CN107876763A - A kind of Nb Si alloy preparation methods with oriented freezing organization feature - Google Patents

A kind of Nb Si alloy preparation methods with oriented freezing organization feature Download PDF

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CN107876763A
CN107876763A CN201711127782.5A CN201711127782A CN107876763A CN 107876763 A CN107876763 A CN 107876763A CN 201711127782 A CN201711127782 A CN 201711127782A CN 107876763 A CN107876763 A CN 107876763A
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CN107876763B (en
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刘伟
熊华平
陈冰清
李能
黄帅
秦仁耀
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AECC Beijing Institute of Aeronautical Materials
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30Process control
    • B22F10/36Process control of energy beam parameters
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20Direct sintering or melting
    • B22F10/25Direct deposition of metal particles, e.g. direct metal deposition [DMD] or laser engineered net shaping [LENS]
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30Process control
    • B22F10/32Process control of the atmosphere, e.g. composition or pressure in a building chamber
    • B22F10/322Process control of the atmosphere, e.g. composition or pressure in a building chamber of the gas flow, e.g. rate or direction
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30Process control
    • B22F10/36Process control of energy beam parameters
    • B22F10/366Scanning parameters, e.g. hatch distance or scanning strategy
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00Processes of additive manufacturing
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/045Alloys based on refractory metals
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C27/00Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/02Alloys based on vanadium, niobium, or tantalum
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency

Abstract

The invention belongs to the preparing technical field of high-temperature structural material, more particularly to a kind of powder feeding formula Laser Rapid Prototyping Technique, more particularly to a kind of Nb Si alloy preparation methods with oriented freezing organization feature.The present invention prepares the Nb Si bianry alloys with oriented freezing organization feature using binary channels powder feeding formula Laser Rapid Prototyping Technique, and using commercially available pure element powder as raw material, without especially preparing spherical powder or pre-alloying powder, raw material set-up procedure is simple.Using binary channels powder-feeding method, Nb powder can be effectively avoided to mix non-uniform phenomenon caused by density difference with Si powder, and then from being had an impact to alloying component.In addition Nb powder and Si the powder reaction in-situ under laser action, produce in powder reaction in-situ effect, can further refining alloy microscopic structure.Alloy is by Nb solid solution phases and Nb3The phase composition of Si phases two, Nb solid solution phases and Nb is presented parallel to the microscopic structure in shaping direction3Si phases, which orient, is alternately arranged feature, and phase size is only 1/10 or so of Nb Si bianry alloys prepared by traditional directional solidification processes.

