CN109332680A - A kind of nano-oxide particles for high energy beam 3D printing/nickel base superalloy composite spherical powder and preparation method thereof - Google Patents
A kind of nano-oxide particles for high energy beam 3D printing/nickel base superalloy composite spherical powder and preparation method thereof Download PDFInfo
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- CN109332680A CN109332680A CN201811319601.3A CN201811319601A CN109332680A CN 109332680 A CN109332680 A CN 109332680A CN 201811319601 A CN201811319601 A CN 201811319601A CN 109332680 A CN109332680 A CN 109332680A
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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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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Abstract
The present invention discloses a kind of nano-oxide particles for high energy beam 3D printing/nickel base superalloy composite spherical powder, and nano-scale oxide enhances distribution of particles in the surface of micron-size spherical Ni-base Superalloy Powder；For the Ni-base Superalloy Powder purity 99% or more, partial size is 20-50 μm；The nano-scale oxide enhancing particle uses nanometer Y2O3、ThO2Or Al2O3Powder, powder diameter 30-100nm, the mass fraction of addition are 1-10%.Such composite spherical powder particle diameter distribution is narrow, sphericity is high, good fluidity, meets the requirement of 3D printing technique, and Nano-size Reinforced Particle is distributed in individual particle in 3D printing finished-product material, and 3D printing fabricated part is had excellent performance.Invention additionally discloses a kind of preparation methods of the nano-oxide particles for high energy beam 3D printing/nickel base superalloy composite spherical powder.
Description
Technical field
The invention belongs to 3D printing manufacturing technology field, in particular to a kind of nano-oxide for high energy beam 3D printing
Particle/nickel base superalloy composite spherical powder and preparation method thereof.
Background technique
Nickel base superalloy is widely used in the fields such as space flight, aviation because of its excellent high-temperature service performance.Compared to
The processing methods such as traditional casting, machine cut, it is complicated, high that the 3D printing of the high energy beams such as laser, electron beam can break through spatial form
The limitation of the conditions such as warm working has evolved into the main forming side of high-precision, complex-shaped nickel base superalloy aerospace parts
Method.And 3D printing powder body material is the key factor of determining 3D printing final product quality, decides the forming capacity of 3D printing technique
Boundary.
In recent years, dispersed oxide enhancing (ODS) nickel base superalloy is because having superior inoxidizability, intensity under high temperature
Etc. performances, adapt to work under severe extreme condition, be widely used in the fields such as aerospace turbogenerator.Oxide is more
It dissipates enhancing nickel base superalloy and mainly passes through some high-fire resistances of addition, inert oxide (Y2O3、ThO2、Al2O3) particle,
It is distributed evenly in matrix to improve its high-temperature behavior.
3D printing technique, which prepares nano-ceramic particle enhancing nickel base superalloy component, to be had compared with high-tech difficulty.Nanometer
Surface caused by the huge specific surface of grain can make between particle there are extremely strong agglomeration, and ceramic particle and matrix gold
It is big to belong to density variation, is easier to cause reunion, segregation, reduces reinforced phase particle to the strengthening effect of parent metal.
In view of the above-mentioned problems, nano-oxide particles/nickel base superalloy of high energy beam 3D printing is all made of prefabricated nanometer
Oxide particle/nickel base superalloy composite granule technology path.Currently, prefabricated nano-oxide particles/nickel-base high-temperature closes
Gold is all made of the method for the dispersion of long-time high-energy ball milling/compound.And high-energy ball milling method long-time mixed-powder can greatly drop
The sphericity of low powder particle, causes powder fluidity to decline to a great extent, and seriously affects the forming quality of high energy beam 3D printing；And
It is difficult to thoroughly solve the problems, such as that nanoscale enhancing particle is easy to reunite, causes Nano-size Reinforced Particle in the finished product of high energy beam 3D printing
Reunion and segregation.
Summary of the invention
The purpose of the present invention is to provide a kind of nano-oxide particles for high energy beam 3D printing/nickel-base high-temperature conjunction
Golden composite spherical powder, particle diameter distribution is narrow, sphericity is high, good fluidity, meets the requirement of 3D printing technique, 3D printing finished product
Nano-size Reinforced Particle is distributed in individual particle in material, and 3D printing fabricated part is had excellent performance.
It is another object of the present invention to provide a kind of nano-oxide particles for high energy beam 3D printing/Ni-based height
The advantages that there is the preparation method of temperature alloy composite spherical powder raw material to choose extensively, and preparation method is simple, at low cost.
