CN103949639A - Method for preparing Nb-Si based superhigh-temperature alloy by SLM (selective laser melting) technology - Google Patents
Method for preparing Nb-Si based superhigh-temperature alloy by SLM (selective laser melting) technology Download PDFInfo
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Abstract
The invention belongs to the technical field of preparation of high-temperature alloy, and particularly relates to a method for preparing NbSi superhigh-temperature alloy by SLM (selective laser melting) technology. SLM equipment is utilized, the process parameters are reasonably set, and an NbSi alloy forming piece is directly prepared by a CAD (computer-aided design) model in a one-step way. The prepared NbSi alloy has the characteristics of high density, fewer defects, fine phase size and uniform distribution, and mainly consists of Nbss solid solution and Nb5Si3 strengthening phase. The NbSi alloy prepared by the method has the advantages that a die is not needed, the interface reaction is avoided, the alloy pollution is reduced, the content of impurities is reduced, the utilization rate of material is high, and the comprehensive yield and production efficiency of the NbSi alloy can be improved.
Description
Technical field
The invention belongs to high temperature alloy preparing technical field, particularly a kind of method of utilizing laser selective melting technology to prepare NbSi supertherm.
Background technology
Along with High Performance Aeroengine, combustion gas turbine are towards high flow capacity ratio, high thrust-weight ratio, high inlet temperature future development, the operating temperature of the hot-end components such as turbo blade improves constantly, and turbine inlet temperature (TIT) is also in continuous lifting.At present, the maximum operation (service) temperature of the third generation nickel-base high-temperature single crystal alloy using in jet engine has reached 1100～1150 DEG C, approaches 85% of this alloy melting point, then the potentiality that promote are little, therefore in the urgent need to the structural material of development of new.At present, refractory silicide is because of its excellent combination property, become the focus direction of superhigh temperature structural material research field, and wherein Nb-Si based ultra-high temperature alloy have high-melting-point (>1750 DEG C), low-density (6.6-7.2g/cm
3), the advantages such as good elevated temperature strength and certain fracture toughness, fatigue behaviour and machinability, become one of new type high temperature structural metallic materials having competitiveness.Nb-Si base alloy is by Nb
sSsolid solution and intermetallic compound Nb
5si
3form, rely on the Nb of high tenacity
sSsolid solution bears plastic deformation, improves Room-Temperature Fracture Toughness, relies on hard crisp silicide phase Nb
5si
3bear the mechanical load under high temperature, improve elevated temperature strength.
In recent years, NbSi supertherm research emphasis is aspect alloy designs and preparation technology.Alloying Design is mainly to add Ti, Al, Hf, Cr, platinum metal (Re, Ru etc.), Wo, Ta, Mo, rare earth element (Ho, Dy, Y), B, C, Ge, Zr, V, Sn, N, Fe, In.Adding of alloying element can significantly improve the coupling between the performances such as its Room-Temperature Fracture Toughness, high temperature creep strength and high-temperature oxidation resistance.Aspect preparation technology, Nb-Si base alloy is because its fusing point is high, oxidizable, contain fragility phase and a large amount of Ti and contour active elements of Hf, preparation technology is very restricted, and mainly contains at present vacuum non-consumable/consumable arc-melting, vacuum induction melting, directional solidification, powder metallurgy and model casting etc.In the NbSi alloy structure that vacuum arc melting obtains, often there is component segregation phenomenon, easily occur thick primary phase, Nb
3si metastable phase and crackle etc., oxygen content and other impurity content are higher, are unfavorable for the direct application of high-temperature structural material.When powder metallurgy NbSi alloy, easily cause crackle to produce at the stress of sintering and cooling generation, thereby affect the combination property of alloy, the impact of sintering temperature alloy tissue is very large, sintering temperature difference, the tissue composition of products therefrom is also different, grain size difference, and composition mutually also may be different (as Nb
3the appearance of Si phase); Vacuum induction melting can keep all even high-purities of alloying component, and shortcoming is that melt temperature is inhomogeneous, and the degree of superheat is low, easily forms the defects such as poured short.Directional solidification can be eliminated most of transverse grain boundaries, effectively controls microstructure and the chemical composition of alloy, and obtains the foundry goods of low defect, becomes just gradually the main technique means of preparing niobium silicon supertherm.But traditional directional solidification shortcoming mainly contains: process of setting cooldown rate is low, cause alloy structure alligatoring and grow up, limit the raising of alloy property, in addition owing to containing the very strong element of chemism under the high temperature such as Hf, Ti in NbSi supertherm, therefore be at high temperature very easy to and the crucible generation interfacial reaction contacting, cause alloy to pollute, oxygen content increases, foundry goods is mingled with increase, and mechanical performance declines.Model casting Nb-Si base alloy, its shell holds warm ability will exceed 2000 DEG C, be no more than 1700 DEG C but hold warm ability for the shell of high-temperature structural material model casting at present more, and at high temperature react with Nb-Si base alloy, be difficult to meet Nb-Si base alloy model casting forming requirements.
