WO2015109658A1 - 3d打印机用的金属粉末及其制备方法 - Google Patents

3d打印机用的金属粉末及其制备方法 Download PDF

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Publication number
WO2015109658A1
WO2015109658A1 PCT/CN2014/074722 CN2014074722W WO2015109658A1 WO 2015109658 A1 WO2015109658 A1 WO 2015109658A1 CN 2014074722 W CN2014074722 W CN 2014074722W WO 2015109658 A1 WO2015109658 A1 WO 2015109658A1
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Prior art keywords
metal powder
printer
powder
submicron
average particle
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PCT/CN2014/074722
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English (en)
French (fr)
Inventor
陈钢强
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宁波广博纳米新材料股份有限公司
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Priority to US15/113,055 priority Critical patent/US10065240B2/en
Publication of WO2015109658A1 publication Critical patent/WO2015109658A1/zh

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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
    • B22F9/082—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 atomising using a fluid
    • 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
    • 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
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • 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
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102—Metallic powder coated with organic material
    • 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
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/105—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing inorganic lubricating or binding agents, e.g. metal salts
    • 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
    • B22F1/14—Treatment of metallic powder
    • B22F1/148—Agglomerating
    • 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5873—Removal of material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/56—After-treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/10—Formation of a green body
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20—Direct sintering or melting
    • 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
    • B22F9/082—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 atomising using a fluid
    • B22F2009/084—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 atomising using a fluid combination of methods
    • 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
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/15—Nickel or cobalt
    • 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
    • B22F2302/00—Metal Compound, non-Metallic compound or non-metal composition of the powder or its coating
    • B22F2302/45—Others, including non-metals
    • 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
    • B22F2304/00—Physical aspects of the powder
    • B22F2304/05—Submicron size 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
    • B22F2304/00—Physical aspects of the powder
    • B22F2304/10—Micron size particles, i.e. above 1 micrometer up to 500 micrometer
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Definitions

  • the invention relates to the technical field of all raw materials of a 3D printer, in particular to a metal powder for a 3D printer and a preparation method thereof.
  • the metal powder is a metal powder composed of a plurality of submicron-sized metal particles having an average particle diameter of 10 to 50 ⁇ m.
  • 3D printing technology has become one of the most emerging technologies in the world. This new production approach, along with other digital production models, will drive the realization of the third industrial revolution.
  • One of the major bottlenecks that constrain the rapid development of 3D printing technology is printed materials, especially metal printed materials. R&D and production of better and more versatile metal materials is key to improving 3D printing technology.
  • various metal powders with fine particle size, uniform particle size, high sphericity, and low oxygen content are required.
  • high-end metal powders are mainly imported. Foreign manufacturers often bundle high-priced sales of raw materials and equipment, which greatly restricts the development of metal 3D printing technology in China.
  • the preparation method of the metal powder mainly includes an atomization method, a rotating electrode method, and the like.
  • the metal powder prepared by vacuum atomization has the characteristics of high sphericity, uniform composition and low oxygen content, and is widely used.
  • the average particle size of the metal powder prepared by the atomization method is limited, the average particle diameter is 10-50 ⁇ m, and the fine powder yield is low, and it has not been possible to prepare a submicron-sized metal powder by atomization.
  • the smaller the particle size of the metal powder the faster the melting rate, and the printing speed and accuracy can be improved.
  • the metal powder has a submicron particle size (particle size diameter of 100 ⁇ ⁇ to 1.0 ⁇ m)
  • the dispersibility of the metal powder is deteriorated, resulting in difficulty in transporting the metal powder, which limits the submicron metal powder in 3D printing manufacturing.
  • Applications. How to obtain a metal powder suitable for 3D printing manufacturing is one of the key issues in 3D printing technology.
  • the present invention has been made in view of the above-mentioned deficiencies of the prior art, and provides a metal powder for a 3D printer which has various advantages of submicron particles and a dispersibility and transportability of atomized metal powder.
  • the technical solution adopted by the present invention is: a metal powder for a 3D printer, which is a submicron-sized metal powder obtained by physical vapor deposition or chemical vapor deposition.
  • the metal powder has an average particle diameter of 0.1 to 3 ⁇ m; the submicron-sized metal powder having an average particle diameter of 0.1 to 3 ⁇ m is agglomerated into a metal powder for an average particle diameter of 10 to 50 ⁇ m 3D printer.
  • the metal powder type used in the above 3D printer of the present invention may be a pure metal powder or an alloy powder.
