WO2018121688A1 - 3d printing spherical powder preparation method utilizing plasma - Google Patents

3d printing spherical powder preparation method utilizing plasma Download PDF

Info

Publication number
WO2018121688A1
WO2018121688A1 PCT/CN2017/119529 CN2017119529W WO2018121688A1 WO 2018121688 A1 WO2018121688 A1 WO 2018121688A1 CN 2017119529 W CN2017119529 W CN 2017119529W WO 2018121688 A1 WO2018121688 A1 WO 2018121688A1
Authority
WO
WIPO (PCT)
Prior art keywords
powder
printing
spherical
plasma
metal
Prior art date
Application number
PCT/CN2017/119529
Other languages
French (fr)
Chinese (zh)
Inventor
江民德
Original Assignee
江民德
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 江民德 filed Critical 江民德
Publication of WO2018121688A1 publication Critical patent/WO2018121688A1/en

Links

Classifications

    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making 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
    • 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
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
    • 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
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/065—Spherical particles
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
    • C04B35/62665—Flame, plasma or melting treatment
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62695—Granulation or pelletising

Definitions

  • the invention relates to the technical field of a method for preparing a 3D printing powder, in particular to a method for preparing a spherical 3D printing powder by using plasma.
  • the method has the advantages of simple process and low energy consumption, and the prepared 3D printing powder has high purity and concentrated distribution, and the method not only improves the product quality of the 3D printing powder, but also obtains a 3D printing powder with a high sphericity. Spherical particles, loose bulk ratio, stable quality, small deformation of the product, low production cost (about 1/5-1/6 of the price of imported 3D printing powder), it is worth promoting.
  • the present invention provides the following technical solutions:
  • a method for preparing spherical 3D printing powder by using plasma comprising the following steps:
  • At least one of metal powder, prealloy powder, ceramic powder is sent to a plasma flame, plasma high temperature treatment, the temperature of the plasma flame is 10000-30000 ° C;
  • a high temperature plasma flame melts at least one of the metal powder, the prealloy powder, and the ceramic powder of the step 1) into droplets, and the molten droplets form a sphere under surface tension;
  • the spherical liquid droplets are dropped by gravity into a cooling device through which the powdered argon gas is fed, and the spherical liquid droplets are rapidly cooled under the protection of the powdered argon gas to prepare a spherical 3D printing powder; or
  • the spherical droplets are dropped into water under the action of gravity or dripped into a cooling device containing water to prepare a spherical 3D printing powder.
  • the plasma flame has a temperature of 11,000 to 29000 ° C, for example, 11,000 ° C, 12500 ° C, 15000 ° C, 18000 ° C, 20000 ° C, 25000 ° C or 29000 ° C.
  • the metal powder has a particle diameter of 20 to 100 ⁇ m; the prealloyed powder has a particle diameter of 20 to 100 ⁇ m; and the ceramic powder has a particle diameter of 20 to 100 ⁇ m.
  • the metal powder is at least one selected from the group consisting of a metal element, a metal oxide, a metal carbide, a metal nitride or a metal silicide.
  • the metal element in powder form is at least one selected from the group consisting of titanium powder, copper powder, tantalum powder, tantalum powder, molybdenum powder, tungsten powder or aluminum powder.
  • the metal oxide is at least one selected from the group consisting of calcium oxide, zirconium oxide, titanium oxide or magnesium oxide
  • the metal carbide is at least one selected from the group consisting of calcium carbide, zirconium carbide, titanium carbide or magnesium carbide
  • metal nitride And at least one selected from the group consisting of calcium nitride, zirconium nitride, titanium nitride or magnesium nitride
  • the metal silicide is at least one selected from the group consisting of calcium silicide, zirconium silicide, titanium silicide or magnesium silicide
  • the metal carbide is selected from the group consisting of At least one of calcium carbide, zirconium carbide, titanium carbide or magnesium carbide.
  • the prealloy is selected from at least one of a cobalt chromium tungsten alloy, a titanium alloy or a stainless steel alloy.
  • the prealloy is selected from at least one of a superalloy or a corrosion resistant alloy.
  • the prealloy is selected from the group consisting of dental repairing alloys.
  • the ceramic powder is selected from the group consisting of cermet powders.
  • the cermet powder is at least one selected from the group consisting of an oxide-based cermet, a carbide-based cermet, a nitride-based cermet, a boride-based cermet, and a silicide-based cermet.
  • the oxide-based ceramic powder includes, but is not limited to, an oxide composed of an oxide such as alumina, zirconia, magnesia, silica, or cerium oxide, and a composite of metal tungsten, chromium or cobalt. Base ceramic powder.
  • the carbide-based cermet includes, but is not limited to, a carbide compounded with a metal such as titanium carbide, silicon carbide, tungsten carbide or the like and a metal such as cobalt, nickel, chromium, tungsten or molybdenum.
  • a metal such as titanium carbide, silicon carbide, tungsten carbide or the like
  • a metal such as cobalt, nickel, chromium, tungsten or molybdenum.
  • Base cermet is not limited to, a carbide compounded with a metal such as titanium carbide, silicon carbide, tungsten carbide or the like and a metal such as cobalt, nickel, chromium, tungsten or molybdenum.
  • the nitride-based cermet includes, but is not limited to, a nitride, such as titanium nitride, boron nitride, silicon nitride, or tantalum nitride, as a matrix, and is compounded with a portion of the metal material.
  • a nitride such as titanium nitride, boron nitride, silicon nitride, or tantalum nitride, as a matrix, and is compounded with a portion of the metal material.
  • the boride-based cermet includes, but is not limited to, titanium boride, lanthanum boride, vanadium boride, chromium boride, zirconium boride, tungsten boride, molybdenum boride, lanthanum boride, boron
  • the boride such as bismuth is a matrix and is compounded with a part of the metal material.
  • the silicide-based cermet includes, but is not limited to, manganese silicide, iron silicide, cobalt silicide, nickel silicide, titanium silicide, zirconium silicide, tantalum silicide, vanadium silicide, tantalum silicide, tantalum silicide, molybdenum silicide, Tungsten silicide, silicon germanium or the like is a silicide matrix and is compounded with a part or a trace amount of a metal material.
  • the corrosion-resistant alloy is a conventional corrosion-resistant alloy known in the art, such as an iron-based alloy (such as a corrosion-resistant stainless steel alloy, etc.); a nickel-based alloy (such as a Ni-Cr alloy, a Ni-Cr-Mo alloy). , Ni-Cu alloy, etc.).
  • the high temperature alloy is a conventional high temperature alloy known in the art, for example, a metal material which is based on iron, nickel and cobalt and can work for a long time under a high temperature of 600 ° C and a certain stress.
  • the dental repair alloy is a conventional dental repair alloy known in the art, such as a cobalt chromium tungsten alloy, an amalgam, a gold alloy, a titanium alloy or a nickel chromium alloy.
