CN108161017A - It is a kind of for metal powder of 3D printing and preparation method thereof - Google Patents

It is a kind of for metal powder of 3D printing and preparation method thereof Download PDF

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Publication number
CN108161017A
CN108161017A CN201810007084.XA CN201810007084A CN108161017A CN 108161017 A CN108161017 A CN 108161017A CN 201810007084 A CN201810007084 A CN 201810007084A CN 108161017 A CN108161017 A CN 108161017A
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metal powder
printing
powder
aerosolization
preparation
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CN108161017B (en
Inventor
李广兵
杨炽洪
杨汉波
林金才
肖海斌
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Guangdong Yin Na Science And Technology Co Ltd
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Guangdong Yin Na Science And Technology Co Ltd
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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
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F1/0003
    • 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
    • B33Y70/00Materials specially adapted for additive manufacturing
    • 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
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0844Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid in controlled atmosphere
    • 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
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0848Melting process before atomisation

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Powder Metallurgy (AREA)

Abstract

The present invention relates to a kind of preparation methods of the metal powder for 3D printing, include the following steps:S1:Simple metal silk is imported into the chamber full of the first inert gas;S2:Simple metal silk aerosolization is obtained metal powder, and be collected by the effect in the cavity through aerosolization operating voltage;S3:The metal powder being collected into is sieved, obtains screening metal powder;S4:Screening metal powder is washed and dried, obtains the metal powder for 3D printing, wherein:First purity inert gas is 99.99%, a diameter of 0.1 1.0mm of the simple metal silk.The present invention prepares metal powder by aerosolization method, and preparation process is simple, and capacity usage ratio is high;The features such as metal powder for 3D printing that this preparation method obtains can reach high sphericity, low reflecting rate, low oxygen content, particle diameter distribution is narrow, it is very suitable for 3D printing equipment.