  • the invention also provides a preparation method of a metal powder for a 3D printer, and the specific preparation steps include:
  • step (3) Stir the mixed slurry in step (3) through a centrifugal spray granulator (centrifugal spray granulator or centrifugal granulation spray dryer) or a pressure spray granulator (pressure spray granulator or pressure) Spray Drying Granulator)
  • a centrifugal spray granulator centrifugal spray granulator or centrifugal granulation spray dryer
  • a pressure spray granulator pressure spray granulator or pressure
  • Spray Drying Granulator A metal powder for 3D printing having a spherical shape and an average particle diameter of 10 to 50 ⁇ m was prepared.
  • the above step (4) obtaining the average diameter of the metal powder for 3D printing can obtain the desired metal powder size by adjusting the rotational speed of the centrifugal spray or the pressure of the pressure spray and other control parameters, and the solid-liquid ratio of the slurry;
  • the pressure of the pressure spray granulator is 6-30 kg/cm 2 (ie 0.6).
  • the pressure of the pressure spray granulator is 6-30 kg/cm 2 (ie 0.6).
  • the process parameters involved in the above two granulation machines ie the operating parameters (ie the operating parameters applicable to both the pressure spray granulator and the centrifugal spray granulator) can be controlled at:
  • the inlet temperature of the dry air is 200-350 °C, the outlet temperature of dry air is 80-150 °C ;
  • the flow rate of dry air is 100-300 Nm 3 /h (the standard hour is the volume flow under standard conditions);
  • the feed rate of the pressure spray granulator or the centrifugal spray granulator is 5-20 kg/h.
  • the submicron-sized metal powder according to the step (1) of the present invention has an average particle diameter of 0.5 to 2 ⁇ m, and the metal powder having the particle diameter is used for the agglomeration process of the granulation process, which is more advantageous for each submicron metal.
  • the powders are agglomerated with each other and the structure is more stable.
  • the metal powder for the 3D printer according to the step (4) of the present invention has an average particle diameter of 20 to 30 ⁇ m, and the use of the metal powder of the particle size range is more advantageous for application on a 3D printer.
  • the metal powder of the present invention may be a pure metal powder such as titanium, nickel or copper, or a nickel-based alloy powder such as NiCr21Fel8Mo9, NiCrl9Nb5Mo3 or the like; a titanium-based alloy powder such as Ti6A14V; an aluminum-based alloy powder, for example Al-SilOMg, A1SU2, etc.; Fe-based alloy powders, such as GP1-stainless steel, 316 L, etc., and other metal powders that can be used for 3D printing, such as Co28Cr6Mo, CoCr-2LC.
  • a pure metal powder such as titanium, nickel or copper, or a nickel-based alloy powder such as NiCr21Fel8Mo9, NiCrl9Nb5Mo3 or the like
  • a titanium-based alloy powder such as Ti6A14V
  • an aluminum-based alloy powder for example Al-SilOMg, A1SU2, etc.
  • Fe-based alloy powders such as GP1-stain
  • the liquid described in the above step (2) of the present invention may be water, ethanol or other organic solution (e.g., isopropanol, methanol, etc.).
  • the above organic binder of the present invention such as polyvinyl alcohol, ethyl cellulose or special metal ore powder granulation binder, etc. (such as the model produced by Baoding Jingsu Biotechnology Co., Ltd.: HY-1 metallurgical ore powder)
  • Pellet adhesive model:
  • the metal powder for a 3D printer of the present invention is obtained by agglomerating a submicron-sized metal powder having a particle diameter of 0.1 to 3 ⁇ m into a metal powder having an average particle diameter of 10 to 50 ⁇ m by a granulation process, not a a complete integrated metal powder, but a plurality of submicron metal powders are bonded to each other.
  • the metal powder for the 3D printer has various advantages of submicron particles (such as high sphericity, Uniform composition, low oxygen content, and dispersibility and transportability of atomized metal powder, thus solving the problem of dispersion and transportation of submicron metal powder in 3D printing, making submicron metal powder in 3D
  • submicron particles such as high sphericity, Uniform composition, low oxygen content, and dispersibility and transportability of atomized metal powder
  • the metal powder slurry having a small solid-liquid ratio can obtain a smaller metal powder at the same centrifugal spray rotation speed or the same pressure spray pressure, because at the same rotation speed, the discharge is performed.
  • the droplet diameter is equivalent, because the metal powder content in the droplet is small, the droplet is dried, and less metal powder is shrunk into a smaller diameter metal powder. Therefore, the solid-liquid ratio of 0.25-2.0 is successfully selected in the present invention.
