CN103949639B - The method that a kind of selective laser smelting technology prepares Nb-Si based ultra-high temperature alloy - Google Patents

The method that a kind of selective laser smelting technology prepares Nb-Si based ultra-high temperature alloy Download PDF

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CN103949639B
CN103949639B CN201410211026.0A CN201410211026A CN103949639B CN 103949639 B CN103949639 B CN 103949639B CN 201410211026 A CN201410211026 A CN 201410211026A CN 103949639 B CN103949639 B CN 103949639B
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selective laser
supertherm
powder
alloy
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CN103949639A (en
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张虎
孙少波
贾丽娜
李震
徐惠彬
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Beihang University
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Abstract

The invention belongs to high temperature alloy preparing technical field, particularly to a kind of selective laser smelting technology (Selective Laser Melting, SLM) method preparing NbSi supertherm, utilize selective laser melting unit, being arranged by rational technological parameter, directly completed the preparation of NbSi Alloy Forming part by cad model one step, the NbSi alloy consistency of preparation is high, defect is few, mainly by Nbss solid solution and Nb5Si3Hardening constituent forms, and phase size is tiny and is evenly distributed.This method prepares NbSi alloy without mould, it is to avoid interfacial reaction, reduces alloy contamination, reduces and is mingled with content, and stock utilization is high, can improve combination property and the production efficiency of NbSi alloy.

Description

The method that a kind of selective laser smelting technology prepares Nb-Si based ultra-high temperature alloy
Technical field
The invention belongs to high temperature alloy preparing technical field, utilize selective laser smelting technology to prepare particularly to one The method of NbSi supertherm.
Background technology
Along with High Performance Aeroengine, combustion gas turbine are sent out towards high flow capacity ratio, high thrust-weight ratio, high inlet temperature direction Exhibition, the operating temperature of the hot-end components such as turbo blade improves constantly, and turbine inlet temperature (TIT) is also constantly promoting.At present, jet is sent out The maximum operation (service) temperature of the third generation nickel-base high-temperature single crystal alloy used in motivation has reached 1100~1150 DEG C, close to being somebody's turn to do The 85% of alloy melting point, then the potentiality promoted are little, therefore in the urgent need to developing novel structural material.At present, infusibility silication Thing, because of the combination property of its excellence, becomes the focus direction of superhigh temperature structural material research field, and wherein Nb-Si based ultra-high temperature Alloy has high-melting-point (> 1750 DEG C), low-density (6.6-7.2g/cm3), good elevated temperature strength and certain fracture toughness, The advantage such as fatigue behaviour and machinability, one of new type high temperature structural metallic materials becoming great competitiveness.Nb-Si base alloy By NbSSSolid solution and intermetallic compound Nb5Si3Constitute, rely on the Nb of high tenacitySSSolid solution bears plastic deformation, improves Room-Temperature Fracture Toughness, relies on the most crisp silicide phase Nb5Si3Bear the mechanical load under high temperature, improve elevated temperature strength.
In recent years, NbSi supertherm research emphasis is in terms of alloy design and preparation technology.Alloying Design is main Be 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.The addition of alloying element can significantly improve its Room-Temperature Fracture Toughness, high temperature creep strength and high temperature antioxygen Coupling between the performances such as change ability.In terms of preparation technology, Nb-Si base alloy is high due to its fusing point, oxidizable, containing fragility Mutually and the contour active element of substantial amounts of Ti and Hf, preparation technology is very restricted, currently mainly have vacuum non-consumable/from Consumption electric arc melting, vacuum induction melting, directional solidification, powder metallurgy and model casting etc..The NbSi that vacuum arc melting obtains Alloy structure often exists component segregation phenomenon, thick primary phase, Nb easily occur3Si metastable phase and crackle etc., oxygen contains Amount and other impurity content are higher, are unfavorable for the direct application of high-temperature structural material.During powder metallurgy NbSi alloy, sintering and The stress that cooling produces is easily caused crackle and produces, thus affects the combination property of alloy, the sintering temperature shadow to alloy structure Ringing very big, sintering temperature is different, and the tissue composition of products therefrom is also different, and grain size is different, composition be likely to mutually difference (as Nb3The appearance of Si phase);Vacuum induction melting can keep the most even high-purity of alloying component, and shortcoming is that melt temperature is uneven, mistake Temperature is low, easily forms the defects such as poured short.Directional solidification can eliminate major part transverse grain boundaries, effectively controls the microcosmic of alloy Tissue and chemical composition, and obtain the foundry goods of low defect, it is increasingly becoming the main technique means preparing niobium silicon supertherm. But traditional directional solidification shortcoming mainly has: process of setting cooldown rate is low, causes alloy structure to be roughened and grows up, limiting The raising of alloy property, additionally, due to NbSi supertherm contains the element that under the high temperature such as Hf, Ti, chemism is the strongest, because of This is at high temperature very easy to and the crucible generation interfacial reaction contacted, and causes alloy contamination, and oxygen content increases, and foundry goods is mingled with increasing Adding, mechanical performance declines.Model casting Nb-Si base alloy, its shell temperature capability more than 2000 DEG C, but will be currently used for height The shell temperature capability of temperature structural material model casting is less than 1700 DEG C more, and at high temperature occurs anti-with Nb-Si base alloy Should, it is difficult to meet Nb-Si base alloy model casting forming requirements.