Description

It is a kind of for metal powder of 3D printing and preparation method thereof
Technical field
The invention belongs to the technical field of 3D printing material, more particularly to a kind of metal powders and its preparation for 3D printing Method.
Background technology
3D printing dusty material is the key that restrict 3D printing technique to promote and apply, and the country is limited by powder-making technique, particulate Diameter powder prepares difficult, and powder yield is low, oxygen and other impurity content height etc., easily occurs powder fusing during 3D printing State is uneven, leads in product that oxide inclusion content is high, compactness is poor, intensity is low, structure is uneven.
At present, as 3D printing with metal powder technology of preparing mainly prepares metal powder, but prepared by this method with gas atomization Metal powder there is the defects of sphericity is low, reflecting rate is high, oxygen content is high and particle diameter distribution is wide.
Invention content
(1) technical problems to be solved
To solve the above-mentioned problems, the purpose of the present invention is to provide a kind of metal powder for 3D printing and its preparation sides Method, the metal powder for 3D printing that this preparation method obtains can reach high sphericity, low reflecting rate, low oxygen content, grain size The features such as narrowly distributing, is very suitable for 3D printing equipment.
(2) technical solution
In order to achieve the above object, the main technical schemes that the present invention uses include:
A kind of preparation method of metal powder for 3D printing, includes the following steps:
S1:Simple metal silk is imported into the chamber full of the first inert gas:
S11:Chamber is evacuated to setting vacuum degree, is filled with the first inert gas to normal pressure, then is evacuated to described set Determine vacuum degree,
S12:The first inert gas is filled with to setting pressure, and after setting aerosolization operating voltage, simple metal silk is imported Chamber;
S2:Simple metal silk aerosolization is obtained metal powder, gone forward side by side by the effect in the cavity through aerosolization operating voltage Row is collected;
S3:The metal powder being collected into is sieved, obtains screening metal powder;
S4:Screening metal powder is washed and is dried, obtains the metal powder for 3D printing,
Wherein:
Step S11 is at least recycled 3 times, and the vacuum degree that sets in step S11 is 1Pa, by the setting of the vacuum degree, The oxygen content of whole system can be efficiently reduced, conducive to the preparation of follow-up 3D printing metal powder,
The pressure that sets in step S12 as 0-1.5MPa, the aerosolization operating voltage that sets as 20-45kv, Under the pressure and operating voltage of setting, the mixture of generation micro droplets and nanometer powder after aerosolization can be made,
First purity inert gas be 99.99%, first inert gas for helium, neon, argon gas, Krypton, It is one or more in xenon, radon gas and nitrogen,
A diameter of 0.1-1.0mm of the simple metal silk.
Preferably, the metal powder is copper powder, silver powder or stainless steel powder.
Preferably, it in step S2, prepares metal powder and includes the following steps:
S21:Wire, by setpoint frequency aerosolization, forms micron order drop and nanoscale powder under aerosolization operating voltage The mixture at end;
S22:The drop condenses to form micron-size spherical metal powder through cooling gas, and is collected;
Wherein:Aerosolization setpoint frequency is 2Hz in step S21.
Preferably, it in step S3, is sieved using stainless steel, the aperture of the stainless steel sieve is 325 mesh.
Preferably, step S4 includes the following steps:
S41:It is 5-8 hours in 0.5% the second inert gas environment that metal powder, which will be sieved, and be placed on oxygen concentration, then Powder by weight:Absolute ethyl alcohol=1:5 mixing, disperse 10 minutes in 120W ultrasonic disperse equipment, stand 3 minutes and outwell Upper strata dispersion liquid leaves bottom micron particles, repeats the above process 3 times;
S42:Bottom micron particles are dried or dried, obtain the metal powder for 3D printing,
Wherein:Mixture of the metal powder for 3D printing for micron metal powder and Nano metal powder, the nanometer Metal powder is coated on a micron uranium powder surface,
Second inert gas be helium, neon, argon gas, Krypton, xenon, radon gas and nitrogen in it is one or more,
It is described dry or drying temperature be less than 80 DEG C.
Preferably, it is dispersed with carbon material in absolute ethyl alcohol.
Preferably, the carbon material is one or more in graphite, carbon nanotube, graphene.
Preferably, by weight, the dosage of the carbon material is the 0.01% of absolute ethyl alcohol dosage.
According to another aspect of the present invention, a kind of metal powder for 3D printing, the metal powder are according to above-mentioned system Preparation Method prepares gained, and the purity of the metal powder is more than 99.90%, and the grain size of the metal powder is 7.9-63.3 μm.
Further, the oxygen content of the metal powder is less than 0.076%.
(3) advantageous effect
The invention has the advantages that:
The present invention prepares metal powder by aerosolization method, and preparation process is simple, and capacity usage ratio is high;This preparation method obtains To the metal powder for 3D printing can reach high sphericity, it is non-the features such as low reflecting rate, low oxygen content, particle diameter distribution is narrow Often suitable 3D printing equipment.
Description of the drawings
Fig. 1 is scanning electron microscope (SEM) photo of 3D printing metal powder of the present invention
Specific embodiment
With reference to specific embodiment, the present invention is further explained.It should be understood that these embodiments are merely to illustrate this hair It is bright rather than limit the scope of the invention.