  • the technical effect of preparing the above metal powder having an average diameter of 10 to 50 micrometers is achieved. By this granulation method, a powder smaller than the atomized metal powder can be obtained.
  • the metal powder is then passed through a screening machine to remove un-agglomerated loose powder and oversized powder to obtain a metal powder of the desired size.
  • This metal powder has various advantages of submicron particles and dispersibility and transportability of atomized metal powder, enabling submicron metal powders to be used in existing 3D printing equipment.
  • Figure 1 Scanning electron micrograph of submicron metal powder.
  • Figure 3 Scanning electron micrograph of copper-based alloy powder with an average particle size of 1.0 ⁇ m.
  • Figure 4. Scanning electron micrograph of copper-based alloy powder with an average particle size of 40 microns.
  • Figure 5 Scanning electron micrograph of titanium-based alloy powder with an average particle size of 0.5 ⁇ m.
  • Figure 7 Scanning electron micrograph of nickel-based alloy powder with an average particle size of 0.25 ⁇ m.
  • Figure 8 Scanning electron micrograph of a nickel-based alloy powder with an average particle size of 30 microns.
  • Figure 9 Scanning electron micrograph of pure metal nickel powder with an average particle size of 0.5 ⁇ m.
  • Figure 10 Scanning electron micrograph of pure metal nickel powder with an average particle size of 40 microns.
  • the equipment involved in the invention such as a pressure spray granulator or a centrifugal spray granulator, is a commercially available product, and the specific working principle is as follows: the feed liquid is input through a pump, sprays a mist droplet, and then the same hot air (dry air) The cocurrent flow is reduced, the powder particles are collected by the bottom discharge port, the exhaust gas and its tiny powder are separated by a cyclone, the exhaust gas is discharged by the exhaust fan, and the powder is collected by the powder cylinder disposed at the lower end of the cyclone, and the fan outlet can also be Equipped with a secondary dust removal device, the pressure, flow rate, and orifice size are adjusted according to product specifications to obtain the desired spherical particles in a certain proportion.
  • Physical vapor deposition method The copper-based alloy as a raw material is dissolved in the crucible, and the gas (hydrogen, argon, nitrogen, etc.) enters from the inlet pipe in the plasma transfer arc torch, is plasmaized by the external power source, and A plasma transfer arc is generated between the plasma transfer arc torches (ie, the lower end of the plasma transfer arc generated by the plasma transfer arc torch is connected to the metal liquid surface in the crucible); the metal is evaporated and vaporized by the plasma transfer arc; Adding a room temperature inert gas or nitrogen to the metal vapor at a high speed through a polycooling pipe to reduce the temperature of the metal vapor to
  • a copper-based alloy powder having an average particle diameter of 1.0 ⁇ m is obtained (Fig. 3) (the above physical vapor deposition method is a conventional method in the industry, which is described in detail in this step); and then a solid-liquid ratio of 1.5:1 is prepared with ethanol.
  • the weight of the organic binder polyvinyl alcohol
  • the metal powder slurry was prepared into a spherical metal powder by a centrifugal spray granulator.
  • the rotational speed of the centrifugal spray granulator was controlled at 12,000 rpm, the inlet temperature of the dry air of the centrifugal spray granulator was 200 ° C, the outlet temperature was 90 ° C, and the dry air flow rate was 220 Nm 3 /h.
  • the metal powder slurry was fed at a rate of 12 kg/h.
  • the dry granulated metal powder was collected by a cyclone, and the ultrafine metal powder was collected through a filter bag.
  • the metal powder collected by the cyclone was classified by a shaker to obtain a metal powder having an average particle diameter of 40 ⁇ m (Fig. 4).
  • the metal powder collected in the filter bag and the metal powder separated by the sieve are recovered and prepared into a metal powder slurry.
  • Example 2 A titanium-based alloy powder having an average particle diameter of 0.5 ⁇ m (Fig. 5) produced by physical vapor deposition, and a metal powder slurry having a solid-liquid ratio of 2:1.
  • the weight of the organic binder (ethyl cellulose) was 1.5% by weight of the solid.
  • the metal powder slurry was prepared into a spherical metal powder by a centrifugal spray granulator. The speed of the centrifugal spray granulator is controlled at
  • the inlet temperature of dry air is 350 ° C
  • the outlet temperature is 120 ° C
  • the dry air flow rate is 250 Nm 3 /h.