Moreover, above-mentioned several method is prepared NbSi alloy and is required to crucible or mould, is difficult to directly preparation and has spy Sizing and the alloy components of labyrinth (variable cross-section, inner chamber or cooling duct), generally require more machining and rear place Reason, technique is loaded down with trivial details, the low waste simultaneously easily causing alloy material of production efficiency.Therefore, exploitation one is prepared more efficiently The method of Nb-Si based ultra-high temperature alloy is the most vital.
Summary of the invention
The present invention prepares, for traditional method, the problem that NbSi based ultra-high temperature alloy exists just, it is provided that a kind of laser choosing The method that district's smelting technology (Selective Laser Melting, SLM) quickly prepares NbSi based ultra-high temperature alloy.
Selective laser fusing (SLM) technology is to be tied with rapid prototyping (rapid prototyping) technology by laser melting coating A kind of up-to-date advanced manufacturing technology altogether.SLM be capable of 3 D complex structural elements without mould, high performance Quickly preparation.Its process is mainly: utilizes computer to obtain the three-dimensional CAD physical model of parts, then utilizes delamination software Carry out hierarchy slicing in component height direction, and the three-D profile information of parts is converted into two-dimensional silhouette information, and generation is swept Retouch path.Laser beam, according to the scanning pattern specified successively melt deposition metal or alloy powder, is piled up and is formed 3D solid zero Part.Through material and process optimization, once-forming consistency can be higher than 95%, and shaped alloys can directly meet industrial requirement. SLM technology is applicable to difficult processing, high-performance refractory metal and the preparation of alloy.
The technical scheme that the present invention utilizes SLM technology to prepare NbSi supertherm is:
Using the pre-alloyed NbSi supertherm powder prepared of Powder In Argon Atomization, NbSi powder is spherical in shape or nearly ball Shape, diameter is between 10~60 μm.Followed by precinct laser fusion (selective laser melting, SLM) technique pair Nb-Si alloy powder carries out quick shaping to be prepared.Set rational laser forming parameter (laser power, laser beam flying speed, Sweep span and paving powder thickness), utilize high energy laser beam to make NbSi alloy powder melt.Additionally, in precinct laser fusion technique In, powder smelting/solidification is exceedingly fast, rate of cooling high (105~106K/s), therefore can prepare tiny, uniform, stable Rapidly solidified alloy tissue, thus obtain the NbSi supertherm part of excellent in mechanical performance.
