrous alloy and preparation method being easier to obtain.With yttrium nitride for strengthening phase
Fe-Cr-W-M (M is one or more in the metallic elements such as Ti, Zr, Al) alloy is in existing skill
Art have not been reported.
Summary of the invention
The present invention is directed to the weak point that existing dispersed oxide ferrous alloy exists, it is provided that a kind of
With ferrous alloy that nano silicon nitride yttrium is main dispersion-strengtherning phase and preparation method.
One nano silicon nitride yttrium dispersion strengthening iron-base alloy of the present invention, it includes matrix and enhancing
Phase；
Described matrix includes by percentage to the quality:
Cr:12-17%, preferably 12-16%, more preferably 13-15%；
W:1-4%, 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 enhancing includes yttrium nitride mutually；
The quality of described yttrium nitride is the 0.3-1% of substrate quality, preferably 0.3%-0.7%, enters
One step is preferably 0.3%-0.5%.
One nano silicon nitride yttrium dispersion strengthening iron-base alloy of the present invention, 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, tensile strength of 500 DEG C
>=1140MPa, the tensile strength >=850MPa of 600 DEG C.
The preparation method of the present invention a kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy, including following
Step:
Step one
Yttrium nitride powder is weighed 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 includes 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
For 30-60h；Described M one in the metallic element such as Ti, Zr, Al at least one；
Step 2
To step one gained mechanical alloying powder load jacket, vacuum degassing, soldering and sealing, then
Hot-pressed, carry out hot rolling or forge hot, high annealing after shaping successively, obtain yttrium nitride more
Dissipate reinforced iron-base alloy；Time hot-pressed, control temperature and be 900-1000 DEG C；Hot rolling or
During forge hot, control temperature and be 950-1150 DEG C；During high annealing, controlling temperature is
1050-1200℃。
The preparation method of the present invention a kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy, step one
In, the granularity of yttrium nitride powder is less than or equal to 30 μm, further preferably less than equal to 10 μm；
The granularity of iron(-)base powder is less than or equal to 150 μm (-100 mesh), is preferably less than equal to
106 μm (-150 mesh), further preferably less than equal to 75 μm (-200 mesh).
The preparation method of the present invention a kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy, step one
In, the preparation method of described matrix alloy powder is:
Join by the matrix alloy component of design and take raw material, through vacuum induction melting, argon atomization,
Obtain the granularity matrix alloy powder less than or equal to 150 μm (-100 mesh).
The preparation method of the present invention a kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy, step one
In, described protective atmosphere one in argon, helium.
The preparation method of the present invention a kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy, step one
In, during ball milling, controlling ball material mass ratio is 8-12:1.
The preparation method of the present invention a kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy, step 2
In, time hot-pressed, control extrusion ratio is 6-15:1；During hot rolling, control total deformation
Amount is 50-80%；During forge hot, control total deformation is 30-60%；During high annealing, control
Annealing time is 1-2h.
Advantages of the present invention and good effect:
The present invention use non-oxide system high stability yttrium nitride granule as dispersion-strengtherning phase,
Fragility yttrium nitride, in Process During High Energy Ball Milling, is easily broken into be smaller in size than 10nm tiny
Grain, is dispersed among alloy substrate, in powder forming subsequently, heat treatment process,
High stability yttrium nitride not with alloy constituent element generation chemical reaction, it is to avoid particle growth, it is ensured that
Dispersion-strengthened effect, puies forward heavy alloyed mechanical property.
The present invention is prepared at powder, the oxygen of powder adsorption in forming process, when hot forming,
Formation steady oxide can be reacted with the active element in alloy, become the second hardening constituent, make
Obtain the oxygen of inevitable absorption in technical process, be utilized effectively.Due to alloy unit in matrix
Element is evenly distributed, the oxide the formed disperse that is evenly distributed in alloy substrate.
Compared with oxide-dispersed alloy, alloy substrate of the present invention do not has added Oxides
Hardening constituent is grown up core as oxide, and prepared by powder, the direct shape of oxygen of absorption in forming process
Become dispersed oxide to be distributed in the base, effectively overcome in oxide-dispersed alloy and adsorb
Oxygen causes the defect that oxide hardening constituent is grown up.
