CN108213422A - A kind of preparation method of carbon containing high-entropy alloy composite material - Google Patents
A kind of preparation method of carbon containing high-entropy alloy composite material Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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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
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- B22F10/64—Treatment of workpieces or articles after build-up by thermal means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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- B22F10/36—Process control of energy beam parameters
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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- B22F10/366—Scanning parameters, e.g. hatch distance or scanning strategy
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- 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
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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]
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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Abstract
The invention discloses a kind of preparation methods of carbon containing high-entropy alloy composite material, include the following steps：(1) high entropy prealloy powder is prepared；It is made of in high entropy prealloy powder at least four metallic elements in Fe, Co, Cr, Ni and Mn and C element；(2) selective laser melting (SLM) molding is carried out to high entropy prealloy powder, and part after molding is subjected to subsequent heat treatment to get to carbon containing high-entropy alloy.The present invention, as matrix, can be ensured after selective laser melting (SLM) molding, still with preferable plasticity using the high-entropy alloy of the excellent plasticities such as FeCoCrNi；Interstitial element C is introduced simultaneously, the yield strength and ultimate strength of matrix are significantly improved by solution strengthening；Degree of supercooling during precinct laser fusion is very high, and interstitial element C is equably dissolved into matrix, and no coarse Carbide segregation is precipitated, so as to ensure that the plasticity of material.The product of high-compactness (＞ 99%) is obtained during the preparation method of the present invention by the way of precinct laser fusion.
Description
Technical field
The invention belongs to alloy fields more particularly to a kind of use selective laser smelting technology to prepare carbon containing high-entropy alloy and answer
The method of condensation material.
Background technology
High-entropy alloy refer at least quaternary and more than transition group alloying element with equimolar or close to equimolar ratio
The alloy combined.Although the composition of high-entropy alloy is more complicated, single-phase supersaturated solid solution can be formed.High entropy
Alloy has good mechanical performance, corrosion resistance and antioxygenic property.
Gap carbon is added into high-entropy alloy, is a kind of good method for strengthening high-entropy alloy.At present, high-entropy alloy master
It to use and be prepared the methods of vacuum arc melting.However melting cooling velocity itself is relatively low, it is coarse hard in carbon containing high-entropy alloy
Matter carbide is easily segregated in grain boundaries, the mechanical property of attacking material.And founding is not easy to shape the part of labyrinth, no
Conducive to some practical application requests of high-entropy alloy.In order to which carbon containing high-entropy alloy is preferably applied in engineering, research increases material
It is particularly important that manufacturing method prepares the uniform carbon containing high-entropy alloy part of complicated shape, tissue.
One of the mode of precinct laser fusion as increasing material manufacturing can not only manufacture the extremely complex workpiece of shape, gram
The problems such as material difficult processing is low with stock utilization are taken；Also, since precinct laser fusion process has the characteristics that cooling rate is high,
Tiny uniform, the material interior element of material structure prepared using the technology is evenly distributed, satisfactory mechanical property.
Material prepared by precinct laser fusion has complicated shape, so the schedule of reinforcement that can be used is limited.There is research
Person is closed micro-crack and micropore in selective laser fusing sample by hot isostatic pressing, so as to further improve precinct laser
Melt the mechanical property of sample.But the process for improving properties of sample using hot isostatic pressing increases industry energy consumption, reduces product
Precision, weaken the engineering significance of precinct laser fusion.
For precinct laser fusion part subsequent reinforced it is difficult the problem of, seek it is a kind of low cost, suitable for precinct laser
The high-entropy alloy of subsequent reinforced is melted, explores printing and the heat treatment process of high-entropy alloy selective laser fusion technology, further
It is those skilled in the art's urgent problem to be solved to improve the mechanical property of materials.
Invention content
The technical problems to be solved by the invention are to overcome the shortcomings of to mention in background above technology and defect, provide one
The method that kind prepares carbon containing high-entropy alloy using selective laser smelting technology.
