CN107523733A - A kind of directional solidification Nb Si based multicomponent alloys - Google Patents
A kind of directional solidification Nb Si based multicomponent alloys Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/04—Influencing the temperature of the metal, e.g. by heating or cooling the mould
- B22D27/045—Directionally solidified castings
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
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Abstract
The invention discloses a kind of Nb Si based multicomponent alloys that one kind can prepare aero-turbine or airspace engine hot-end component such as working-blade, guide vane, jet pipe, combustion chamber etc. by directional solidification.Designed by alloy compositions, and the tissue signature of this kind of alloy is changed dramatically in reference to directional solidification, efficiently control the microstructure and chemical composition of alloy, eliminate most of transverse grain boundaries, obtain the casting of low defect, by being suitably heat-treated, the alloy has excellent temperature-room type plasticity, Toughness, high/low temperature intensity.
Description
Technical field
The invention belongs to ultra high temperature alloy material field, is related to a kind of hot junction that can be applied on aero-gas turbine
Part, specially a kind of directional solidification Nb-Si based multicomponent alloys and preparation method thereof.
Background technology
The high thrust-weight ratio aero-engine hot-end component of a new generation needs the higher high-temperature structural material of temperature capability.Nb-Si
There is based alloy high-melting-point (>=1750 DEG C), low-density (≤7.2g/cm3) and good processing characteristics, target temperature in use to reach
To 1200~1400 DEG C, turn into for the high most potential candidate material of thrust-weight ratio aero-engine hot-end component of a new generation,
It is one of the study hotspot in present material field.
The high thrust-weight ratio aero-engine hot-end component of a new generation is very harsh to superhigh temperature structural material performance requirement, it is necessary to
Reach combination property balance in elevated temperature strength, creep resistance, Toughness, inoxidizability and density etc..From material structure
Said in angle, the key performance such as above-mentioned intensity, toughness and environmental stability should by different phases or tissue come undertake, it is necessary to using
Heterogeneous structure matching theory is designed to meet the requirement of material combination property balance.Nb-Si based alloys are exactly a kind of with above-mentioned
The superhigh temperature structural material of new generation of heterogeneous structure feature.The basic composition of Nb-Si based alloys mutually consolidate by the Nb bases including plasticity and toughness
Solution (Nbss) mutually and at high temperature keeps the intermetallic compound Nb of high intensity5Si3Phase, Nbss phases provide Toughness, and
Nb5Si3Elevated temperature strength, creep resistance and high-temperature oxidation resistance are mutually provided.Nbss/Nb5Si3Duplex structure is Nb-Si based alloys
The organization foundation of obdurability matching, by optimizing Nbss/Nb5Si3Tissue, Nb-Si based alloys are made both to have kept certain room temperature tough
Property, there is good high-temperature behavior again.For Nb-Si based alloys, how critical problem is by design of alloy and work
Skill optimizes to realize the Strengthening and Toughening matching of Nb-Si based alloys at a room temperature and a high temperature.
In traditional Nb-Si based alloys component and tissue/performance study, the addition of trace element is generally investigated to alloy
The effect of the formation of some phases in tissue, so as to further study its influence to performance.Such as Publication No. CN106048356
Chinese invention patent, wherein the addition element Zr and micro Y in Nb alloys, Y addition are 0.03-0.3at.%, and Zr's adds
Dosage is 0-8at.%, and B addition is 1-10at.%, and have studied alloying element by way of electric arc melting+heat treatment
To tissue and property relationship.The Chinese invention patents such as Publication No. CN101235460A, CN101608268A, CN101974712,
And US6428910, US5942055 etc. foreign patent have studied associated alloys element and Nb-Si based alloy high-temperatures resist
Oxidisability, the relation of mechanical property.But the studies above only by carrying out melting once to alloy after, or burnt by plasma
The mode of knot is molded, then the mode by post processing, not prepares Nb-Si bases by the way of liquid metal cools down directional solidification
Multicomponent alloy, do not improve the Strengthening and Toughening matching of Nb-Si alloys inherently.And the present inventor is by largely grinding
Study carefully discovery, for Nb-Si based alloys, the elemental constituent of alloy and solidification mode there is collaboration to influence final tissue and performance
Effect, both together decide on phase composition and the phase morphology of alloy, and the tissue final to alloy and performance play the effect of key.
