CN109317671A - A kind of method that laser gain material prepares high-entropy alloy - Google Patents

A kind of method that laser gain material prepares high-entropy alloy Download PDF

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Publication number
CN109317671A
CN109317671A CN201810929883.2A CN201810929883A CN109317671A CN 109317671 A CN109317671 A CN 109317671A CN 201810929883 A CN201810929883 A CN 201810929883A CN 109317671 A CN109317671 A CN 109317671A
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entropy alloy
laser
gain material
layer
laser gain
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任旭东
焦加飞
童照鹏
李琳
杨宇
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Jiangsu University
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Jiangsu University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20—Direct sintering or melting
    • B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F12/00—Apparatus or devices specially adapted for additive manufacturing; Auxiliary means for additive manufacturing; Combinations of additive manufacturing apparatus or devices with other processing apparatus or devices
    • B22F12/10—Auxiliary heating means
    • B22F12/17—Auxiliary heating means to heat the build chamber or platform
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B22F3/15—Hot isostatic pressing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE 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
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30—Process control
    • B22F10/36—Process control of energy beam parameters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/60—Treatment of workpieces or articles after build-up
    • B22F10/64—Treatment of workpieces or articles after build-up by thermal means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Powder Metallurgy (AREA)

Abstract

The present invention relates to a kind of method that laser gain material prepares high-entropy alloy, A is comprised the following steps that, by substrate polishing, cleaning and drying, and it is preheated；B, ball-milling treatment is carried out to proportioned high-entropy alloy powder, it is to be deposited after mixing evenly；C, it is required according to blocky high-entropy alloy component performance, the laser technical parameters of every layer of sedimentary of pre-designed processing；D, according to preset every layer of laser technical parameters, layer-by-layer variable element laser gain material processing is carried out in substrate surface；E, it after to be processed, after prepared bulk alloy component slow cooling to room temperature, is separated from substrate with the method for wire cutting by material component is increased, hip treatment then is carried out to it.The present invention shortens its production cycle, reduces cost while meeting molded part performance, can also prepare complex-shaped large scale part.