Description

A kind of Nb-Si alloy preparation methods with oriented freezing organization feature
Technical field
The invention belongs to the preparing technical field of high-temperature structural material, more particularly to a kind of powder feeding formula laser fast forming skill Art, more particularly to a kind of Nb-Si alloy preparation methods with oriented freezing organization feature.
Background technology
Nb-Si alloys are one of most potential candidates of following high-performance gas turbogenerator material, are expected to take the lead in Applied to some high temperature fixed components and high temperature rotatable parts in advanced aero gas turbine engine.
Being presently used for preparing the directional solidification processes of Nb-Si based ultra-high temperature alloys includes:Czochralski directional solidifications (C-DS), electron beam directional solidification (EBDS), light suspension directional solidification (OFZ) and global orientation solidification (IDS).
C-DS prepares material and uses czochralski method, and during alloy is prepared, melt is constantly reduced, and this causes the life of material Long speed is difficult to accurately control, therefore does not have to this method substantially at present and prepare Nb-Si based ultra-high temperature alloys.
During EBDS prepares material, the stabilization of its melt is maintained by the gravity and surface tension of itself, because And the specimen shape prepared is simple, size is smaller, high energy consumption;The generation of electron beam needs high vacuum, then high saturated vapour pressure Element highly volatile, cause composition not accurate, these all limit its application in terms of Nb-Si based ultra-high temperature alloys.
OFZ turns into the master for preparing Nb-Si based ultra-high temperature alloys because the requirement ratio without crucible pollution and to vacuum is relatively low Want method, but OFZ has highly energy-consuming, the specimen size of preparation is small, it is in irregular shape the shortcomings of, prepare Nb-Si bases with the method Supertherm has the trend gradually substituted by new directional solidification processes.
It is that the alloy mother metal of preparation is once completely melt in special ceramic crucible that IDS, which prepares cardinal principle, insulation A period of time makes alloy melt composition uniform, then with certain speed pull crucible, allows crucible and melt to enter liquid together In metal or other cooling mediums, so as to realize the oriented growth of material, but high activity Nb-Si alloy melts are by ceramic crucible Constraint, therefore the impurity such as oxygen can be brought into unavoidably.
In addition, Nb-Si alloy structures prepared by above-mentioned several directional freeze methods are thicker, mechanical property is difficult to ensure that.
The content of the invention
The present invention is to overcome above mentioned problem, there is provided one kind is fusing thermal source using high energy laser beam, and preparation has tiny The method of the Nb-Si bianry alloys of oriented freezing organization feature.
The present invention technical solution be,
Using pure Nb powder and pure Si powder as raw material, prepare to have using binary channels powder feeding formula Laser Rapid Prototyping Technique and determine To the Nb-Si alloys of Peculiarities of Solidification Structure, alloy is by Nb based solid solutions phase and Nb3Nb is presented in the phase composition of Si phases two, microscopic structure Solid solution phase and Nb3Si phases, which orient, is alternately arranged feature, and preparation process comprises the following steps:
(1) commercially available pure Nb powder and pure Si powder are sieved by metallic screen respectively, obtains even-grained pure Nb powder and pure Si Powder;
(2) the pure Nb and pure Si powder obtained step (1) be respectively placed in two of Stereolithography it is independent In powder feeder, using high-purity argon gas as load powder air-flow and protection gas;
(3) according to the Nb-Si binary alloys of required preparation, the powder feeding rate of pure Nb powder and pure Si powder is adjusted;
(4) laser and powder are coaxially sent out, laser and powder synchronizing moving, and only scan a road in one direction Secondary, in the presence of laser, Nb, Si powder melts on forming board forms molten bath, and as powder and laser travel forward, Molten bath solidifies, and obtains one layer of sedimentary;
(5) after layer surface temperature to be deposited is reduced to less than 100 DEG C, next sedimentary preparation is carried out;
(6) coaxial head of powder and laser rises a deposit thickness, then the sedimentary obtained using step (4) as base Body, repeat step (4) obtain another sedimentary;
(7) repeat step (5) and step (6), completed until prepared by the Nb-Si alloys of required height, treat that alloy temperature drops Taken out after to room temperature, obtain the Nb-Si alloys with oriented freezing organization feature.
The pure Nb powder that screening obtains in step (1), the average grain diameter of pure Si powder is 50~100 μm.
Powder air-flow velocity is carried in step (2):5~10L/min, protection air-flow speed:10~30L/min.
Total powder feeding rate of pure Nb powder and pure Si powder is 5~20g/min in step (3).
Forming board is the DZ125 alloys of directional solidification state in step (4), alloy directionally solidified to be oriented parallel to powder feeding formula Laser fast forming direction.
Laser power is set in step (4):1000~3000W, laser are in out-of-focus appearance, defocus distance:0~20mm, Laser scan rate:400~800mm/min.
The present invention has the advantage that and beneficial effect