In a word, the present invention is with fragility yttrium nitride as 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；Crush yttrium nitride granule by high-energy ball milling, obtain particle size less than 10nm
Fine particle, even dispersion be distributed in matrix produce dispersion-strengtherning effect, prepare high-performance
Ferrous alloy material.Due to tiny yttrium nitride granule not with alloy constituent element generation chemical reaction,
Particle growth can be prevented effectively from, it is ensured 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；With
Time, the oxygen that technical process introduces, it is utilized effectively by forming oxide dispersion intensifying phase,
Can effectively reduce the difficulty that powder is prepared, stored, transports, reduce powder preparation cost.This
Invented technology is simple, prepares high performance material difficulty low, efficiently solves technical process absorption
A difficult problem for this puzzlement field of powder metallurgy of oxygen, is conducive to being prepared on a large scale the high property of stable performance
Can dispersion strengthening iron-base alloy.
Accompanying drawing explanation
Accompanying drawing 1 is the Fe-13.6Cr-3.3W-0.3YN (mass fraction) prepared by embodiment 1
Alloy microscopic structure transmission photo.
From figure 1 it appears that matrix is uniform-distribution with the diameter hardening constituent less than 6nm
Granule.
Detailed description of the invention
The present invention uses high-energy ball milling, prepares nano silicon nitride yttrium dispersion strengthening iron-base alloy, under
Face combines example, and the present invention will be further described.
Comparative example 1:
Design alloying component, described alloy includes following component by percentage to the quality:
Cr:13.6%；W:3.3%；Y2O3: 0.3；Surplus is Fe；
Testing raw materials used is that (composition is Fe-13.6Cr-3.3W to atomization pre-alloyed powder, matter
Amount mark) and Y2O3Powder.Wherein, the granularity of pre-alloyed powder is less than or equal to 75 μm (-200
Mesh), Y2O3The mean diameter of powder is less than or equal to 30nm.Pre-alloyed powder adds
Mass fraction is the Y of 0.3%2O3Powder, mix rearmounted enter in ball grinder, be filled with after evacuation
High-purity argon gas, ball milling, rotational speed of ball-mill is 350rpm, and Ball-milling Time controls to be 48h, obtains
Granularity is less than or equal to the mechanical alloying powder of 13 μm.The powder of mechanical alloying is loaded steel
Jacket, evacuation degasification, soldering and sealing, then at 950 DEG C of extrusion moldings, then extruded bars is existed
950 DEG C carry out the rolling that overall reduction is 70%, finally by alloy at 1050 DEG C of 1h that anneal.
The alloy of preparation, matrix grain size is about 600nm, even dispersion distribution nanometer in matrix
Y2O3Particle (10-20nm), its average particle size particle size is 14nm, room temperature, 500 DEG C and
The tensile strength of 600 DEG C is respectively 1135MPa, 898MPa and 654MPa, elongation of having no progeny
Rate is respectively 15.7%, 15% and 17.5%.
Embodiment 1:
Design alloying component is: Fe-13.6Cr-3.3W-0.3YN (mass fraction)
Testing raw materials used is that (composition is Fe-13.6Cr-3.3W to atomization pre-alloyed powder, matter
Amount mark) and YN powder.Wherein, the granularity of pre-alloyed powder is less than or equal to 75 μm (-200
Mesh), the mean diameter of YN powder is less than or equal to 10 μm.Matter is added in pre-alloyed powder
Amount mark is the YN powder of 0.3%, mix rearmounted enter in ball grinder, be filled with height after evacuation
Pure argon, ball milling, rotational speed of ball-mill is 350rpm, and Ball-milling Time controls to be 48h, obtains grain
Degree is less than or equal to the mechanical alloying powder of 12 μm.The powder of mechanical alloying is loaded ladle
Set, evacuation degasification, soldering and sealing, then extruded at 950 DEG C, then by extruded bars at 950 DEG C
Carry out the rolling that overall reduction is 70%, finally by alloy at 1050 DEG C of 1h that anneal.Preparation
Alloy, matrix grain size is about 500nm, and in matrix, even dispersion is distributed the most tiny
Nanoparticle, its particle size be less than 6nm (see accompanying drawing 1), room temperature, 500 DEG C and
The tensile strength of 600 DEG C is respectively 1461MPa, 1127MPa and 825MPa, elongation of having no progeny
Rate is respectively 14.7%, 16.6% and 19.2%.