  • step 1) at least one of the metal powder, the prealloy powder, and the ceramic powder is fed into the plasma flame by using an automatic continuous powder feeding device.
  • step 1) at least one of the metal powder, the prealloy powder, and the ceramic powder is fed into the plasma flame in an amount of 10-30 g/min, for example, 10 g/min, 15 g. /min, 20g/min, 25g/min or 30g/min.
  • the power of the plasma is between 15 and 100 kW, for example 30 kW, 40 kW or 50 kW.
  • the plasma gas is argon, and the purity of the argon gas is 99.99%.
  • the powder feeding argon gas flow rate of 0.4-1.2m 3 / h for example, 0.4m 3 /h,0.5m 3 /h,0.6m 3 /h,0.7 m 3 /h,0.8m 3 /h,0.9m 3 /h,1.0m 3 /h,1.1m 3 / h or 1.2m 3 / h.
  • the powdered argon gas can not only accelerate the cooling of the spherical droplets into a solid, but also prevent oxidation thereof.
  • the purity of the powdered argon gas is from 99.99 to 99.999%.
  • the cooling device is selected from the group consisting of stainless steel drums.
  • step 2) the powder dropped into the water may be subjected to a filtration drying heat treatment step to obtain a final spherical 3D printing powder.
  • the present invention also provides a 3D printing powder prepared by the above method.
  • the 3D printing powder has a spherical shape, and the 3D printing powder has a particle diameter of 10 to 100 ⁇ m, preferably 30 to 80 ⁇ m, for example, 30 to 50 ⁇ m.
  • the spherical 3D printing powder having a particle diameter of 10 to 100 ⁇ m has a ball formation probability of 90% to 100%.
  • the 3D printing powder has a median diameter (D 50 ) of 20 to 50 ⁇ m, preferably 30 to 40 ⁇ m.
  • the 3D printing powder is a cobalt chromium tungsten alloy powder.
  • the present invention also provides the use of the above 3D printing powder for a 3D printing process article.
  • the 3D printing powder is used for industrial production of materials having special requirements of various varieties, low yields and high melting points.
  • the article may be a dental restoration.
  • the article may be a part, a component, an integral device, an appliance or a craft, or the like.
  • the 3D printing powder is a 3D printed cobalt chrome-tungsten alloy powder, and the article is used in the field of repairing teeth and the like.
  • the invention does not require refining, deoxidation, slag formation, slag treatment, air ball formation, atomization and the like, and the spherical 3D printing powder obtained has a smooth surface, uniform distribution, no pollution, and a large loose ratio. , good mobility, is currently a spherical shape with greater advantages.
  • the invention utilizes plasma to prepare 3D printing powder, realizes simple and rapid preparation of 3D printing powder, has simple process, low energy consumption, no dust pollution, and the obtained 3D printing powder has a spherical surface, good fluidity and low cost, and is worthy of substantial Promotion.
  • the invention utilizes water to quench the prepared 3D printing powder, so that the ball forming probability of the prepared product is greatly improved, and the water cooling greatly reduces the preparation cost and improves the working efficiency for the preparation process, and is particularly suitable for multi-purpose. Industrial production of materials with special requirements for varieties, low yields and high melting points.
  • the invention is designed to be suitable for both ceramic raw materials which are not oxidized and metals and/or alloys which are difficult to be oxidized by designing different cooling treatment methods, and has wider applicability and is easier to promote and implement.
  • a method for preparing a spherical 3D printing powder by using a plasma using a prealloyed powder (titanium vanadium aluminum alloy) or a metal powder (titanium powder) as a raw material, preparing a spherical 3D printing powder by plasma,
  • the specific preparation steps are as follows: pre-alloy powder or metal powder is fed into a plasma flame, the feeding amount is 10-50 g/min, the power of the control plasma is 15 kW; the plasma gas is argon gas, and the flow rate is 2.5 m 3 /h;
  • the plasma flame is 10000-30000 ° C high temperature to melt the pre-alloy powder or metal powder into droplets (instantaneous processing time is about 0.01-0.1 s), the molten droplets form a sphere under the surface tension, and the spherical droplets are under the action of gravity.
  • the powdered argon gas introduced into the cooling device can achieve good protection against oxidation of the prepared 3D printing powder.
  • the 3D printing powder prepared in this example has a spherical shape and a particle size composition of 10-100 ⁇ m.
  • a method for preparing a spherical 3D printing powder by using a plasma, and preparing a 3D printing powder by using a cobalt chromium tungsten prealloyed powder as a raw material the specific preparation step is: pre-alloying cobalt chromium tungsten
  • the powder is fed into a plasma flame with a feed rate of 15 g/min, the plasma control power is 20 kW, the ion gas is argon gas, and the flow rate is 2-3 m 3 /h; the cobalt chromium tungsten is passed through a plasma flame at a high temperature of 10000-30000 ° C.
  • the pre-alloyed powder is melted into droplets (the instantaneous treatment time is about 0.01-0.1 s), and the molten droplets form a sphere under the surface tension, and the spherical droplets are dropped by gravity into a stainless steel bucket containing pure water. Further, the filter drying heat treatment is carried out to obtain spherical 3D-printed cobalt-chromium-tungsten powder having a ball probability of 95% or more.
  • the 3D printing powder prepared in this example has a spherical shape and a particle size composition of 10-100 ⁇ m.
  • a method for preparing a spherical 3D printing powder by using a plasma, and preparing a 3D printing powder by using titanium powder as a raw material the specific preparation step is: feeding titanium powder into a plasma flame, feeding The amount of 18g/min is controlled, the power of the plasma is 15-20kW; the ion gas is argon, the flow rate is 2.3m 3 /h; the titanium powder is melted into droplets by the high temperature of 10000-30000 ° C (preferably 15000 ° C) of the plasma flame.
  • the instantaneous treatment time is about 0.01-0.1 s
  • the molten droplets form a sphere under the action of surface tension
  • the spherical droplets are dropped by gravity into a stainless steel bucket containing pure water, and then subjected to filtration drying heat treatment.
  • a spherical 3D printed titanium powder having a ball formation probability of 95% or more was obtained.
  • the 3D printing powder prepared in this example has a spherical shape and a particle size composition of 10-100 ⁇ m.
  • the spherical 3D printing powder prepared by the multi-step process has a smooth surface, controllable particle size composition and good fluidity, and is currently a superior method for preparing spherical 3D printing powder.
  • the invention does not require refining, deoxidation, slag formation, slag treatment, air ball formation, atomization and the like, and the spherical 3D printing powder obtained has a smooth surface, uniform distribution, no pollution, and a large loose ratio. , good mobility, is currently a spherical shape with greater advantages.
  • the invention utilizes plasma to prepare 3D printing powder, realizes simple and rapid preparation of 3D printing powder, has simple process, low energy consumption, no dust pollution, and the obtained 3D printing powder has a spherical surface, good fluidity and low cost, and is worthy of substantial Promotion.
  • the spherical 3D printing powder prepared by the method of the present invention is suitable for the 3D printing technology of teeth and is suitable for the repair of teeth.

