CN107523733B - A kind of directional solidification Nb-Si based multicomponent alloy - Google Patents
A kind of directional solidification Nb-Si based multicomponent alloy Download PDFInfo
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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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- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
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- 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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- 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.It is designed by alloy compositions, and it changed dramatically the tissue signature of this kind of alloy in conjunction with directional solidification, efficiently control the microstructure and chemical component of alloy, eliminate most of transverse grain boundaries, obtain the casting of low defect, by being suitably heat-treated, which has excellent temperature-room type plasticity, Toughness, high/low temperature intensity.
Description
Technical field
The invention belongs to ultra high temperature alloy material fields, are related to a kind of hot end that can be applied on aero-gas turbine
Component, specially a kind of directional solidification Nb-Si based multicomponent alloy and preparation method thereof.
Background technique
The high thrust 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 performance, target to be reached using temperature
To 1200~1400 DEG C, become for the high most potential candidate material of thrust ratio aero-engine hot-end component of a new generation,
It is one of the research hotspot in present material field.
The high thrust ratio aero-engine hot-end component of a new generation is very harsh to superhigh temperature structural material performance requirement, it is necessary to
Elevated temperature strength, creep resistance, Toughness, inoxidizability and in terms of reach comprehensive performance balance.From material structure
It is said in angle, the key performances such as above-mentioned intensity, toughness and environmental stability should be undertaken by different phases or tissue, need to apply
The design of heterogeneous structure matching theory is to meet the requirement that material comprehensive performance balances.Nb-Si based alloy is exactly a kind of with above-mentioned
The superhigh temperature structural material of new generation of heterogeneous structure feature.Mutually the Nb base including plasticity and toughness is solid for the basic composition of Nb-Si based alloy
Solution (Nbss) mutually and at high temperature keeps high-intensitive intermetallic compound Nb5Si3Phase, Nbss phase provide Toughness, and
Nb5Si3Elevated temperature strength, creep resistance and high-temperature oxidation resistance are mutually provided.Nbss/Nb5Si3Duplex structure is Nb-Si based alloy
The matched organization foundation of obdurability, by optimizing Nbss/Nb5Si3Tissue makes Nb-Si based alloy both keep certain room temperature tough
Property, and there is good high-temperature behavior.For Nb-Si based alloy, how critical problem is by design of alloy and work
Skill optimizes to realize the Strengthening and Toughening matching of Nb-Si based alloy at a room temperature and a high temperature.
In traditional Nb-Si based alloy component and tissue/performance study, the addition of microelement is usually investigated to alloy
The effect of the formation of certain phases in tissue, to further study its influence to performance.Such as Publication No. CN106048356
Chinese invention patent, the addition element Zr and micro Y in Nb alloy, wherein the additive amount of Y is 0.03-0.3at.%, and Zr's adds
Dosage is 0-8at.%, and the additive amount of B is 1-10at.%, and has 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 patents to have studied associated alloys element and Nb-Si based alloy high-temperature anti-
Oxidisability, the relationship of mechanical property.But the studies above only by alloy carry out melting once after, or by plasma burning
The mode of knot forms, and using the mode of post-processing, not prepares Nb-Si base by the way of the cooling directional solidification of liquid metal
Multicomponent alloy, there is no the Strengthening and Toughening matchings for inherently improving Nb-Si alloy.And the present inventor is by largely grinding
Study carefully discovery, for Nb-Si based alloy, the elemental constituent of alloy and solidification mode have synergy to final tissue and performance
Effect, the two codetermine phase composition and the phase morphology of alloy, and the tissue final to alloy and performance play crucial effect.
Summary of the invention
The present invention exactly aiming at the problem that Nb-Si based multicomponent alloy high/low temperature Strengthening and Toughening performance is difficult to match, provides one
Class Nb-Si based multicomponent alloy, is designed and column that transverse grain boundaries that directional solidification method obtains are few by reasonable constituent optimization
Shape crystalline substance tissue makes the high/low temperature mechanical property of alloy significantly improve, can be applied to Turbine Blade component, combustion chamber etc.
Turbogenerator hot-end component.