The content of the invention
The present invention is exactly the problem of being difficult to matching for Nb-Si based multicomponent alloy high/low temperature Strengthening and Toughening performances, there is provided one
Class Nb-Si based multicomponent alloys, are designed by rational constituent optimization, and the post that the obtained transverse grain boundaries of directional solidification method are few
The brilliant tissue of shape, makes the high/low temperature mechanical property of alloy significantly improve, can be applied to Turbine Blade part, combustion chamber etc.
Turbogenerator hot-end component.
Complete technical scheme of the invention includes：
A kind of directional solidification Nb-Si based multicomponent alloys, it is characterised in that the alloy is made up of the element of following content：
12%≤Si≤25%, 20%≤Ti≤28%, 1%≤Cr≤24%, 1%≤Al≤10%, 2%≤Hf≤10%, 0.5%
<Y≤5%, surplus Nb, above constituent content are atomic percent.
A kind of directional solidification Nb-Si based multicomponent alloys, it is characterised in that the alloy is using Nb as matrix, by following content
Element composition：14%≤Si≤25%, 20%≤Ti≤28%, 1%≤Cr≤24%, 1%≤Al≤10%, 2%≤Hf
≤ 10%, 0<Zr≤10%, surplus Nb, above constituent content are atomic percent.
A kind of directional solidification Nb-Si based multicomponent alloys, it is characterised in that the alloy is using Nb as matrix, by following content
Element composition：14%≤Si≤25%, 20%≤Ti≤28%, 1%≤Cr≤24%, 1%≤Al≤10%, 2%≤Hf
≤ 10%, 0<Zr≤10%, 0.5%<Y≤5%, surplus Nb, above constituent content are atomic percent.
Further, after described alloy melting, oriented solidification processing, then thermally treated acquisition：Wherein described determines
It it is 1700-2100 DEG C, drawing velocity 1.2-100mm/min to setting temperature, before directional solidification, in directional solidification temperature
Pull is proceeded by after 30min；Heat treatment temperature is 1000-1500 DEG C, and the time is 1~50 hour.
Further, the preparation technology of the alloy comprises the following steps：
(1) alloy of the component is prepared into prealloy mother's ingot using vacuum non-consumable electric arc melting first, to ensure
State the uniformity of alloying component；
(2) use liquid metal cooling method directional solidification, with yttrium or zirconium oxide coating alumina ceramics or
Person's yttria-coated ceramic aluminium oxide ceramics is shell, and described Nb-Si Quito is obtained under certain drawing velocity and holding temperature
First alloy；
(3) by directional freeze method prepare alloy carry out homogenization heat treatment, obtain fine microstructures uniformly, excellent performance
Nb-Si based multicomponent alloys.
Further, the alloy structure includes Nbss phases and Nb5Si3Hardening constituent, wherein Nbss phases content are 20-60%,
Nb5Si3Phase content is 20-60%.
Further, the alloy structure includes 0-25%Cr2Nb phases.
Further, the room temperature tensile intensity ＞ 1000MPa of the alloy, room temperature elongation percentage ＞ 0.85%, room temperature fracture
Toughness ＞ 26.5MPam1/2, high temperature endurance performance is more than 300 hours under 1250 DEG C/80MPa.
The present invention is relative to the advantages of prior art：
1. the design of alloy compositions, first, in the hexa-atomic alloys of Nb-Si-Ti-Cr-Al-Hf, NbSSWith the phase of silicide phase
The factor such as composition, size, pattern and distribution and phase boundary surface intensity together decides on the mechanical property of alloy.Alloying component and lattice
Phase angle influences surface energy and lattice displacement gesture respectively, and when the ratio of surface energy and lattice displacement gesture is more than 6.3, alloy is to prolong
Property alloy.The content of Ti, Zr and Y element influences surface energy and lattice displacement gesture simultaneously, can also improve lattice phase angle.Only
When Ti is more than 20at.%, the ratio of the two could increase with the increase of Ti contents, and alloy is more prone at room temperature
Plastic deformation behavior.Secondly, on the basis of hexa-atomic alloy system, addition Y and/or Zr element has been separately designed, and combinations thereof
Alloy compositions system, further, for each alloy element, by calculating, designing and test, researched and analysed correlation
Tissue, has obtained the reasonable content of different-alloy element.