  • the metal powder slurry was fed at a rate of 10 kg/h.
  • the dry granulated metal powder was collected by a cyclone, and the ultrafine metal powder was collected through a filter bag.
  • the metal powder collected by the cyclone was classified by a shaker to obtain a metal powder having an average particle diameter of 45 ⁇ m (Fig. 6).
  • the metal powder collected in the filter bag and the metal powder separated by the sieve are recovered and prepared into a metal powder slurry.
  • the weight of the organic binder (manufactured by Baoding Jingsu Biotechnology Co., Ltd.: HY-1 metallurgical ore fines binder) is 1.5% by weight of solids.
  • the metal powder slurry was prepared into a spherical metal powder by a centrifugal spray granulator.
  • the rotation speed of the centrifugal spray was controlled at 25,000 rpm, the inlet temperature of the dry air was 200 ° C, the outlet temperature was 90 ° C, and the dry air flow rate was 220 Nm 3 /h.
  • the metal powder slurry was fed at a rate of 10 kg/h.
  • the dry granulated metal powder was collected by a cyclone, and the ultrafine metal powder was collected through a filter bag.
  • the metal powder collected by the cyclone was classified by a shaker to obtain a metal powder having an average particle diameter of 30 ⁇ m (Fig. 8).
  • the metal powder collected in the filter bag and the metal powder separated by the sieve are recovered and prepared into a metal powder slurry.
  • Pure metal nickel powder (Fig. 9) having an average particle diameter of 0.5 ⁇ m produced by physical vapor deposition was prepared, and a metal powder slurry having a solid-liquid ratio of 1.5:1 was prepared with methanol.
  • the weight of the organic binder was 1.0% by weight of the solid.
  • the metal powder slurry was prepared into a spherical metal powder by a pressure spray granulator. The pressure of the pressure spray was controlled at 15 kg/cm 2 , the inlet temperature of the dry air was 250 ° C, the outlet temperature was 95 ° C, and the dry air flow rate was 250 Nm 3 /h.
  • the metal powder slurry was fed at a rate of 12 kg/h.
  • the dry granulated metal powder was collected by a cyclone, and the ultrafine metal powder was collected through a filter bag.
  • the metal powder collected by the cyclone was classified by a shaker to obtain a metal powder having an average particle diameter of 40 ⁇ m (Fig. 10).
  • the metal powder collected in the filter bag and the metal powder separated by the sieve are recovered and prepared into a metal powder slurry.
  • the metal powder for the 3D printer prepared in the above embodiment can be seen from the drawings, the structure is not a complete integrated metal powder, but a plurality of submicron metal powders are bonded and agglomerated with each other, therefore,
  • the metal powder for the 3D printer has various advantages of submicron particles (such as high sphericity, uniform composition, low oxygen content), and dispersibility and transportability of atomized metal powder.
  • the 3D printer prepared by the above embodiment uses metal powder for 3D printing, and the 3D printer uses metal powder to be sprayed onto the heating model table in the protective chamber of the protective gas through the nozzle of the 3D printer to form a layer by layer to form a 3D printing.
  • the product has the advantages of good dispersibility in the nozzle spraying process and smooth metal powder transportation. In the layer-by-layer printing process, the contact area of each layer of metal powder at the junction is sufficiently ensured to be bonded and fastened.

