CN105132844A - Method for improving high-temperature oxidation resistance of Nb-Si-based multicomponent alloy - Google Patents
Method for improving high-temperature oxidation resistance of Nb-Si-based multicomponent alloy Download PDFInfo
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Abstract
The invention discloses a method for improving the high-temperature oxidation resistance of Nb-Si-based multicomponent alloy and belongs to the field of ultrahigh-temperature alloy materials. According to the method, high-energy laser beams are made to act on the surface of an Nb-Si-based multicomponent alloy sample under the protection of argon gas by means of a laser melting device by conducting preheating and setting melting technological parameters reasonably, so that the surface of the alloy is molten and solidified rapidly, and a surface remelting layer with fine, a uniform and compact structure is formed, and thus the high-temperature oxidation resistance of the Nb-Si-based multicomponent alloy is improved by refining the structure. According to the method, the phenomenon that cracks are generated easily in the rapid solidification process of brittle alloy is avoided effectively by adding the preheating procedure; meanwhile, the surface remelting layer and a base body are combined in a metallurgy mode, falling is unlikely to happen when the alloy is in service, and the practicability is high.
Description
Technical field
The invention belongs to ultra high temperature alloy material field, relate to a kind of method improving the high-temperature oxidation resistance of ultrahigh temperature alloy, particularly a kind of method utilizing Alloy by Laser Surface Remelting technology to improve Nb-Si based multicomponent alloy high-temperature oxidation resistance.
Background technology
Along with aviation aircraft towards long boat time, the high speed of a ship or plane, high seaworthiness and high security future development, also more and more higher to the requirement of aircraft engine, the specific targets being reflected in engine are exactly higher thrust-weight ratio, longer time between overhaul.The raising of engine thrust-weight ratio and working efficiency, also improves the performance requriements of the engine blade material of core the most thereupon.What be widely used in aero engine turbine blades at present is nickel-base alloy, there is the over-all propertieies such as excellent intensity, toughness, oxidation-resistance and fatigue property, but along with the further increase of thrust-weight ratio, the use temperature of nickel base superalloy is more than 1100 DEG C, reach more than 80% of alloy melting point, this seriously governs the further lifting of aero-engine performance, is thus necessary to research and develop to hold the stronger high temperature structural material of warm ability.
Nb-Si based ultra-high temperature alloy, also claims Nb-Si base in-situ composite, has high-melting-point (>1750 DEG C), low density (6.6-7.2g/cm
3), the advantage such as good hot strength and certain fracture toughness property, fatigue property and workability, become one of high temperature structural material having competitive power.Nb-Si base alloy is primarily of Nb based solid solution (Nb
sS) and intermetallic compound Nb
5si
3form.According to the principle of design of matrix material, Nb
sSthere is provided temperature-room type plasticity and toughness, Nb
5si
3hot strength and antioxidant property are provided mutually.Meanwhile, in alloy, add the alloying elements such as Ti, Cr, Al and Hf and form Nb-Si based multicomponent alloy, the over-all propertieies such as its Toughness, hot strength and oxidation-resistance can be improved further.
Although Nb-Si based multicomponent alloy has excellent mechanical property, its antioxidant property poor is under the high temperature conditions a large bottleneck of this alloy practical application of restriction.The method of the antioxidant property of the raising Nb-Si based multicomponent alloy that present stage adopts is for adding alloy element and using oxidation resistant coating.Add the elements such as Cr, Ti and Hf and can carry heavy alloyed high-temperature oxidation resistance, but be unfavorable for the raising of the mechanical behavior under high temperature of alloy; Oxidation resistant coating (as Mo-Si-B coating) can put forward heavy alloyed oxidation-resistance to a certain extent, but closes because coating and alloy belong to heterojunction, there is the risk of peeling off.Therefore, still need to continue a kind of effective method improving Nb-Si based multicomponent alloy high-temperature oxidation resistance of research and development, to ensure the reliability of Nb-Si based multicomponent alloy under arms in process as blade of aviation engine material.
Summary of the invention
The present invention, just for the Nb-Si based multicomponent alloy problem that oxidisability is poor under the high temperature conditions, under the prerequisite taking into account mechanical property, provides a kind of method improving Nb-Si based multicomponent alloy high-temperature oxidation resistance.High energy laser beam is utilized to make Nb-Si based multicomponent alloy surface melting, tiny, uniform alloy structure is formed after rapid solidification, extraneous oxygen can be suppressed in hot environment to alloy internal divergence, thus carry heavy alloyed high-temperature oxidation resistance by structure refinement, and to form surface remelting layer identical with alloying constituent, and metallurgically combine, be not easy to peel off in military service process.Simultaneously, because Nb-Si based multicomponent alloy toughness is poor, easily crack under rapid solidification condition, the present invention adopts the laser beam alloy under low energy densities condition to carry out preheating, effectively can suppress the generation of crackle, to ensure the compactness of alloy surface remelted layer.