Moreover, above-mentioned several method is prepared NbSi alloy and is all needed crucible or mould, be difficult to the alloy components that directly preparation has specific dimensions and labyrinth (variable cross-section, inner chamber or cooling duct), often need more machined and post processing, technique is loaded down with trivial details, and the low while of production efficiency is easily caused the waste of alloy material.Therefore, develop a kind of method of preparing more efficiently Nb-Si based ultra-high temperature alloy vital beyond doubt.
Summary of the invention
The present invention prepares for conventional method the problem that NbSi based ultra-high temperature alloy exists just, provides a kind of laser selective melting technology (Selective Laser Melting, SLM) to prepare fast the method for NbSi based ultra-high temperature alloy.
Laser selective melting (SLM) technology is a kind of up-to-date advanced manufacturing technology that laser melting coating and rapid prototyping (rapid prototyping) technology are combined.SLM can realize 3 D complex structure parts without mould, high performance quick preparation.Its process is mainly: utilize computer to obtain the three-dimensional CAD physical model of parts, then utilize delamination software to carry out hierarchy slicing in component height direction, and the three-D profile information of parts is converted into two-dimensional silhouette information, and generate scanning pattern.Laser beam, according to the successively melt deposition metal or alloy powder of scanning pattern of specifying, is piled up and is formed Three-dimensional Entity Components.Through material and process optimization, the density of once-forming can be higher than 95%, and shaping alloy can directly meet industrial requirement.SLM technology is applicable to the preparation of difficult processing, high-performance refractory metal and alloy.
The technical scheme that the present invention utilizes SLM technology to prepare NbSi supertherm is:
The pre-alloyed NbSi supertherm powder that adopts Powder In Argon Atomization to prepare, NbSi powder is spherical in shape or subsphaeroidal, and diameter is between 10～60 μ m.Utilize subsequently precinct laser fusion (selective laser melting, SLM) technique to carry out Quick-forming preparation to Nb-Si alloy powder.Set rational laser forming parameter (laser power, laser beam flying speed, sweep span and paving powder thickness), utilize high energy laser beam to make the fusing of NbSi alloy powder.In addition,, in precinct laser fusion technique, powder smelting/solidify is exceedingly fast, cooling velocity high (10
5～10
6k/s), therefore can prepare tiny, even, stable rapidly solidified alloy tissue, thereby obtain the NbSi supertherm part of mechanical property excellence.