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Abstract

一种3D打印机用的金属粉末，是由许多亚微米级的金属颗粒通过造粒工艺团聚成10-50微米的金属粉末。由于该金属粉末是由亚微米金属颗粒组合，它的熔点低、熔融速度快，可以提高金属3D打印机的打印速度以及打印构件的精度。同时金属粉末的平均粒径又与现有的3D打印机用的雾化金属粉相当，具有良好的分散性和输送性，可以适用于现有的3D打印机设备。

Description

说 明 书
3D打印机用的金属粉末及其制备方法
技术领域：
本发明涉及 3D打印机所有原料技术领域，具体涉及一种用于 3D打印机的金属粉末 及其制备方法。 该金属粉末是由许多亚微米级的金属粒子组成的平均粒径为 10-50微米 的金属粉末。
背景技术：
3D打印技术目前已成为全球最关注的新兴技术之一。这种新型的生产方式与其他数 字化生产模式一起将推动第三次工业革命的实现。制约 3D 打印技术迅速发展的其中一 大瓶颈是打印材料， 特别是金属打印材料。 研发和生产性能更好和通用性更强的金属材 料是提升 3D打印技术的关键。 在高性能金属构件直接采用 3D打印技术制造方面， 需 要粒径细、 粒径均匀、 高球形度、 低氧含量的各类金属粉末。 目前高端的金属粉末主要 依赖进口。 而国外厂商常将原材料与设备捆绑高价销量， 极大地制约了我国的金属 3D 打印技术的发展。
金属粉末的制备方法主要有雾化法、 旋转电极法等。 其中采用真空雾化法制备的金 属粉末具有球形度高、 成分均匀、 氧含量低等特点， 受到广泛应用。 雾化法制备的金属 粉末的平均粒径受到限制， 平均粒径在 10-50微米， 并且细粉得率低， 目前还无法采用 雾化法来制备亚微米级金属粉末。 一般来讲， 金属粉末粒径越小， 熔融速度越快， 可以 提高打印速度和精度。但当金属粉末粒径达到亚微米级 (粒度直径 1 00ηΓΠ〜1 .0μ m)时， 金属粉末的分散性变差， 导致金属粉末输送困难， 限制了亚微米级的金属粉末在 3D打 印制造中的应用。 如何获得一种适合于 3D打印制造中的金属粉是 3D打印技术的关键 问题之一。
发明内容：
本发明针对现有技术的上述不足， 提供一种使金属粉末既具有亚微米粒子的各种优 点， 又具有雾化金属粉末的分散性和输送性的 3D打印机用的金属粉末。
为了解决上述技术问题， 本发明采用的技术方案为： 一种 3D打印机用的金属粉末， 该金属粉末为先采用物理气相沉积法或化学气相沉积法制备亚微米级金属粉末，所得的 亚微米级金属粉末的平均粒径为 0.1-3微米；该平均粒径为 0.1-3微米的亚微米级金属粉 末通过造粒团聚成平均粒径 10-50微米 3D打印机用的的金属粉末。
本发明上述的 3D打印机用的金属粉末种类可以是纯金属粉或合金粉。 本发明还提供一种 3D打印机用的金属粉末的制备方法， 具体制备步骤包括：
( 1 ) 先采用物理气相沉积法或化学气相沉积法制备出亚微米级金属粉末， 所得的 亚微米级金属粉末的平均粒径为 0.1-3微米；
(2) 将步骤 （1 ) 所得的平均粒径为 0.1-3微米的亚微米级金属粉末与液体混合、 配制成金属粉浆料； 上述金属粉浆料的亚微米级金属粉末与液体的重量比（即固液重量 比） 为 0.25-2.0:1 ;
(3 )在步骤（2)所得的金属粉浆料中加入亚微米级金属粉末（固体）重量 0.1-10% 的有机粘合剂， 搅拌混合均匀；
( 4)将步骤（3 )搅拌混合均匀的浆料通过离心喷雾造粒机（离心喷雾造粒器或称 离心造粒喷雾干燥机） 或压力喷雾造粒机 （压力喷雾造粒器或称压力喷雾干燥造粒机） 制备成球形、 平均粒径为 10-50微米的 3D打印用的金属粉末。
