WO2023216401A1 - Method for reducing oxygen in powder for 3d printing - Google Patents

Method for reducing oxygen in powder for 3d printing Download PDF

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WO2023216401A1
WO2023216401A1 PCT/CN2022/103594 CN2022103594W WO2023216401A1 WO 2023216401 A1 WO2023216401 A1 WO 2023216401A1 CN 2022103594 W CN2022103594 W CN 2022103594W WO 2023216401 A1 WO2023216401 A1 WO 2023216401A1
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powder
metal powder
printing
screening
satellite
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PCT/CN2022/103594
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French (fr)
Chinese (zh)
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陈刚
曲选辉
秦明礼
章林
朱科研
陶麒鹦
丁旺旺
陈佳男
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北京科技大学
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • 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
    • B22F10/30—Process control
    • B22F10/34—Process control of powder characteristics, e.g. density, oxidation or flowability
    • 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
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • 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

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  • the invention belongs to the field of powder metallurgy, and relates to a method for reducing oxygen in 3D printing powder, and in particular to a method for reducing the oxygen content of gas atomized or water-gas combined atomized metal powder for 3D printing.
  • 3D printing directly prints materials in a bottom-up, layer-by-layer accumulation method, which can achieve direct shaping and personalized customization of complex shapes, solving the problems of low production efficiency and waste of raw materials caused by traditional processing methods.
  • Atomized metal powder is an important raw material for 3D printing, and the performance of atomized powder is the key to affecting the performance of 3D printed parts.
  • the oxygen content and inclusions of atomized metal powder are one of the important factors affecting the 3D printing forming process and the performance of the parts.
  • high-end materials such as titanium alloys, high-strength stainless steel, and nickel-based high-temperature alloys, reducing their oxygen content and inclusions can help improve the mechanical properties of formed parts.
  • metal powders for 3D printing are mostly prepared using gas atomization or water-gas combined atomization processes.
  • the collision of metal droplets will lead to the presence of a large amount of satellite powder on the powder surface.
  • the existence of satellite powder will not only cause Reducing the fluidity and bulk density of the powder, and its finer particle size, will increase the oxygen content and inclusions in the powder, thereby affecting the performance of the printed parts. Therefore, the elimination of satellite powder on the surface of atomized metal powder particles is crucial to 3D printing technology.
  • the production of satellite powder can be controlled by adjusting the process parameters of gas atomization or water-gas combined atomization.
  • gas atomization or water-gas combined atomization it is difficult to completely eliminate satellite powder with currently commercially available atomized powders. It can be seen that at this stage, there is an urgent need to develop an effective post-processing method to eliminate satellite powder on the surface of atomized powder particles for 3D printing, so as to reduce the oxygen content and inclusions of the powder, improve the fluidity and bulk density of the powder, and further enhance the 3D Performance of printed parts.
  • the present invention proposes a method for modifying gas atomized or water-gas joint atomized metal powder based on air flow mill technology.
  • the oxygen content and inclusions of the metal powder are further reduced. , thereby improving the quality of powder raw materials and the performance of 3D printed formed parts.
  • the present invention uses air flow mill technology to modify gas atomized and water-gas combined atomized metal powders.
  • the basic principle is that the gas flow rate and grinding air pressure in the airflow mill equipment cause the atomized metal powders to collide and rub against each other in the equipment chamber.
  • the shear force and collision force between particles will knock off the satellite powder on the surface of the metal powder, and then pass through Screening removes satellite powder to reduce the oxygen content and inclusions in the powder.
  • the sphericity and bulk density of powder particles will also be improved.
  • a method for reducing oxygen in 3D printing powder including the following steps:
  • Step 1) Sieve commercially available atomized metal powder with a sieve to remove impurities in the powder;
  • Step 2 Place the commercially available atomized metal powder obtained by screening in an airflow mill equipment for surface treatment to improve the surface morphology of the powder;
  • Step 3 Place the surface-treated atomized metal powder obtained by airflow milling under a high-purity argon or nitrogen atmosphere for screening, and then vacuum seal and package it.
  • the commercially available atomized metal powders are four powders: 316L stainless steel, Ti-6Al-4V titanium alloy, CM247LC nickel-based high-temperature alloy and AlSi10Mg aluminum alloy.
  • the raw materials are prepared by atomization method, and the particle size range is 15-63 ⁇ m. , there are more satellite powders in the powder, and the sphericity is 60% to 80%.
  • step 2 nitrogen or argon is used as the protective atmosphere and working gas during the jet mill treatment.