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Structural Engineering (AREA)
  • Materials Engineering (AREA)
  • Civil Engineering (AREA)
  • Composite Materials (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Plasma & Fusion (AREA)
  • Thermal Sciences (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention discloses a 3D printing spherical powder preparation method utilizing plasma, the method comprising: employing a metal powder, a pre-alloyed powder, or a ceramic powder as raw materials; feeding the raw material powders into a high-temperature plasma flame; melting the powders to provide liquid drops to form spheres by the effect of surface tension; cooling the same to obtain a 3D printing powder. The plasma flame has a temperature of 10000-30000°C, and power of 15-100 kW. The method is implemented without employing a plurality of processes in a conventional gas spray method, and is simple in process and high in efficiency, and produces no dust pollution. The powder prepared by the method has a spherical surface and favorable fluidity, and is low in cost.

Description

一种利用等离子体制备球形3D打印粉的方法Method for preparing spherical 3D printing powder by using plasma 技术领域Technical field
本发明涉及一种3D打印粉的制备方法技术领域，具体是涉及一种利用等离子体制备球形3D打印粉的方法。The invention relates to the technical field of a method for preparing a 3D printing powder, in particular to a method for preparing a spherical 3D printing powder by using plasma.
背景技术Background technique
目前，国内外使用3D打印粉时一般要求流动性非常好的球形粉末，这是因为非球形普通的粉末颗粒形状复杂，流动差，送粉不均，导致打印出来的产品质量不均。虽然目前主要有利用气体喷雾法制备此类球形粉末，但是工艺复杂，生产成本高，适用范围有限(只适用于熔点低于2000℃以下的材料)。At present, the use of 3D printing powder at home and abroad generally requires spherical powder with very good fluidity. This is because the non-spherical ordinary powder particles have a complicated shape, poor flow, and uneven powder feeding, resulting in uneven quality of printed products. Although such a spherical powder is mainly prepared by a gas spray method, the process is complicated, the production cost is high, and the scope of application is limited (only applicable to materials having a melting point below 2000 ° C).
现今的3D打印技术在各个领域广泛推广使用，优质的3D打印粉成了炙手可热的重要资源。而目前大部分的优质3D打印粉主要依赖于进口(主要是德国采用气体喷雾法生产的3D打印粉)，价格昂贵，大约在每公斤5000-6000元之间。Today's 3D printing technology is widely used in various fields, and high-quality 3D printing powder has become an important resource. At present, most of the high-quality 3D printing powder relies mainly on imports (mainly 3D printing powder produced by gas spray method in Germany), which is expensive, about 5,000-6,000 yuan per kilogram.
发明内容Summary of the invention
本发明的目的在于提供一种利用等离子体制备球形3D打印粉的方法。所述方法具有工艺简单，能耗低，制备得到的3D打印粉的纯度高，分布集中，采用所述方法不仅提高了3D打印粉的产品质量，而且得到的3D打印粉为球形度较高的球形颗粒物，松装比重大，质量稳定，产品烧结变形小，生产成本低(约为进口3D打印粉价格的1/5-1/6之间)，值得大幅推广。It is an object of the present invention to provide a method of preparing a spherical 3D printing powder using plasma. The method has the advantages of simple process and low energy consumption, and the prepared 3D printing powder has high purity and concentrated distribution, and the method not only improves the product quality of the 3D printing powder, but also obtains a 3D printing powder with a high sphericity. Spherical particles, loose bulk ratio, stable quality, small deformation of the product, low production cost (about 1/5-1/6 of the price of imported 3D printing powder), it is worth promoting.
为实现上述目的，本发明提供如下技术方案：To achieve the above object, the present invention provides the following technical solutions:
一种利用等离子体制备球形3D打印粉的方法，所述方法包括如下步骤：A method for preparing spherical 3D printing powder by using plasma, the method comprising the following steps:
1)将金属粉、预合金粉、陶瓷粉中的至少一种送入等离子火焰，进行等离子高温处理，所述等离子火焰的温度为10000-30000℃；1) at least one of metal powder, prealloy powder, ceramic powder is sent to a plasma flame, plasma high temperature treatment, the temperature of the plasma flame is 10000-30000 ° C;
2)高温等离子火焰将步骤1)的金属粉、预合金粉、陶瓷粉中的至少一种熔化成液滴，熔化的液滴在表面张力作用下形成球；2) a high temperature plasma flame melts at least one of the metal powder, the prealloy powder, and the ceramic powder of the step 1) into droplets, and the molten droplets form a sphere under surface tension;
所述球形液滴在重力作用下滴落到通有送粉氩气的冷却装置中，所述球形液滴在送粉氩气的保护作用下迅速冷却，制备得到球形3D打印粉；或者，The spherical liquid droplets are dropped by gravity into a cooling device through which the powdered argon gas is fed, and the spherical liquid droplets are rapidly cooled under the protection of the powdered argon gas to prepare a spherical 3D printing powder; or
所述球形液滴在重力作用下滴落到水中或滴落到装有水的冷却装置中，制备得到球形3D打印粉。The spherical droplets are dropped into water under the action of gravity or dripped into a cooling device containing water to prepare a spherical 3D printing powder.
作为本发明进一步的方案：步骤1)中，所述等离子火焰的温度为11000-29000℃，例如为11000℃，12500℃，15000℃，18000℃，20000℃，25000℃或29000℃。As a further aspect of the present invention, in the step 1), the plasma flame has a temperature of 11,000 to 29000 ° C, for example, 11,000 ° C, 12500 ° C, 15000 ° C, 18000 ° C, 20000 ° C, 25000 ° C or 29000 ° C.
作为本发明进一步的方案：步骤1)中，所述金属粉的粒径为20-100μm；所述预合金粉的粒径为20-100μm；所述陶瓷粉的粒径为20-100μm。As a further aspect of the present invention, in the step 1), the metal powder has a particle diameter of 20 to 100 μm; the prealloyed powder has a particle diameter of 20 to 100 μm; and the ceramic powder has a particle diameter of 20 to 100 μm.
作为本发明进一步的方案：步骤1)中，所述金属粉选自粉末形式的如下物质中的至少一种：金属单质、金属氧化物、金属碳化物、金属氮化物或金属硅化物。As a further aspect of the present invention, in the step 1), the metal powder is at least one selected from the group consisting of a metal element, a metal oxide, a metal carbide, a metal nitride or a metal silicide.
优选地，粉末形式的金属单质选自钛粉、铜粉、钽粉、铌粉、钼粉、钨粉或铝粉中的至少一种。Preferably, the metal element in powder form is at least one selected from the group consisting of titanium powder, copper powder, tantalum powder, tantalum powder, molybdenum powder, tungsten powder or aluminum powder.
优选地，金属氧化物选自氧化钙、氧化锆、氧化钛或氧化镁中的至少一种；金属碳化物选自碳化钙、碳化锆、碳化钛或碳化镁中的至少一 种；金属氮化物选自氮化钙、氮化锆、氮化钛或氮化镁中的至少一种；金属硅化物选自硅化钙、硅化锆、硅化钛或硅化镁中的至少一种；金属碳化物选自碳化钙、碳化锆、碳化钛或碳化镁中的至少一种。Preferably, the metal oxide is at least one selected from the group consisting of calcium oxide, zirconium oxide, titanium oxide or magnesium oxide; the metal carbide is at least one selected from the group consisting of calcium carbide, zirconium carbide, titanium carbide or magnesium carbide; metal nitride And at least one selected from the group consisting of calcium nitride, zirconium nitride, titanium nitride or magnesium nitride; the metal silicide is at least one selected from the group consisting of calcium silicide, zirconium silicide, titanium silicide or magnesium silicide; and the metal carbide is selected from the group consisting of At least one of calcium carbide, zirconium carbide, titanium carbide or magnesium carbide.
优选地，所述预合金选自钴铬钨合金、钛合金或不锈钢合金中的至少一种。Preferably, the prealloy is selected from at least one of a cobalt chromium tungsten alloy, a titanium alloy or a stainless steel alloy.
优选地，所述预合金选自高温合金或耐腐蚀合金中的至少一种。Preferably, the prealloy is selected from at least one of a superalloy or a corrosion resistant alloy.
优选地，所述预合金选自牙科修复用合金。Preferably, the prealloy is selected from the group consisting of dental repairing alloys.
优选地，所述陶瓷粉选自金属陶瓷粉。Preferably, the ceramic powder is selected from the group consisting of cermet powders.
优选地，所述金属陶瓷粉选自氧化物基金属陶瓷、碳化物基金属陶瓷、氮化物基金属陶瓷、硼化物基金属陶瓷、硅化物基金属陶瓷中的至少一种。Preferably, the cermet powder is at least one selected from the group consisting of an oxide-based cermet, a carbide-based cermet, a nitride-based cermet, a boride-based cermet, and a silicide-based cermet.
作为示例性地，所述氧化物基陶瓷粉包括但不限于以氧化铝、氧化锆、氧化镁、氧化硅、氧化铍等氧化物为基体，与金属钨、铬或钴复合而成的氧化物基陶瓷粉。Illustratively, the oxide-based ceramic powder includes, but is not limited to, an oxide composed of an oxide such as alumina, zirconia, magnesia, silica, or cerium oxide, and a composite of metal tungsten, chromium or cobalt. Base ceramic powder.