上述步骤 （4) 3D打印用的金属粉末的平均直径的获得可以通过调节离心喷雾的转 速或压力喷雾的压力和其他控制参数以及浆料的固液比等得到所需的金属粉末大小； 为 了实现上述粒径的产品， 本发明步骤 （4 ) 所述的离心喷雾造粒机的转速控制在 10000-40000转 /分； 压力喷雾造粒机的压力为 6-30kg/cm2 (即 0. 6-3兆帕）； 对上述二 种造粒机器涉及到的工艺参数即操作参数（即压力喷雾造粒机和离心喷雾造粒机均适用 的操作参数） 可控制在： 干燥空气的进口温度为 200-350 °C、 干燥空气的出口温度为 80-150°C ;干燥空气的流量为 100-300 Nm3/h (标方每小时即指标准状况下的体积流量）； 金属粉浆料在压力喷雾造粒机或离心喷雾造粒机的进料速度为 5-20kg/h。
作为优选， 本发明步骤（1 )所述的亚微米级金属粉末的平均粒径为 0.5-2微米， 采 用该粒径的金属粉， 再进行造粒工艺团聚过程， 更利于各亚微米级金属粉末彼此之间的 团聚， 结构更加稳固。
作为优选， 本发明步骤（4)所述的 3D打印机用的金属粉末其平均粒径为 20-30微 米， 采用该粒径范围的金属粉末， 更利于在 3D打印机上的应用。
作为优选， 本发明所述的金属粉末可以为钛、镍、铜等纯金属粉， 也可以是镍基合金粉， 例如 NiCr21Fel8Mo9 、 NiCrl9Nb5Mo3等； 钛基合金粉， 例如 Ti6A14V ； 铝基合金 粉， 例如 Al-SilOMg 、 A1SU2等； 铁基合金粉， 例如 GP1-不锈钢、 316 L等以及可用 于 3D打印的其他金属粉， 例如 Co28Cr6Mo 、 CoCr-2LC 。
本发明上述步骤 （2) 中所述的液体可以是水、 乙醇或者其他有机溶液 （如异丙醇， 甲醇等）。 本发明上述的有机粘合剂如聚乙烯醇、 乙基纤维素或者专用的金属矿粉造粒粘合剂 等 （如保定京素生物科技有限公司生产的型号为： HY-1的冶金矿粉球团粘合剂、 型号：
G-S的钢渣粉球团粘合剂等）。
本发明的优点和有益效果：
1.本发明 3D打印机用的金属粉末， 采用的是将亚微米级（粒径为 0.1-3微米）金属 粉末通过造粒工艺团聚成平均粒径 10-50微米的金属粉末而成， 不是一个完整的一体化 的金属粉末， 而是有多个亚微米级的金属粉末彼此粘结团聚而成， 因此， 该 3D打印机 用的金属粉末既具有亚微米粒子的各种优点 （如球形度高、 成分均匀、 氧含量低）， 又 具有雾化金属粉末的分散性和输送性， 因此， 解决了亚微米级金属粉末在 3D打印中分 散和输送困难的问题， 使亚微米级的金属粉末在 3D 打印技术中的应用成为可能， 本发 明的实施使得 3D 打印技术得到进一步的发展。
2.本发明 3D打印机用的金属粉末的制备方法， 采用在金属粉浆料里添加固体重量 0.1-5 %的有机粘合剂， 金属粉浆料通过离心喷雾造粒机、压力喷雾造粒机或其他造粒设 备制备成球形状的、 平均直径在 10-50微米的金属粉末工艺。 金属粉末的平均直径可以 通过调节离心喷雾的转速或压力喷雾的压力以及浆料的固液比得到所需的金属粉末大 小。 特别是调节浆料的固液比， 可以得到较小的金属粉末。 经过本发明实验可得在相同 的离心喷雾的转速下或相同的压力喷雾的压力下， 固液比小的金属粉浆料可以得到较小 金属粉末， 这是因为在相同的转速下， 喷出的液滴直径相当， 由于在液滴中的金属粉粒 含量少， 液滴经过干燥， 较少的金属粉粒收缩成较小直径的金属粉末因此， 本发明选用 0.25-2.0的固液比成功实现制备上述平均直径在 10-50微米金属粉体的技术效果。 通过 这种造粒方法， 可以得到比雾化的金属粉更小的粉末。 然后金属粉末通过分筛机， 除去 未成团的散粉和超大的粉团， 得到所需大小的金属粉末。 这种金属粉末既具有亚微米粒 子的各种优点， 又具有雾化金属粉末的分散性和输送性， 能够使亚微米的金属粉在现有 3D打印设备得到应用。
附图说明
图 1 亚微米级金属粉末的扫描电镜图。
图 2 3D打印机用的金属粉末 （I) 扫描电镜图。
图 3 平均粒径 1.0微米的铜基合金粉扫描电镜图。
图 4 平均粒径 40微米的铜基合金粉末扫描电镜图。 图 5 平均粒径 0.5微米的钛基合金粉扫描电镜图。
图 6 平均粒径 45微米的钛基合金粉末扫描电镜图。
图 7 平均粒径 0.25微米的镍基合金粉扫描电镜图。
图 8 平均粒径 30微米的镍基合金粉末扫描电镜图。