The invention provides a kind of method improving Nb-Si based multicomponent alloy high-temperature oxidation resistance, comprise the following steps:
(1) with the Nb-Si based multicomponent alloy element of certain atomic ratio for synthesis material, preparation Nb-Si based multicomponent alloy sample;
(2) Nb-Si based multicomponent alloy sample is fixed on the table, be filled with shielding gas after tightness system vacuumizes and carry out atmosphere protection;
(3) laser beam is according to the scanning pattern preset and processing parameter, carries out pre-heating scan to Nb-Si based multicomponent alloy specimen surface;
(4) after preheating terminates, amendment processing parameter, laser beam is scanned Nb-Si based multicomponent alloy surface according to the scanning pattern preset, and alloy surface melts and solidifies, and forms remelted layer;
(5) closure systems, takes out when parts are cooled to room temperature, and whole preparation process is carried out in protective atmosphere;
(6) be placed in alumina crucible by without surface remelting process with through the sample of Alloy by Laser Surface Remelting process, then put into high temperature resistance furnace static oxidization, all samples before oxidation test all by accurate measurement size;
(7), after oxidation test terminates, after utilizing scanning electron microscopic observation to be oxidized, the cross section of sample, compares the difference without surface remelting process and the antioxidant property through Alloy by Laser Surface Remelting processing sample.
Nb-Si based multicomponent alloy selected in step (1) is prepared by non-consumable vacuum arc melting and obtains.
In step (3), before surface remelting, laser beam is utilized to carry out preheating to specimen surface, concrete pre-thermal parameter: laser power 250 ~ 400W, sweep velocity 1500 ~ 2000mm/s, sweep span 0.10 ~ 0.25mm, scanning times 5 ~ 10 times.
In step (4), utilize high energy laser beam irradiated sample surface, alloy surface is melted, produce remelted layer, melting characteristic parameter: laser power 350 ~ 500W, sweep velocity 100 ~ 300mm/s, sweep span 0.05 ~ 0.15mm, scanning times 1 ~ 2 time.
Described Nb-Si based multicomponent alloy composition counts Nb-16Si-24Ti-2Cr-2Al-2Hf with atomic percent.
Described Nb-Si based multicomponent alloy composition counts Nb-18Si-24Ti-2Cr-2Al-2Hf with atomic percent.
Described Nb-Si based multicomponent alloy composition counts Nb-20Si-24Ti-2Cr-2Al-2Hf with atomic percent.
Described Nb-Si based multicomponent alloy composition counts Nb-22Si-24Ti-2Cr-2Al-2Hf with atomic percent.
In step (6), utilize short time high temperature oxidation experiment to evaluate the oxidation-resistance of sample, oxidation experiment parameter is: temperature 1250 DEG C, insulation 2h.
The Alloy by Laser Surface Remelting Nb-Si based multicomponent alloy prepared, the surface remelting layer tissue that cool to room temperature obtains is by tiny Nb
sSsosoloid and Nb
5si
3strengthening phase form, phase size <1 μm, is evenly distributed, and density is high, and crackle content is few, and surface remelting layer and matrix alloy associativity better.
Feature of the present invention is:
(1) preparation of alloy of the present invention female ingot is simple, is namely obtained the Nb-Si based multicomponent alloy of heterogeneity by non-consumable arc melting technology.
(2) the present invention is directed to the Nb-Si based multicomponent alloy that Toughness is poor, adopt simple pre-heating step, effectively control the generation of crackle in rapid solidification, thus obtain fine and close surface remelting layer;
(3) prepared in the present invention Alloy by Laser Surface Remelting layer is metallurgically combined with matrix, is not easy to peel off in military service process, practical.
(4) method therefor of the present invention is simple and practical, under the prerequisite taking into account mechanical property, makes the short time high temperature oxidation-resistance of Nb-Si based multicomponent alloy improve more than 8 times.In addition, the present invention can also be generalized to other ultra high temperature alloy material fields.