  • the gas pressure is 0.10 ⁇ 0.80MPa
  • the rotation speed is 1000 ⁇ 4000r/min
  • the treatment time is 5 ⁇ 60min.
  • the screening process described in step 3) is to carry out screening under a high-purity argon or nitrogen atmosphere, and then vacuum seal packaging.
  • the screening particle size range is 15-63 ⁇ m, and the high-purity argon or Nitrogen purity is 99.99wt.%.
  • the surface-treated metal powder obtained in step 2) has a particle size range of 1 to 63 ⁇ m. Scanning electron microscope observation shows that the number of satellite powders is significantly reduced, the sphericity is increased, and the number and size of inclusions are reduced.
  • the sieved metal powder obtained in step 3 has a particle size ranging from 15 to 63 ⁇ m. Compared with the untreated aerosolized powder, the oxygen content is significantly reduced, and the powder fluidity is improved.
  • the metal powder processed in steps 1), 2) and 3) has a significantly lower oxygen content and a significantly lower number of satellite powders. The number of inclusions is reduced, the bulk density is increased, and the powder flowability is improved.
  • the invention proposes a 3D printing powder oxygen reduction method, which is characterized by the fact that there is no adhering satellite powder on the surface of the powder particles after airflow milling, the oxygen content is significantly reduced, and the powder sphericity reaches more than 90%, which helps to improve 3D printing. Performance of printed parts.
  • the present invention is suitable for atomized powders of different material systems, including titanium alloys, iron-based alloys and nickel-based high-temperature alloys.
  • the invention has a short working time, operates at room temperature, and is protected by inert gas. Therefore, the impurities of the powder can be effectively controlled.
  • the process of the present invention is short, simple to operate, high in raw material utilization and low in cost.
  • the microscopic morphology of the four powders obtained by the present invention including airflow mill modified 316L stainless steel, Ti-6Al-4V titanium alloy, CM247LC nickel-based high-temperature alloy and AlSi10Mg aluminum alloy, is smooth and has no satellite powder, and the powder sphericity is within Over 89%, liquidity improved;
  • Figure 1 is an SEM microscopic morphology of atomized 316L stainless steel powder before and after airflow milling in Example 1 of the present invention.
  • the picture (a) shows the morphology of 316L stainless steel powder before jet milling
  • the picture (b) shows the morphology of 316L stainless steel powder after jet milling.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Automation & Control Theory (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

A method for reducing oxygen in a powder for 3D printing, which belongs to the field of powder metallurgy. The method comprises: firstly, screening a commercially available atomized metal powder by using a sieve, so as to remove impurities in the powder; placing the commercially available atomized metal powder obtained from screening in a jet mill apparatus for a surface treatment, so as to improve the surface morphology of the powder; and placing the atomized metal powder obtained from a jet milling treatment and a surface treatment in a high-purity argon or nitrogen atmosphere for screening, and subjecting same to vacuum sealed packaging. Satellite powders do not adhere to the surfaces of powder particles obtained from the jet milling treatment, the oxygen content is significantly reduced, and the sphericity degree of the powder reaches 90% or more, such that the performance of a 3D printed and formed part can be improved. The method is suitable for atomized powders of different material systems, including a titanium alloy, an iron-based alloy, a nickel-based high-temperature alloy, etc., and is short in terms of technological process, easy to operate, high in terms of the utilization rate of raw materials, and low in terms of cost.

Description

一种3D打印粉末降氧方法A method for reducing oxygen in 3D printing powder 技术领域Technical field
本发明属于粉末冶金领域，涉及一种3D打印粉末降氧方法，尤其涉及一种降低3D打印用气雾化或水气联合雾化金属粉末氧含量的方法。The invention belongs to the field of powder metallurgy, and relates to a method for reducing oxygen in 3D printing powder, and in particular to a method for reducing the oxygen content of gas atomized or water-gas combined atomized metal powder for 3D printing.