The present invention utilizes the method that SLM technology prepares NbSi supertherm, and preparation process specifically includes 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 the height direction Hierarchy slicing sliding-model control, slice thickness uniformly (0.03~0.1mm), and comprises cross-sectional profiles information and the laser of part Machining path, by multilayer wall information and save as stl file, and is transferred to SLM selective laser melting systems;
(2) forming board is fixed on liftable workbench, after sealing device evacuation, is filled with high-purity argon gas (99.99%) carrying out atmosphere protection, powder feed system uniform spreading a layer thickness on substrate is the NbSi to be processed of 0.03~0.1mm Supertherm powder;
(3) laser beam is according to scanning pattern set in advance, is optionally scanned the powder on substrate, and powder melts Change and solidify, forming cladding layer;Concrete preparation parameter: laser power 350~500W, scanning speed 200~400mm/s, Sweep span 0.05~0.15mm;
(4), after completing a plane scan, substrate declines the distance of a thickness, and on first cladding layer again on uniform spreading A layer thickness is the NbSi alloy powder of 0.03~0.1mm;
(5) above-mentioned (3)-(4) step is repeated, until NbSi based ultra-high temperature alloy machines;
In the present invention, preparation NbSi supertherm uses Ti6Al4V forming board, and substrate thickness is 10mm;
The present invention use the method that powder is prepared in argon atomization and SLM technique combines prepare NbSi supertherm, The interaction of powder and laser beam is different from other traditional powder metallurgical technique process, and it melts/and solidification behavior is different from Traditional method.This technical scheme major advantage is:
(1) SLM technology utilizes laser beam layer by layer deposition NbSi supertherm powder, is directly completed by cad model one step The preparation of NbSi alloy.Preparation process, without preparing crucible, mould or powder jacket etc., reduces scale error;SLM technology is permissible Effectively avoid the interfacial reaction of high temperature alloy and crucible, mould etc., reduce alloy contamination, reduce and be mingled with content;SLM process has Argon gas atmosphere is protected, and the NbSi alloy of the condition of high temperature is had protected effect, is prevented effectively from the oxidation of alloy, carries heavy alloyed combining Close performance.
(2), during SLM technology prepares superhigh temperature NbSi alloy process, during powder smelting, liquid phase bath temperature is high, size very Little, setting time is extremely short, therefore rate of cooling high (105~106K/s), for height nonequilibrium freezing, setting time is extremely short, energy Effectively reduce the microsegregation of NbSi supertherm, and alloy consistency relatively prior powder metallurgy technique is higher, have thin Little, uniform, stable rapid solidification structure, thus obtain the NbSi supertherm part of excellent in mechanical performance;
(3) SLM is applicable to prepare the alloy component of the NbSi of various labyrinth, and especially internal have complicated abnormal shape knot Structure (cavity, cooling duct), the alloy component that traditional method cannot manufacture;NbSi alloying technology is simple and quick, eliminate in preparation Design with manufacture mold process, it is to avoid traditional machining and post processing, use manpower and material resources sparingly;The most undressed, unnecessary NbSi pre-alloyed powder can recycle and reuse, and stock utilization is high;
(4) utilize the NbSi supertherm consistency that SLM technology shapes high, alloy mainly by Nbss solid solution and Nb5Si3Hardening constituent forms, and is evenly distributed, and phase size the most tiny (less than 1 μm) reaches nanoscale, much smaller than traditional method Prepare phase size.The comprehensive mechanical property of NbSi alloy can improve in this tissue signature that SLM obtains.
Accompanying drawing illustrates:
Accompanying drawing 1 SLM technology shapes Nb-18Si-24Ti-2Cr-2Al-2Hf alloy XRD figure spectrum;
Accompanying drawing 2 SLM technology shapes Nb-18Si-24Ti-2Cr-2Al-2Hf alloy scanning electron microscopic picture;
Accompanying drawing 3 SLM technology shapes Nb-16Si-22Ti-4Cr-2Al-2Hf alloy XRD figure spectrum;
Accompanying drawing 4 SLM technology shapes Nb-16Si-22Ti-4Cr-2Al-2Hf alloy scanning electron microscopic picture.
Detailed description of the invention
Below in conjunction with example, the present invention is further elaborated, but the invention is not limited in specific embodiment.