作为示例性地，所述碳化物基金属陶瓷包括但不限于以碳化钛、碳化硅、碳化钨等碳化物为基体，与金属钴、镍、铬、钨、钼等金属复合而成的碳化物基金属陶瓷。Illustratively, the carbide-based cermet includes, but is not limited to, a carbide compounded with a metal such as titanium carbide, silicon carbide, tungsten carbide or the like and a metal such as cobalt, nickel, chromium, tungsten or molybdenum. Base cermet.
作为示例性地，所述氮化物基金属陶瓷包括但不限于以氮化钛、氮化硼、氮化硅、氮化钽等氮化物为基体，与部分金属材料复合而成。Illustratively, the nitride-based cermet includes, but is not limited to, a nitride, such as titanium nitride, boron nitride, silicon nitride, or tantalum nitride, as a matrix, and is compounded with a portion of the metal material.
作为示例性地，所述硼化物基金属陶瓷包括但不限于以硼化钛、硼化钽、硼化钒、硼化铬、硼化锆、硼化钨、硼化钼、硼化铌、硼化铪等硼化物为基体，与部分金属材料复合而成。Illustratively, the boride-based cermet includes, but is not limited to, titanium boride, lanthanum boride, vanadium boride, chromium boride, zirconium boride, tungsten boride, molybdenum boride, lanthanum boride, boron The boride such as bismuth is a matrix and is compounded with a part of the metal material.
作为示例性地，所述硅化物基金属陶瓷包括但不限于以硅化锰、硅化铁、硅化钴、硅化镍、硅化钛、硅化锆、硅化铌、硅化钒、硅化铌、硅化钽、硅化钼、硅化钨、硅化钡等为硅化物基体，与部分或微量金属 材料复合而成。Illustratively, the silicide-based cermet includes, but is not limited to, manganese silicide, iron silicide, cobalt silicide, nickel silicide, titanium silicide, zirconium silicide, tantalum silicide, vanadium silicide, tantalum silicide, tantalum silicide, molybdenum silicide, Tungsten silicide, silicon germanium or the like is a silicide matrix and is compounded with a part or a trace amount of a metal material.
本发明中，所述耐腐蚀合金为本领域已知的常规耐腐蚀合金，例如为铁基合金(如耐腐蚀不锈钢合金等)；镍基合金(如Ni-Cr合金，Ni-Cr-Mo合金，Ni-Cu合金等)。所述高温合金为本领域已知的常规高温合金，例如为铁、镍、钴为基，能在600℃以上的高温及一定应力作用下长期工作的一类金属材料。所述牙科修复用合金为本领域已知的常规牙科修复用合金，例如为钴铬钨合金、银汞合金、金合金、钛合金或镍铬合金。In the present invention, the corrosion-resistant alloy is a conventional corrosion-resistant alloy known in the art, such as an iron-based alloy (such as a corrosion-resistant stainless steel alloy, etc.); a nickel-based alloy (such as a Ni-Cr alloy, a Ni-Cr-Mo alloy). , Ni-Cu alloy, etc.). The high temperature alloy is a conventional high temperature alloy known in the art, for example, a metal material which is based on iron, nickel and cobalt and can work for a long time under a high temperature of 600 ° C and a certain stress. The dental repair alloy is a conventional dental repair alloy known in the art, such as a cobalt chromium tungsten alloy, an amalgam, a gold alloy, a titanium alloy or a nickel chromium alloy.
作为本发明进一步的方案：步骤1)中，采用自动连续送粉装置将金属粉、预合金粉、陶瓷粉中的至少一种送入等离子火焰中。As a further aspect of the present invention, in the step 1), at least one of the metal powder, the prealloy powder, and the ceramic powder is fed into the plasma flame by using an automatic continuous powder feeding device.
作为本发明进一步的方案：步骤1)中，所述金属粉、预合金粉、陶瓷粉中的至少一种送入等离子火焰的送入量为10-30g/min，例如为10g/min、15g/min、20g/min、25g/min或30g/min。As a further aspect of the present invention, in the step 1), at least one of the metal powder, the prealloy powder, and the ceramic powder is fed into the plasma flame in an amount of 10-30 g/min, for example, 10 g/min, 15 g. /min, 20g/min, 25g/min or 30g/min.
作为本发明进一步的方案：步骤1)中，所述等离子体的功率为15-100kW，例如为30kW、40kW或50kW。所述等离子气体为氩气，所述氩气的纯度为99.99％。所述等离子气体的流量为2.0-3.0m 3/h，例如为2.0m 3/h、2.1m 3/h、2.2m 3/h、2.3m 3/h、2.4m 3/h、2.5m 3/h、2.6m 3/h、2.7m 3/h、2.8m 3/h、2.9m 3/h或3.0m 3/h。 As a further solution of the invention: in step 1), the power of the plasma is between 15 and 100 kW, for example 30 kW, 40 kW or 50 kW. The plasma gas is argon, and the purity of the argon gas is 99.99%. The plasma gas flow rate of 2.0-3.0m 3 / h, for example, 2.0m 3 /h,2.1m 3 /h,2.2m 3 /h,2.3m 3 /h,2.4m 3 /h,2.5m 3 /h,2.6m 3 /h,2.7m 3 /h,2.8m 3 /h,2.9m 3 / h or 3.0m 3 / h.
作为本发明进一步的方案：步骤2)中，所述送粉氩气的流量为0.4-1.2m 3/h，例如为0.4m 3/h、0.5m 3/h、0.6m 3/h、0.7m 3/h、0.8m 3/h、0.9m 3/h、1.0m 3/h、1.1m 3/h或1.2m 3/h。所述送粉氩气不仅可以加速使球形液滴冷却成固体，还可以防止其氧化。 As a further embodiment of the present invention: 2) in step, the powder feeding argon gas flow rate of 0.4-1.2m 3 / h, for example, 0.4m 3 /h,0.5m 3 /h,0.6m 3 /h,0.7 m 3 /h,0.8m 3 /h,0.9m 3 /h,1.0m 3 /h,1.1m 3 / h or 1.2m 3 / h. The powdered argon gas can not only accelerate the cooling of the spherical droplets into a solid, but also prevent oxidation thereof.
作为本发明进一步的方案：所述送粉氩气的纯度为99.99-99.999％。As a further aspect of the present invention, the purity of the powdered argon gas is from 99.99 to 99.999%.
作为本发明进一步的方案：步骤2)中，所述冷却装置选自不锈钢桶。As a further aspect of the invention: in step 2), the cooling device is selected from the group consisting of stainless steel drums.
作为本发明进一步的方案：步骤2)中，滴落到水中的粉末可以经过过滤烘干热处理步骤，得到最终的球形3D打印粉。As a further aspect of the present invention: in step 2), the powder dropped into the water may be subjected to a filtration drying heat treatment step to obtain a final spherical 3D printing powder.
本发明还提供一种3D打印粉，所述3D打印粉是采用上述方法制备得到的。The present invention also provides a 3D printing powder prepared by the above method.
作为本发明进一步的方案：所述3D打印粉呈球形，所述3D打印粉的粒径为10-100μm，优选为30-80μm，例如为30-50μm。As a further aspect of the present invention, the 3D printing powder has a spherical shape, and the 3D printing powder has a particle diameter of 10 to 100 μm, preferably 30 to 80 μm, for example, 30 to 50 μm.
作为本发明进一步的方案：所述粒径为10-100μm的球形3D打印粉的成球概率在90％-100％。As a further aspect of the present invention, the spherical 3D printing powder having a particle diameter of 10 to 100 μm has a ball formation probability of 90% to 100%.
作为本发明进一步的方案：所述3D打印粉的中值粒径(D 50)为20-50μm，优选为30-40μm。 As a further aspect of the present invention, the 3D printing powder has a median diameter (D 50 ) of 20 to 50 μm, preferably 30 to 40 μm.
作为本发明进一步的方案：所述3D打印粉为钴铬钨合金粉。As a further aspect of the present invention, the 3D printing powder is a cobalt chromium tungsten alloy powder.
本发明还提供上述3D打印粉的用途，用于3D打印工艺制品。The present invention also provides the use of the above 3D printing powder for a 3D printing process article.
作为本发明进一步的方案：所述3D打印粉用于多品种、少产量和高熔点的具有特种要求的材料的工业化生产。As a further aspect of the present invention, the 3D printing powder is used for industrial production of materials having special requirements of various varieties, low yields and high melting points.
作为本发明进一步的方案：所述制品可以是牙科修复制品。As a further aspect of the invention: the article may be a dental restoration.
作为本发明进一步的方案：所述制品可以是零件、部件、整体设备、用具或工艺品等。As a further aspect of the invention: the article may be a part, a component, an integral device, an appliance or a craft, or the like.
作为本发明进一步的方案：所述3D打印粉为3D打印钴铬钨合金粉，所述制品用于牙齿的修补等领域中。As a further aspect of the present invention, the 3D printing powder is a 3D printed cobalt chrome-tungsten alloy powder, and the article is used in the field of repairing teeth and the like.
与现有技术相比，本发明的有益效果是：Compared with the prior art, the beneficial effects of the present invention are:
本发明不需要精炼、脱氧、造渣、捞渣处理、鼓气成球、雾化等多道工序制取，制得的球形3D打印粉，表面光滑，分布均匀，无污染，松装比重大，流动性好，是目前具有较大优势的球形。The invention does not require refining, deoxidation, slag formation, slag treatment, air ball formation, atomization and the like, and the spherical 3D printing powder obtained has a smooth surface, uniform distribution, no pollution, and a large loose ratio. , good mobility, is currently a spherical shape with greater advantages.
本发明利用等离子体制备3D打印粉，实现了简易快速的制备3D打印粉，工艺简单，能耗低，无粉尘污染，且所得的3D打印粉表面为球形，流动性好，成本低，值得大幅推广。The invention utilizes plasma to prepare 3D printing powder, realizes simple and rapid preparation of 3D printing powder, has simple process, low energy consumption, no dust pollution, and the obtained 3D printing powder has a spherical surface, good fluidity and low cost, and is worthy of substantial Promotion.