技术背景technical background
3D打印通过一种自下而上、逐层堆积的方式直接打印材料，可以实现直接成形和复杂形状的个性化定制，解决了传统加工方法生产效率低、原材料浪费的问题。雾化金属粉末是3D打印的重要原料，而雾化粉末的性能是影响3D打印制件性能的关键所在。特别地，雾化金属粉末的氧含量和夹杂物等，是影响3D打印成形工艺及其制件性能的重要因素之一。针对钛合金、高强不锈钢、镍基高温合金等高端材料而言，降低其氧含量和夹杂物，有助于提高成形件的力学性能。目前，3D打印用金属粉末大多是利用气雾化或水气联合雾化工艺制备的，在雾化过程中金属液滴的相撞会导致粉末表面存在大量的卫星粉，卫星粉的存在不仅会降低粉末的流动性和松装密度，而且其粒径较细，会增加粉末的氧含量和夹杂，进而影响打印件的性能。因此，雾化金属粉末颗粒表面卫星粉的消除，对于3D打印技术而言至关重要。3D printing directly prints materials in a bottom-up, layer-by-layer accumulation method, which can achieve direct shaping and personalized customization of complex shapes, solving the problems of low production efficiency and waste of raw materials caused by traditional processing methods. Atomized metal powder is an important raw material for 3D printing, and the performance of atomized powder is the key to affecting the performance of 3D printed parts. In particular, the oxygen content and inclusions of atomized metal powder are one of the important factors affecting the 3D printing forming process and the performance of the parts. For high-end materials such as titanium alloys, high-strength stainless steel, and nickel-based high-temperature alloys, reducing their oxygen content and inclusions can help improve the mechanical properties of formed parts. At present, metal powders for 3D printing are mostly prepared using gas atomization or water-gas combined atomization processes. During the atomization process, the collision of metal droplets will lead to the presence of a large amount of satellite powder on the powder surface. The existence of satellite powder will not only cause Reducing the fluidity and bulk density of the powder, and its finer particle size, will increase the oxygen content and inclusions in the powder, thereby affecting the performance of the printed parts. Therefore, the elimination of satellite powder on the surface of atomized metal powder particles is crucial to 3D printing technology.
一般情况下，通过调整气雾化或水气联合雾化的工艺参数可以控制卫星粉的产生，但是目前市售的雾化粉末均难以实现卫星粉的完全消除。可见，现阶段亟需开发一种消除3D打印用雾化粉末颗粒表面卫星粉的有效后处理方法，以降低粉末的氧含量和夹杂物，以及提高粉末的流动性和松装密度，进一步提升3D打印成形件的性能。In general, the production of satellite powder can be controlled by adjusting the process parameters of gas atomization or water-gas combined atomization. However, it is difficult to completely eliminate satellite powder with currently commercially available atomized powders. It can be seen that at this stage, there is an urgent need to develop an effective post-processing method to eliminate satellite powder on the surface of atomized powder particles for 3D printing, so as to reduce the oxygen content and inclusions of the powder, improve the fluidity and bulk density of the powder, and further enhance the 3D Performance of printed parts.
针对上述问题，本发明提出了基于气流磨技术对气雾化或水气联合雾化金属粉末进行改性处理的方法，通过消除粉末颗粒表面的卫星粉，进一步降低金属粉末的氧含量和夹杂物，从而提高粉末原料的质量和3D打印成形件的性能。In response to the above problems, the present invention proposes a method for modifying gas atomized or water-gas joint atomized metal powder based on air flow mill technology. By eliminating satellite powder on the surface of the powder particles, the oxygen content and inclusions of the metal powder are further reduced. , thereby improving the quality of powder raw materials and the performance of 3D printed formed parts.
发明内容Contents of the invention
本发明利用气流磨技术对气雾化和水气联合雾化金属粉末进行改性处理，通过去除粉末表面的卫星粉，降低粉末的氧含量和夹杂物，提高粉末流动性和松装密度。基本原理在于，气流磨设备中的气体流速及研磨气压使得雾化金属粉末在设备仓室内发生相互碰撞、摩擦，颗粒间的剪切力和碰撞力将金属粉末表面的卫星粉打掉，然后通过筛分将卫星粉筛除，达到降低粉末氧含量和夹杂物的目的。同时，粉末颗粒的球形度和松装密度也将得到提高。The present invention uses air flow mill technology to modify gas atomized and water-gas combined atomized metal powders. By removing satellite powder on the surface of the powder, the oxygen content and inclusions of the powder are reduced, and the fluidity and bulk density of the powder are improved. The basic principle is that the gas flow rate and grinding air pressure in the airflow mill equipment cause the atomized metal powders to collide and rub against each other in the equipment chamber. The shear force and collision force between particles will knock off the satellite powder on the surface of the metal powder, and then pass through Screening removes satellite powder to reduce the oxygen content and inclusions in the powder. At the same time, the sphericity and bulk density of powder particles will also be improved.