Description

A kind of method that laser gain material prepares high-entropy alloy
Technical field
The invention belongs to alloy material and its preparation technical fields, and in particular to a kind of laser gain material manufacture high-entropy alloy Preparation method.
Background technique
High-entropy alloy is a kind of novel metal material, is to be put forward by TaiWan, China scholar Ye Junwei in 2004. It is to be formed by five kinds or five kinds or more metallic elements by equimolar mass ratio or approximate equimolar mass combination, with conventional alloys Difference, due to high entropy effect and distortion of lattice effect, a bit excellent mechanical performance of the alloy, such as high rigidity, intensity, corrosion resistant Wear resistance is lost, especially mechanical performance also does well at low temperatures and high temperatures, has very high thermal stability and high temperature anti- Oxidisability is with a wide range of applications.Method for preparing high-entropy alloy mainly has at present: founding, powder metallurgy, spray coating method and plating The methods of film.High-entropy alloy microstructure made by these methods is rougher, and tissue is defective, and the production cycle is longer, cost Also relatively high.
Laser gain material manufacture is a kind of novel metal component preparation method, is compared with traditional diamond-making technique, this method tool There is higher cooling rate, reaches 107K/s, high cooling rate can refine crystal grain, keep Elemental redistribution uniform, improve material Expect mechanical property, is a kind of novel effective preparation method that can be used to prepare high-entropy alloy.Functionally graded material component is One kind making center portion and the external high-performance component with different mechanical properties, in the preparation of material by gradient distribution technological design In the process by continuously changing distribution or the working process parameter of each site component content, make material macroscopic properties in space Change of gradient is presented on position, the difference of materials'use performance is required to meet structural detail different parts, reaches optimization The purpose of structure entirety service performance.
Summary of the invention
The present invention can not prepare the technical problem of functionally gradient high-entropy alloy for existing traditional preparation methods, propose A kind of laser gain material prepares the new method of high-entropy alloy.
For achieving the above object, the technical scheme adopted by the invention is as follows: a kind of laser gain material prepares high-entropy alloy Method comprises the following steps that A, by substrate polishing, cleaning and drying, and preheats to it；B, proportioned high entropy is closed Bronze end carries out ball-milling treatment, to be deposited after mixing evenly；C, it is required according to blocky high-entropy alloy component performance, it is pre-designed Process the laser technical parameters of every layer of sedimentary；D, it according to preset every layer of laser technical parameters, is carried out in substrate surface Layer-by-layer variable element laser gain material processing；E, it after to be processed, after prepared bulk alloy component slow cooling to room temperature, is cut with line The method cut is separated material component is increased from substrate, and then carries out hip treatment to it.
In above scheme, in the step A, substrate preheating temperature is to 300 DEG C.
In above scheme, in the step B, by equimolar than mixing, powder purity is each ingredient of high-entropy alloy powder 99.99% or more.
In above scheme, in the step D, high-entropy alloy powder layer-by-layer melt deposition from bottom to top is keeping powder feeding speed In the case that rate is constant, dust distributor couples output with laser coaxial.
In above scheme, the parameter of layer-by-layer variable element laser gain material processing includes laser beam scan path, laser scanning speed And laser power.
In above scheme, in the case where keeping metal powder feed rate certain, dust distributor is opened simultaneously with laser, is made Powder Melting And Solidification in substrate, laser beam scan path are divided into two kinds, a kind of to scan along X-axis in S font, and a kind of along Y-axis is in S word Shape scanning.
In above scheme, laser power 800W-2000W, powder feeding rate 0.7r/min, powder feeding gas pressure 0.9MPa。
In above scheme, whole process carries out in argon atmosphere, and coaxial shielding gas pressure rates are 5L/min；Laser is taken Connecing rate is 50%；Spot diameter is 2mm.
In above scheme, in the step E, heat and other static pressuring processes parameter are as follows: 1100 DEG C of temperature, the duration 3.5 is small When, pressure is 170 MPa.
Beneficial effects of the present invention are as follows: (1) present invention prepares functionally gradient high-entropy alloy by laser gain material manufacture, In deposition process, by successively changing the technological parameter of each sedimentary, prepared alloy center portion and outside is made to possess difference Mechanical property can obtain high-performance, the flawless functionally gradient bulk high-entropy alloy of " interior tough outer strong " or " interior outer tough by force "； (2) the problems such as using gradient distribution technological design, solving low deposition interfacial bonding strength, boundary defect；(3) laser gain material manufactures Inevitably there is hole, micro-crack and residual tension in sample, the sample of preparation is carried out hip treatment, eliminates it Internal hole, micro-crack and residual thermal stress etc., improves its mechanical performance.(4) alloy structure that this method is prepared is Single face-centered cubic crystal structure or body-centered cubic crystal structure, tensile yield strength 500MPa-700MPa are broken general extension Rate is 50% or so, and microhardness is 400HV or so, and exemplar has good mechanical performance.
Figure of description
With reference to the accompanying drawing, technical solution of the present invention is described in detail.
Fig. 1 present invention prepares the schematic diagram of " sandwich " shape functionally gradient bulk high-entropy alloy.
Fig. 2 present invention is in S zigzag scanning path schematic diagram along Y-axis.
Fig. 3 is in S zigzag scanning path schematic diagram along X-axis for the present invention.
Fig. 4 is the XRD spectrum that the present invention prepares " sandwich " shape functionally gradient bulk high entropy alloy material.
Fig. 5 is that the present invention prepares tough outer strong performance profile in " sandwich " shape functionally gradient bulk high entropy alloy material.
Specific embodiment
To facilitate the understanding of the present invention, present invention work is further retouched in detail with reference to the accompanying drawings and detailed description It states.
The present invention provides a kind of laser gain material manufacture " sandwich " shape functionally gradient bulk high-entropy alloy technical solution, The specific steps of which are as follows: choosing five kinds of metallic elements Fe, Co, Ni, Cr, Mn, mixed by equimolar ratio, selected powder is pure Degree is 99.99%.
Stainless steel base is polished with sand paper, then is cleaned with ethyl alcohol, surface impurity is removed, does standard for post-production It is standby.
As shown in Figure 1, the present invention prepares showing for " sandwich " shape functionally gradient bulk Fe, Co, Ni, Cr, Mn high-entropy alloy It is intended to, metal powder Melting And Solidification in substrate forms blocky entity.
Laser gain material manufacture is carried out, as shown in Figures 2 and 3, laser beam scan path, which is divided into, to be scanned along X-axis S font and along Y-axis The scanning of S font.Laser power is 600W-2000W, and powder feeding rate 0.7r/min, powder feeding gas pressure is 0.9MPa；To avoid Material is oxidized, and whole process carries out in argon gas, and coaxial shielding gas pressure rates are 5L/min；Laser lap rate is 50%；Light Spot diameter is 2mm.Laser power is 600W when processing first layer.At the end of first layer, nozzle move vertically upward 0.5mm away from From, and increase laser power to 800W, then carry out second layer increasing material manufacturing.Every layer of end rear nozzle moves 0.5mm vertically upward. Laser power increases to as 1000W when increasing material to third layer and the 4th layer.When to five cladding layers, laser power is down to 800W.It arrives Laser power is down to 600W when six cladding layers, completes until increasing material, and material surface and center portion is made to have different mechanical performances. Sample after molding is cut from substrate using wire cutting, and is cleaned up with ethyl alcohol, then is polished its surface with sand paper, crystal phase Polishing machine polishes it, carries out XRD, its surface topography and object phase constituent are observed in SEM, EDS test.Measure the aobvious of sample Microhardness and residual stress, each value at least measure five times, take its average value, avoid error.Sample is carried out at hot isostatic pressing Reason, the defects of to eliminate its micro-crack and thermal stress.Sample will be stretched and implement tension test, survey its yield strength and elongation percentage.
As shown in figure 4, the XRD spectrum of obtained high-entropy alloy, it can be seen that the alloy is face-centered cubic crystal knot Structure, diffraction maximum is at 43.5 °, 50.6 °, 74 ° and 95 °.
As shown in figure 5, the present invention prepares " sandwich " shape functionally gradient bulk Fe, Co, Ni, Cr, Mn high entropy alloy material Performance, the high-performance of acquisition " interior tough outer strong ", flawless functionally gradient bulk high-entropy alloy.