In order to achieve the above objectives, solution of the invention is:
A kind of nano-oxide particles for high energy beam 3D printing/nickel base superalloy composite spherical powder, nanoscale
Oxide enhances distribution of particles in the surface of micron-size spherical Ni-base Superalloy Powder.
For above-mentioned Ni-base Superalloy Powder purity 99% or more, partial size is 20-50 μm.
Above-mentioned nano-scale oxide enhancing particle uses nanometer Y2O3、ThO2Or Al2O3Powder, powder diameter 30-
100nm, the mass fraction of addition are 1-10%.
A kind of foregoing nano-oxide particles for high energy beam 3D printing/nickel base superalloy composite spherical
The preparation method at end, includes the following steps:
Step 1: dispersion/bonding agent being dissolved in organic solvent and forms dispersion solution, nano-scale oxide is enhanced into particle
It is added in the solution, and is crushed decentralized processing 10-50min through high-energy ultrasonic；
Step 2: the dispersion liquid after break process in step 1 being subjected to ultrasonic agitation 30-70min, forms nanometer enhancing
Grain suspension；
Step 3: the Nano-size Reinforced Particle suspension obtained and uniform is added to step 2 in spherical Ni-base Superalloy Powder
Mixing；
Step 4: then the uniformly mixed solution high-speed stirred 2-4h that step 3 is obtained is dried, sieving processing,
Obtain nano-oxide particles/nickel base superalloy composite spherical powder.
In above-mentioned steps 1, dispersion/bonding agent is polyethylene glycol, and the mass fraction of addition is 0.5-5%.
In above-mentioned steps 1, organic solvent is ethyl alcohol, and the mass fraction of addition is 5-20%.
After adopting the above scheme, compared with the prior art, the invention has the following advantages:
(1) processing of solution group is implemented to nanometer grade powder using dispersing agent, so that nanometer grade powder has excellent dispersibility；
(2) bonding agent in the present invention has the characteristics that bonding is secured, quick, can effectively facilitate enhancing particle and metal powder
The combination of last particle；The mutual coordinated of mixed-powder, bonding agent, at room temperature can rapid link；
(3) the composite powder sphericity is high, and good fluidity can effectively be beaten in 3D as the shaping raw material of 3D printing
Rapid shaping on printing apparatus；
(4) raw material of the present invention is chosen extensively, and preparation method is simple, at low cost.
Detailed description of the invention
Fig. 1 is nanometer Al prepared by the present invention2O3The scanning electron microscope macrograph of/Ni based high-temperature alloy composite powder；
Fig. 2 is nanometer Al prepared by the present invention2O3The scanning electron microscope high power photo of/Ni based high-temperature alloy composite powder.
Specific embodiment
Below with reference to embodiment and Figure of description, the present invention is further illustrated.
Embodiment 1:
A kind of nanometer Al for high energy beam 3D printing2O3/ Ni based high-temperature alloy composite spherical powder and preparation method thereof,
With Ni based high-temperature alloy for 100% mass percentage, nanometer Al2O3Powder accounts for 1%；Nanometer Al2O3Partial size be 40nm, nickel
50 μm of based high-temperature alloy powder diameter.
This nanometer of Al2O3The preparation method of/Ni based high-temperature alloy composite powder:
Step 1: 0.5% polyethylene glycol dispersion/bonding agent is dissolved in 5% alcohol solvent and forms dispersion solution, it will
1%Al2O3Nanoscale enhancing particle is added in the solution, and is crushed decentralized processing 10min through high-energy ultrasonic；
Step 2: the dispersion liquid after break process in step 1 being subjected to ultrasonic agitation 30min, it is outstanding to form Nano-size Reinforced Particle
Supernatant liquid；
Step 3: the Nano-size Reinforced Particle suspension obtained and uniform is added to step 2 in nickel base superalloy spherical powder
Mixing；
Step 4: the uniformly mixed solution that step 3 is obtained carries out high-speed stirred 2h, is then dried, at sieving
Reason, can be obtained nano-oxide particles/nickel base superalloy composite spherical powder.
Embodiment 2:
A kind of nanometer ThO for high energy beam 3D printing2/ Ni based high-temperature alloy composite spherical powder and preparation method thereof,
With Ni-base Superalloy Powder for 100% mass percentage, nanometer ThO2Powder is 2%；Nanometer ThO2Partial size be 30nm,
40 μm of Ni-base Superalloy Powder partial size.