一种3D打印粉末降氧方法，包括以下步骤：A method for reducing oxygen in 3D printing powder, including the following steps:
步骤1)将市售雾化金属粉末用筛网筛分，去除粉末中的杂质；Step 1) Sieve commercially available atomized metal powder with a sieve to remove impurities in the powder;
步骤2)将筛分得到的市售雾化金属粉末置于气流磨设备中进行表面处理，改善粉末表面形貌；Step 2) Place the commercially available atomized metal powder obtained by screening in an airflow mill equipment for surface treatment to improve the surface morphology of the powder;
步骤3)将气流磨处理得到的经过表面处理后的雾化金属粉末置于高纯氩气或氮气气氛下进行筛分，然后真空密封包装。Step 3) Place the surface-treated atomized metal powder obtained by airflow milling under a high-purity argon or nitrogen atmosphere for screening, and then vacuum seal and package it.
进一步地，所述的市售雾化金属粉末为316L不锈钢、Ti-6Al-4V钛合金、CM247LC镍基高温合金和AlSi10Mg铝合金四种粉末，原料由雾化方法制备，粒度范围为15～63μm，粉末中存在较多的卫星粉，球形度为60％～80％。Further, the commercially available atomized metal powders are four powders: 316L stainless steel, Ti-6Al-4V titanium alloy, CM247LC nickel-based high-temperature alloy and AlSi10Mg aluminum alloy. The raw materials are prepared by atomization method, and the particle size range is 15-63 μm. , there are more satellite powders in the powder, and the sphericity is 60% to 80%.
进一步地，步骤2)所述的表面处理，气流磨处理时采用氮气或氩气作为保护气氛和工作气体，气体压力为0.10～0.80MPa，转速为1000～4000r/min，处理时间5～60min。Further, in the surface treatment described in step 2), nitrogen or argon is used as the protective atmosphere and working gas during the jet mill treatment. The gas pressure is 0.10~0.80MPa, the rotation speed is 1000~4000r/min, and the treatment time is 5~60min.
进一步地，步骤3)所述的筛分处理，是在高纯氩气或氮气气氛下进行筛分，然后真空密封包装，筛分粒径范围为15～63μm，所述的高纯氩气或氮气纯度为99.99wt.％。Further, the screening process described in step 3) is to carry out screening under a high-purity argon or nitrogen atmosphere, and then vacuum seal packaging. The screening particle size range is 15-63 μm, and the high-purity argon or Nitrogen purity is 99.99wt.%.
进一步地，步骤2)所得的表面处理后的金属粉末，粒度范围为1～63μm，经扫描电镜观察发现，卫星粉数量明显减少，球形度提高，夹杂物数量和尺寸减小。Furthermore, the surface-treated metal powder obtained in step 2) has a particle size range of 1 to 63 μm. Scanning electron microscope observation shows that the number of satellite powders is significantly reduced, the sphericity is increased, and the number and size of inclusions are reduced.
进一步地，步骤3)所得的筛分后的金属粉末，粒径范围为15～63μm，与未处理的气雾化粉末相比氧含量明显降低，且粉末流动性得到改善。Furthermore, the sieved metal powder obtained in step 3) has a particle size ranging from 15 to 63 μm. Compared with the untreated aerosolized powder, the oxygen content is significantly reduced, and the powder fluidity is improved.
进一步地，经步骤1)、步骤2)与步骤3)处理后的金属粉末与气雾化或水气联合雾化工艺制备的金属粉末相比，粉末氧含量明显降低，卫星粉数量明显减少，夹杂物数量减少，松装密度增大，粉末流动性得到改善。Further, compared with the metal powder prepared by gas atomization or water-gas combined atomization process, the metal powder processed in steps 1), 2) and 3) has a significantly lower oxygen content and a significantly lower number of satellite powders. The number of inclusions is reduced, the bulk density is increased, and the powder flowability is improved.
本发明提出的一种3D打印粉末降氧方法，其特征在于气流磨处理后的粉末颗粒表面不存在黏附的卫星粉，氧含量得到明显降低，粉末球形度达到90％以上，有助于提高3D打印成形件的性能。The invention proposes a 3D printing powder oxygen reduction method, which is characterized by the fact that there is no adhering satellite powder on the surface of the powder particles after airflow milling, the oxygen content is significantly reduced, and the powder sphericity reaches more than 90%, which helps to improve 3D printing. Performance of printed parts.
本发明技术关键点和优点在于：The technical key points and advantages of the present invention are:
1、本发明适用于不同材料体系的雾化粉末，包括钛合金、铁基合金和镍基高温合金等。1. The present invention is suitable for atomized powders of different material systems, including titanium alloys, iron-based alloys and nickel-based high-temperature alloys.