本发明利用水对制备的3D打印粉进行急冷处理，使得制备得到的产 品的成球概率大大提高，同时水冷却对于制备工艺来说大大降低了制备成本，并提高了工作效率，特别适用于多品种、少产量和高熔点的具有特殊要求的材料的工业化的生产。The invention utilizes water to quench the prepared 3D printing powder, so that the ball forming probability of the prepared product is greatly improved, and the water cooling greatly reduces the preparation cost and improves the working efficiency for the preparation process, and is particularly suitable for multi-purpose. Industrial production of materials with special requirements for varieties, low yields and high melting points.
本发明通过设计不同的冷却处理方式，使得所述方法既适合于不发生氧化的陶瓷原料、也适合于难以被氧化的金属和/或合金，适用性更广，更易于推广和实施。The invention is designed to be suitable for both ceramic raw materials which are not oxidized and metals and/or alloys which are difficult to be oxidized by designing different cooling treatment methods, and has wider applicability and is easier to promote and implement.
具体实施方式detailed description
下面结合具体实施例，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的保护范围。此外，应理解，在阅读了本发明所公开的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本发明所限定的保护范围之内。The invention is further illustrated below in conjunction with specific embodiments. It is to be understood that the examples are merely illustrative of the invention and are not intended to limit the scope of the invention. In addition, it is to be understood that various modifications and changes may be made to the present invention without departing from the scope of the invention.
下述实施例中所使用的实验方法如无特殊说明，均为常规方法；下述实施例中所用的试剂、材料等，如无特殊说明，均可从商业途径得到。The experimental methods used in the following examples are conventional methods unless otherwise specified; the reagents, materials and the like used in the following examples are commercially available unless otherwise specified.
实施例1Example 1
本发明实施例中，一种利用等离子体制备球形3D打印粉的方法，以预合金粉(钛钒铝合金)或金属粉(钛粉)为原料，对其进行等离子体制备球形3D打印粉末，具体制备步骤为：将预合金粉或金属粉送入等离子火焰，送入量为10-50g/min，控制等离子体的功率在15kW；等离子气为氩气，流量为2.5m 3/h；通过等离子火焰的10000-30000℃高温将预合金粉或金属粉熔化成液滴(瞬时处理时间为0.01-0.1s左右)，熔化的液滴在表面张力作用下形成球，球形液滴在重力作用下滴落到通有送粉氩气(流量为0.65m 3/h)的不锈钢桶中，冷却装置中通入的送粉氩气可以很好的实现对制备得到的3D打印粉防氧化保护，得到成球概率为95％的球形3D打印粉末。 In the embodiment of the present invention, a method for preparing a spherical 3D printing powder by using a plasma, using a prealloyed powder (titanium vanadium aluminum alloy) or a metal powder (titanium powder) as a raw material, preparing a spherical 3D printing powder by plasma, The specific preparation steps are as follows: pre-alloy powder or metal powder is fed into a plasma flame, the feeding amount is 10-50 g/min, the power of the control plasma is 15 kW; the plasma gas is argon gas, and the flow rate is 2.5 m 3 /h; The plasma flame is 10000-30000 ° C high temperature to melt the pre-alloy powder or metal powder into droplets (instantaneous processing time is about 0.01-0.1 s), the molten droplets form a sphere under the surface tension, and the spherical droplets are under the action of gravity. Dropped into a stainless steel tank with powdered argon (flow rate 0.65m 3 /h), the powdered argon gas introduced into the cooling device can achieve good protection against oxidation of the prepared 3D printing powder. A spherical 3D printing powder with a ball probability of 95%.
本实施例制得的3D打印粉末呈球形，粒度组成为10-100μm。The 3D printing powder prepared in this example has a spherical shape and a particle size composition of 10-100 μm.
实施例2Example 2
本发明实施例中，一种利用等离子体制备球形3D打印粉的方法，以钴铬钨预合金粉为原料，对其进行等离子体制备3D打印粉，具体制备步骤为：将钴铬钨预合金粉送入等离子火焰，送入量为15g/min，控制等离子体的功率在20kW；离子气为氩气，流量为2-3m 3/h；通过等离子火焰的10000-30000℃高温将钴铬钨预合金粉熔化成液滴(瞬时处理时间为0.01-0.1s左右)，熔化的液滴在表面张力作用下形成球，球形液滴在重力作用下滴落到装有纯净水的不锈钢桶中，再进行过滤烘干热处理，得到成球概率为95％以上的球形3D打印钴铬钨粉。 In the embodiment of the present invention, a method for preparing a spherical 3D printing powder by using a plasma, and preparing a 3D printing powder by using a cobalt chromium tungsten prealloyed powder as a raw material, the specific preparation step is: pre-alloying cobalt chromium tungsten The powder is fed into a plasma flame with a feed rate of 15 g/min, the plasma control power is 20 kW, the ion gas is argon gas, and the flow rate is 2-3 m 3 /h; the cobalt chromium tungsten is passed through a plasma flame at a high temperature of 10000-30000 ° C. The pre-alloyed powder is melted into droplets (the instantaneous treatment time is about 0.01-0.1 s), and the molten droplets form a sphere under the surface tension, and the spherical droplets are dropped by gravity into a stainless steel bucket containing pure water. Further, the filter drying heat treatment is carried out to obtain spherical 3D-printed cobalt-chromium-tungsten powder having a ball probability of 95% or more.
本实施例制得的3D打印粉末呈球形，粒度组成为10-100μm。The 3D printing powder prepared in this example has a spherical shape and a particle size composition of 10-100 μm.
实施例3Example 3
本发明实施例中，一种利用等离子体制备球形3D打印粉的方法，以钛粉为原料，对其进行等离子体制备3D打印粉，具体制备步骤为：将钛粉送入等离子火焰，送入量18g/min，控制等离子体的功率在15-20kW；离子气为氩气，流量为2.3m 3/h；通过等离子焰的10000-30000℃(优选15000℃)高温将钛粉熔化成液滴(瞬时处理时间为0.01-0.1s左右)，熔化的液滴在表面张力作用下形成球，球形液滴在重力作用下滴落到装有纯净水的不锈钢桶中，再进行过滤烘干热处理，得到成球概率为95％以上的球形3D打印钛粉。 In the embodiment of the present invention, a method for preparing a spherical 3D printing powder by using a plasma, and preparing a 3D printing powder by using titanium powder as a raw material, the specific preparation step is: feeding titanium powder into a plasma flame, feeding The amount of 18g/min is controlled, the power of the plasma is 15-20kW; the ion gas is argon, the flow rate is 2.3m 3 /h; the titanium powder is melted into droplets by the high temperature of 10000-30000 ° C (preferably 15000 ° C) of the plasma flame. (The instantaneous treatment time is about 0.01-0.1 s), the molten droplets form a sphere under the action of surface tension, and the spherical droplets are dropped by gravity into a stainless steel bucket containing pure water, and then subjected to filtration drying heat treatment. A spherical 3D printed titanium powder having a ball formation probability of 95% or more was obtained.
本实施例制得的3D打印粉末呈球形，粒度组成为10-100μm。The 3D printing powder prepared in this example has a spherical shape and a particle size composition of 10-100 μm.
从上述实施例1-3可以看出，采用本发明所述的方法，在制备3D打印粉末的过程中不需要喷雾法、精炼、脱氧、造渣、捞渣处理、鼓气成球、雾化等多道工序制取，制得的球形3D打印粉，表面光滑，粒度组成可控， 流动性好，是目前较为优越的制备球形3D打印粉的方法。It can be seen from the above Examples 1-3 that, by the method of the present invention, no spraying, refining, deoxidation, slagging, slag treatment, air blasting, or atomization are required in the process of preparing the 3D printing powder. The spherical 3D printing powder prepared by the multi-step process has a smooth surface, controllable particle size composition and good fluidity, and is currently a superior method for preparing spherical 3D printing powder.
本发明不需要精炼、脱氧、造渣、捞渣处理、鼓气成球、雾化等多道工序制取，制得的球形3D打印粉，表面光滑，分布均匀，无污染，松装比重大，流动性好，是目前具有较大优势的球形。The invention does not require refining, deoxidation, slag formation, slag treatment, air ball formation, atomization and the like, and the spherical 3D printing powder obtained has a smooth surface, uniform distribution, no pollution, and a large loose ratio. , good mobility, is currently a spherical shape with greater advantages.
本发明利用等离子体制备3D打印粉，实现了简易快速的制备3D打印粉，工艺简单，能耗低，无粉尘污染，且所得的3D打印粉表面为球形，流动性好，成本低，值得大幅推广。The invention utilizes plasma to prepare 3D printing powder, realizes simple and rapid preparation of 3D printing powder, has simple process, low energy consumption, no dust pollution, and the obtained 3D printing powder has a spherical surface, good fluidity and low cost, and is worthy of substantial Promotion.
在上述过程当中，利用本发明方法制备的球形3D打印粉适合于牙齿的3D打印技术，适合于牙齿的修补。Among the above processes, the spherical 3D printing powder prepared by the method of the present invention is suitable for the 3D printing technology of teeth and is suitable for the repair of teeth.
以上，对本发明的实施方式进行了说明。但是，本发明不限定于上述实施方式。凡在本发明的精神和原则之内，所做的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and scope of the present invention are intended to be included within the scope of the present invention.