Embodiment 1
SLM technology is utilized to prepare Nb-18Si-24Ti-2Cr-2Al-2Hf (at.%, atomic percent) supertherm: The SLM selective laser melting systems used specifically includes that Nd-YAG laser instrument, for shaping the computer system of control, powder feeding System and argon gas atmosphere protection device;
1. selecting the Nb-18Si-24Ti-2Cr-2Al-2Hf pre-alloying powder utilizing Powder In Argon Atomization to prepare, powder becomes Spherical or subsphaeroidal, diameter is between 10~60 μm;
2., according to alloy part shape to be processed, utilize computer to set up three-dimensional CAD model, and high at model with Slice Software Degree carries out hierarchy slicing sliding-model control on direction, and slice thickness uniformly (thickness is 0.05mm), and comprises part to be processed Cross-sectional profiles information and scanning machining path, by multilayer wall information and save as stl file, and be transferred to SLM laser In selective melting system;
3. powder is loaded in forming cavity, the Ti6Al4V forming board that thickness is 10mm is fixed on liftable work On platform;The forming cavity first evacuation sealed, then pours high-purity argon gas (99.99%) and protects.Powder feed system is utilized to exist On substrate, uniform spreading a layer thickness is the Nb-18Si-24Ti-2Cr-2Al-2Hf supertherm powder of 0.05mm;
4. laser beam is according to scanning pattern set in advance and preparation parameter, sweeps the powder preset on substrate Retouching, powder smelting also solidifies, and forms cladding layer;Concrete preparation parameter: laser power 400W, scanning speed 250mm/s, sweeps Retouch spacing 0.10mm;
5., after completing a plane scan, substrate declines the distance of a thickness, and on first cladding layer again on uniform spreading A layer thickness is the Nb-18Si-24Ti-2Cr-2Al-2Hf alloy powder of 0.05mm;
6. repeat above-mentioned (5), (6) step, until Nb-18Si-24Ti-2Cr-2Al-2Hf supertherm part processes Become, be then shut off system, take out when parts are cooled to room temperature;Whole preparation process is carried out in argon atmosphere;
By accompanying drawing 1 it can be seen that SLM shapes Nb-18Si-24Ti-2Cr-2Al-2Hf alloy structure mainly by NbSSSolid solution Body and Nb5Si3Two phase compositions.Light color is Nbss solid solution mutually, and dark color is Nb mutually5Si3Phase.
By accompanying drawing 2 it can be seen that SLM shapes Nb-18Si-24Ti-2Cr-2Al-2Hf alloy consistency height, there is no crackle Produce.Nbss phase and Nb5Si3The size of phase the most tiny (< 1 μm), reaches nanometer phase degree, and biphase is evenly distributed, and presents Significantly rapid solidification structure feature, can improve the combination property of NbSi supertherm.
Embodiment 2
SLM technology is utilized to prepare Nb-16Si-22Ti-4Cr-2Al-2Hf (at.%, atomic percent) supertherm: The SLM selective laser melting systems used specifically includes that Nd-YAG laser instrument, for shaping the computer system of control, powder feeding System and argon gas atmosphere protection device;
1. selecting the Nb-16Si-22Ti-4Cr-2Al-2Hf pre-alloying powder utilizing Powder In Argon Atomization to prepare, powder becomes Spherical or subsphaeroidal, diameter is between 10~60 μm;
2., according to alloy part shape to be processed, utilize computer to set up three-dimensional CAD model, and high at model with Slice Software Degree carries out hierarchy slicing sliding-model control on direction, and slice thickness uniformly (thickness is 0.08mm), and comprises part to be processed Cross-sectional profiles information and scanning machining path, by multilayer wall information and save as stl file, and be transferred to SLM laser In selective melting system;
3. powder is loaded in forming cavity, the Ti6Al4V forming board that thickness is 10mm is fixed on liftable work On platform, the forming cavity of sealing first evacuation, then pours high-purity argon gas (99.99%) and protects.Powder feed system is utilized to exist On substrate, uniform spreading a layer thickness is the Nb-16Si-22Ti-4Cr-2Al-2Hf supertherm powder of 0.08mm;
4. laser beam is according to scanning pattern set in advance and preparation parameter, sweeps the powder preset on substrate Retouching, powder smelting also solidifies, and forms cladding layer;Concrete preparation parameter: laser power 400W, scanning speed 300mm/s, sweeps Retouch spacing 0.06mm;
5., after completing a plane scan, substrate declines the distance of a thickness, and on first cladding layer again on uniform spreading A layer thickness is the Nb-16Si-22Ti-4Cr-2Al-2Hf alloy powder of 0.08mm;
6. repeat above-mentioned (5), (6) step, until Nb-16Si-22Ti-4Cr-2Al-2Hf supertherm part processes Become, be then shut off system, take out when parts are cooled to room temperature;Whole preparation process is carried out in argon atmosphere;
By accompanying drawing 3 and accompanying drawing 4 it can be seen that SLM shapes Nb-16Si-22Ti-4Cr-2Al-2Hf alloy consistency height, deposit In a small amount of pore (size < 1 μm), there is no the defect such as space and fire check.Shaped alloys is by nanoscale NbssPhase and Nb5Si3Phase (light color is Nbss solid solution to composition mutually, and dark color is Nb mutually5Si3Phase), size the most tiny (< 1 μm), and biphase be evenly distributed, Present obvious rapid solidification structure feature, the combination property of NbSi supertherm can be improved.