2、本发明工作时间短，于室温下操作，且由惰性气体保护。所以，粉末的杂质可以得到有效控制。2. The invention has a short working time, operates at room temperature, and is protected by inert gas. Therefore, the impurities of the powder can be effectively controlled.
3、本发明工艺流程短，操作简单，原料利用率高，成本低。3. The process of the present invention is short, simple to operate, high in raw material utilization and low in cost.
本发明的技术效果如下：The technical effects of the present invention are as follows:
(1)本发明所得到的气流磨改性316L不锈钢、Ti-6Al-4V钛合金、CM247LC镍基高温合金和AlSi10Mg铝合金四种粉末的氧含量和夹杂物含量得到显著降低；(1) The oxygen content and inclusion content of the four powders of jet mill modified 316L stainless steel, Ti-6Al-4V titanium alloy, CM247LC nickel-based high-temperature alloy and AlSi10Mg aluminum alloy obtained by the present invention are significantly reduced;
(2)本发明所得到的气流磨改性316L不锈钢、Ti-6Al-4V钛合金、CM247LC镍基高温合金和AlSi10Mg铝合金四种粉末的微观形貌表面光滑无卫星粉，粉末球形度均在89％以上，流动性得到改善；(2) The microscopic morphology of the four powders obtained by the present invention, including airflow mill modified 316L stainless steel, Ti-6Al-4V titanium alloy, CM247LC nickel-based high-temperature alloy and AlSi10Mg aluminum alloy, is smooth and has no satellite powder, and the powder sphericity is within Over 89%, liquidity improved;
(3)本发明所得的气流磨改性316L不锈钢、Ti-6Al-4V钛合金、CM247LC镍基高温合金和AlSi10Mg铝合金四种粉末的中位径变窄，D50在33～35μm范围内，松装密度增大，铺粉性能得到提高。(3) The median diameters of the four powders of jet mill modified 316L stainless steel, Ti-6Al-4V titanium alloy, CM247LC nickel-based high-temperature alloy and AlSi10Mg aluminum alloy obtained by the present invention become narrower, and the D50 is in the range of 33 to 35 μm. The packing density increases and the powder spreading performance is improved.
附图说明Description of the drawings
图1为本发明实施例1中经气流磨处理前后的雾化316L不锈钢粉末SEM显微形貌图。其中，(a)图显示为气流磨处理前的316L不锈钢粉末形貌，(b)图为气流磨处理后的316L不锈钢粉末形貌。Figure 1 is an SEM microscopic morphology of atomized 316L stainless steel powder before and after airflow milling in Example 1 of the present invention. Among them, the picture (a) shows the morphology of 316L stainless steel powder before jet milling, and the picture (b) shows the morphology of 316L stainless steel powder after jet milling.
具体实施方式Detailed ways
通过阅读下文中的优选实施方式详细描述，这使本领域从业者更了解本发明的优点和益处。The following detailed description of the preferred embodiments will provide those skilled in the art with a better understanding of the advantages and benefits of the present invention.
实施例1Example 1
1.以雾化316L不锈钢粉末为原料，其中氧含量为0.037wt.％；D10＝12.2μm，D50＝30.5μm，D90＝53.6μm；球形度75％；流动性23.4s/50g；松装密度3.86g/cm 3，经SEM观察可发现粉末存在卫星粉，如图1(a)所示。 1. Use atomized 316L stainless steel powder as raw material, in which the oxygen content is 0.037wt.%; D10=12.2μm, D50=30.5μm, D90=53.6μm; sphericity 75%; fluidity 23.4s/50g; bulk density 3.86g/cm 3 . SEM observation shows that satellite powder exists in the powder, as shown in Figure 1(a).
2.将上述原料钛粉筛分后，放入气流磨设备中进行表面处理，采用高纯氮气作为保护气氛和工作气氛，气体压力0.40MPa，转速2000r/min，处理时间10min，使得卫星粉不再黏附在金属粉末表面，而是处于游离状态。2. After screening the above raw material titanium powder, put it into the airflow mill equipment for surface treatment. Use high-purity nitrogen as the protective atmosphere and working atmosphere. The gas pressure is 0.40MPa, the rotation speed is 2000r/min, and the processing time is 10min, so that the satellite powder does not It then adheres to the surface of the metal powder, but is in a free state.