The present invention prepares the Nb-Si with oriented freezing organization feature using binary channels powder feeding formula Laser Rapid Prototyping Technique Bianry alloy, using commercially available pure element powder as raw material, without especially preparing spherical powder or pre-alloying powder, raw material prepare Process is simple.Using binary channels powder-feeding method, Nb powder and Si powder can be effectively avoided to be mixed caused by density difference uneven Phenomenon, and then alloying component is had an impact.In addition Nb powder and Si the powder reaction in-situ under laser action, produce in situ in powder Response effect, can further refining alloy microscopic structure.Alloy is by Nb solid solution phases and Nb3The phase composition of Si phases two, parallel into Nb solid solution phases and Nb is presented in the microscopic structure in shape direction3Si phases, which orient, is alternately arranged feature, and phase size is only that tradition orientation is solidifying Gu 1/10 or so of Nb-Si bianry alloys prepared by technique.Eliminating traditional founding Nb-Si techniques institute, inevitably composition is inclined Analysis, uneven microstructure, the problems such as coarse grains, it is not necessary to which crucible constrains, and avoids electrode, crucible etc. and is closed to high activity Nb-Si The pollution of golden melt, alloy comprehensive mechanical property are good.
Embodiment
The present invention is further elaborated below, but the invention is not limited in specific embodiment.
Using pure Nb powder and pure Si powder as raw material, being prepared using Laser Rapid Prototyping Technique has oriented freezing organization special The Nb-Si alloys of sign, alloy is by Nb solid solution phases and Nb3Nb solid solution phases and Nb is presented in the phase composition of Si phases two, microscopic structure3Si Mutually orientation is alternately arranged, and preparation process comprises the following steps:
(1) commercially available pure Nb powder and pure Si powder are sieved by metallic screen respectively, it is 50~100 μm pure to obtain average grain diameter Nb powder and pure Si powder;
(2) the pure Nb and pure Si powder obtained step (1) be respectively placed in two of Stereolithography it is independent In powder feeder, the two powder feeders can individually adjust rotating speed, and then adjust the mixed proportion of powder, and using high-purity argon gas as load powder Air-flow and protection gas, carry powder air-flow velocity:5~10L/min, protection air-flow speed:10~30L/min;
(3) according to the Nb-Si binary alloys of required preparation, the powder feeding rate of pure Nb powder and pure Si powder is adjusted, Total powder feeding rate of Nb powder and Si powder is 5~20g/min;
(4) forming board is the DZ125 alloys of directional solidification state, and alloy directionally solidified to be oriented parallel to powder feeding formula laser fast Rapid-result shape direction.
(5) laser and powder are coaxially sent out, laser and powder synchronizing moving, and only scan a road in one direction Secondary, laser power is set to:1000~3000W, laser defocus distance:0~20mm, laser scan rate:400~800mm/min, In the presence of laser, Nb, Si powder reaction in-situ on forming board, and as powder and laser travel forward, molten bath is coagulated Gu obtain one layer of sedimentary;
(6) after layer surface temperature to be deposited is reduced to less than 100 DEG C, next sedimentary preparation is carried out;
(7) coaxial head of powder and laser rises a deposit thickness, then the sedimentary obtained using step (5) as base Body, repeat step (5) obtain another sedimentary;
(8) repeat step (5) and step (6), completed until prepared by the Nb-Si alloys of required height, treat that alloy temperature drops Taken out after to room temperature, obtaining thin wall shape has the Nb-Si alloys of oriented freezing organization feature.
Embodiment
A kind of Nb-16Si alloy preparation methods with oriented freezing organization feature:
(1) commercially available pure Nb powder and pure Si powder are sieved by metallic screen, obtain particle mean size be about 80 μm pure Nb powder and Pure Si powder.
(2) the pure Nb and pure Si powder obtained step (1) be respectively placed in two of Stereolithography it is independent In powder feeder, using high-purity argon gas as load powder air-flow and protection gas, 6L/min, protection air-flow speed:25L/min;
(3) Nb-16Si binary alloys are calculated as according to atomic percent, adjust sending for pure Nb powder and pure Si powder Powder speed, the powder feeding rate of wherein Nb powder are:The powder feeding rate of 9.46g/min, Si powder is:0.54g/min.
(4) it is 300mm × 300mm × 50mm DZ125 alloys for forming board using size;
(5) laser and powder are coaxially sent out, laser and powder synchronizing moving, and only scan a road in one direction It is secondary, 2000 W, laser defocus distance:13mm, laser scan rate:600mm/min, in the presence of laser, Nb, Si powder exists Fusing forms molten bath on forming board, and as powder and laser travel forward, molten bath solidification, obtains width about 2mm, thickness is about For 0.6mm, length about 15mm one layer of sedimentary;
(6) after layer surface temperature to be deposited is reduced to less than 100 DEG C, next sedimentary preparation is carried out;
(7) coaxial head of powder and laser rises a deposit thickness, then the sedimentary obtained using step (5) as base Body, repeat step (5) obtain another sedimentary;
(8) repeat step (6) and step (7), completed until prepared by highly about 10mm Nb-Si alloys, treat alloy temperature Taken out after being down to room temperature, obtain the Nb-Si alloys with oriented freezing organization feature, on alloy cross section Nb based solid solutions and Nb3Only about 1 μm of Si phase sizes.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the scope of the invention, every utilization The equivalent structure or equivalent flow conversion that present specification is done, or directly or indirectly it is used in other correlation techniques neck Domain, it is included within the scope of the present invention.