The present invention utilizes SLM technology to prepare the method for NbSi supertherm, and preparation process specifically comprises the following steps:
(1) utilize computer design to go out the three-dimensional CAD model of part, and with Slice Software, model is carried out in short transverse the processing of hierarchy slicing discretization, slice thickness is (0.03～0.1mm) evenly, and the cross-sectional profiles information that comprises part and Laser Processing path, by multilayer slice information and save as stl file, and be transferred to SLM laser selective melting system;
(2) forming board is fixed on liftable workbench, after sealing device vacuumizes, be filled with high-purity argon gas (99.99%) and carry out atmosphere protection, the powder feed system NbSi supertherm powder to be processed that uniform spreading a layer thickness is 0.03～0.1mm on substrate;
(3) laser beam, according to predefined scanning pattern, optionally scans the powder on substrate, and powder smelting also solidifies, and forms cladding layer; Concrete preparation parameter: laser power 350～500W, sweep speed 200～400mm/s, sweep span 0.05～0.15mm;
(4) complete after a plane scan the decline distance of a bed thickness of substrate, and the NbSi alloy powder that formerly uniform spreading last layer thickness is 0.03～0.1mm again on cladding layer;
(5) repeat above-mentioned (3)-(4) step, until NbSi based ultra-high temperature alloy machines;
In the present invention, preparation NbSi supertherm adopts Ti6Al4V forming board, and substrate thickness is 10mm;
In the present invention, adopt argon gas atomization to prepare the method that powder and SLM technique combines and prepare NbSi supertherm, the interaction of powder and laser beam is different from other traditional powder metallurgical technique process, and it melts/solidify behavior and is different from conventional method.This technical scheme major advantage is:
(1) SLM technology is utilized laser beam layer by layer deposition NbSi supertherm powder, is directly completed the preparation of NbSi alloy by cad model one step.Preparation process is without preparing crucible, mould or powder jacket etc., error reduced in size; SLM technology can effectively be avoided the interfacial reaction of high temperature alloy and crucible, mould etc., reduces alloy and pollutes, and reduces and is mingled with content; SLM process has argon gas atmosphere protection, and the NbSi alloy of the condition of high temperature is had to protection effect, effectively avoids the oxidation of alloy, puies forward heavy alloyed combination property.
(2) SLM technology is prepared in superhigh temperature NbSi alloy process, and when powder smelting, liquid phase bath temperature is high, small-sized, setting time is extremely short, therefore cooling velocity high (10
5～10
6k/s), for height nonequilibrium freezing, setting time is extremely short, can effectively reduce the microsegregation of NbSi supertherm, and alloy density is higher compared with prior powder metallurgy technique, there is tiny, even, stable rapid solidification tissue, thereby obtain the NbSi supertherm part of mechanical property excellence;
(3) SLM is applicable to the alloy component of the NbSi for preparing various labyrinths, and especially inside has complicated abnormal shape structure (cavity, cooling duct), the alloy component that conventional method cannot be manufactured; Preparation NbSi alloying technology is simple and quick, removed design and mfg. moulding die process from, avoided traditional machined and post processing, uses manpower and material resources sparingly; Undressed, unnecessary NbSi pre-alloyed powder can recycle and reuse simultaneously, and stock utilization is high;
(4) the NbSi supertherm density of utilizing SLM technology to be shaped is high, and alloy is mainly by Nbss solid solution and Nb
5si
3hardening constituent composition, is evenly distributed, and phase size is extremely tiny (to be less than 1 μ m), to reach nanoscale, prepare phase size much smaller than conventional method.The comprehensive mechanical property of NbSi alloy can improve in this tissue signature that SLM obtains.
Brief description of the drawings:
Accompanying drawing 1SLM technology shaping Nb-18Si-24Ti-2Cr-2Al-2Hf alloy XRD collection of illustrative plates;
Accompanying drawing 2SLM technology shaping Nb-18Si-24Ti-2Cr-2Al-2Hf alloy ESEM picture;
Accompanying drawing 3SLM technology shaping Nb-16Si-22Ti-4Cr-2Al-2Hf alloy XRD collection of illustrative plates;
Accompanying drawing 4SLM technology shaping Nb-16Si-22Ti-4Cr-2Al-2Hf alloy ESEM picture.
Detailed description of the invention
Below in conjunction with example, the present invention is further elaborated, but the present invention is not limited to specific embodiment.
