CN104084592A - 一种制备三维打印用球形粉末材料的方法 - Google Patents
一种制备三维打印用球形粉末材料的方法 Download PDFInfo
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- CN104084592A CN104084592A CN201410362878.XA CN201410362878A CN104084592A CN 104084592 A CN104084592 A CN 104084592A CN 201410362878 A CN201410362878 A CN 201410362878A CN 104084592 A CN104084592 A CN 104084592A
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- 239000000463 material Substances 0.000 title claims abstract description 43
- 238000010146 3D printing Methods 0.000 title abstract description 11
- 238000000498 ball milling Methods 0.000 claims abstract description 35
- 210000002381 Plasma Anatomy 0.000 claims abstract description 32
- 239000002994 raw material Substances 0.000 claims abstract description 25
- 239000007789 gas Substances 0.000 claims abstract description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Chemical compound data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 16
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C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 229910000861 Mg alloy Inorganic materials 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N copper Chemical compound 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CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract 2
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound 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Abstract
本发明公开了一种制备三维打印用球形粉末材料的方法，包括原料选取，高能球磨和射频等离子体球化步骤，所述原料选取步骤所选原料为金属或合金粉末，所述高能球磨步骤在氩气保护下进行，球磨介质为石油醚，所述金属或合金粉末为铝合金粉末、钛合金粉末、镍基合金粉末、不锈钢粉末或钨合金粉末，所述射频等离子体球化步骤总气流量100～200L/min，等离子体输入功率50～100kW，系统出气口负压为-1000Pa～-2000Pa，送粉量为50～150g/min。本发明所制得球形粉末，球形度高，粒度均匀，含氧量低，缺陷少和流动性好，适用于3D打印；本发明制备三维打印用球形粉末材料的方法还具有过程精确可控的优点。
Description
技术领域
[0001] 本发明属于三维制造技术领域，涉及一种制造三维打印耗材的方法，特别涉及一 种制备三维打印用球形粉末材料的方法。
背景技术
[0002] 三维打印又称3D打印，是当前全球最受关注的新兴技术之一，被MIT的《科技评 论》杂志评选为2014年十大最具突破性的科技创新之一。作为一个战略性新兴产业，3D打 印技术及相关产业正在高速发展，麦肯锡预测，到2025年，3D打印相关产业规模有望达到 0. 2万亿至0. 6万亿美元。
[0003] 3D打印粉末材料是制约3D打印技术推广应用的关键，目前制备3D打印粉末材料 的方法主要有机械研磨法、自蔓延高温合成法、雾化法、旋转电极法、化学气相沉积法；机械 研磨法工序简单、成本低，但效率和纯度较低，难以用于工业化生产；自蔓延高温合成法虽 然工艺简单，易得到细粉，但氧含量较高、形状不规则，如加有微合金化元素，反应尤其不易 充分，粉末成分均匀性差；雾化法主要用于金属或合金粉末的制备，对于一些可熔的氧化物 陶瓷材料，难以获得细微陶瓷粉体，且由于存在坩埚污染，无法保证纯度；旋转电极法可以 制备高纯度的金属粉末，但制备的粉末较粗，平均粒径一般在100〜150 μ m以上；化学气相 沉积法制备的粉末粒径均匀，但粉末后处理工序繁杂，生产能耗较高。
[0004] 目前，国内高端的3D打印粉末材料主要依赖进口，而国外厂商常将原材料与设备 捆绑高价销量（售价约为国产3D打印粉末材料价格的5〜10倍），极大地制约了我国3D 打印技术的发展。
[0005] 因此，有必要开发一种价格更低、性能更好、通用性更强的3D打印材料以拓展3D 打印技术应用和推广。
发明内容
[0006] 有鉴于此，本发明的目的在于提供一种制备三维打印用球形粉末材料的方法。
[0007] 为达到上述目的，本发明提供如下技术方案：
[0008] -种制备三维打印用球形粉末材料的方法，包括原料选取，高能球磨和射频等离 子体球化步骤，所述原料选取步骤所选原料为金属或合金粉末，所述高能球磨步骤在氩气 保护下进行，球磨介质为石油醚。
[0009] 作为本发明制备三维打印用球形粉末方法的优选，所述金属或合金粉末为铝合 金粉、不锈钢粉、钛合金粉、镍基合金粉、钨合金粉、钴铬合金粉、镁合金粉或铜粉，其粒径 ^ 100 μ m〇