The complete technical solution of the present invention includes:
A kind of directional solidification Nb-Si based multicomponent alloy, which is characterized in that the alloy is made 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, the above constituent content are atomic percent.
A kind of directional solidification Nb-Si based multicomponent alloy, which is characterized 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, the above constituent content is atomic percent.
A kind of directional solidification Nb-Si based multicomponent alloy, which is characterized 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, the above constituent content are atomic percent.
Further, after the alloy melting, oriented solidification processing, then thermally treated acquisition: determine described in wherein
It is 1700-2100 DEG C, drawing velocity 1.2-100mm/min to setting temperature, before directional solidification, in directional solidification temperature
Start to carry out pull after 30min；Heat treatment temperature is 1000-1500 DEG C, and the time is 1~50 hour.
Further, the preparation process of the alloy includes the following steps:
(1) vacuum non-consumable electric arc melting is used to prepare prealloy mother's ingot first the alloy of the component, 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 Quito Nb-Si 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, have excellent performance
Nb-Si based multicomponent alloy.
Further, the alloy structure includes Nbss phase and Nb5Si3Hardening constituent, wherein Nbss phase content is 20-60%,
Nb5Si3Phase content is 20-60%.
Further, the alloy structure includes 0-25%Cr2Nb phase.
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 greater than 300 hours under 1250 DEG C/80MPa.
The present invention compared with the existing technology the advantages of be:
1. the design of alloy compositions, firstly, in the hexa-atomic alloy of Nb-Si-Ti-Cr-Al-Hf, NbSSWith the phase of silicide phase
The mechanical property of the factors such as ingredient, size, pattern and distribution and phase boundary surface intensity co-determination alloy.Alloying component and lattice
Phase angle influences surface respectively can be with lattice displacement gesture, and when surface can be greater than 6.3 with the ratio of lattice displacement gesture, alloy is to prolong
Property alloy.The content of Ti, Zr and Y element influences surface simultaneously can also be improved lattice phase angle with lattice displacement gesture.Only
When Ti is greater than 20at.%, the ratio of the two could increase with the increase of Ti content, and alloy is more prone to produce at room temperature
Plastic deformation behavior.Secondly, addition Y and/or Zr element has been separately designed on the basis of hexa-atomic alloy system, and combinations thereof
Alloy compositions system correlation has further been researched and analysed by calculating, design and experiment for each alloy element
Tissue, has obtained the reasonable content of different-alloy element.
2. further, by alloy compositions design in conjunction with solidification mode, leading on the basis of the design of above-mentioned alloy compositions
The design in supersolidification path, optimizing tissue and performance.In the prior art, it for the production of Nb-Si multicomponent alloy, mostly uses
After being designed with alloy compositions, electric arc melting obtains the mode of ingot casting.The Y and/or Zr that the present invention passes through addition 0.5at.% or more
Constituent content solidifies after electric arc melting homogenizes, then in a manner of directional solidification, and in conjunction with 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 reinforced phases such as Nb and Nbss
Cloth has unexpectedly refined silicide phase and solid solution phase, improves single-phase Nb5Si3、NbSSThe spies such as elasticity modulus, hardness
Property, so that phase size and uniformity etc. are optimized, obtain the Nb of threadiness5Si3Mutually it is distributed to NbSSOn matrix, wherein fiber
Average length be greater than 20 μm, alloy property has breakthrough improvement.
Detailed description of the invention
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.
Specific embodiment
The present invention is further elaborated below in conjunction with example, but the invention is not limited to specific embodiments.