This nanometer of ThO2The preparation method of/Ni based high-temperature alloy composite powder:
Step 1: 1% polyethylene glycol dispersion/bonding agent being dissolved in 10% alcohol solvent and form dispersion solution, will received
Meter level enhancing particle is added in the solution, and is crushed decentralized processing 25min through high-energy ultrasonic；
Step 2: the dispersion liquid after break process in step 1 being subjected to ultrasonic agitation 40min, it is outstanding to form Nano-size Reinforced Particle
Supernatant liquid；
Step 3: the Nano-size Reinforced Particle suspension obtained and uniform is added to step 2 in nickel base superalloy spherical powder
Mixing；
Step 4: the uniformly mixed solution that step 3 is obtained carries out high-speed stirred 3h, is then dried, at sieving
Reason, can be obtained nano-oxide particles/nickel base superalloy composite spherical powder.
Embodiment 3:
A kind of nanometer Y for high energy beam 3D printing2O3/ Ni based high-temperature alloy composite spherical powder and preparation method thereof, with
Ni-base Superalloy Powder is 100% mass percentage, Y2O3Powder is 3%；Nanometer Y2O3Partial size be 50nm, Ni-based height
20 μm of temperature alloy powder diameter.
This nanometer of Y2O3The preparation method of/Ni based high-temperature alloy composite powder:
Step 1: 1% polyethylene glycol dispersion/bonding agent being dissolved in 10% alcohol solvent and forms dispersion solution, by nanometer
Grade enhancing particle is added in the solution, and is crushed decentralized processing 30min through high-energy ultrasonic；
Step 2: the dispersion liquid after break process in step 1 being subjected to ultrasonic agitation 40min, it is outstanding to form Nano-size Reinforced Particle
Supernatant liquid；
Step 3: the Nano-size Reinforced Particle suspension obtained and uniform is added to step 2 in nickel base superalloy spherical powder
Mixing；
Step 4: the uniformly mixed solution that step 3 is obtained carries out high-speed stirred 3h, is then dried, at sieving
Reason, can be obtained nano-oxide particles/nickel base superalloy composite spherical powder.
Embodiment 4:
A kind of nanometer Al for high energy beam 3D printing2O3/ Ni based high-temperature alloy composite spherical powder and preparation method thereof,
With Ni-base Superalloy Powder for 100% mass percentage, nanometer Al2O3Powder is 5%；Nanometer Al2O3Partial size be
30nm, 50 μm of Ni-base Superalloy Powder partial size.
This nanometer of Al2O3The preparation method of/Ni based high-temperature alloy composite powder:
Step 1: 2% polyethylene glycol being dissolved in 15% ethyl alcohol and forms dispersion solution, by nanoscale Al2O3Powder is added
Into the solution, mixed solution is obtained；
Step 2: the mixed solution obtained in step 1 being put into biomixer and handles 40min, then by mixed solution
It takes out；
Step 3: the mixed solution after step 2 break process being subjected to ultrasonic agitation 60min, it is outstanding to form nanoreinforcement material
Supernatant liquid；
Step 4: the nanoreinforcement material suspension obtained is added to step 3 in Ni-base Superalloy Powder and is uniformly mixed
It closes；
Step 5: the uniformly mixed solution that step 4 is obtained carries out high-speed stirred 3h, is then dried, at sieving
Reason, obtains composite powder.
Embodiment 5:
A kind of nanometer Y for high energy beam 3D printing2O3/ Ni based high-temperature alloy composite spherical powder and preparation method thereof, with
Ni-base Superalloy Powder is 100% mass percentage, nanometer Y2O3Powder is 10%；Nanoscale Y2O3Partial size be
100nm, 50 μm of Ni-base Superalloy Powder partial size.
This nanometer of Y2O3The preparation method of/Ni based high-temperature alloy composite powder:
Step 1: 5% polyethylene glycol dispersion/bonding agent being dissolved in 20% alcohol solvent and form dispersion solution, will received
Meter level enhancing particle is added in the solution, and is crushed decentralized processing 50min through high-energy ultrasonic；
Step 2: the dispersion liquid after break process in step 1 being subjected to ultrasonic agitation 70min, it is outstanding to form Nano-size Reinforced Particle
Supernatant liquid；
Step 3: the Nano-size Reinforced Particle suspension obtained and uniform is added to step 2 in nickel base superalloy spherical powder
Mixing；
Step 4: the uniformly mixed solution that step 3 is obtained carries out high-speed stirred 4h, is then dried, at sieving
Reason, can be obtained nano-oxide particles/nickel base superalloy composite spherical powder.
As depicted in figs. 1 and 2, composite spherical powder according to the present invention has nano-scale oxide enhancing distribution of particles
Feature in the surface of micrometer nickel based alloy spherical powder, using Ni-base Superalloy Powder as raw material, nano-oxide particles
For reinforcing material, polyethylene glycol is dispersion/bonding agent, and ethyl alcohol is organic solvent, passes through solution mixing, dispersion, dry preparation.