2. on the basis of the design of above-mentioned alloy compositions, further, alloy compositions are designed and combined with solidification mode, led to
The design in supersolidification path, optimizing tissue and performance.In the prior art, it is use for the production of Nb-Si multicomponent alloys more
After being designed with alloy compositions, electric arc melting obtains the mode of ingot casting.Y and/or Zr of the invention by adding more than 0.5at.%
Constituent content, after electric arc melting homogenizes, then solidified in a manner of directional solidification, with reference to the mode of heat treatment, to obtain Nb-Si more
First alloy.By improving the elements such as Y, Zr, Ti in Nb5Si3、Nb3Si and Cr2Point of the toughness phase such as the enhancing such as Nb phase and Nbss
Cloth, silicide phase and solid solution phase are unexpectedly refined, improved single-phase Nb5Si3、NbSSModulus of elasticity, the spy such as hardness
Property so that phase size and uniformity etc. are optimized, and obtain the Nb of threadiness5Si3Distributed mutually is to NbSSOn matrix, wherein fiber
Average length be more than 20 μm, alloy property has breakthrough improvement.
Brief description of the drawings
Fig. 1 is the XRD spectrum after the oriented solidification of alloy selected by the embodiment of the present invention 1 and heat treatment；
Fig. 2 is the organization chart after the oriented solidification of alloy selected by the embodiment of the present invention 1 and heat treatment；
Fig. 3 is the room temperature tensile properties figure after the oriented solidification of alloy selected by the embodiment of the present invention 1 and heat treatment；
Fig. 4 is the high temperature endurance performance figure after the oriented solidification of alloy selected by the embodiment of the present invention 1 and heat treatment.
Embodiment
The present invention is further elaborated below in conjunction with example, but the invention is not limited in specific embodiment.
The embodiment of the present invention 1,2,3 is respectively Nb-16Si-26Ti-5Cr-2Al-2Hf-1.5Y, Nb-16Si- from component
24Ti-4Cr-2Al-2Hf-3Zr, Nb-16Si-24Ti-4Cr-2Al-2Hf-0.8Y-5Zr alloy, through vacuum non-consumable electric arc
Melting technique obtains alloy mother's ingot, is then molded using directional solidification liquid metal cooling method, then directional solidificating alloy rod is entered
Row vacuum heat is tested, and concrete technology step is as follows：
(1) according to Nb-16Si-26Ti-5Cr-2Al-2Hf-1.5Y, Nb-16Si-24Ti-4Cr-2Al-2Hf-3Zr, Nb-
16Si-24Ti-4Cr-2Al-2Hf-0.8Y-5Zr nominal composition is matched, and weighs the Nb that purity is higher than 99.90wt%,
The raw material such as Ti, Si, Cr, Al, Hf, raw material surface is cleaned (including pickling, alkali cleaning scale removal, using acetone
And/or alcohol degreases) and polishing, drying and processing then is carried out to raw material, carried out after drying with high Accuracy Electronic Balance
Weigh, packaged raw material wait melting.
(2) packaged raw material are placed in vacuum arc melting furnace crucible, and by the former material of the volatile loss of Si, Al
Material is placed in crucible bottom, starts to vacuumize, when vacuum reaches 1.0 × 10-3High-purity argon gas is filled with after Pa, melts vacuum arc
Pressure in furnace reaches 1-5Pa or so and starts melting, and congruent melting is refined 5 times, master alloy ingot overturn after melting each time, really
It is uniform to protect its composition.
(3) to master alloy ingot carry out wire cutting, cut on master alloy ingot φ 14mm pole several, remove pole table
Face and the oxide skin of end face, are dried after being cleaned with acetone, and encapsulation is standby.
(4) cylindrical rod after encapsulation is placed in self-control yttrium pipe, and earthenware and pole is together placed in very
In empty directional solidification furnace, start to vacuumize heating, when vacuum reaches 1.0 × 10-3High-purity argon gas is filled with after Pa to 1-5Pa,
30min is incubated after temperature reaches 1700-2100 DEG C, starts to carry out pull with 1.2-100mm/min drawing velocity, enters
Fast quenching in Ga-In-Sn alloys, furnace cooling.
(5) alloy bar is taken out from yttrium pipe, and polishes off remnants yttrium and oxide on surface,
Dried after cleaning.
(6) the directional solidificating alloy rod obtained by the 5th step is placed in vacuum heat treatment furnace, is evacuated to 1.0 × 10-2Pa it
After start to warm up, when vacuum is evacuated to 1.0 × 10-3Start to be filled with high-purity argon gas after Pa, protected when temperature rises to 1000-1500 DEG C
Warm 50h, furnace cooling.