Embodiment 1
In the present embodiment, a diameter of 1mm of pure stainless steel wire, an aerosolization filament length is set as 20cm, the first indifferent gas Body purity is 99.99%.
A kind of preparation method of metal powder for 3D printing of the invention is as follows:
S1:Pure stainless steel wire is full of to the chamber of the first inert gas around importing,
S11:Equipment is evacuated to 1Pa, is filled with the first inert gas (nitrogen) to normal pressure, then be evacuated to 1Pa, is recycled 3 times, oxygen content is made finally to be less than 300ppm;
- filling with inert gas-is vacuumized repeatedly to vacuumize, and is in order to reduce the oxygen content in equipment, to avoid oxygen to gold Belong to the influence of powder;When oxygen content is higher than 300ppm, prepared oxygen content in power is high, can make the parts mechanics of final 3D printing Performance is not up to standard;
S12:The first inert gas is then charged with to 1.5MPa, after setting aerosolization operating voltage 45KV, by simple metal silk Import chamber;
The production of metal powder is protected using the first atmosphere of inert gases;
S2:Simple metal silk aerosolization is obtained metal powder, gone forward side by side by the effect in the cavity through aerosolization operating voltage Row is collected,
S21:Wire presses the frequency aerosolization of 2Hz under 45KV voltages, forms micron order drop and nanometer grade powder Mixture;
S22:Drop condenses to form micron-size spherical metal powder through cooling gas, and is collected;
S3:The metal powder being collected into using the stainless steel of 325 mesh is sieved, obtains screening metal powder;
S4:Screening metal powder is washed and is dried, obtains the metal powder for 3D printing,
S41:Metal powder will be sieved to be placed in the second inert gas (nitrogen) environment that oxygen concentration is 0.5% 5 hours, Then powder by weight:Absolute ethyl alcohol (dispersion liquid may be water)=1:5 mixing, divide in 120W ultrasonic disperse equipment It dissipates 10 minutes, stands 3 minutes and outwell upper strata dispersion liquid, leave bottom micron particles, repeat the above process 3 times, until upper strata is clear Washing lotion becomes clarification;
Wherein, by weight, 0.01% graphite is dispersed in absolute ethyl alcohol, helps to increase final products powder Mobility promotes print procedure;Meanwhile graphite addition can cause pulvurent carbonaceous amount too high too much, and finished product is made to become fragile;
S42:Bottom micron particles are dried or dried at 80 DEG C, obtain the metal powder for 3D printing.
The purity of obtained metal powder is more than 99.90%, and oxygen content is less than 0.076%, and grain size is 15-45 μm.
Embodiment 2
In the present embodiment, a diameter of 0.1mm of fine silver silk, one time aerosolization filament length is set as 20cm, purity inert gas It is 99.99%.
A kind of preparation method of metal powder for 3D printing of the invention is as follows:
S1:Fine silver filament winding is imported into the chamber full of the first inert gas (nitrogen and helium),
S11:Equipment is evacuated to 1Pa, is filled with the first inert gas to normal pressure, then be evacuated to 1Pa, recycles 3 times, makes Oxygen content will finally be less than 300ppm;
- filling with inert gas-is vacuumized repeatedly to vacuumize, and is in order to reduce the oxygen content in equipment, to avoid oxygen to gold Belong to the influence of powder;When oxygen content is higher than 300ppm, prepared oxygen content in power is high, can make the parts mechanics of final 3D printing Performance is not up to standard;
S12:The first inert gas is then charged with to 0.1MPa, after setting aerosolization operating voltage 20KV, by simple metal silk Import chamber;
The production of metal powder is protected using the first atmosphere of inert gases;
S2:Simple metal silk aerosolization is obtained metal powder, gone forward side by side by the effect in the cavity through aerosolization operating voltage Row is collected,
S21:Wire presses the frequency aerosolization of 2Hz under 20KV voltages, forms micron order drop and nanometer grade powder Mixture;
S22:Drop condenses to form micron-size spherical metal powder through cooling gas, and is collected;
S3:The metal powder being collected into using the stainless steel of 325 mesh is sieved, obtains screening metal powder;
S4:Screening metal powder is washed and is dried, obtains the metal powder for 3D printing,
S41:Metal powder will be sieved to be placed in the second inert gas (nitrogen and helium) environment that oxygen concentration is 0.5% 5 hours, then powder by weight:Absolute ethyl alcohol (dispersion liquid may be water)=1.5:5 mixing, in 120W ultrasonic disperses Disperse 10 minutes in equipment, stand and outwell upper strata dispersion liquid in 3 minutes, leave bottom micron particles, repeat the above process 3 times, directly Become to upper strata cleaning solution and clarify;
Wherein, by weight, 0.01% graphite and the mixture of graphene are dispersed in absolute ethyl alcohol, helps to increase Add the mobility of final products powder, promote print procedure;Meanwhile graphite addition can cause pulvurent carbonaceous amount too high too much, make Finished product becomes fragile;
S42:Bottom micron particles are dried or dried at 80 lower DEG C, obtain the metal powder for 3D printing.
The purity of obtained metal powder is more than 99.90%, and oxygen content is less than 0.076%, and grain size is 15-53 μm.
Embodiment 3
In the present embodiment, a diameter of 0.5mm of fine copper silk, one time aerosolization filament length is set as 20cm, purity inert gas It is 99.99%.
A kind of preparation method of metal powder for 3D printing of the invention is as follows:
S1:Fine copper filament winding is imported into the chamber full of the first inert gas (nitrogen, argon gas and helium),