Embodiment 1
Utilize SLM technology to prepare Nb-18Si-24Ti-2Cr-2Al-2Hf (at.%, atomic percent) supertherm: the SLM laser selective melting system of use mainly comprises: Nd-YAG laser instrument, for be shaped control computer system, powder feed system and argon gas atmosphere protective device;
1. select the Nb-18Si-24Ti-2Cr-2Al-2Hf pre-alloying powder that utilizes Powder In Argon Atomization to prepare, powder globulate or subsphaeroidal, diameter is between 10～60 μ m;
2. according to alloy part shape to be processed, utilize computer to set up three-dimensional CAD model, and in model short transverse, carry out the processing of hierarchy slicing discretization with Slice Software, slice thickness is (thickness is 0.05mm) evenly, and the cross-sectional profiles information that comprises part to be processed and scanning machining path, by multilayer slice information and save as stl file, and be transferred in SLM laser selective melting system;
3. powder is packed in forming cavity, the Ti6Al4V forming board that is 10mm by thickness is fixed on liftable workbench; First the forming cavity of sealing vacuumizes, and then pours high-purity argon gas (99.99%) and protects.Utilize the powder feed system Nb-18Si-24Ti-2Cr-2Al-2Hf supertherm powder that uniform spreading a layer thickness is 0.05mm on substrate;
4. laser beam, according to predefined scanning pattern and preparation parameter, scans the powder preseting on substrate, and powder smelting also solidifies, and forms cladding layer; Concrete preparation parameter: laser power 400W, sweep speed 250mm/s, sweep span 0.10mm;
5. complete after a plane scan the decline distance of a bed thickness of substrate, and the Nb-18Si-24Ti-2Cr-2Al-2Hf alloy powder that formerly uniform spreading last layer thickness is 0.05mm again on cladding layer;
6. repeat above-mentioned (5), (6) step, until Nb-18Si-24Ti-2Cr-2Al-2Hf supertherm part machines, then shutdown system is taken out in the time that parts are cooled to room temperature; Whole preparation process is carried out in argon shield atmosphere;
Can be found out by accompanying drawing 1, SLM shaping Nb-18Si-24Ti-2Cr-2Al-2Hf alloy structure is mainly by Nb
sSsolid solution and Nb
5si
3two phase compositions.Light color is Nbss solid solution mutually, and dark color is Nb mutually
5si
3phase.
Can be found out by accompanying drawing 2, SLM shaping Nb-18Si-24Ti-2Cr-2Al-2Hf alloy density is high, does not have crackle to produce.Nbss phase and Nb
5si
3the size of phase is extremely tiny, and (<1 μ m), reaches nanophase degree, and two-phase is evenly distributed, and presents obvious rapid solidification tissue signature, can improve the combination property of NbSi supertherm.
Embodiment 2
Utilize SLM technology to prepare Nb-16Si-22Ti-4Cr-2Al-2Hf (at.%, atomic percent) supertherm: the SLM laser selective melting system of use mainly comprises: Nd-YAG laser instrument, for be shaped control computer system, powder feed system and argon gas atmosphere protective device;
1. select the Nb-16Si-22Ti-4Cr-2Al-2Hf pre-alloying powder that utilizes Powder In Argon Atomization to prepare, powder globulate or subsphaeroidal, diameter is between 10～60 μ m;
2. according to alloy part shape to be processed, utilize computer to set up three-dimensional CAD model, and in model short transverse, carry out the processing of hierarchy slicing discretization with Slice Software, slice thickness is (thickness is 0.08mm) evenly, and the cross-sectional profiles information that comprises part to be processed and scanning machining path, by multilayer slice information and save as stl file, and be transferred in SLM laser selective melting system;
3. powder is packed in forming cavity, the Ti6Al4V forming board that is 10mm by thickness is fixed on liftable workbench, and first the forming cavity of sealing vacuumizes, and then pours high-purity argon gas (99.99%) and protects.Utilize the powder feed system Nb-16Si-22Ti-4Cr-2Al-2Hf supertherm powder that uniform spreading a layer thickness is 0.08mm on substrate;
4. laser beam, according to predefined scanning pattern and preparation parameter, scans the powder preseting on substrate, and powder smelting also solidifies, and forms cladding layer; Concrete preparation parameter: laser power 400W, sweep speed 300mm/s, sweep span 0.06mm;
5. complete after a plane scan the decline distance of a bed thickness of substrate, and the Nb-16Si-22Ti-4Cr-2Al-2Hf alloy powder that formerly uniform spreading last layer thickness is 0.08mm again on cladding layer;
6. repeat above-mentioned (5), (6) step, until Nb-16Si-22Ti-4Cr-2Al-2Hf supertherm part machines, then shutdown system is taken out in the time that parts are cooled to room temperature; Whole preparation process is carried out in argon shield atmosphere;
Can be found out by accompanying drawing 3 and accompanying drawing 4, SLM shaping Nb-16Si-22Ti-4Cr-2Al-2Hf alloy density is high, and (size <1 μ m), does not have the defect such as space and fire check a small amount of pore.Shaping alloy is by nanoscale Nb
ssphase and Nb
5si
3(light color is Nbss solid solution mutually, and dark color is Nb mutually in phase composition
5si
3phase), size is extremely tiny, and (<1 μ m), and two-phase is evenly distributed, and presents obvious rapid solidification tissue signature, can improve the combination property of NbSi supertherm.