Claims (9)

1. a kind of method that laser gain material prepares high-entropy alloy, which is characterized in that comprise the following steps that
A, by substrate polishing, cleaning and drying, and it is preheated；
B, ball-milling treatment is carried out to proportioned high-entropy alloy powder, it is to be deposited after mixing evenly；
C, it is required according to blocky high-entropy alloy component performance, the laser technical parameters of every layer of sedimentary of pre-designed processing；
D, according to preset every layer of laser technical parameters, layer-by-layer variable element laser gain material processing is carried out in substrate surface；
E, after to be processed, after prepared bulk alloy component slow cooling to room temperature, material component will be increased with the method for wire cutting It is separated from substrate, hip treatment then is carried out to it.
2. the method that a kind of laser gain material according to claim 1 prepares high-entropy alloy, which is characterized in that the step A In, substrate preheating temperature is to 300 DEG C.
3. the method that a kind of laser gain material according to claim 1 prepares high-entropy alloy, which is characterized in that the step B In, for each ingredient of high-entropy alloy powder by equimolar than mixing, powder purity is 99.99% or more.
4. the method that a kind of laser gain material according to claim 1 prepares high-entropy alloy, which is characterized in that the step D In, high-entropy alloy powder layer-by-layer melt deposition from bottom to top, in the case where keeping powder feeding rate constant, dust distributor and laser Coaxial coupling output.
5. the method that a kind of laser gain material according to claim 4 prepares high-entropy alloy, which is characterized in that layer-by-layer variable element The parameter of laser gain material processing includes laser beam scan path, laser scanning speed and laser power.
6. the method that a kind of laser gain material according to claim 4 prepares high-entropy alloy, which is characterized in that keeping metal In the case that powder powder feeding rate is certain, dust distributor is opened simultaneously with laser, makes powder Melting And Solidification in substrate, laser scanning Path is divided into two kinds, a kind of to scan along X-axis in S font, it is a kind of along Y-axis in the scanning of S font.
7. the method that a kind of laser gain material according to claim 4 prepares high-entropy alloy, which is characterized in that laser power is 800W-2000W, powder feeding rate 0.7r/min, powder feeding gas pressure 0.9MPa.
8. the method that a kind of laser gain material according to claim 4 prepares high-entropy alloy, which is characterized in that whole process exists It is carried out in argon atmosphere, coaxial shielding gas pressure rates are 5L/min；Laser lap rate is 50%；Spot diameter is 2mm.
9. the method that a kind of laser gain material according to claim 1 prepares high-entropy alloy, which is characterized in that the step E In, heat and other static pressuring processes parameter are as follows: 1100 DEG C of temperature, the duration 3.5 hours, pressure was 170 MPa.
CN201810929883.2A 2018-08-15 2018-08-15 A kind of method that laser gain material prepares high-entropy alloy Pending CN109317671A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109972019A (en) * 2019-04-30 2019-07-05 上海交通大学 A kind of medium entropy alloy material and application method for increasing material manufacturing
CN112935252A (en) * 2021-03-04 2021-06-11 西北工业大学 Method for preparing high-toughness eutectic high-entropy alloy based on selective laser melting technology
US20220241854A1 (en) * 2019-02-20 2022-08-04 Hamilton Sundstrand Corporation Method for identifying and forming viable high entropy alloys via additive manufacturing