Claims (10)

  1. 一种利用等离子体制备球形3D打印粉的方法，其特征在于，所述方法包括如下步骤：A method for preparing a spherical 3D printing powder by using a plasma, characterized in that the method comprises the following steps:
    1)将金属粉、预合金粉、陶瓷粉中的至少一种送入等离子火焰，进行等离子高温处理，所述等离子火焰的温度为10000-30000℃；1) at least one of metal powder, prealloy powder, ceramic powder is sent to a plasma flame, plasma high temperature treatment, the temperature of the plasma flame is 10000-30000 ° C;
    2)高温等离子火焰将步骤1)的金属粉、预合金粉、陶瓷粉中的至少一种熔化成液滴，熔化的液滴在表面张力作用下形成球；2) a high temperature plasma flame melts at least one of the metal powder, the prealloy powder, and the ceramic powder of the step 1) into droplets, and the molten droplets form a sphere under surface tension;
    所述球形液滴在重力作用下滴落到通有送粉氩气的冷却装置中，所述球形液滴在送粉氩气的保护作用下迅速冷却，制备得到球形3D打印粉；或者，The spherical liquid droplets are dropped by gravity into a cooling device through which the powdered argon gas is fed, and the spherical liquid droplets are rapidly cooled under the protection of the powdered argon gas to prepare a spherical 3D printing powder; or
    所述球形液滴在重力作用下滴落到水中或滴落到装有水的冷却装置中，制备得到球形3D打印粉。The spherical droplets are dropped into water under the action of gravity or dripped into a cooling device containing water to prepare a spherical 3D printing powder.
  2. 根据权利要求1所述的利用等离子体制备球形3D打印粉的方法，其特征在于，步骤1)中，等离子火焰的温度为11000-29000℃，例如为11000℃，12500℃，15000℃，18000℃，20000℃，25000℃或29000℃。The method for preparing a spherical 3D printing powder by using the plasma according to claim 1, wherein in the step 1), the temperature of the plasma flame is 11000 to 29000 ° C, for example, 11000 ° C, 12500 ° C, 15000 ° C, 18000 ° C. , 20000 ° C, 25000 ° C or 29000 ° C.
  3. 根据权利要求1或2所述的利用等离子体制备球形3D打印粉的方法，其特征在于，步骤1)中，所述金属粉的粒径为20-100μm；所述预合金粉的粒径为20-100μm；所述陶瓷粉的粒径为20-100μm。The method for preparing a spherical 3D printing powder by plasma according to claim 1 or 2, wherein in the step 1), the metal powder has a particle diameter of 20-100 μm; and the pre-alloyed powder has a particle diameter of 20-100 μm; the ceramic powder has a particle diameter of 20 to 100 μm.
    优选地，步骤1)中，所述金属粉选自粉末形式的如下物质中的至少一种：金属单质、金属氧化物、金属碳化物、金属氮化物或金属硅化物。Preferably, in step 1), the metal powder is selected from at least one of the following substances in the form of a powder: a metal element, a metal oxide, a metal carbide, a metal nitride or a metal silicide.
    优选地，粉末形式的金属单质选自钛粉、铜粉、钽粉、铌粉、钼粉、钨粉或铝粉中的至少一种。Preferably, the metal element in powder form is at least one selected from the group consisting of titanium powder, copper powder, tantalum powder, tantalum powder, molybdenum powder, tungsten powder or aluminum powder.
    优选地，所述预合金选自钴铬钨合金、钛合金或不锈钢合金中的至少一种。Preferably, the prealloy is selected from at least one of a cobalt chromium tungsten alloy, a titanium alloy or a stainless steel alloy.
    优选地，所述预合金选自高温合金或耐腐蚀合金中的至少一种。Preferably, the prealloy is selected from at least one of a superalloy or a corrosion resistant alloy.
    优选地，所述预合金选自牙科修复用合金。Preferably, the prealloy is selected from the group consisting of dental repairing alloys.
    优选地，所述陶瓷粉选自金属陶瓷粉。Preferably, the ceramic powder is selected from the group consisting of cermet powders.
    优选地，步骤1)中，采用自动连续送粉装置将金属粉、预合金粉、陶瓷粉中的至少一种送入等离子火焰中。Preferably, in the step 1), at least one of the metal powder, the prealloy powder and the ceramic powder is fed into the plasma flame by using an automatic continuous powder feeding device.
  4. 根据权利要求1-3中任一项所述的利用等离子体制备球形3D打印粉的方法，其特征在于，步骤1)中，所述金属粉、预合金粉、陶瓷粉中的至少一种送入等离子火焰的送入量为10-30g/min，例如为10g/min、15g/min、20g/min、25g/min或30g/min。The method for preparing a spherical 3D printing powder by plasma according to any one of claims 1 to 3, wherein in the step 1), at least one of the metal powder, the prealloy powder, and the ceramic powder is sent The feed rate of the plasma flame is 10-30 g/min, for example 10 g/min, 15 g/min, 20 g/min, 25 g/min or 30 g/min.
  5. 根据权利要求1-4中任一项所述的利用等离子体制备球形3D打印粉的方法，其特征在于，步骤1)中，所述等离子体的功率为15-100kW，例如为30kW、40kW或50kW。The method for preparing a spherical 3D printing powder by plasma according to any one of claims 1 to 4, wherein in the step 1), the power of the plasma is 15-100 kW, for example, 30 kW, 40 kW or 50kW.
    优选地，所述等离子气体的流量为2.0-3.0m 3/h，例如为2.0m 3/h、2.1m 3/h、2.2m 3/h、2.3m 3/h、2.4m 3/h、2.5m 3/h、2.6m 3/h、2.7m 3/h、2.8m 3/h、2.9m 3/h或3.0m 3/h。 Preferably, the plasma gas flow rate of 2.0-3.0m 3 / h, for example, 2.0m 3 /h,2.1m 3 /h,2.2m 3 /h,2.3m 3 /h,2.4m 3 / h, 2.5m 3 /h,2.6m 3 /h,2.7m 3 /h,2.8m 3 /h,2.9m 3 / h or 3.0m 3 / h.
    优选地，所述等离子气体为氩气，所述氩气的纯度为99.99-99.999％。Preferably, the plasma gas is argon, and the purity of the argon gas is 99.99-99.999%.
  6. 根据权利要求1-5中任一项所述的利用等离子体制备球形3D打印粉的方法，其特征在于，步骤2)中，所述送粉氩气的流量为0.4-1.2m 3/h，例如为0.4m 3/h、0.5m 3/h、0.6m 3/h、0.7m 3/h、0.8m 3/h、0.9m 3/h、1.0m 3/h、1.1m 3/h或1.2m 3/h。 The method for preparing a spherical 3D printing powder by plasma according to any one of claims 1 to 5, wherein in the step 2), the flow rate of the powdered argon gas is 0.4-1.2 m 3 /h, for example, 0.4m 3 /h,0.5m 3 /h,0.6m 3 /h,0.7m 3 /h,0.8m 3 /h,0.9m 3 /h,1.0m 3 /h,1.1m 3 / h or 1.2m 3 /h.
    优选地，所述送粉氩气的纯度为99.99-99.999％。Preferably, the powdered argon gas has a purity of 99.99-99.999%.
  7. 根据权利要求1-6中任一项所述的利用等离子体制备球形3D打印粉的方法，其特征在于，步骤2)中，所述冷却装置选自不锈钢桶。The method for preparing a spherical 3D printing powder by plasma according to any one of claims 1 to 6, wherein in the step 2), the cooling device is selected from a stainless steel barrel.
    优选地，步骤2)中，滴落到水中的粉末经过过滤烘干热处理步骤，得到最终的球形3D打印粉。Preferably, in step 2), the powder dropped into the water is subjected to a filtration drying heat treatment step to obtain a final spherical 3D printing powder.
  8. 一种3D打印粉，所述3D打印粉是采用权利要求1-7中任一项所述的利用等离子体制备球形3D打印粉的方法制备得到的。A 3D printing powder prepared by the method for preparing a spherical 3D printing powder by plasma according to any one of claims 1-7.
  9. 根据权利要求8所述的3D打印粉，其特征在于，所述3D打印粉呈球形，所述3D打印粉的粒径为10-100μm，优选为30-80μm，例如为30-50μm。The 3D printing powder according to claim 8, wherein the 3D printing powder has a spherical shape, and the 3D printing powder has a particle diameter of 10 to 100 μm, preferably 30 to 80 μm, for example, 30 to 50 μm.
    优选地，所述粒径为10-100μm的球形3D打印粉的成球概率在90％-100％。Preferably, the spherical 3D printing powder having a particle diameter of 10 to 100 μm has a ball formation probability of 90% to 100%.
    优选地，所述3D打印粉的中值粒径(D 50)为20-50μm，优选为30-40μm。 Preferably, the 3D printing powder has a median diameter (D 50 ) of 20 to 50 μm, preferably 30 to 40 μm.
    优选地，所述3D打印粉为钴铬钨合金粉。Preferably, the 3D printing powder is a cobalt chromium tungsten alloy powder.
  10. 权利要求8或9所述的3D打印粉的用途，用于3D打印工艺制品。Use of the 3D printing powder of claim 8 or 9 for a 3D printing process article.
    优选地，所述3D打印粉用于多品种、少产量和高熔点的具有特种要求的材料的工业化生产。Preferably, the 3D printing powder is used for industrial production of materials with special requirements of multiple varieties, low yields and high melting points.
    优选地，所述制品是牙科修复制品。Preferably, the article is a dental restoration.
    优选地，所述制品是零件、部件、整体设备、用具或工艺品。Preferably, the article is a part, component, unitary device, appliance or handicraft.
    优选地，所述3D打印粉为3D打印钴铬钨合金粉，所述制品用于牙齿的修补领域中。Preferably, the 3D printing powder is a 3D printed cobalt chrome-tungsten alloy powder, and the article is used in the field of dental repair.
PCT/CN2017/119529 2016-12-29 2017-12-28 3d printing spherical powder preparation method utilizing plasma WO2018121688A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201611247222.9 2016-12-29
CN201611247222.9A CN106670452A (en) 2016-12-29 2016-12-29 Method for preparing spherical 3D printing powder through plasma shaping