The foregoing is only the preferred embodiments of the present invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes description of the present invention to do; 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 (12)
1. utilize laser selective melting technology to prepare a method for NbSi supertherm, it is characterized in that, preparation process comprises the following steps:
(1). according to NbSi Alloy Forming part shape to be processed, set up drip molding cad model, then in short transverse, it is carried out to hierarchy slicing processing to be divided into the section of even thickness, cross-sectional profiles information and machining path that section comprises Alloy Forming part, and the file of cutting into slices imports in laser selective melting equipment;
(2). in laser selective melting equipment, forming board is fixed on liftable workbench, after sealing device vacuumizes, be filled with protective gas and carry out atmosphere protection, powder feed system is uniform spreading one deck NbSi supertherm to be processed powder on substrate, and powder thickness equates with slice thickness in step (1);
(3). laser beam, according to predefined scanning pattern, optionally scans the powder on substrate, and powder smelting also solidifies, and forms cladding layer;
(4). in completing steps (3) after a plane scan, the decline distance of a bed thickness of substrate, and uniform spreading last layer NbSi alloy powder again on the cladding layer of formation in step (3);
(5). repeat above-mentioned steps (3)-(4), until NbSi alloy machines; Then shutdown system is taken out in the time that parts are cooled to room temperature; Whole preparation process is carried out in protective atmosphere.
2. a kind of method of utilizing laser selective melting technology to prepare NbSi supertherm according to claim 1, is characterized in that, the slice thickness described in step (1) is 0.03～0.1mm.
3. a kind of method of utilizing laser selective melting technology to prepare NbSi supertherm according to claim 1, it is characterized in that, NbSi alloy powder selected in step (2) is prepared by Powder In Argon Atomization and obtains, spherical in shape or subsphaeroidal, diameter 10～60 μ m.
4. a kind of method of utilizing laser selective melting technology to prepare NbSi supertherm according to claim 1, is characterized in that, the protective gas described in step (2) is high-purity argon gas, and purity is 99.99%.
5. a kind of method of utilizing laser selective melting technology to prepare NbSi supertherm according to claim 1; it is characterized in that; in step (2), the NbSi alloy powder thickness of evenly laying on substrate is 0.03～0.1mm, and described protective atmosphere is argon gas atmosphere.
6. a kind of method of utilizing laser selective melting technology to prepare NbSi supertherm according to claim 1, is characterized in that, in step (3), forms cladding layer; Concrete preparation parameter: laser power 350～500W, sweep speed 200～400mm/s, sweep span 0.05～0.15mm;
7. a kind of method of utilizing laser selective melting technology to prepare NbSi supertherm according to claim 1, is characterized in that, in step (4), then the NbSi alloy powder thickness of evenly laying is 0.03～0.1mm.
8. a kind of method of utilizing laser selective melting technology to prepare NbSi supertherm according to claim 1, is characterized in that, described forming board adopts Ti6Al4V forming board.
9. a kind of method of utilizing laser selective melting technology to prepare NbSi supertherm according to claim 8, is characterized in that, described Ti6Al4V forming board thickness is 10mm.
10. a kind of method of utilizing laser selective melting technology to prepare NbSi supertherm according to claim 1, is characterized in that, described NbSi alloy powder composition is counted Nb-18Si-24Ti-2Cr-2Al-2Hf with atomic percent.
11. a kind of methods of utilizing laser selective melting technology to prepare NbSi supertherm according to claim 1, is characterized in that, described NbSi alloy powder composition is counted Nb-16Si-22Ti-4Cr-2Al-2Hf with atomic percent.
12. according to the prepared NbSi supertherm drip molding of any method of claim 1-12, it is characterized in that, the NbSi base alloy density that cool to room temperature obtains is high, and Main Tissues is by Nbss solid solution and Nb
5si
3hardening constituent composition, phase size <1 μ m and being evenly distributed.
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