3.将气流磨处理后的金属粉末进行筛分处理，在高纯氩气下进行筛分，筛分粒径范围为15～63μm，高纯氩气纯度为99.99wt.％，然后真空密封包装，对处理后粉末进行氧含量、粒度分布、球形度、形貌、流动性、松装密度表征。3. Sieve the metal powder processed by the jet mill and sieve it under high-purity argon gas. The sieving particle size range is 15-63 μm, and the purity of the high-purity argon gas is 99.99wt.%, and then vacuum sealed and packaged. , the treated powder was characterized for oxygen content, particle size distribution, sphericity, morphology, fluidity and bulk density.
4.上述处理后的316L不锈钢粉末，经检测，氧含量0.010wt.％；D10＝23.1μm，D50＝33.5μm，D90＝55.1μm；球形度92％；流动性20.7s/50g；松装密度4.03g/cm 3；且粉末表面已不存在卫星粉，如图1(b)所示。 4. After the above treatment, the 316L stainless steel powder was tested and found that the oxygen content was 0.010wt.%; D10=23.1μm, D50=33.5μm, D90=55.1μm; sphericity 92%; fluidity 20.7s/50g; bulk density 4.03g/cm 3 ; and there is no satellite powder on the powder surface, as shown in Figure 1(b).
实施例2Example 2
1.以雾化Ti-6Al-4V钛合金粉末为原料，其中氧含量0.150wt.％；D10＝13.5μm，D50＝28.6μm，D90＝51.4μm；球形度76％；流动性33.5s/50g；松装密度2.38g/cm 3，经SEM观察可发现粉末存在卫星粉。 1. Use atomized Ti-6Al-4V titanium alloy powder as raw material, with oxygen content 0.150wt.%; D10=13.5μm, D50=28.6μm, D90=51.4μm; sphericity 76%; fluidity 33.5s/50g ; The bulk density is 2.38g/cm 3 , and satellite powder can be found in the powder through SEM observation.
2.将上述原料钛粉经过筛分后，放入气流磨设备中进行表面处理，采用高纯氮气作为保护气氛和工作气氛，气体压力0.30MPa，转速2500r/min，处理时间10min，使得卫星粉不再黏附在金属粉末表面，而是处于游离状态。2. After screening the above raw titanium powder, put it into the airflow mill equipment for surface treatment. Use high-purity nitrogen as the protective atmosphere and working atmosphere. The gas pressure is 0.30MPa, the rotation speed is 2500r/min, and the processing time is 10min, so that the satellite powder It no longer adheres to the surface of the metal powder, but is in a free state.
3.将气流磨处理后的金属粉末进行筛分处理，在高纯氩气下进行筛分，筛分粒径范围为15～63μm，高纯氩气纯度为99.99wt.％，然后真空密封包装，对处理后粉末进行氧含量、粒度分布、球形度、形貌、流动性、松装密度表征。3. Sieve the metal powder processed by the jet mill and sieve it under high-purity argon gas. The sieving particle size range is 15-63 μm, and the purity of the high-purity argon gas is 99.99wt.%, and then vacuum sealed and packaged. , the treated powder was characterized for oxygen content, particle size distribution, sphericity, morphology, fluidity and bulk density.
4.上述处理后的Ti-6Al-4V钛合金粉末，经检测，氧含量0.100wt.％；D10＝19.2μm， D50＝32.1μm，D90＝53.4μm；球形度90％；流动性31.1s/50g；松装密度2.41g/cm 3；且粉末表面已不存在卫星粉。 4. The Ti-6Al-4V titanium alloy powder after the above treatment has been tested and found that the oxygen content is 0.100wt.%; D10=19.2μm, D50=32.1μm, D90=53.4μm; sphericity 90%; fluidity 31.1s/ 50g; bulk density 2.41g/cm 3 ; and there is no satellite powder on the powder surface.
实施例3Example 3
1.以雾化CM247LC镍基高温合金粉末为原料，其中氧含量0.050wt.％；D10＝20.5μm，D50＝35.6μm，D90＝63.5μm；球形度68％；流动性14.2s/50g；松装密度5.24g/cm 3，经SEM观察可发现粉末存在卫星粉。 1. Use atomized CM247LC nickel-based superalloy powder as raw material, in which the oxygen content is 0.050wt.%; D10=20.5μm, D50=35.6μm, D90=63.5μm; sphericity 68%; fluidity 14.2s/50g; loose The packing density is 5.24g/cm 3 , and satellite powder can be found in the powder through SEM observation.