Embodiment 2:
Fe-13.9Cr-4.0W-1YN (mass fraction)
Testing raw materials used is that (composition is Fe-13.9Cr-4.0W to atomization pre-alloyed powder, matter
Amount mark) and YN powder.Wherein, the granularity of pre-alloyed powder is less than or equal to is 75 μm (-200
Mesh), the mean diameter of YN powder is less than or equal to 10 μm.Matter is added in pre-alloyed powder
Amount mark is the YN powder of 1%, mix rearmounted enter in ball grinder, be filled with high-purity after evacuation
Argon, ball milling, rotational speed of ball-mill is 300rpm, and Ball-milling Time controls to be 60h, obtains granularity
Mechanical alloying powder less than or equal to 10 μm.The powder of mechanical alloying is loaded ladle
Set, evacuation degasification, soldering and sealing, then extruded at 1000 DEG C, then extruded bars is existed
1000 DEG C carry out the rolling that overall reduction is 60%, finally by alloy at 1050 DEG C of 1h that anneal.
The alloy of preparation, matrix grain size is about 500nm, and in matrix, even dispersion is distributed greatly
Measuring tiny nanoparticle, its average particle size particle size is 8nm, room temperature, 500 DEG C and 600 DEG C
Tensile strength be respectively 1590MPa, 1307MPa and 895MPa, elongation after fracture divides
It is not 12.5%, 14.1% and 16.7%.
Embodiment 3:
Fe-15.2Cr-3.7W-0.5YN (mass fraction)
Test raw materials used for atomization pre-alloyed powder (composition is Fe-15.2Cr-3.7W, mass fraction)
With YN powder.Wherein, the granularity of pre-alloyed powder is less than or equal to 75 μm (-200 mesh),
The mean diameter of YN powder is less than or equal to 10 μm.Mass fraction is added in pre-alloyed powder
Be the YN powder of 0.5%, mix rearmounted enter in ball grinder, be filled with high-purity argon gas after evacuation,
Ball milling, rotational speed of ball-mill is 300rpm, and Ball-milling Time controls to be 60h, obtains granularity and is less than
Mechanical alloying powder in 9.5 μm.The powder of mechanical alloying is loaded steel capsule, takes out
Vacuum degassing, soldering and sealing, then extruded at 1000 DEG C, then by extruded bars at 1050 DEG C
Carry out the forging that overall reduction is 40%, finally by alloy at 1050 DEG C of 1h that anneal.Preparation
Alloy, matrix grain size is about 500nm, and in matrix, even dispersion is distributed the most tiny
Nanoparticle, its average particle size particle size is 7nm, anti-room temperature, 500 DEG C and 600 DEG C
Tensile strength is respectively 1506MPa, 1164MPa and 879MPa, and elongation after fracture is respectively
13.5%, 14.2% and 15.3%.
Embodiment 4:
Fe-14.2Cr-3.7W-1.0Ti-0.5YN (mass fraction)
Test raw materials used for atomization pre-alloyed powder (composition is Fe-15.2Cr-3.7W, mass fraction)
With YN powder.Wherein, the granularity of pre-alloyed powder is less than or equal to 75 μm (-200 mesh),
The mean diameter of YN powder is less than or equal to 10 μm.Mass fraction is added in pre-alloyed powder
Be the YN powder of 0.5%, mix rearmounted enter in ball grinder, be filled with high-purity argon gas after evacuation,
Ball milling, rotational speed of ball-mill is 300rpm, and Ball-milling Time controls to be 60h, obtains granularity and is less than
Mechanical alloying powder in 9 μm.The powder of mechanical alloying is loaded steel capsule, takes out true
Empty degasification, soldering and sealing, then extruded at 900 DEG C, then extruded bars is carried out at 1150 DEG C
Overall reduction is the forging of 40%, finally by alloy at 1100 DEG C of 2h that anneal.The alloy of preparation,
Matrix grain size is about 500nm, and in matrix, even dispersion is distributed the most tiny nanometer
Particle, its average particle size particle size is 7nm, in room temperature, 500 DEG C and the tensile strength of 600 DEG C
Being respectively 1595MPa, 1435MPa and 910MPa, elongation after fracture is respectively 10.5%,
13.2% and 14.3%.