Claims (6)

  1. A kind of 1. Nb-Si alloy preparation methods with oriented freezing organization feature, it is characterised in that:With pure Nb powder and pure Si Powder is raw material, and preparing the Nb-Si with oriented freezing organization feature using binary channels powder feeding formula Laser Rapid Prototyping Technique closes Gold, alloy is by Nb based solid solutions phase and Nb3Nb solid solution phases and Nb is presented in the phase composition of Si phases two, microscopic structure3Si phases orient alternating Arrayed feature, preparation process comprise the following steps:
    (1) commercially available pure Nb powder and pure Si powder are sieved by metallic screen respectively, obtains even-grained pure Nb powder and pure Si powder;
    (2) the pure Nb and pure Si powder obtained step (1) is respectively placed in two independent powder feedings of Stereolithography In device, using high-purity argon gas as load powder air-flow and protection gas;
    (3) according to the Nb-Si binary alloys of required preparation, the powder feeding rate of pure Nb powder and pure Si powder is adjusted;
    (4) laser and powder are coaxially sent out, laser and powder synchronizing moving, and only scan a passage in one direction, In the presence of laser, Nb, Si powder melts on forming board forms molten bath, and as powder and laser travel forward, molten bath Solidification, obtains one layer of sedimentary;
    (5) after layer surface temperature to be deposited is reduced to less than 100 DEG C, next sedimentary preparation is carried out;
    (6) coaxial head of powder and laser rises a deposit thickness, then the sedimentary obtained using step (4) as matrix, weight Multiple step (4) obtains another sedimentary;
    (7) repeat step (5) and step (6), completed until prepared by the Nb-Si alloys of required height, treat that alloy temperature is down to room Taken out after temperature, obtain the Nb-Si alloys with oriented freezing organization feature.
  2. 2. a kind of Nb-Si alloy preparation methods with oriented freezing organization feature according to claim 1, its feature exist In:The pure Nb powder that screening obtains in step (1), the average grain diameter of pure Si powder is 50~100 μm.
  3. 3. a kind of Nb-Si alloy preparation methods with oriented freezing organization feature according to claim 1, its feature exist In:Powder air-flow velocity is carried in step (2):5~10L/min, protection air-flow speed:10~30L/min.
  4. 4. a kind of Nb-Si alloy preparation methods with oriented freezing organization feature according to claim 1, its feature exist In:Total powder feeding rate of pure Nb powder and pure Si powder is 5~20g/min in step (3).
  5. 5. a kind of Nb-Si alloy preparation methods with oriented freezing organization feature according to claim 1, its feature exist In:Forming board is the DZ125 alloys of directional solidification state in step (4), alloy directionally solidified to be oriented parallel to powder feeding formula laser Quick-forming direction.
  6. 6. a kind of Nb-Si alloy preparation methods with oriented freezing organization feature according to claim 1, its feature exist In:Laser power is set in step (4):1000~3000W, laser are in out-of-focus appearance, defocus distance:0~20mm, laser are swept Retouch speed:400~800mm/min.
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Cited By (2)

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CN111910184A (en) * 2020-08-06 2020-11-10 沈阳中钛装备制造有限公司 Laser cladding method
CN111945150A (en) * 2020-07-24 2020-11-17 中国航发北京航空材料研究院 Preparation method of TiAlN coating

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CN111910184A (en) * 2020-08-06 2020-11-10 沈阳中钛装备制造有限公司 Laser cladding method

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