2.将上述原料CM247LC镍基高温合金粉末经过筛分后，放入气流磨设备中进行表面处理，采用高纯氮气作为保护气氛和工作气氛，气体压力0.50MPa，转速3000r/min，处理时间10min，使得卫星粉不再黏附在金属粉末表面，而是处于游离状态。2. After screening the above raw material CM247LC nickel-based high-temperature alloy powder, put it into the airflow mill equipment for surface treatment. Use high-purity nitrogen as the protective atmosphere and working atmosphere. The gas pressure is 0.50MPa, the rotation speed is 3000r/min, and the processing time is 10min. , so that the satellite powder no longer adheres to the surface of the metal powder, but is in a free state.
3.将气流磨处理后的金属粉末进行筛分处理，在高纯氩气下进行筛分，筛分粒径范围为15～63μm，高纯氩气纯度为99.99wt.％，然后真空密封包装，对处理后粉末进行氧含量、粒度分布、球形度、形貌、流动性、松装密度表征。3. Sieve the metal powder processed by the jet mill and sieve it under high-purity argon gas. The sieving particle size range is 15-63 μm, and the purity of the high-purity argon gas is 99.99wt.%, and then vacuum sealed and packaged. , the treated powder was characterized for oxygen content, particle size distribution, sphericity, morphology, fluidity and bulk density.
4.上述处理后的CM247LC镍基高温合金粉末，经检测，氧含量0.020wt.％；D10＝18.9μm，D50＝33.2μm，D90＝54.1μm；球形度93％；流动性12.1s/50g；松装密度5.34g/cm 3；且粉末表面已不存在卫星粉。 4. After the above treatment, the CM247LC nickel-based superalloy powder was tested and found that the oxygen content was 0.020wt.%; D10=18.9μm, D50=33.2μm, D90=54.1μm; sphericity 93%; fluidity 12.1s/50g; The bulk density is 5.34g/cm 3 ; and there is no satellite powder on the powder surface.
实施例4Example 4
1.以雾化AlSi10Mg铝合金粉末为原料，其中氧含量0.035wt.％；D10＝18.5μm，D50＝29.4μm，D90＝50.6μm；球形度79％；流动性45.3s/50g；松装密度1.30g/cm 3。 1. Using atomized AlSi10Mg aluminum alloy powder as raw material, the oxygen content is 0.035wt.%; D10=18.5μm, D50=29.4μm, D90=50.6μm; sphericity 79%; fluidity 45.3s/50g; bulk density 1.30g/cm 3 .
2.将上述原料AlSi10Mg铝合金粉末经过筛分后，放入气流磨设备中进行表面处理，采用高纯氮气作为保护气氛和工作气氛，气体压力0.20MPa，转速1000r/min，处理时间10min，使得卫星粉不再黏附在金属粉末表面，而是处于游离状态。2. After screening the above raw material AlSi10Mg aluminum alloy powder, put it into the airflow mill equipment for surface treatment. Use high-purity nitrogen as the protective atmosphere and working atmosphere. The gas pressure is 0.20MPa, the rotation speed is 1000r/min, and the processing time is 10min, so that The satellite powder no longer adheres to the surface of the metal powder, but is in a free state.
3.将气流磨处理后的金属粉末进行筛分处理，在高纯氩气下进行筛分，筛分粒径范围为15～63μm，高纯氩气纯度为99.99wt.％，然后真空密封包装，对处理后粉末进行氧含量、粒度分布、球形度、形貌、流动性、松装密度表征。3. Sieve the metal powder processed by the jet mill and sieve it under high-purity argon gas. The sieving particle size range is 15-63 μm, and the purity of the high-purity argon gas is 99.99wt.%, and then vacuum sealed and packaged. , the treated powder was characterized for oxygen content, particle size distribution, sphericity, morphology, fluidity and bulk density.
4.上述处理后的AlSi10Mg铝合金粉末，氧含量0.020wt.％；D10＝23.3μm， D50＝34.2μm，D90＝52.7μm；球形度90％；流动性39.6s/50g；松装密度1.51g/cm 3。 4. AlSi10Mg aluminum alloy powder after the above treatment, oxygen content 0.020wt.%; D10=23.3μm, D50=34.2μm, D90=52.7μm; sphericity 90%; fluidity 39.6s/50g; bulk density 1.51g /cm 3 .