Publications (1)

Publication Number Publication Date
WO2018121688A1 true WO2018121688A1 (en) 2018-07-05

Family

ID=58873025

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2017/119529 WO2018121688A1 (en) 2016-12-29 2017-12-28 3d printing spherical powder preparation method utilizing plasma

Country Status (2)

Country Link
CN (2) CN106670452A (en)
WO (1) WO2018121688A1 (en)

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109290585A (en) * 2018-11-07 2019-02-01 深圳市圆梦精密技术研究院 Prepare the device and preparation method thereof of spherical powder
CN110124591A (en) * 2019-05-29 2019-08-16 郑州大学 Sub-micron or nano particle cladding spherical powder and preparation method thereof
CN111085690A (en) * 2020-01-10 2020-05-01 北京矿冶科技集团有限公司 Spherical rhenium powder plasma preparation method with high powder feeding rate, spherical rhenium powder and rhenium product
CN111318717A (en) * 2020-03-23 2020-06-23 黑龙江省科学院高技术研究院 Regeneration method for recovering metal powder through 3D printing
CN112820872A (en) * 2019-11-15 2021-05-18 深圳市贝特瑞纳米科技有限公司 Ternary cathode material, preparation method thereof and lithium ion battery
CN113134616A (en) * 2021-04-19 2021-07-20 山东理工大学 Plasma preparation method of metal-based ceramic 3D printing composite powder
CN113134618A (en) * 2021-04-19 2021-07-20 山东理工大学 Metal-based ceramic 3D printing composite powder plasma preparation device
CN113927038A (en) * 2021-10-14 2022-01-14 广东省科学院新材料研究所 TiAl alloy powder for 3D printing and preparation method thereof
CN113941703A (en) * 2021-10-18 2022-01-18 合肥工业大学 Method for preparing spherical bronze powder for 3D printing through microwave heating
CN114101693A (en) * 2020-08-31 2022-03-01 厦门稀土材料研究所 Low-oxygen europium nickel powder for 3D printing and preparation method thereof
CN114247894A (en) * 2020-09-25 2022-03-29 安泰天龙钨钼科技有限公司 Method for preparing large-particle-size spherical tungsten powder by radio frequency plasma method
CN114346247A (en) * 2020-09-28 2022-04-15 广东省科学院材料与加工研究所 Wire material for preparing 3D printing alloy powder and powder preparation method
CN114653959A (en) * 2022-03-30 2022-06-24 中南大学 Spherical tantalum powder, preparation thereof and application thereof in 3D printing
CN115041699A (en) * 2022-07-22 2022-09-13 华材(山东)新材料有限公司 Production method of spherical zirconium powder for 3D printing

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3216545B2 (en) 2016-03-07 2022-09-28 Heraeus Deutschland GmbH & Co. KG Precious metal based powder and its use in the preparation of components
CN106670452A (en) * 2016-12-29 2017-05-17 江民德 Method for preparing spherical 3D printing powder through plasma shaping
CN107252894A (en) * 2017-06-15 2017-10-17 中北大学 A kind of preparation method of gear division 3D printing cobalt-based composite ceramic powder
WO2019056643A1 (en) * 2017-09-20 2019-03-28 江民德 Method for producing neodymium-iron-boron composite magnetic material
CN108941596A (en) * 2018-09-03 2018-12-07 湖南伊澍智能制造有限公司 A kind of 3D printing special alloy powder and preparation method thereof
CN109749486B (en) * 2019-01-21 2021-07-23 长沙族兴新材料股份有限公司 Method for preparing round non-floating type silver aluminum pigment
CN110102751B (en) * 2019-04-18 2021-04-30 电子科技大学 Plasma preparation technology for metal particle oxidation resistant layer
CN110449594B (en) * 2019-07-23 2022-05-24 中国航天空气动力技术研究院 Method for reducing oxygen content of titanium powder prepared by hydrogenation and dehydrogenation method
CN110845234B (en) * 2019-12-04 2021-10-29 江西科技师范大学 Spherical hollow ZrTiO4Ceramic powder and preparation method and application thereof
JP7318819B2 (en) * 2020-09-08 2023-08-01 株式会社プロテリアル Ni-based alloy powder and manufacturing method of laminate-molded product using this Ni-based alloy powder
CN114394604B (en) * 2022-01-20 2024-04-02 上海海事大学 Preparation method of superhard spherical tungsten boride powder

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3909241A (en) * 1973-12-17 1975-09-30 Gte Sylvania Inc Process for producing free flowing powder and product
US3974245A (en) * 1973-12-17 1976-08-10 Gte Sylvania Incorporated Process for producing free flowing powder and product
US4162283A (en) * 1977-12-08 1979-07-24 Swiss Aluminium Ltd. Method of melting magnetically weak particles of arbitrary shape into substantially spherically-shaped globules
CN87101648A (en) * 1987-02-27 1987-08-19 江西九江有色金属冶炼厂 Spheroidization tantalum powder and reparation technology thereof
JPH0625717A (en) * 1992-07-06 1994-02-01 Tsukishima Kikai Co Ltd Method and device for producing globular grain by high-frequency plasma
CN102672189A (en) * 2012-05-17 2012-09-19 赣州海盛钨钼集团有限公司 Preparation method of spherical tungsten powder
CN103386492A (en) * 2013-07-19 2013-11-13 江西悦安超细金属有限公司 Preparation method for superfine spherical stainless steel powder
CN105522161A (en) * 2015-12-25 2016-04-27 中国科学院重庆绿色智能技术研究院 Rapid large-scale preparing method for small-grain-size spherical powder for 3D printing
CN105537602A (en) * 2015-12-25 2016-05-04 中国科学院重庆绿色智能技术研究院 Rapid large-scale preparing method for spherical ultra-high-temperature alloy powder for 3D printing
CN105562700A (en) * 2015-12-31 2016-05-11 龙岩紫荆创新研究院 Plasma preparation method of spherical titanium powder for 3D printing
CN106670452A (en) * 2016-12-29 2017-05-17 江民德 Method for preparing spherical 3D printing powder through plasma shaping