Claims (7)
1. a nano silicon nitride yttrium dispersion strengthening iron-base alloy, including matrix and enhancing phase；It is special
Levy and be:
Described matrix is made up of following component 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 enhancing includes yttrium nitride mutually；
The quality of described yttrium nitride is the 0.3%-0.7% of substrate quality.
A kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy the most according to claim 1；
It is characterized in that:
Described matrix is made up of following component 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 enhancing includes yttrium nitride mutually；
The quality of described yttrium nitride is the 0.3%-0.5% of substrate quality.
3. according to a kind of nano silicon nitride yttrium dispersion strengthened iron described in claim 1-2 any one
Base alloy, it is characterised in that: the room temperature tensile intensity of described yttrium nitride dispersion strengthening iron-base alloy
For >=1450MPa, the tensile strength of 500 DEG C be >=1100MPa, the tensile strength of 600 DEG C is
≥800MPa。
4. prepare nano silicon nitride yttrium dispersion strengthening iron-base alloy as claimed in claim 3 for one kind
Method；It is characterized in that, comprise the steps:
Step one
Yttrium nitride powder is weighed 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 includes 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
For 30-60h；Described M is at least one in Ti, Zr, Al；
In step one, the granularity of yttrium nitride powder is less than or equal to 10 μm；Matrix alloy powder
Granularity is less than or equal to 150 μm；
Step 2
Step one gained mechanical alloying powder is loaded jacket, vacuum degassing, soldering and sealing, then
Hot-pressed, carry out hot rolling or forge hot, high annealing after shaping successively, obtain yttrium nitride more
Dissipate reinforced iron-base alloy；Hot-pressed temperature is 900-1000 DEG C；Hot rolling or hot forging temperature are
950-1150℃；High temperature anneal temperature is 1050-1200 DEG C.
A kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy the most according to claim 4
Preparation method, it is characterised in that: in step one, described protective atmosphere is in argon, helium
One.
A kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy the most according to claim 4
Preparation method, it is characterised in that: in step one, during ball milling, controlling ball material mass ratio is 8-12:
1。
A kind of nano silicon nitride yttrium dispersion strengthening iron-base alloy the most according to claim 4
Preparation method, it is characterised in that: in step 2, time hot-pressed, controlling extrusion ratio is
6-15:1；During hot rolling, control total deformation is 50-80%；During forge hot, control total deformation
Amount is 30-60%；During high annealing, control annealing time is 1-2h.
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| TWI607093B (en) * | 2015-06-01 | 2017-12-01 | 國立臺灣科技大學 | Metal alloy composite material and method for making the same |
| CN108907209B (en) * | 2018-07-27 | 2020-04-07 | 中南大学 | Oxide dispersion strengthening iron-based alloy powder and characterization method thereof |
| CN110607487B (en) * | 2019-10-09 | 2021-03-02 | 北京钢研高纳科技股份有限公司 | ODS-Fe3Al alloy, alloy product and preparation method thereof |
| CN114178534B (en) * | 2020-08-25 | 2023-12-12 | 香港大学 | Antibacterial stainless steel powder and preparation method and application thereof |
| CN112170854B (en) * | 2020-10-14 | 2021-06-15 | 中南大学 | Method for preparing nano spherical oxide dispersion strengthening phase |
| CN114686722B (en) * | 2022-05-06 | 2023-04-18 | 浙江百川导体技术股份有限公司 | Rare earth nitride dispersion strengthening brass alloy and preparation method thereof |
| CN114807668B (en) * | 2022-05-06 | 2022-11-01 | 浙江百川导体技术股份有限公司 | Rare earth nitride dispersion strengthening titanium-doped copper alloy and preparation method thereof |
| CN115446302B (en) * | 2022-08-31 | 2024-04-19 | 鞍钢股份有限公司 | Iron-based intermediate with uniformly dispersed nano particles and preparation and use methods thereof |
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