Accompanying drawing illustrates:
Accompanying drawing 1Nb-16Si-24Ti-2Cr-2Al-2Hf alloy XRD figure is composed;
Accompanying drawing 2Nb-16Si-24Ti-2Cr-2Al-2Hf alloy, without process of the present invention, is oxidized the scanning electron microscopic picture of front and back;
Accompanying drawing 3Nb-16Si-24Ti-2Cr-2Al-2Hf alloy, through process of the present invention, is oxidized the scanning electron microscopic picture of front and back;
Accompanying drawing 4Nb-20Si-24Ti-2Cr-2Al-2Hf alloy XRD figure is composed;
The scanning electron microscopic picture of accompanying drawing 5Nb-20Si-24Ti-2Cr-2Al-2Hf alloy after process of the present invention.
Embodiment
Below in conjunction with example, the present invention is further elaborated, but the present invention is not limited to specific embodiment.
Embodiment 1
Utilize Alloy by Laser Surface Remelting technology to improve Nb-Si based multicomponent alloy high-temperature oxidation resistance, the laser fusion system of use mainly comprises: Nd-YAG laser apparatus, department of computer science unify argon gas atmosphere protector, and step is as follows:
1. with Nb, Si, Ti, Cr, Al, Hf for synthesis material, utilize vacuum non-consumable arc melting technology to obtain the female ingot of Nb-16Si-24Ti-2Cr-2Al-2Hf alloy, utilize Linear cut to cut sample, and specimen surface is polished, dry up for subsequent use after cleaning;
2. fixed on the table by Nb-16Si-24Ti-2Cr-2Al-2Hf alloy sample, the forming cavity vacuum state that first will seal, is then filled with high-purity argon gas (99.99%) and protects;
3. laser beam is according to the scanning pattern preset and parameter, pre-heating scan is carried out to Nb-16Si-24Ti-2Cr-2Al-2Hf alloy sample surface, concrete pre-thermal parameter: laser power 300W, sweep velocity 1800mm/s, sweep span 0.20mm, scanning times 8 times;
4. laser beam is according to the scanning pattern preset and parameter, Nb-16Si-24Ti-2Cr-2Al-2Hf alloy sample surface is scanned, specimen surface melts and solidifies, form remelted layer, concrete remelting parameter: laser power 400W, sweep velocity 100mm/s, sweep span 0.10mm, scanning times 1 time;
5. closure systems, takes out when parts are cooled to room temperature, and whole preparation process is carried out in protective atmosphere;
6. be placed in alumina crucible by without surface remelting process with through the sample of Alloy by Laser Surface Remelting process, then put into high temperature resistance furnace and carry out 1250 DEG C, the static oxidization of 2h, all samples before oxidation test all by accurate measurement size;
7., after oxidation test terminates, after utilizing scanning electron microscopic observation to be oxidized, the cross section of sample, compares the difference without surface remelting process and the antioxidant property through Alloy by Laser Surface Remelting processing sample.
As can be seen from accompanying drawing 1, the surface remelting tissue of Alloy by Laser Surface Remelting Nb-16Si-24Ti-2Cr-2Al-2Hf alloy is primarily of Nb
sSsosoloid and Nb
5si
3two phase composites.Light color is Nb mutually
sSsosoloid, dark color is Nb mutually
5si
3phase.
As can be seen from accompanying drawing 2 and accompanying drawing 3, be oxidized 2h under 1250 DEG C of conditions after, oxidational losses thickness without Alloy by Laser Surface Remelting process alloy sample is about 67.3 μm (accompanying drawings 2), and the oxidational losses thickness of Alloy by Laser Surface Remelting process alloy is 7.9 μm (accompanying drawings 3), show that Alloy by Laser Surface Remelting treatment technology can make the high-temperature oxidation resistance of Nb-Si based multicomponent alloy improve more than 8 times.