In order to solve the above technical problems, technical solution proposed by the present invention is：A kind of carbon containing high-entropy alloy composite wood is provided
The preparation method of material, includes the following steps：
(1) high entropy prealloy powder is prepared；By at least four metals member in Fe, Co, Cr, Ni and Mn in high entropy prealloy powder
Element and C element composition；
(2) selective laser melting (SLM) molding is carried out to high entropy prealloy powder, and part after molding is subjected to subsequent heat treatment,
Obtain carbon containing high-entropy alloy.
Above-mentioned preparation method, it is preferred that the molar content of carbon atom is not higher than 5% in high entropy prealloy powder.
Above-mentioned preparation method, it is preferred that the molar content of carbon atom is 1-4% in high entropy prealloy powder.
Above-mentioned preparation method, it is preferred that high entropy prealloy powder is prepared as raw material using metal simple-substance and metal carbides.
Above-mentioned preparation method, it is preferred that the metal simple-substance in simple substance Fe, Co, Cr, Ni, Mn at least four；
The one kind of the metal carbides in chromium carbide, cementite, carbonization nickel.
Above-mentioned preparation method, it is preferred that the heat treatment includes annealing, and precipitation strength is carried out after annealing.
Above-mentioned preparation method, it is preferred that the condition of the annealing is：Part is warming up to 350~450 in 1~2h
DEG C, 2~5h is kept the temperature, is higher than 9 × 10 in vacuum degree-3Under conditions of Pa, less than 100 DEG C are cooled to the furnace.
Above-mentioned preparation method, it is preferred that the condition of the precipitation strength is：Part is warming up to 800~1000 DEG C, is protected
Warm 15min~50min takes out part, is air-cooled to room temperature.
Above-mentioned preparation method, it is preferred that scanning is successively scanned using checkerboard type；Deflection angle when successively scanning, deflection
Angle is 50~70 °.
Above-mentioned preparation method, it is preferred that the process conditions of precinct laser fusion are：Scanning laser power for 300~
400W, 600~2000mm/s of sweep speed, spot diameter are 70~100 μm, and 90~130 μm of sweep span, powdering thickness is 30
~50 μm.
Above-mentioned preparation method, it is preferred that during precinct laser fusion, oxygen content is less than 2000ppm, chamber inner pressure in chamber
Power is 30~40mbar；Basal plate preheating temperature is 100 DEG C.
Above-mentioned preparation method, it is preferred that specifically include following steps：
(1) metal carbides and metal simple-substance is taken to be prepared into high entropy prealloy powder as raw material；
(2) threedimensional model of part to be prepared is established on computers, and imported into the former of precinct laser fusion
In, and molding technique parameter is set；
(3) high entropy prealloy powder prepared by step (1) is placed in selective laser melting (SLM) molding equipment and supplied in powder cylinder, and
Inert gas is passed through into working chamber, metal substrate is preheated；
(4) selective laser melting (SLM) molding is carried out, and part after molding is annealed and precipitation strength.
Above-mentioned preparation method, it is preferred that the method for being prepared into high entropy prealloy powder is gas atomization, centrifugal atomization
With one kind in nodularization method.
Above-mentioned preparation method, it is preferred that the high entropy pre-alloyed powder granularity being prepared is 15~45 μm.
Compared with prior art, the advantage of the invention is that：
(1) present invention can ensure using the high-entropy alloy of the excellent plasticities such as FeCoCrNi as matrix in precinct laser
After melt-forming, still with preferable plasticity；Interstitial element C is introduced simultaneously, matrix is significantly improved by solution strengthening
Yield strength and ultimate strength；Degree of supercooling during precinct laser fusion is very high, and interstitial element C is equably dissolved into matrix
Interior, no coarse Carbide segregation is precipitated, so as to ensure that the plasticity of material.
(2) high-compactness (＞ 99%) is obtained by the way of precinct laser fusion during preparation method of the invention
Product, suitable for the part of forming shape complexity；Part after molding is without mechanical processing, and stock utilization is high, shaping speed
Soon.
