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WO2018121688A1 - 一种利用等离子体制备球形3d打印粉的方法 - Google Patents

一种利用等离子体制备球形3d打印粉的方法 Download PDF

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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
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powder
printing
spherical
plasma
metal
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French (fr)
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江民德
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • 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.

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  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
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  • Structural Engineering (AREA)
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Abstract

本发明公开了一种利用等离子体制备球形3D打印粉的方法，以金属粉、预合金粉或陶瓷粉为原料，将原料粉送入高温等离子火焰，粉末熔化成液滴，液滴在表面张力作用下成球，然后冷却得到3D打印粉末，其中等离子火焰温度为10000-30000℃，等离子体的功率为15-100KW。本发明不需要传统气体喷雾法制备的多道工序，工艺简单，效率高，无粉尘污染，制得的粉末表面为球形，流动性好，成本低。

Description

一种利用等离子体制备球形3D打印粉的方法 技术领域
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。
背景技术
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)。
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。
发明内容
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。
为实现上述目的，本发明提供如下技术方案：
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：
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℃；
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；
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，
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。
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℃。
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。
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。
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。
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。
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。
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。
优选地，所述预合金选自牙科修复用合金。
优选地，所述陶瓷粉选自金属陶瓷粉。
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。
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。
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。
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。
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。
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。
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。
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。
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。
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。
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。
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％。
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。
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。
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。
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。
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％。
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。
作为本发明进一步的方案：所述3D打印粉为钴铬钨合金粉。
本发明还提供上述3D打印粉的用途，用于3D打印工艺制品。
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。
作为本发明进一步的方案：所述制品可以是牙科修复制品。
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。
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。
与现有技术相比，本发明的有益效果是：
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。
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。
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。
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。
具体实施方式
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。
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。
实施例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。
本实施例制得的3D打印粉末呈球形，粒度组成为10-100μm。
实施例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。
本实施例制得的3D打印粉末呈球形，粒度组成为10-100μm。
实施例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。
本实施例制得的3D打印粉末呈球形，粒度组成为10-100μm。
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。
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。
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。
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。
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。

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：
    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℃；
    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；
    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，
    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。
  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℃。
  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。
    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。
    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。
    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。
    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。
    优选地，所述预合金选自牙科修复用合金。
    优选地，所述陶瓷粉选自金属陶瓷粉。
    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。
  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。
  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。
    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。
    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％。
  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。
    优选地，所述送粉氩气的纯度为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。
    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。
  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。
  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。
    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％。
    优选地，所述3D打印粉的中值粒径(D 50)为20-50μm，优选为30-40μm。
    优选地，所述3D打印粉为钴铬钨合金粉。
  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。
    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。
    优选地，所述制品是牙科修复制品。
    优选地，所述制品是零件、部件、整体设备、用具或工艺品。
    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。
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