Embodiment 2
Utilize Alloy by Laser Surface Remelting technology to improve Nb-Si based multicomponent alloy high-temperature oxidation resistance, the laser fusion system of use mainly comprises: Nd-YAG laser apparatus, department of computer science unify argon gas atmosphere protector, and step is as follows:
1. with Nb, Si, Ti, Cr, Al, Hf for synthesis material, utilize vacuum non-consumable arc melting technology to obtain the female ingot of Nb-20Si-24Ti-2Cr-2Al-2Hf alloy, utilize Linear cut to cut sample, and specimen surface is polished, dry up for subsequent use after cleaning;
2. fixed on the table by Nb-20Si-24Ti-2Cr-2Al-2Hf alloy sample, the forming cavity vacuum state that first will seal, is then filled with high-purity argon gas (99.99%) and protects;
3. laser beam is according to the scanning pattern preset and parameter, pre-heating scan is carried out to Nb-20Si-24Ti-2Cr-2Al-2Hf alloy sample surface, concrete pre-thermal parameter: laser power 300W, sweep velocity 1800mm/s, sweep span 0.20mm, scanning times 8 times;
4. laser beam is according to the scanning pattern preset and parameter, Nb-20Si-24Ti-2Cr-2Al-2Hf alloy sample surface is scanned, specimen surface melts and solidifies, form remelted layer, concrete remelting parameter: laser power 400W, sweep velocity 100mm/s, sweep span 0.10mm, scanning times 1 time;
5. closure systems, takes out when parts are cooled to room temperature, and whole preparation process is carried out in protective atmosphere;
6. be placed in alumina crucible by without surface remelting process with through the sample of Alloy by Laser Surface Remelting process, then put into high temperature resistance furnace and carry out 1250 DEG C, the static oxidization of 2h, all samples before oxidation test all by accurate measurement size;
7., after oxidation test terminates, after utilizing scanning electron microscopic observation to be oxidized, the cross section of sample, compares the difference without surface remelting process and the antioxidant property through Alloy by Laser Surface Remelting processing sample.
As can be seen from accompanying drawing 4 and accompanying drawing 5, the surface remelting layer density of Alloy by Laser Surface Remelting Nb-20Si-24Ti-2Cr-2Al-2Hf alloy is high, and the defects such as crackle, pore and space are less.Nb
sSphase and Nb
5si
3the size of phase is extremely tiny (<1 μm), reach nanophase rank, and two-phase is evenly distributed, and presents obvious rapid solidification structure feature.
The foregoing is only the preferred embodiments of the present invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (10)
1. improve a method for Nb-Si based multicomponent alloy high-temperature oxidation resistance, it is characterized in that, preparation process comprises the following steps:
(1) with the Nb-Si based multicomponent alloy element of certain atomic ratio for synthesis material, preparation Nb-Si based multicomponent alloy sample;
(2) Nb-Si based multicomponent alloy sample is fixed on the table, be filled with shielding gas after tightness system vacuumizes and carry out atmosphere protection;
(3) laser beam is according to the scanning pattern preset and processing parameter, carries out pre-heating scan to Nb-Si based multicomponent alloy specimen surface;
(4) after preheating terminates, amendment processing parameter, laser beam is scanned Nb-Si based multicomponent alloy surface according to the scanning pattern preset, and alloy surface melts and solidifies, and forms remelted layer;
(5) closure systems, takes out when parts are cooled to room temperature, and whole preparation process is carried out in protective atmosphere;
(6) be placed in alumina crucible by without surface remelting process with through the sample of Alloy by Laser Surface Remelting process, then put into high temperature resistance furnace and carry out static oxidization, all samples before oxidation test all by accurate measurement size;
(7), after oxidation test terminates, after utilizing scanning electron microscopic observation to be oxidized, the cross section of sample, compares the difference without surface remelting process and the antioxidant property through Alloy by Laser Surface Remelting processing sample.
2. a kind of method improving Nb-Si based multicomponent alloy high-temperature oxidation resistance according to claim 1, is characterized in that, Nb-Si based multicomponent alloy selected in step (1) is prepared by non-consumable vacuum arc melting and obtains.
3. a kind of method improving Nb-Si based multicomponent alloy high-temperature oxidation resistance according to claim 1, it is characterized in that, in step (3), before surface remelting, laser beam is utilized to carry out preheating to specimen surface, concrete pre-thermal parameter: laser power 250 ~ 400W, sweep velocity 1500 ~ 2000mm/s, sweep span 0.10 ~ 0.25mm, scanning times 5 ~ 10 times.
4. a kind of method improving Nb-Si based multicomponent alloy high-temperature oxidation resistance according to claim 1, it is characterized in that, in step (4), utilize high energy laser beam irradiated sample surface, alloy surface is melted, produce remelted layer, melting characteristic parameter: laser power 350 ~ 500W, sweep velocity 100 ~ 300mm/s, sweep span 0.05 ~ 0.15mm, scanning times 1 ~ 2 time.
5. a kind of method improving Nb-Si based multicomponent alloy high-temperature oxidation resistance according to claim 1, is characterized in that, described Nb-Si based multicomponent alloy composition counts Nb-16Si-24Ti-2Cr-2Al-2Hf with atomic percent.
6. a kind of method improving Nb-Si based multicomponent alloy high-temperature oxidation resistance according to claim 1, is characterized in that, described Nb-Si based multicomponent alloy composition counts Nb-18Si-24Ti-2Cr-2Al-2Hf with atomic percent.