Selection group is divided into Nb-16Si-26Ti-5Cr-2Al-2Hf-1.5Y, Nb-16Si- to the embodiment of the present invention 1,2,3 respectively
The alloy of 24Ti-4Cr-2Al-2Hf-3Zr, Nb-16Si-24Ti-4Cr-2Al-2Hf-0.8Y-5Zr, through vacuum non-consumable electric arc
Melting technique obtains alloy mother's ingot, then using directional solidification liquid metal cooling method form, then to directional solidificating alloy stick into
The experiment of row vacuum heat treatment, the specific process steps are as follows:
(1) according to Nb-16Si-26Ti-5Cr-2Al-2Hf-1.5Y, Nb-16Si-24Ti-4Cr-2Al-2Hf-3Zr, Nb-
The nominal composition of 16Si-24Ti-4Cr-2Al-2Hf-0.8Y-5Zr is matched, and the Nb that purity is higher than 99.90wt% is weighed,
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, is carried out after drying with high Accuracy Electronic Balance
It weighs, 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 degree reaches 1.0 × 10-3It is filled with high-purity argon gas after Pa, keeps vacuum arc molten
Pressure in furnace reaches 1-5Pa or so and starts melting, and congruent melting is refined 5 times, overturn after melting to master alloy ingot each time, really
It is uniform to protect its ingredient.
(3) to master alloy ingot carry out wire cutting, cut on master alloy ingot φ 14mm pole several, remove pole table
The oxide skin in face and end face is dried after being cleaned with acetone, is encapsulated spare.
(4) cylindrical rod after encapsulation is placed in self-control yttrium pipe, and ceramic tube and pole is placed in very together
In empty directional solidification furnace, start to vacuumize heating, when vacuum degree reaches 1.0 × 10-3High-purity argon gas is filled with after Pa to 1-5Pa,
30min is kept the temperature after temperature reaches 1700-2100 DEG C, is started to carry out pull with the drawing velocity of 1.2-100mm/min, be entered
Fast quenching in Ga-In-Sn alloy, furnace cooling.
(5) alloy bar is taken out from yttrium pipe, and polishes off remaining yttrium and oxide on surface,
It is dried after cleaning.
(6) the resulting directional solidificating alloy stick of step 5 is placed in vacuum heat treatment furnace, is evacuated to 1.0 × 10-2Pa it
After start to warm up, empty pump to 1.0 × 10 surely-3Start to be filled with high-purity argon gas after Pa, the guarantor when temperature rises to 1000-1500 DEG C
Warm 50h, furnace cooling.
(7) the heat treatment coupon cross section of step 6 acquisition, longitudinal section are cut with wire cutting, with waterproof abrasive paper and abrasive pastes
The polishing and polishing for carrying out sample, prepare metallographic specimen and XRD analysis sample.Stick bottom end is oriented in distance with wire cutting method
The axial location of 50mm-140mm cuts Three Points Bending Specimen and high-temperature and durable sample is several, Three Points Bending Specimen having a size of
30mm × 6mm × 3mm, high-temperature and durable specimen length are 60mm, and the size of active section is 30mm × 2mm × 3mm.
(8) Three Points Bending Specimen is placed on universal electrical test machine equipment and carries out fracture toughness and room temperature tensile, room temperature
Elongation percentage test, each alloy bar cut 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 phase, α-Nb5Si3Phase 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
It aligns.The specific performance of embodiment 1 is as shown in Figure 3-4 and listed by table 1, after the oriented solidification of alloy and heat treatment, room temperature
Tensile strength is up to 1050MPa or more, and room temperature elongation percentage is greater than 0.85%.Room-Temperature Fracture Toughness is more than 26.5MPam1/2,
High temperature endurance performance is greater than 300 hours under 1250 DEG C/80MPa.The property of table 1 embodiment 1-3 and comparative experiments embodiment 4-6
It can data.
The performance data of 1 embodiment 1-6 of table
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 alloy.The Room-Temperature Fracture Toughness of the alloy of this method preparation 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 less than 10 hours, as shown in table 1, well below this
The invention performance.
Embodiment 5 is in order to verify the effect that Ti content in invention is greater than 18at.%, using orientation described in the present invention
Freezing method is prepared for Nb-16Si-15Ti-4Cr-2Al-2Hf-0.8Y-5Zr alloy.After the Ti content in alloy declines, 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 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, it should
Nb in the alloy structure that directional solidification method described in patent prepares5Si3Phase elongated fibers length is more than 20 μm, and size is big
The vermiform Nb described in patent CN1024180255Si3Size, each performance is as shown in table 1, far below alloy described in this patent
Performance.
The above description is only a preferred embodiment of the present invention, is not intended to limit the scope of the invention, all utilizations
Equivalent structure or equivalent flow shift made by present specification is applied directly or indirectly in other relevant technologies
Field is included within the scope of the present invention.