图 9 平均粒径 0.5微米的纯金属镍粉扫描电镜图。
图 10 平均粒径 40微米的纯金属镍粉末扫描电镜图。
图 11 3D打印机用的金属粉末 （II) 扫描电镜图。
具体实 51^式
下面通过实施例进一步详细描述本发明， 但本发明不仅仅局限于以下实施例。 本发明涉及到的设备如压力喷雾造粒机或离心喷雾造粒机等均为市售产品，具体工 作原理为： 料液通过泵输入， 喷出雾状液滴， 然后同热空气 （干燥空气） 并流下降， 粉 粒由塔底排料口收集， 废气及其微小粉末经过旋风分离器分离， 废气由抽风机排出， 粉 末由设在旋风分离器下端的粉筒收集， 风机出口处还可装备二级除尘装置， 按产品规格 要求调节压力、 流量、 喷孔的大小， 得到所需的按一定大小比例的球形颗粒。
实施例 1
采用物理气相沉积法： 将作为原料的铜基合金在坩埚中溶解， 气体 （氢气、 氩气、 氮气等）从等离子体转移弧炬中的进气管进入、 通过外加电源被等离子化， 在坩埚和等 离子体转移弧炬之间产生等离子体转移弧（即等离子体转移弧炬产生的等离子体转移弧 下端与坩埚中的金属液面相接）； 金属通过等离子体转移弧被蒸发、 汽化； 金属蒸气通 过聚冷管道， 将室温的惰性气体或氮气高速加入到金属蒸气中， 使金属蒸气温度降到
30CTC以下， 得到平均粒径为 1.0微米的铜基合金粉 (图 3) (上述物理气相沉积法为行业 常规方法， 在此步骤详细赘述）； 然后与乙醇配成固液比为 1.5:1的金属粉浆料。 有机粘 合剂 （聚乙烯醇） 的重量为固体重量的 2%。 通过离心喷雾造粒器把金属粉浆料制备成 球形状的金属粉末。离心喷雾造粒器的转速控制在 12000转 /分，离心喷雾造粒器的干燥 空气的进口温度为 200 °C， 出口温度为 90°C， 干燥空气流量为 220Nm3/h。 金属粉浆料 的进料速度为 12kg/h。 干燥造粒后的金属粉末通过旋风器收集， 超细的金属粉末通过滤 袋收集。 旋风器收集的金属粉末用振动筛分级， 得到平均粒径为 40微米的金属粉末 (图 4)。 滤袋收集的金属粉末和分筛踢除的金属粉末回收再制备成金属粉浆料。
实施例 2: 采用物理气相沉积法生产的平均粒径为 0.5微米的钛基合金粉 (图 5)，与水配成固液 比为 2:1的金属粉浆料。有机粘合剂（乙基纤维素）的重量为固体重量的 1.5 %。通过离 心喷雾造粒器把金属粉浆料制备成球形状的金属粉末。 离心喷雾造粒机的转速控制在
12000 转 /分， 干燥空气的进口温度为 350°C， 出口温度为 120°C， 干燥空气流量为 250Nm3/h。 金属粉浆料的进料速度为 10kg/h。 干燥造粒后的金属粉末通过旋风器收集， 超细的金属粉末通过滤袋收集。 旋风器收集的金属粉末用振动筛分级， 得到平均粒径为 45微米的金属粉末 (图 6)。 滤袋收集的金属粉末和分筛踢除的金属粉末回收再制备成金 属粉浆料。
实施例 3:
采用物理气相沉积法生产的平均粒径为 0.25微米的镍基合金粉 (图 7)， 与乙醇配成 固液比为 1:1的金属粉浆料。 有机粘合剂 （保定京素生物科技有限公司生产的型号为： HY-1的冶金矿粉球团粘合剂） 的重量为固体重量的 1.5 %。 通过离心喷雾造粒器把金属 粉浆料制备成球形状的金属粉末。离心喷雾的转速控制在 25000转 /分，干燥空气的进口 温度为 200°C， 出口温度为 90°C， 干燥空气流量为 220Nm3/h。 金属粉浆料的进料速度 为 10kg/h。 干燥造粒后的金属粉末通过旋风器收集， 超细的金属粉末通过滤袋收集。 旋 风器收集的金属粉末用振动筛分级， 得到平均粒径为 30微米的金属粉末 (图 8)。 滤袋收 集的金属粉末和分筛踢除的金属粉末回收再制备成金属粉浆料。
实施例 4:
采用物理气相沉积法生产的平均粒径为 0.5微米的纯金属镍粉 (图 9)，与甲醇配成固 液比为 1.5:1的金属粉浆料。有机粘合剂的重量为固体重量的 1.0%。通过压力喷雾造粒 器把金属粉浆料制备成球形状的金属粉末。压力喷雾的压力控制在 15kg/cm2， 干燥空气 的进口温度为 250°C， 出口温度为 95°C， 干燥空气流量为 250Nm3/h。 金属粉浆料的进 料速度为 12kg/h。干燥造粒后的金属粉末通过旋风器收集， 超细的金属粉末通过滤袋收 集。 旋风器收集的金属粉末用振动筛分级， 得到平均粒径为 40微米的金属粉末 (图 10)。 滤袋收集的金属粉末和分筛踢除的金属粉末回收再制备成金属粉浆料。