S11:Equipment is evacuated to 1Pa, is filled with the first inert gas to normal pressure, then be evacuated to 1Pa, recycles 3 times, makes Oxygen content will finally be less than 300ppm;
- filling with inert gas-is vacuumized repeatedly to vacuumize, and is in order to reduce the oxygen content in equipment, to avoid oxygen to gold Belong to the influence of powder;When oxygen content is higher than 300ppm, prepared oxygen content in power is high, can make the parts mechanics of final 3D printing Performance is not up to standard;
S12:The first inert gas is then charged with to 0.1MPa, after setting aerosolization operating voltage 35KV, by simple metal silk Import chamber;
The production of metal powder is protected using the first atmosphere of inert gases;
S2:Simple metal silk aerosolization is obtained metal powder, gone forward side by side by the effect in the cavity through aerosolization operating voltage Row is collected,
S21:Wire presses the frequency aerosolization of 2Hz under 35KV voltages, forms micron order drop and nanometer grade powder Mixture;
S22:Drop condenses to form micron-size spherical metal powder through cooling gas, and is collected;
S3:The metal powder being collected into using the stainless steel of 325 mesh is sieved, obtains screening metal powder;
S4:Screening metal powder is washed and is dried, obtains the metal powder for 3D printing,
S41:Metal powder will be sieved and be placed on the second inert gas (nitrogen, argon gas and helium) that oxygen concentration is 0.5% 5 hours in environment, then powder by weight:Absolute ethyl alcohol (dispersion liquid may be water)=2:5 mixing, in 120W ultrasounds Disperse 10 minutes in dispersing apparatus, stand 3 minutes and outwell upper strata dispersion liquid, leave bottom micron particles, repeat the above process 3 It is secondary, until upper strata cleaning solution becomes clarification;
Wherein, by weight, 0.01% graphite and the mixture of graphene are dispersed in absolute ethyl alcohol, helps to increase Add the mobility of final products powder, promote print procedure;Meanwhile graphite addition can cause pulvurent carbonaceous amount too high too much, make Finished product becomes fragile;
S42:Bottom micron particles are dried or dried at 80 lower DEG C, obtain the metal powder for 3D printing.
The purity of obtained metal powder is more than 99.90%, and oxygen content is less than 0.076%, and grain size is 15-53 μm.
It should be noted that:
1st, under the vacuum degree set in step s 11, oxygen content that can efficiently in removing system, convenient for follow-up noble gas Process in body atmosphere;
2nd, in step S12 pressure and operating voltage setting, the mixing of micron order drop and nanometer grade powder can be obtained Object makes micron particles and nano particle exist jointly, and final product 3D printing metal powder can be made to have excellent performance, nanoscale The reflectivity of particle is very low, and the nano particle on micron powder surface can significantly reduce reflection of the metal powder surface to laser, subtract Few damage to 3D printing equipment laser.Reducing power needed for printing, (influence to laser is reflected on powder surface:Laser shines After being mapped to powder surface, if powder surface reflectivity is high, most of laser can enter optical device by backtracking, lead to light It learns device heating and generates miniature deformation, influence of this miniature deformation to laser is very big);
Voltage, frequency and grain size are not simple linear relationship.It is found after analysis of experiments, there are multiple valves for voltage Value.Wherein at a threshold values, more than this threshold values, there is no micron-sized powder in the powder of production, in another threshold values Place, after the threshold values, the powder produced is a millimeter grade particles entirely, without micron particles and nano-scale particle.At two Between threshold values, there are an optimization points, and on this aspect, the yield highest of powder, performance is best.
3rd, the first inert gas and the second inert gas can be gas of the same race or gas not of the same race, but gas purity requires to have Difference, this is to the requirement of environment oxygen content difference in different process step.Since powder is in first inert gas environment The condition of high temperature, powder easily aoxidize, therefore to purity and its sensitivity.Powder in second inert gas environment is in room temperature shape State, powder is not oxidizable, therefore no so high to the purity requirement of gas.Inert gas includes but not limited to:Helium, neon Gas, argon gas, Krypton, xenon, radon gas and nitrogen etc..
4th, the carbon material added in absolute ethyl alcohol, can play the role of increase powder mobility, in addition to graphite, Except carbon nanotube and graphene, other can play the carbon material of similar action, the material of even other materials can be used in The technical program.
5th, it as shown in Figure 1, being detected by being scanned electron microscope (SEM) to product 3D printing metal powder, finds logical The technical program is crossed, has obtained the high powder of sphericity;It can be seen that product is micron and the mixture of nano powder, while micro- Nano level powder is attached on the particle of meter level.
6th, metal powder of the present invention includes but not limited to copper powder, silver powder and stainless steel powder.
Finally it should be noted that:Above-described embodiments are merely to illustrate the technical scheme rather than to it Limitation;Although the present invention is described in detail referring to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: It can still modify to the technical solution recorded in previous embodiment or to which part or all technical features into Row equivalent replacement;And these modifications or substitutions, it does not separate the essence of the corresponding technical solution various embodiments of the present invention technical side The range of case.