Claims (1)
1. a kind of preparation method of directional solidification Nb-Si based multicomponent alloy, which is characterized in that the alloy by following content member
Element composition: 12%≤Si≤25%, 20%≤Ti≤28%, 1%≤Cr≤24%, 1%≤Al≤10%, 2%≤Hf≤
10%, 0.5% < Y≤5%, 3≤Zr≤10%, surplus Nb, the above constituent content are atomic percent, and the orientation is solidifying
Gu in Nb-Si based multicomponent alloy tissue, Nb5Si3Mutually it is distributed in NbSSOn matrix, specific steps include:
Nb, Ti, Si that purity is higher than 99.90wt%, Cr, Al are weighed, Hf raw material clean raw material surface, including
Pickling, alkali cleaning scale removal are degreased and are polished using acetone and/or alcohol, then carry out drying and processing to raw material,
It is weighed after drying with high Accuracy Electronic Balance, packaged raw material wait melting；
(2) packaged raw material are placed in vacuum arc melting furnace crucible, and the raw material of the volatile loss of Si, Al is set
In crucible bottom, start to vacuumize, when vacuum degree reaches 1.0 × 10-3It is filled with high-purity argon gas after Pa, makes vacuum arc melting furnace
Interior pressure reaches 1-5Pa and starts melting, and congruent melting is refined 5 times, overturn after melting to master alloy ingot each time, it is ensured that its ingredient
Uniformly；
(3) wire cutting is carried out to master alloy ingot, is cut on master alloy ingotPole several, remove pole surface
And the oxide skin of end face, it dries, encapsulates spare after being cleaned with acetone；
(4) cylindrical rod after encapsulation is placed in self-control yttrium pipe, and ceramic tube and pole is placed in vacuum together and determined
Into consolidation furnace, start to vacuumize heating, when vacuum degree reaches 1.0 × 10-3High-purity argon gas is filled with to 1-5Pa after Pa, works as temperature
Degree keeps the temperature 30min after reaching 1700-2100 DEG C, start to carry out pull with the drawing velocity of 1.2mm/min, close into Ga-In-Sn
Fast quenching in gold, furnace cooling；
(5) alloy bar is taken out from yttrium pipe, and polishes off remaining yttrium and oxide on surface, cleaning
After dry；
(6) the resulting directional solidificating alloy stick of step 5 is placed in vacuum heat treatment furnace, is evacuated to 1.0 × 10-2It is opened after Pa
Begin to heat up, surely empty pump to 1.0 × 10-3Start to be filled with high-purity argon gas after Pa, the heat preservation when temperature rises to 1000-1500 DEG C
50h, furnace cooling；
(7) the heat treatment coupon cross section of step 6 acquisition, longitudinal section are cut with wire cutting, is carried out with waterproof abrasive paper and abrasive pastes
The polishing and polishing of sample, prepare metallographic specimen and XRD analysis sample；Stick bottom end 50mm- is oriented in distance with wire cutting method
The axial location of 140mm cuts Three Points Bending Specimen and high-temperature and durable sample is several, Three Points Bending Specimen having a size of 30mm ×
6mm × 3mm, high-temperature and durable specimen length are 60mm, and the size of active section is 30mm × 2mm × 3mm；
(8) Three Points Bending Specimen is placed on universal electrical test machine equipment and carries out fracture toughness and room temperature tensile, room temperature extension
Rate test, each alloy bar cut 6 Three Points Bending Specimens and 3 tensile samples, and final performance is averaged；
The alloy structure includes Nbss phase and Nb5Si3Hardening constituent, wherein Nbss phase content is 20-60%, Nb5Si3Phase content is
20-60%；
The alloy structure includes 0-25%Cr2Nb phase；Room temperature tensile the intensity > 1000MPa, room temperature elongation percentage > of the alloy
0.85%, Room-Temperature Fracture Toughness > 26.5MPam1/2, high temperature endurance performance is greater than 300 hours under 1250 DEG C/80MPa.
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Granted publication date: 20191203 Termination date: 20200904 |