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103658647A (en) * 2013-12-10 2014-03-26 华南理工大学 SLM device based on four lasers and two stations and machining method
CN104841930A (en) * 2015-06-05 2015-08-19 哈尔滨工程大学 High-entropy alloy powder for 3D (three-dimensional) printing and method for preparing high-entropy alloy coating by using high-entropy alloy powder
CN105562694A (en) * 2015-12-31 2016-05-11 中国钢研科技集团有限公司 Hot isostatic pressing three-control method suitable for additive manufacturing parts
CN105665704A (en) * 2016-03-11 2016-06-15 上海拓宝机电科技有限公司 Metal laser selective melting method
CN107130124A (en) * 2017-04-21 2017-09-05 北京科技大学 A kind of method that increases material manufacturing technology shapes high-entropy alloy
CN108555295A (en) * 2017-08-24 2018-09-21 中国工程物理研究院材料研究所 A kind of laser solid forming method of high-entropy alloy component

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103658647A (en) * 2013-12-10 2014-03-26 华南理工大学 SLM device based on four lasers and two stations and machining method
CN104841930A (en) * 2015-06-05 2015-08-19 哈尔滨工程大学 High-entropy alloy powder for 3D (three-dimensional) printing and method for preparing high-entropy alloy coating by using high-entropy alloy powder
CN105562694A (en) * 2015-12-31 2016-05-11 中国钢研科技集团有限公司 Hot isostatic pressing three-control method suitable for additive manufacturing parts
CN105665704A (en) * 2016-03-11 2016-06-15 上海拓宝机电科技有限公司 Metal laser selective melting method
CN107130124A (en) * 2017-04-21 2017-09-05 北京科技大学 A kind of method that increases material manufacturing technology shapes high-entropy alloy
CN108555295A (en) * 2017-08-24 2018-09-21 中国工程物理研究院材料研究所 A kind of laser solid forming method of high-entropy alloy component

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20220241854A1 (en) * 2019-02-20 2022-08-04 Hamilton Sundstrand Corporation Method for identifying and forming viable high entropy alloys via additive manufacturing
CN109972019A (en) * 2019-04-30 2019-07-05 上海交通大学 A kind of medium entropy alloy material and application method for increasing material manufacturing
CN109972019B (en) * 2019-04-30 2021-10-22 上海交通大学 Medium-entropy alloy material for additive manufacturing and application method
CN112935252A (en) * 2021-03-04 2021-06-11 西北工业大学 Method for preparing high-toughness eutectic high-entropy alloy based on selective laser melting technology

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Application publication date: 20190212