The foregoing is only the preferred embodiments of the present invention, not thereby limit the scope of the claims of the present invention, every utilization Equivalent structure or equivalence flow process that description of the invention content is made convert, or are directly or indirectly used in other relevant technology Field, is the most in like manner included in the scope of patent protection of the present invention.

Claims (8)

1. one kind utilizes the method that selective laser smelting technology prepares NbSi supertherm, it is characterised in that preparation process bag Include following steps:
(1). according to NbSi supertherm drip molding shape to be processed, set up drip molding cad model, then in short transverse On to its carry out hierarchy slicing process to be divided into section in uniform thickness, section comprise Alloy Forming part cross-sectional profiles letter Breath and machining path, and section file is imported in the melting unit of selective laser, described slice thickness is 0.03~0.1mm;
(2). in the melting unit of selective laser, Ti6Al4V forming board is fixed on liftable workbench, sealing device Being filled with protective gas after evacuation and carry out atmosphere protection, powder feed system uniform spreading one layer NbSi superhigh temperature to be processed on substrate is closed Bronze end, powder thickness is equal with slice thickness in step (1), and selected NbSi supertherm powder is by Powder In Argon Atomization It is prepared, spherical in shape or subsphaeroidal, diameter 10~60 μm;
(3). the NbSi supertherm powder on substrate, according to scanning pattern set in advance, is optionally carried out by laser beam Scanning, powder smelting also solidifies, and forms cladding layer;
(4). completing in step (3) after a plane scan, substrate declines the distance of a thickness, and is formed in step (3) Cladding layer on uniform spreading last layer NbSi supertherm powder again;
(5). repeat the above steps (3)-(4), until NbSi supertherm part machines;It is then shut off system, treats parts It is cooled to during room temperature take out;Whole preparation process is carried out in protective atmosphere.
A kind of method utilizing selective laser smelting technology to prepare NbSi supertherm the most according to claim 1, its Being characterised by, the protective gas described in step (2) is high-purity argon gas, and purity is 99.99%.
A kind of method utilizing selective laser smelting technology to prepare NbSi supertherm the most according to claim 1, its It is characterised by, in step (3), forms cladding layer;Concrete preparation parameter: laser power 350~500W, scanning speed 200 ~400mm/s, sweep span 0.05~0.15mm.
A kind of method utilizing selective laser smelting technology to prepare NbSi supertherm the most according to claim 1, its Being characterised by, in step (4), then the NbSi supertherm powder thickness uniformly laid is 0.03~0.1mm.
A kind of method utilizing selective laser smelting technology to prepare NbSi supertherm the most according to claim 1, its Being characterised by, described Ti6Al4V forming board thickness is 10mm.
A kind of method utilizing selective laser smelting technology to prepare NbSi supertherm the most according to claim 1, its Being characterised by, described NbSi supertherm powdered ingredients is calculated as Nb-18Si-24Ti-2Cr-2Al-with atomic percent 2Hf。
A kind of method utilizing selective laser smelting technology to prepare NbSi supertherm the most according to claim 1, its Being characterised by, described NbSi supertherm powdered ingredients is calculated as Nb-16Si-22Ti-4Cr-2Al-with atomic percent 2Hf。
8. prepare the side of NbSi supertherm according to the selective laser smelting technology that utilizes described in any one of claim 1-7 Method, it is characterised in that it is high to be cooled to the NbSi supertherm consistency that room temperature obtains, Main Tissues by Nbss solid solution and Nb5Si3 hardening constituent forms, phase size < 1 μm and being evenly distributed.
CN201410211026.0A 2014-05-19 2014-05-19 The method that a kind of selective laser smelting technology prepares Nb-Si based ultra-high temperature alloy Expired - Fee Related CN103949639B (en)

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