上述实施例制备的 3D打印机用金属粉末， 从附图可以得知， 其结构不是一个完整 的一体化的金属粉末，而是有多个亚微米级的金属粉末彼此粘结团聚而成， 因此，该 3D 打印机用的金属粉末既具有亚微米粒子的各种优点（如球形度高、成分均匀、氧含量低）， 又具有雾化金属粉末的分散性和输送性。 将上述实施例制备的 3D打印机用金属粉末用于 3D打印， 3D打印机用金属粉末通 过 3D打印机的喷嘴喷撒到具有防护性气体的防护室中的加热模型工作台上逐层打印， 形成 3D打印产品； 在喷嘴喷撒过程具有分散性好， 金属粉末输送顺利的优点， 在逐层 打印过程充分保证相接处的每层金属粉末的接触面积增大， 粘结紧固。

Claims

权利 要求 书
1.一种 3D打印机用的金属粉末， 其特征在于： 该金属粉末为先采用物理气相沉积 法或化学气相沉积法制备成平均粒径为 0.1-3微米的亚微米级金属粉末， 该平均粒径为 0.1-3微米的金属粉末通过造粒团聚成平均粒径 10-50微米 3D打印机用的的金属粉末。
2.根据权利要求 1所述的 3D打印机用的金属粉末， 其特征在于： 所述的金属粉末 为纯金属粉或合金粉。
3.根据权利要求 1所述的 3D打印机用的金属粉末， 其特征在于： 所述的亚微米级 金属粉末的平均粒径为 0.5-2微米； 所述的 3D打印机用的金属粉末其平均粒径为 20-30 微米。
4.一种 3D打印机用的金属粉末的制备方法， 其特征在于： 具体制备步骤包括：
( 1 ) 先采用物理气相沉积法或化学气相沉积法制备出亚微米级金属粉末， 所得的 亚微米级金属粉末的平均粒径为 0.1-3微米；
(2) 将步骤 （1 ) 所得的平均粒径为 0.1-3微米的亚微米级金属粉末与液体混合、 配制成金属粉浆料； 上述金属粉浆料的亚微米级金属粉末液体的重量比为 0.25-2.0:1；
(3 ) 在步骤 （2) 所得的金属粉浆料中加入亚微米级金属粉末重量 0.1-10%的有机 粘合剂， 搅拌混合均匀；
(4)将步骤（3 )搅拌混合均匀的浆料通过离心喷雾造粒机或压力喷雾造粒机制备 成球形状的、 平均粒径为 10-50微米的 3D打印用的金属粉末。
5.根据权利要求 4所述的 3D打印机用的金属粉末的制备方法， 其特征在于： 步骤
( 1 ) 所述的亚微米级金属粉末的平均粒径为 0.5-2微米。
6.根据权利要求 5所述的 3D打印机用的金属粉末的制备方法， 其特征在于： 步骤 (4) 所述的 3D打印机用的金属粉末其平均粒径为 20-30微米。
7.根据权利要求 4所述的 3D打印机用的金属粉末的制备方法， 其特征在于： 所述 的金属粉末为钛、 镍或铜的纯金属粉， 或者是镍基合金粉、 钛基合金粉、 铝基合金粉或 铁基合金粉的合金金属粉。
8.根据权利要求 4所述的 3D打印机用的金属粉末的制备方法， 其特征在于： 步骤
(2) 中所述的液体为水、 乙醇、 异丙醇或甲醇。
9.根据权利要求 4所述的 3D打印机用的金属粉末的制备方法， 其特征在于： 步骤
(3 ) 中所述的有机粘合剂为聚乙烯醇、 乙基纤维素或者金属矿粉造粒粘合剂。
10.根据权利要求 4所述的 3D打印机用的金属粉末的制备方法， 其特征在于： 步骤 (4) 所述的离心喷雾造粒机的转速控制在 10000-40000转 /分； 压力喷雾造粒机的压力 为 6-30kg/cm2 ; 上述压力喷雾造粒机或离心喷雾造粒机其他操作参数控制在： 干燥空气 的进口温度为 200-350°C和出口温度为 80-150°C ; 干燥空气的流量为 100-300 Nm3/h; 金 属粉浆料在压力喷雾造粒机或离心喷雾造粒机的进料速度为 5-20 kg/h。
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