(7) heat treatment coupon cross section, the longitudinal section obtained the 6th step is cut with wire cutting, with waterproof abrasive paper and abrasive pastes
The polishing and polishing of sample are carried out, prepares metallographic specimen and XRD analysis sample.With wire cutting method in distance orientation rod bottom
50mm-140mm axial location cuts Three Points Bending Specimen and high-temperature and durable sample is some, and Three Points Bending Specimen size is
30mm × 6mm × 3mm, high-temperature and durable specimen length are 60mm, and the size of its active section is 30mm × 2mm × 3mm.
(8) Three Points Bending Specimen is placed on universal electrical experiment machine equipment and carries out fracture toughness and room temperature tensile, room temperature
Elongation percentage is tested, and each alloy bar cuts 6 Three Points Bending Specimens and 3 tensile samples, and final performance is averaged.
(9) high-temperature and durable sample is placed in the high-temperature behavior test machine equipped with thermocouple and heating system and tensioning system
On tested, three high-temperature and durable samples are cut on each alloy coupon, are averaged.
Tissue that embodiment 1 obtains as shown in figure 1, directional solidificating alloy mainly by Nbss phases, α-Nb5Si3Mutually and γ-
Nb5Si3Phase composition.The microstructure of embodiment 1 is as shown in Fig. 2 alloy passes through directional solidification, and each phase is substantially along solidification direction
Align.The specific performance of embodiment 1 as shown in Figure 3-4 with table 1 listed by, alloy it is oriented solidification and heat treatment after, room temperature
Tensile strength is up to more than 1050MPa, and room temperature elongation percentage is more than 0.85%.Room-Temperature Fracture Toughness is more than 26.5MPam1/2,
High temperature endurance performance is more than 300 hours under 1250 DEG C/80MPa.Table 1 embodiment 1-3 and contrast experiment's embodiment 4-6 property
Can data.
The embodiment 1-6 of table 1 performance data
Embodiment 4 is prepared for Nb-16Si-26Ti-5Cr-2Al- in order to verify advantages of the present invention, using arc melting method
2Hf-1.5Y alloys.The Room-Temperature Fracture Toughness of the alloy prepared by this method is less than 15MPam1/2, room temperature tensile intensity is small
Creep rupture life under 400MPa, 0,1250 DEG C/80MPa of temperature-room type plasticity is less than 10 hours, as shown in table 1, well below this
The described performance of invention.
Embodiment 5 is in order to verify effect of the Ti contents more than 18at.% in invention, using orientation described in the present invention
Freezing method is prepared for Nb-16Si-15Ti-4Cr-2Al-2Hf-0.8Y-5Zr alloys.After the Ti contents in alloy decline, alloy
Room-Temperature Fracture Toughness be less than 12MPam1/2, room temperature tensile intensity is less than 350MPa, 0,1250 DEG C/80MPa of temperature-room type plasticity
Creep rupture life is less than 30h, and as shown in table 1, these performances are also well below performance of the present invention.
Embodiment 6 is prepared for Nb-16Si-15Ti-4Cr-2Al- using the directional solidification method described in patent CN102418025
2Hf-0.8Y-5Zr alloy, Nb in alloy structure5Si3Vermiform is showed, it is not elongated fibrous described in this patent, should
Nb in the alloy structure that directional solidification method described in patent prepares5Si3For phase elongated fibers length more than 20 μm, size is big
In the vermiform Nb described in patent CN1024180255Si3Size, each performance is as shown in table 1, far below the alloy described in this patent
Performance.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the scope of the invention, every utilization
The equivalent structure or equivalent flow conversion that present specification is made, or directly or indirectly it is used in other related technologies
Field, it is included within the scope of the present invention.
Claims (8)
1. a kind of directional solidification Nb-Si based multicomponent alloys, it is characterised in that the alloy is made up of the element of following content：
12%≤Si≤25%, 20%≤Ti≤28%, 1%≤Cr≤24%, 1%≤Al≤10%, 2%≤Hf≤10%, 0.5%
<Y≤5%, surplus Nb, above constituent content are atomic percent.
2. a kind of directional solidification Nb-Si based multicomponent alloys, it is characterised in that the alloy is using Nb as matrix, by following content
Element forms：14%≤Si≤25%, 20%≤Ti≤28%, 1%≤Cr≤24%, 1%≤Al≤10%, 2%≤Hf≤
10%, 0<Zr≤10%, surplus Nb, above constituent content are atomic percent.