Claims (10)

1. a kind of preparation method of metal powder for 3D printing, it is characterised in that:Include the following steps:
S1:Simple metal silk is imported into the chamber full of the first inert gas:
S11:Chamber is evacuated to setting vacuum degree, is filled with the first inert gas to normal pressure, then is evacuated to the setting very Reciprocal of duty cycle,
S12:The first inert gas is filled with to setting pressure, and after setting aerosolization operating voltage, simple metal silk is imported into chamber;
S2:Simple metal silk aerosolization is obtained metal powder, and received by the effect in the cavity through aerosolization operating voltage Collection;
S3:The metal powder being collected into is sieved, obtains screening metal powder;
S4:Screening metal powder is washed and is dried, obtains the metal powder for 3D printing,
Wherein:
Step S11 is at least recycled 3 times, the vacuum degree that sets in step S11 as 1Pa,
The pressure that sets in step S12 as 0-1.5MPa, the aerosolization operating voltage that sets as 20-45kv,
First purity inert gas be 99.99%, first inert gas for helium, neon, argon gas, Krypton, xenon, It is one or more in radon gas and nitrogen,
A diameter of 0.1-1.0mm of the simple metal silk.
2. the preparation method of the metal powder according to claim 1 for 3D printing, it is characterised in that:The metal powder is Copper powder, silver powder or stainless steel powder.
3. the preparation method of the metal powder according to claim 1 for 3D printing, it is characterised in that:In step S2, system Standby metal powder includes the following steps:
S21:Wire by setpoint frequency aerosolization, forms micron order drop and nanometer grade powder under aerosolization operating voltage Mixture;
S22:The drop condenses to form micron-size spherical metal powder through cooling gas, and is collected;
Wherein:Aerosolization setpoint frequency is 2Hz in step S21.
4. the preparation method of the metal powder according to claim 1 for 3D printing, it is characterised in that:In step S3, make It is sieved with stainless steel, the aperture of the stainless steel sieve is 325 mesh.
5. the preparation method of the metal powder according to claim 1 for 3D printing, it is characterised in that:Under step S4 includes State step:
S41:Metal powder will be sieved to be placed in the second inert gas environment that oxygen concentration is 0.5% 5-8 hours, then by weight Amount part compares powder:Absolute ethyl alcohol=(1-2):5 mixing, disperse 10 minutes in 120W ultrasonic disperse equipment, stand 3 minutes and outwell Upper strata dispersion liquid leaves bottom micron particles, repeats the above process 3 times;
S42:Bottom micron particles are dried or dried, obtain the metal powder for 3D printing,
Wherein:Mixture of the metal powder for 3D printing for micron metal powder and Nano metal powder, the nano metal Powder is coated on a micron uranium powder surface,
Second inert gas be helium, neon, argon gas, Krypton, xenon, radon gas and nitrogen in it is one or more,
It is described dry or drying temperature be less than 80 DEG C.
6. the preparation method of the metal powder according to claim 5 for 3D printing, it is characterised in that:In step S41, nothing Carbon material is dispersed in water-ethanol.
7. the preparation method of the metal powder according to claim 6 for 3D printing, it is characterised in that:The carbon material is It is one or more in graphite, carbon nanotube, graphene.
8. the preparation method of the metal powder for 3D printing described according to claim 6 or 7, it is characterised in that:By weight Meter, the dosage of the carbon material are the 0.01% of absolute ethyl alcohol dosage.
9. a kind of metal powder for 3D printing, it is characterised in that:The metal powder is according to claim any one of 1-8 Preparation method prepare gained, the purity of the metal powder is more than 99.90%, and the grain size of the metal powder is 7.9-63.3 μm.
10. the metal powder according to claim 9 for 3D printing, it is characterised in that:The oxygen content of the metal powder is small In 0.076%.
CN201810007084.XA 2018-01-04 2018-01-04 Metal powder for 3D printing and preparation method thereof Active CN108161017B (en)

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