The above examples only illustrate the technical idea of the present invention, and this does not limit the scope of protection of the present invention, all
According to the technical idea provided by the invention, any changes made on the basis of the technical scheme each falls within the scope of the present invention
Within.
Claims (6)
1. a kind of nano-oxide particles for high energy beam 3D printing/nickel base superalloy composite spherical powder, feature exist
In: nano-scale oxide enhances distribution of particles in the surface of micron-size spherical Ni-base Superalloy Powder.
2. a kind of nano-oxide particles/nickel base superalloy for high energy beam 3D printing as described in claim 1 is compound
Spherical powder, it is characterised in that: for the Ni-base Superalloy Powder purity 99% or more, partial size is 20-50 μm.
3. a kind of nano-oxide particles/nickel base superalloy for high energy beam 3D printing as described in claim 1 is compound
Spherical powder, it is characterised in that: the nano-scale oxide enhancing particle uses nanometer Y2O3、ThO2Or Al2O3Powder, powder grain
Diameter is 30-100nm, and the mass fraction of addition is 1-10%.
4. a kind of nano-oxide particles/nickel base superalloy for high energy beam 3D printing as described in claim 1 is compound
The preparation method of spherical powder, it is characterised in that include the following steps:
Step 1: dispersion/bonding agent being dissolved in organic solvent and forms dispersion solution, nano-scale oxide enhancing particle is added
Decentralized processing 10-50min is crushed into the solution, and through high-energy ultrasonic；
Step 2: the dispersion liquid after break process in step 1 being subjected to ultrasonic agitation 30-70min, it is outstanding to form Nano-size Reinforced Particle
Supernatant liquid；
Step 3: the Nano-size Reinforced Particle suspension obtained is added to step 2 in spherical Ni-base Superalloy Powder and is uniformly mixed
It closes；
Step 4: then the uniformly mixed solution high-speed stirred 2-4h that step 3 is obtained is dried, sieving processing, obtains
Nano-oxide particles/nickel base superalloy composite spherical powder.
5. preparation method as claimed in claim 4, it is characterised in that: in the step 1, dispersion/bonding agent is polyethylene glycol,
The mass fraction of addition is 0.5-5%.
6. preparation method as claimed in claim 4, it is characterised in that: in the step 1, organic solvent is ethyl alcohol, addition
Mass fraction is 5-20%.
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| CN110465662A (en) * | 2019-08-09 | 2019-11-19 | 华南理工大学 | A kind of original position regulates and controls 4D Method of printing and the application of Nitinol functional characteristic |
| CN111926207A (en) * | 2020-08-27 | 2020-11-13 | 北京科技大学 | Method for preparing nickel-based alloy |
| CN111926208A (en) * | 2020-08-27 | 2020-11-13 | 北京科技大学 | Method for preparing niobium-based alloy with superfine oxide dispersed phase |
| CN112045183A (en) * | 2020-08-27 | 2020-12-08 | 湘潭大学 | Method for preparing ODS (oxide dispersion strengthened) reinforced heat-resistant aluminum alloy by adopting laser cladding forming |
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| CN112045183A (en) * | 2020-08-27 | 2020-12-08 | 湘潭大学 | Method for preparing ODS (oxide dispersion strengthened) reinforced heat-resistant aluminum alloy by adopting laser cladding forming |
| CN112063910A (en) * | 2020-08-27 | 2020-12-11 | 湘潭大学 | Method for preparing ODS ferrite-based alloy and application thereof |
| CN111926207B (en) * | 2020-08-27 | 2021-12-14 | 北京科技大学 | Method for preparing nickel-based alloy |
| CN112045183B (en) * | 2020-08-27 | 2022-12-20 | 湘潭大学 | Method for preparing ODS (oxide dispersion strengthened) heat-resistant aluminum alloy by adopting laser cladding forming |
| CN114160789A (en) * | 2021-12-09 | 2022-03-11 | 西安交通大学 | Method for enhancing performance of 3D printed metal product through surface coating of printing raw material |
| CN114959392A (en) * | 2022-06-14 | 2022-08-30 | 广东省科学院新材料研究所 | Nano titanium particle reinforced magnesium-based composite material and preparation method and application thereof |
| CN115156525A (en) * | 2022-06-22 | 2022-10-11 | 广东省科学院新材料研究所 | Active modification spherical magnesium alloy powder based on electrostatic self-assembly and preparation method and application thereof |
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