(3) carbon containing high-entropy alloy of the invention is different from other two-phases or multiphase high-entropy alloy, after molding group
In knitting, the second phase has been provided with certain original dimension, can not make its diminution；Present invention system by way of precinct laser fusion
Standby carbon containing high-entropy alloy, internal carbon are evenly distributed, and carbides-free is precipitated.Therefore the present invention passes through precipitation strength heat
Processing, can effectively control the scale of intermetallic compound, nano level carbon compound is precipitated, effective to promote material in itself
Intensity, and hardly lose plasticity.
(4) because most of metal can be combined with interstitial element C, carbon compound hardening constituent is formed, so this is a kind of
The schedule of reinforcement of universality can be widely used in and strengthen high-entropy alloy prepared by precinct laser fusion, so the invention has
There are great meaning and value.
Description of the drawings
Fig. 1 is the pictorial diagram that the embodiment of the present invention 1 prepares high-entropy alloy composite material.
Fig. 2 is the stretching experiment curve graph that the embodiment of the present invention 1 prepares high-entropy alloy composite material.
Fig. 3 is the picture of the carbon distributional analysis of high-entropy alloy composite material prepared by the embodiment of the present invention 1.
Specific embodiment
For the ease of understanding the present invention, done more entirely below in conjunction with Figure of description and preferred embodiment to inventing herein
Face meticulously describes, but protection scope of the present invention is not limited to specific examples below.
Unless otherwise defined, all technical terms used hereinafter are generally understood meaning phase with those skilled in the art
Together.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention's
Protection domain.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1：
The present invention provides a kind of preparation methods of carbon containing high-entropy alloy composite material, include the following steps：
(1) Fe, Co, Cr, Ni metal simple-substance and chromium carbide are chosen as raw material, Fe, Cr, Ni, Co, C in composite material
Atomic ratio be 1：1：1：1：0.05, high entropy prealloy powder is prepared using gas atomization；Wherein, it is removed on a small quantity not in alloying element powder
Other impurity are free of outside evitable impurity oxygen element, the other elements ingredient in addition to Fe, Co, Cr, Ni, C is free of in raw material；
High 15~55 μm of entropy prealloy powder powder diameter range, D50 are controlled at 45 μm；
(2) three-dimensional part model is established on computers, plans component scan path, and scanning is successively swept using checkerboard type
It retouches；Deflection angle when successively scanning, deflection angle are 65 °；
(3) using the technological forming of precinct laser fusion：Scanning laser power be 400W, sweep speed 800mm/s, hot spot
A diameter of 90 μm, 120 μm of sweep span, powdering thickness is 50 μm；
(4) for the inert gas used for argon gas, equipment, will using being passed directly into argon gas in a manner that gas circulation is combined
The indoor oxygen content of chamber is reduced to 2000ppm once, cavity indoor pressure 30mbar；
(5) substrate is preheated, preheating temperature is 100 DEG C, again by manual powdering in substrate after the completion of basal plate preheating
The high entropy pre-alloyed powder that upper tiling a layer thickness is 40 μm；
(6) after forming parts, room temperature is furnace-cooled to, part is taken out, carries out stress relief annealing：400 DEG C are warming up in 1h, is protected
Warm 3h, vacuum degree 8 × 10-3Pa cools to 100 DEG C with the furnace, and part is taken out in blow-on, is air-cooled to room temperature.
(7) precipitation strength heat treatment is carried out：800 DEG C are warming up to, part is placed in stove at high temperature, 30min is kept the temperature, opens
Stove takes out part, is air-cooled to room temperature by high temperature, obtains carbon containing high-entropy alloy, pictorial diagram is as shown in Figure 1.
Part prepared by the precinct laser fusion method, surface is without apparent warping phenomenon.By drainage to this implementation
The part of example is tested, and the consistency for measuring the high-entropy alloy composite material is 99.5%；The stretching experiment engineering of part is bent
Line is as shown in Fig. 2, before heat treatment：Yield strength is 638MPa, tensile strength 797MPa, and elongation percentage reaches 13.5%；At heat
After reason：Yield strength is 706MPa, tensile strength 903MPa, elongation percentage 12.8%.