3. a kind of directional solidification Nb-Si based multicomponent alloys, it is characterised in that the alloy is using Nb as matrix, by following content
Element forms：14%≤Si≤25%, 20%≤Ti≤28%, 1%≤Cr≤24%, 1%≤Al≤10%, 2%≤Hf≤
10%, 0<Zr≤10%, 0.5%<Y≤5%, surplus Nb, above constituent content are atomic percent.
4. the directional solidification Nb-Si based multicomponent alloys according to claim any one of 1-3, it is characterised in that described conjunction
After golden melting, oriented solidification processing, then thermally treated acquisition：Wherein described directional solidification temperature is 1700-2100 DEG C, is taken out
Pulling rate degree is 1.2-100mm/min, and before directional solidification, pull is proceeded by after directional solidification temperature 30min；Heat treatment
Temperature is 1000-1500 DEG C, and the time is 1~50 hour.
5. the directional solidification Nb-Si based multicomponent alloys according to claim any one of 1-4, it is characterised in that after melting again
The concrete technology of oriented solidification comprises the following steps：
(1) alloy of the component is prepared into prealloy mother's ingot using vacuum non-consumable electric arc melting first, to ensure the conjunction
The uniformity of golden composition；
(2) use liquid metal cooling method directional solidification, with yttrium either zirconium oxide coating alumina ceramics or oxygen
It is shell to change yttrium coating alumina ceramics, and described Nb-Si Quito member is obtained under certain drawing velocity and holding temperature and is closed
Gold；
(3) alloy prepared by directional freeze method is subjected to homogenization heat treatment, it is uniform, excellent performance obtains fine microstructures
Nb-Si based multicomponent alloys.
6. the directional solidification Nb-Si based multicomponent alloys according to claim any one of 1-5, it is characterised in that the alloy
Tissue includes Nbss phases and Nb5Si3Hardening constituent, wherein Nbss phases content are 20-60%, Nb5Si3Phase content is 20-60%.
7. directional solidification Nb-Si based multicomponent alloys according to claim 6, it is characterised in that the alloy structure includes
0-25%Cr2Nb phases.
8. the directional solidification Nb-Si based multicomponent alloys described in claim any one of 1-7, it is characterised in that the room of the alloy
Warm tensile strength ＞ 1000MPa, room temperature elongation percentage ＞ 0.85%, Room-Temperature Fracture Toughness ＞ 26.5MPam1/2, 1250 DEG C/
High temperature endurance performance is more than 300 hours under 80MPa.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108085526A (en) * | 2017-12-15 | 2018-05-29 | 中南大学 | A kind of low-density niobium based composites and preparation method |
| CN108277410A (en) * | 2018-01-24 | 2018-07-13 | 北京航空航天大学 | A kind of NbSi alloys with preferred orientation relationship |
| CN108796253A (en) * | 2018-04-24 | 2018-11-13 | 西北工业大学 | A kind of preparation of reactive infiltration Si-Y alloys and tissue modulation method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102418025A (en) * | 2011-12-12 | 2012-04-18 | 北京航空航天大学 | Structure controlled preparation method for Nb-Si-based complex alloy |
| CN106048356A (en) * | 2016-01-28 | 2016-10-26 | 西北工业大学 | Multi-element Nb-Si-based super-high-temperature alloy material and preparing method thereof |
-
2017
- 2017-09-04 CN CN201710784076.1A patent/CN107523733B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102418025A (en) * | 2011-12-12 | 2012-04-18 | 北京航空航天大学 | Structure controlled preparation method for Nb-Si-based complex alloy |
| CN106048356A (en) * | 2016-01-28 | 2016-10-26 | 西北工业大学 | Multi-element Nb-Si-based super-high-temperature alloy material and preparing method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108085526A (en) * | 2017-12-15 | 2018-05-29 | 中南大学 | A kind of low-density niobium based composites and preparation method |
| CN108277410A (en) * | 2018-01-24 | 2018-07-13 | 北京航空航天大学 | A kind of NbSi alloys with preferred orientation relationship |
| CN108277410B (en) * | 2018-01-24 | 2020-11-17 | 北京航空航天大学 | NbSi alloy with preferred orientation relation |
| CN108796253A (en) * | 2018-04-24 | 2018-11-13 | 西北工业大学 | A kind of preparation of reactive infiltration Si-Y alloys and tissue modulation method |
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