7. a kind of method improving Nb-Si based multicomponent alloy high-temperature oxidation resistance according to claim 1, is characterized in that, described Nb-Si based multicomponent alloy composition counts Nb-20Si-24Ti-2Cr-2Al-2Hf with atomic percent.
8. a kind of method improving Nb-Si based multicomponent alloy high-temperature oxidation resistance according to claim 1, is characterized in that, described Nb-Si based multicomponent alloy composition counts Nb-22Si-24Ti-2Cr-2Al-2Hf with atomic percent.
9. a kind of method improving Nb-Si based multicomponent alloy high-temperature oxidation resistance according to claim 1, it is characterized in that, in step (6), utilize short time high temperature oxidation experiment to evaluate the oxidation-resistance of sample, oxidation experiment parameter is: temperature 1250 DEG C, insulation 2h.
10. according to the Alloy by Laser Surface Remelting Nb-Si based multicomponent alloy that any one method of claim 1-9 obtains, it is characterized in that, the surface remelting layer tissue that cool to room temperature obtains is by tiny Nb
sSsosoloid and Nb
5si
3strengthening phase form, phase size <1 μm, is evenly distributed, and density is high, and crackle content is few, and surface remelting layer and matrix alloy associativity better.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106521384A (en) * | 2016-11-03 | 2017-03-22 | 北京航空航天大学 | Method used for improving Nb-Si based alloy oxidation resistance via electron beam remelting |
| CN106756374A (en) * | 2016-12-20 | 2017-05-31 | 哈尔滨工业大学 | Supertherm and preparation method thereof |
| CN107513652A (en) * | 2017-09-05 | 2017-12-26 | 北京航空航天大学 | A kind of quick solidification Nb Si based multicomponent alloys |
| CN108044124A (en) * | 2017-11-14 | 2018-05-18 | 中国航发北京航空材料研究院 | The nearly eutectic Nb-Si-Mo alloy preparation methods of feature are aligned with lamellar structure |
| CN109443916A (en) * | 2018-09-04 | 2019-03-08 | 北京航空航天大学 | The research method of metal bath Free Surface process of setting information |
| CN112132182A (en) * | 2020-08-20 | 2020-12-25 | 上海大学 | Method for rapidly predicting resistivity of ternary gold alloy based on machine learning |
| CN114525462A (en) * | 2022-02-11 | 2022-05-24 | 上海交通大学 | Method for improving high-temperature oxidation resistance of alloy by remelting surface through ultrasonic field and laser |
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| CN103949639A (en) * | 2014-05-19 | 2014-07-30 | 北京航空航天大学 | Method for preparing Nb-Si based superhigh-temperature alloy by SLM (selective laser melting) technology |
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Patent Citations (2)
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106521384A (en) * | 2016-11-03 | 2017-03-22 | 北京航空航天大学 | Method used for improving Nb-Si based alloy oxidation resistance via electron beam remelting |
| CN106521384B (en) * | 2016-11-03 | 2018-03-16 | 北京航空航天大学 | A kind of method that Nb Si based alloy inoxidizability is improved using electron beam remelting technology |
| CN106756374A (en) * | 2016-12-20 | 2017-05-31 | 哈尔滨工业大学 | Supertherm and preparation method thereof |
| CN107513652A (en) * | 2017-09-05 | 2017-12-26 | 北京航空航天大学 | A kind of quick solidification Nb Si based multicomponent alloys |
| CN108044124A (en) * | 2017-11-14 | 2018-05-18 | 中国航发北京航空材料研究院 | The nearly eutectic Nb-Si-Mo alloy preparation methods of feature are aligned with lamellar structure |
| CN109443916A (en) * | 2018-09-04 | 2019-03-08 | 北京航空航天大学 | The research method of metal bath Free Surface process of setting information |
| CN109443916B (en) * | 2018-09-04 | 2020-11-17 | 北京航空航天大学 | Research method of solidification process information of free surface of metal melt |
| CN112132182A (en) * | 2020-08-20 | 2020-12-25 | 上海大学 | Method for rapidly predicting resistivity of ternary gold alloy based on machine learning |
| CN112132182B (en) * | 2020-08-20 | 2024-03-22 | 上海大学 | Method for rapidly predicting resistivity of ternary gold alloy based on machine learning |
| CN114525462A (en) * | 2022-02-11 | 2022-05-24 | 上海交通大学 | Method for improving high-temperature oxidation resistance of alloy by remelting surface through ultrasonic field and laser |
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