High-entropy alloy composite material prepared by the present embodiment precinct laser fusion carries out atom probe analysis (EPMA), photo
(left figure is the distribution of carbon, and right figure is the microscopic structure of corresponding region) as shown in Figure 3.As seen from Figure 3, prepared by the present embodiment
High-entropy alloy composite material, the uniform of carbon be solid-solubilized in matrix, and no apparent Carbide segregation is precipitated.
Embodiment 2：
The present invention provides a kind of preparation methods of carbon containing high-entropy alloy composite material, include the following steps：
(1) Fe, Co, Cr, Ni metal simple-substance and chromium carbide are chosen as raw material, Fe, Cr, Ni, Co, C in composite material
Atomic ratio be 1：1：1：1：0.1, high entropy prealloy powder is prepared using gas atomization；Wherein, it is removed on a small quantity not in alloying element powder
Other impurity are free of outside evitable impurity oxygen element, the other elements ingredient in addition to Fe, Co, Cr, Ni, C is free of in raw material；
High 15~45 μm of entropy prealloy powder powder diameter range, wherein d50 are controlled at 40 μm；
(2) three-dimensional part model is established on computers, plans component scan path, and scanning is successively swept using checkerboard type
It retouches；Deflection angle when successively scanning, deflection angle are 70 °；
(3) technique of the precinct laser fusion used：The scanning laser power be 400W, sweep speed 1000mm/s,
Spot diameter is 80 μm, 110 μm of sweep span, and powdering thickness is 40 μm.
(4) for the inert gas used for argon gas, equipment, will using being passed directly into argon gas in a manner that gas circulation is combined
The indoor oxygen content of chamber is reduced to 2000ppm once, cavity indoor pressure 30mbar；
(5) substrate is preheated, preheating temperature is 100 DEG C, again by manual powdering in substrate after the completion of basal plate preheating
The high entropy pre-alloyed powder that upper tiling a layer thickness is 35 μm；
(6) after forming parts, room temperature is furnace-cooled to, part is taken out, carries out stress relief annealing：450 DEG C are warming up in 1h, is protected
Warm 4h, 8 × 10-3Pa of vacuum degree cool to 100 DEG C with the furnace, and part is taken out in blow-on, is air-cooled to room temperature.
(7) precipitation strength heat treatment is carried out：760 DEG C are warming up to, part is placed in stove at high temperature, 20min is kept the temperature, opens
Stove takes out part, is air-cooled to room temperature by high temperature, obtains carbon containing high-entropy alloy.
Part prepared by the precinct laser fusion method, surface is without apparent warping phenomenon.By drainage to this implementation
Example part is tested, and the consistency for measuring the high-entropy alloy composite material is 99.3%；Before heat treatment：Yield strength is
674MPa, tensile strength 832MPa, elongation percentage reach 9.9%；After heat treatment：Yield strength is 743MPa, and tensile strength is
916MPa, elongation percentage 9.3%.
Embodiment 3：
The present invention provides a kind of preparation methods of carbon containing high-entropy alloy composite material, include the following steps：
(1) Fe, Co, Cr, Ni, Mn metal simple-substance and chromium carbide are chosen as raw material, Fe, Cr in composite material, Ni,
The atomic ratio of Co, Mn, C are 1：1：1：1：1：0.07, high entropy prealloy powder is prepared using gas atomization；Wherein, alloying element powder
In outside a small amount of inevitably impurity oxygen element without other impurity, without in addition to Fe, Co, Cr, Ni, Mn, C in raw material
Other elements ingredient；High 15~45 μm of entropy prealloy powder powder diameter range, wherein d50 are controlled at 35 μm；
(2) three-dimensional part model is established on computers, plans component scan path, and scanning is successively swept using checkerboard type
It retouches；Deflection angle when successively scanning, deflection angle are 63 °；
(3) technique of the precinct laser fusion used：The scanning laser power be 350W, sweep speed 1200mm/s,
Spot diameter is 90 μm, 100 μm of sweep span, and powdering thickness is 35 μm；
(4) for the inert gas used for argon gas, equipment, will using being passed directly into argon gas in a manner that gas circulation is combined
The indoor oxygen content of chamber is reduced to 2000ppm once, cavity indoor pressure 30mbar；
(5) substrate is preheated, preheating temperature is 100 DEG C, again by manual powdering in substrate after the completion of basal plate preheating
The high entropy pre-alloyed powder that upper tiling a layer thickness is 35 μm；
(6) after forming parts, room temperature is furnace-cooled to, part is taken out, carries out stress relief annealing：500 DEG C are warming up in 1h, is protected
Warm 3h, 9 × 10-3Pa of vacuum degree cool to 100 DEG C with the furnace, and part is taken out in blow-on, is air-cooled to room temperature.