Claims (7)

  1. 一种3D打印粉末降氧方法，其特征在于，包括以下步骤：A method for reducing oxygen in 3D printing powder, which is characterized by including the following steps:
    步骤1)将市售雾化金属粉末用筛网筛分，去除粉末中的杂质；Step 1) Sieve commercially available atomized metal powder with a sieve to remove impurities in the powder;
    步骤2)将筛分得到的市售雾化金属粉末置于气流磨设备中进行表面处理，改善粉末表面形貌；Step 2) Place the commercially available atomized metal powder obtained by screening in an airflow mill equipment for surface treatment to improve the surface morphology of the powder;
    步骤3)将气流磨处理得到的经过表面处理后的雾化金属粉末置于高纯氩气或氮气气氛下进行筛分，然后真空密封包装。Step 3) Place the surface-treated atomized metal powder obtained by airflow milling under a high-purity argon or nitrogen atmosphere for screening, and then vacuum seal and package it.
  2. 根据权利要求1所述的一种3D打印粉末降氧方法，其特征在于，所述的市售雾化金属粉末为316L不锈钢、Ti-6Al-4V钛合金、CM247LC镍基高温合金和AlSi10Mg铝合金四种粉末，原料由雾化方法制备，粒度范围为15～63μm，粉末中存在较多的卫星粉，球形度为60％～80％。A 3D printing powder oxygen reduction method according to claim 1, characterized in that the commercially available atomized metal powder is 316L stainless steel, Ti-6Al-4V titanium alloy, CM247LC nickel-based high-temperature alloy and AlSi10Mg aluminum alloy Four kinds of powders, the raw materials are prepared by atomization method, the particle size range is 15-63 μm, there are more satellite powders in the powder, and the sphericity is 60%-80%.
  3. 根据权利要求1所述的一种3D打印粉末降氧方法，其特征在于，步骤2)所述的表面处理，气流磨处理时采用氮气或氩气作为保护气氛和工作气体，气体压力为0.10～0.80MPa，转速为1000～4000r/min，处理时间5～60min。A 3D printing powder oxygen reduction method according to claim 1, characterized in that, in the surface treatment described in step 2), nitrogen or argon is used as the protective atmosphere and working gas during the jet mill treatment, and the gas pressure is 0.10~ 0.80MPa, rotation speed is 1000~4000r/min, processing time is 5~60min.
  4. 根据权利要求1所述的一种3D打印粉末降氧方法，其特征在于，步骤3)所述的筛分处理，是在高纯氩气或氮气气氛下进行筛分，然后真空密封包装，筛分粒径范围为15～63μm，所述的高纯氩气或氮气纯度为99.99wt.％。A 3D printing powder oxygen reduction method according to claim 1, characterized in that the screening process in step 3) is carried out under a high-purity argon or nitrogen atmosphere, and then vacuum-sealed and packaged. The particle size range is 15-63 μm, and the purity of the high-purity argon or nitrogen is 99.99wt.%.
  5. 根据权利要求1所述的一种3D打印粉末降氧方法，其特征在于，步骤2)所得的表面处理后的金属粉末，粒度范围为1～63μm，经扫描电镜观察发现，卫星粉数量明显减少，球形度提高，夹杂物数量和尺寸减小。A 3D printing powder oxygen reduction method according to claim 1, characterized in that the surface-treated metal powder obtained in step 2) has a particle size range of 1 to 63 μm. It is found through scanning electron microscope observation that the number of satellite powders is significantly reduced. , the sphericity is improved, and the number and size of inclusions are reduced.
  6. 根据权利要求1所述的一种3D打印粉末降氧方法，其特征在于，步骤3)所得的筛分后的金属粉末，粒径范围为15～63μm，与未处理的气雾化粉末相比氧含量明显降低，且粉末流动性得到改善。A 3D printing powder oxygen reduction method according to claim 1, characterized in that the screened metal powder obtained in step 3) has a particle size range of 15 to 63 μm. Compared with the untreated aerosolized powder Oxygen content is significantly reduced and powder flowability is improved.
  7. 根据权利要求1所述的一种3D打印粉末降氧方法，其特征在于，经步骤1)、步骤2)与步骤3)处理后的金属粉末与气雾化或水气联合雾化工艺制备的金属 粉末相比，粉末氧含量明显降低，卫星粉数量明显减少，夹杂物数量减少，松装密度增大，粉末流动性得到改善。A 3D printing powder oxygen reduction method according to claim 1, characterized in that the metal powder processed in steps 1), 2) and 3) is prepared by a gas atomization or water gas combined atomization process. Compared with metal powder, the oxygen content of the powder is significantly reduced, the number of satellite powder is significantly reduced, the number of inclusions is reduced, the bulk density is increased, and the powder fluidity is improved.
PCT/CN2022/103594 2022-05-11 2022-07-04 Method for reducing oxygen in powder for 3d printing WO2023216401A1 (en)

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