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101269834B (en) * 2008-05-19 2011-04-06 昆明理工大学 Method for producing nano-ITO powder with plasma electrical arc one-step method
CN104066537B (en) * 2011-12-06 2016-08-31 昭荣化学工业株式会社 Metal dust manufacture plasma device and the method manufacturing metal dust
CN104084594A (en) * 2014-06-05 2014-10-08 中国科学院福建物质结构研究所 Method for preparing microfine spherical niobium powder

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3909241A (en) * 1973-12-17 1975-09-30 Gte Sylvania Inc Process for producing free flowing powder and product
US3974245A (en) * 1973-12-17 1976-08-10 Gte Sylvania Incorporated Process for producing free flowing powder and product
US4162283A (en) * 1977-12-08 1979-07-24 Swiss Aluminium Ltd. Method of melting magnetically weak particles of arbitrary shape into substantially spherically-shaped globules
CN87101648A (en) * 1987-02-27 1987-08-19 江西九江有色金属冶炼厂 Spheroidization tantalum powder and reparation technology thereof
JPH0625717A (en) * 1992-07-06 1994-02-01 Tsukishima Kikai Co Ltd Method and device for producing globular grain by high-frequency plasma
CN102672189A (en) * 2012-05-17 2012-09-19 赣州海盛钨钼集团有限公司 Preparation method of spherical tungsten powder
CN103386492A (en) * 2013-07-19 2013-11-13 江西悦安超细金属有限公司 Preparation method for superfine spherical stainless steel powder
CN105522161A (en) * 2015-12-25 2016-04-27 中国科学院重庆绿色智能技术研究院 Rapid large-scale preparing method for small-grain-size spherical powder for 3D printing
CN105537602A (en) * 2015-12-25 2016-05-04 中国科学院重庆绿色智能技术研究院 Rapid large-scale preparing method for spherical ultra-high-temperature alloy powder for 3D printing
CN105562700A (en) * 2015-12-31 2016-05-11 龙岩紫荆创新研究院 Plasma preparation method of spherical titanium powder for 3D printing
CN106670452A (en) * 2016-12-29 2017-05-17 江民德 Method for preparing spherical 3D printing powder through plasma shaping

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109290585A (en) * 2018-11-07 2019-02-01 深圳市圆梦精密技术研究院 Prepare the device and preparation method thereof of spherical powder
CN110124591A (en) * 2019-05-29 2019-08-16 郑州大学 Sub-micron or nano particle cladding spherical powder and preparation method thereof
CN112820872A (en) * 2019-11-15 2021-05-18 深圳市贝特瑞纳米科技有限公司 Ternary cathode material, preparation method thereof and lithium ion battery
CN111085690A (en) * 2020-01-10 2020-05-01 北京矿冶科技集团有限公司 Spherical rhenium powder plasma preparation method with high powder feeding rate, spherical rhenium powder and rhenium product
CN111085690B (en) * 2020-01-10 2022-11-01 北京矿冶科技集团有限公司 Spherical rhenium powder plasma preparation method with high powder feeding rate, spherical rhenium powder and rhenium product
CN111318717A (en) * 2020-03-23 2020-06-23 黑龙江省科学院高技术研究院 Regeneration method for recovering metal powder through 3D printing
CN114101693A (en) * 2020-08-31 2022-03-01 厦门稀土材料研究所 Low-oxygen europium nickel powder for 3D printing and preparation method thereof
CN114247894A (en) * 2020-09-25 2022-03-29 安泰天龙钨钼科技有限公司 Method for preparing large-particle-size spherical tungsten powder by radio frequency plasma method
CN114346247A (en) * 2020-09-28 2022-04-15 广东省科学院材料与加工研究所 Wire material for preparing 3D printing alloy powder and powder preparation method
CN113134618A (en) * 2021-04-19 2021-07-20 山东理工大学 Metal-based ceramic 3D printing composite powder plasma preparation device
CN113134616A (en) * 2021-04-19 2021-07-20 山东理工大学 Plasma preparation method of metal-based ceramic 3D printing composite powder
CN113134618B (en) * 2021-04-19 2023-01-17 山东理工大学 Metal-based ceramic 3D printing composite powder plasma preparation device
CN113927038A (en) * 2021-10-14 2022-01-14 广东省科学院新材料研究所 TiAl alloy powder for 3D printing and preparation method thereof
CN113941703A (en) * 2021-10-18 2022-01-18 合肥工业大学 Method for preparing spherical bronze powder for 3D printing through microwave heating
CN114653959A (en) * 2022-03-30 2022-06-24 中南大学 Spherical tantalum powder, preparation thereof and application thereof in 3D printing
CN114653959B (en) * 2022-03-30 2023-04-28 中南大学 Spherical tantalum powder, preparation method thereof and application thereof in 3D printing
CN115041699A (en) * 2022-07-22 2022-09-13 华材(山东)新材料有限公司 Production method of spherical zirconium powder for 3D printing

Also Published As

Publication number Publication date
CN106670452A (en) 2017-05-17
CN108247072A (en) 2018-07-06

Similar Documents

Publication Publication Date Title
WO2018121688A1 (en) 3d printing spherical powder preparation method utilizing plasma
CN104475743B (en) A kind of preparation method of superfine spherical titanium and titanium alloy powder
CN104148658B (en) One is prepared increasing material and is manufactured special Ti6Al4V alloy powder process
Antony et al. Processes for production of high-purity metal powders
CN104607823B (en) A kind of manufacture method of spherical self-melting alloy solder
CN105950947B (en) Rich iron high-entropy alloy powder body material and preparation method thereof for 3D printing
US9796022B2 (en) Pollution-free method for recycling iron-based grinding waste
CN102719708A (en) Laser-cladding high-toughness high-hardness nickel-base alloy powder and preparation method thereof
CN104084710B (en) The method for welding of titanium-based amorphous solder, its preparation method and TC4 state alloy
CN105499558B (en) A kind of spherical rhenium alloys powder and preparation method thereof, application
CN102899664A (en) Laser cladding alloy powder and preparation method thereof
CN104060300B (en) The preparation method of titanium aluminum vanadium alloy powder
CN102912188A (en) Laser cladding nickel-based alloy powder and preparation method thereof
CN109112346A (en) A kind of preparation method of increasing material manufacturing copper alloy powder
CN105463451A (en) Method for improving wear resistance and high-temperature resistance of stirring head for stirring and friction welding
CN107695338A (en) A kind of AlSi7Mg dusty materials and preparation method thereof and its application
CN102912189A (en) Laser-cladding cobalt-based alloy powder and method for preparing same
CN109759598A (en) A kind of preparation method of 3D printing GH4169 Ni-base Superalloy Powder
CN109570521A (en) The method that plasma spheroidization prepares metal powder
CN102528016A (en) Powdered alloy steel for metal injection molding and preparation method thereof
CN112981231B (en) High-manganese-nitrogen austenitic stainless steel powder and preparation method thereof
CN102674353A (en) Method for preparing spherical wolfram carbide powder
CN107671281A (en) A kind of compound BN alloy powders and its preparation method and application
CN110625127A (en) Preparation method of cobalt-chromium-nickel-tungsten alloy brazing filler metal powder
CN112662929A (en) Refractory high-entropy alloy and preparation method thereof

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 17887766

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

32PN Ep: public notification in the ep bulletin as address of the adressee cannot be established

Free format text: NOTING OF LOSS OF RIGHTS PURSUANT TO RULE 112(1) EPC (EPO FORM 1205A DATED 05.11.2019)

122 Ep: pct application non-entry in european phase

Ref document number: 17887766

Country of ref document: EP

Kind code of ref document: A1