(7) precipitation strength heat treatment is carried out：830 DEG C are warming up to, part is placed in stove at high temperature, 25min is kept the temperature, opens
Stove takes out part, and room temperature is air-cooled to by high temperature.
Part prepared by the precinct laser fusion method, surface is without apparent warping phenomenon.By drainage to this implementation
Example part is tested, and the consistency for measuring the high-entropy alloy composite material is 99.6%；The stretching experiment engineering curve of part
As shown in Fig. 2, before heat treatment：Yield strength is 625MPa, tensile strength 786MPa, and elongation percentage reaches 16.3%；Heat treatment
Afterwards：Yield strength is 689MPa, tensile strength 891MPa, elongation percentage 16.1%.
Claims (10)
1. a kind of preparation method of carbon containing high-entropy alloy composite material, which is characterized in that include the following steps：
(1) high entropy prealloy powder is prepared；In high entropy prealloy powder by least four metallic elements in Fe, Co, Cr, Ni and Mn and
C element forms；
(2) to high entropy prealloy powder carry out selective laser melting (SLM) molding, and by part after molding carry out subsequent heat treatment to get
To carbon containing high-entropy alloy.
2. preparation method as described in claim 1, which is characterized in that the molar content of carbon atom in high entropy prealloy powder
Not higher than 5%.
3. preparation method as described in claim 1, which is characterized in that the molar content of carbon atom in high entropy prealloy powder
For 1-4%.
4. preparation method as described in claim 1, which is characterized in that prepared using metal simple-substance and metal carbides as raw material high
Entropy prealloy powder.
5. preparation method as claimed in claim 4, which is characterized in that the metal simple-substance is selected from simple substance Fe, Co, Cr, Ni, Mn
In at least four；The one kind of the metal carbides in chromium carbide, cementite, carbonization nickel.
6. preparation method as described in claim 1, which is characterized in that the heat treatment includes annealing, is precipitated after annealing
Strengthen.
7. preparation method as claimed in claim 6, which is characterized in that the condition of the annealing is：Part is risen in 1~2h
Temperature keeps the temperature 2~5h to 350~450 DEG C, is higher than 9 × 10 in vacuum degree-3Under conditions of Pa, less than 100 DEG C are cooled to the furnace.
8. preparation method as claimed in claim 6, which is characterized in that the condition of the precipitation strength is：Part is warming up to
800~1000 DEG C, 15min~50min is kept the temperature, part is taken out, is air-cooled to room temperature.
9. preparation method as described in claim 1, which is characterized in that the process conditions of precinct laser fusion are：Scanning laser
Power is 300~400W, and 600~2000mm/s of sweep speed, spot diameter is 70~100 μm, 90~130 μm of sweep span,
Powdering thickness is 30~50 μm.
10. preparation method as described in claim 1, which is characterized in that specifically include following steps：
(1) metal carbides and metal simple-substance is taken to be prepared into high entropy prealloy powder as raw material；
(2) threedimensional model of part to be prepared is established on computers, and is imported into the former of precinct laser fusion, and
Molding technique parameter is set；
(3) by high entropy prealloy powder prepared by step (1) be placed in selective laser melting (SLM) molding equipment in powder cylinder, and to work
Inert gas is passed through as intracavitary, metal substrate is preheated；
(4) selective laser melting (SLM) molding is carried out, and part after molding is annealed and precipitation strength.
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