[0010] 作为本发明制备三维打印用球形粉末方法的另一种优选，所述高能球磨步骤球料 比为5:1〜10:1，球磨时间为6〜24h，球磨转速为800〜1500r/min。 toon] 作为本发明制备三维打印用球形粉末方法的另一种优选，所述高能球磨后还包括 分级筛选步骤，若球磨后粉体粒径符合要求，则进入射频等离子体球化步骤，反之返回球磨 步骤。
[0012] 作为本发明制备三维打印用球形粉末方法的进一步优选，射频等离子体球 化步骤总气流量100〜200L/min，等离子体输入功率50〜100kW，系统出气口负压 为-lOOOPa 〜-2000Pa，送粉量为 50 〜150g/min。
[0013] 本发明的有益效果在于：
[0014] 本发明制备三维打印用球形粉末材料的方法，首先对金属粉体进行高能球磨，然 后筛选球磨后的粉体，最后对筛选符合要求的粉体进行射频等离子体球化；可以得到球形 度高，粒度均匀，含氧量低，缺陷少和流动性好的适用于3D打印的粉体材料；本发明制备三 维打印用球形粉末材料的方法还具有成本低、过程精确可控的优点；本发明所制得的球形 粉末可用于三维打印制造领域，例如电子束熔融快速成型、粉末床激光烧结成型、激光近净 成型、大型激光烧结成型等，也可用于焊接、表面熔敷、复合材料制备。
附图说明
[0015] 为了使本发明的目的、技术方案和有益效果更加清楚，本发明提供如下附图进行 说明：
[0016] 图1为本发明制备三维打印用球形粉末工艺流程图；
[0017] 图2为实施例2制得球形粉末的微观形貌及粒径分布图；
[0018] 图3为实施例3制得球形粉末的微观形貌及粒径分布图；
[0019] 图4为实施例4制得球形粉末的微观形貌及粒径分布图。
具体实施方式
[0020] 下面将结合附图，对本发明的优选实施例进行详细的描述。
[0021] 实施例1 :
[0022] 本实施例制备三维打印用球形粉末材料的方法如图1所示，包括以下步骤：
[0023] 1)选取原材料：本实施例所选原材料为外购的粉末冶金法制备的铝合金粉末；
[0024] 2)高能球磨：将步骤1所选原材料加入高性能球磨装置进行球磨；
[0025] 本实施例中，球磨罐为玛瑙材质，研磨球选用玛瑙球，球料比为2:1，球磨时间为 2h，球磨转速为1200r/min ;为了控制球磨的速率和防止氧化，本实施例在球磨过程中以石 油醚作为过程控制剂，同时在球磨罐中封入高纯氩气；
[0026] 3)筛选：筛选研磨所得粉体，若球磨后粉体粒径符合要求，则进入射频等离子体 球化步骤，反之返回球磨步骤；
[0027] 4)射频（RF)等离子体球化：干燥步骤3)筛选得到的不规则铝合金粉末，然后送 入射频RF等离子体球化设备中进行球化处理；
[0028] 本实施例中，球化参数设定为，总气流量150L/min，等离子体输入功率20kW，系统 出气口负压为-l〇〇〇Pa，送粉量为200g/min。
[0029] 实施例2 :
[0030] 本实施例制备三维打印用球形粉末材料的方法，包括以下步骤：
[0031] 1)选取原材料：本实施例所选原材料为外购的粉末冶金法制备的不锈钢（不锈钢 316L)粉末；
[0032] 2)高能球磨：将步骤1所选原材料加入高性能球磨装置进行球磨；
[0033] 本实施例中，球磨罐为玛瑙材质，研磨球选用玛瑙球，球料比为4:1，球磨时间为 4h，球磨转速为800r/min ;为了控制球磨的速率和防止氧化，本实施例在球磨过程中以石 油醚作为过程控制剂，同时在球磨罐中封入高纯氩气；
[0034] 3)筛选：筛选研磨所得粉体，若球磨后粉体粒径符合要求，则进入射频等离子体 球化步骤，反之返回球磨步骤；
[0035] 4)射频（RF)等离子体球化：干燥步骤3)筛选得到的不规则铝合金粉末，然后送 入射频RF等离子体球化设备中进行球化处理；
[0036] 本实施例中，球化参数设定为，总气流量120L/min，等离子体输入功率30kW，系统 出气口负压为-lOOOPa，送粉量为150g/min。
[0037] 实施例3 :
[0038] 本实施例制备三维打印用球形粉末材料的方法，包括以下步骤：
[0039] 1)选取原材料：本实施例所选原材料为外购的粉末冶金法制备的钛合金（TC4)粉 末；
[0040] 2)高能球磨：将步骤1所选原材料加入高性能球磨装置进行球磨；
[0041] 本实施例中，球磨罐为WC材质，研磨球选用WC球，球料比为6:1，球磨时间为6h， 球磨转速为600r/min ;为了控制球磨的速率和防止氧化，本实施例在球磨过程中以石油醚 作为过程控制剂，同时在球磨罐中封入高纯氩气；
[0042] 3)筛选：筛选研磨所得粉体，若球磨后粉体粒径符合要求，则进入射频等离子体 球化步骤，反之返回球磨步骤；
[0043] 4)射频（RF)等离子体球化：真空干燥步骤3)筛选得到的不规则铝合金粉末，然 后送入射频RF等离子体球化设备中进行球化处理；
[0044] 本实施例中，球化参数设定为，总气流量100L/min，等离子体输入功率40kW，系统 出气口负压为_ 2000Pa，送粉量为100g/min。
[0045] 实施例4 :
[0046] 本实施例制备三维打印用球形粉末材料的方法，包括以下步骤：
[0047] 1)选取原材料：本实施例所选原材料为外购的粉末冶金法制备的镍基合金粉末 (镍基合金718);
[0048] 2)高能球磨：将步骤1所选原材料加入高性能球磨装置进行球磨；
[0049] 本实施例中，球磨罐为WC材质，研磨球选用WC球，球料比为8:1，球磨时间为8h， 球磨转速为600r/min ;为了控制球磨的速率和防止氧化，本实施例在球磨过程中以石油醚 作为过程控制剂，同时在球磨罐中封入高纯氩气；
[0050] 3)筛选：筛选研磨所得粉体，若球磨后粉体粒径符合要求，则进入射频等离子体 球化步骤，反之返回球磨步骤；
[0051] 4)射频（RF)等离子体球化：干燥步骤3)筛选得到的不规则铝合金粉末，然后送 入射频RF等离子体球化设备中进行球化处理；
[0052] 本实施例中，球化参数设定为，总气流量80L/min，等离子体输入功率60kW，系统 出气口负压为_2000Pa，送粉量为80g/min。
[0053] 实施例5 :
[0054] 本实施例制备三维打印用球形粉末材料的方法，包括以下步骤：
[0055] 1)选取原材料：本实施例所选原材料为外购的粉末冶金法制备的钨合金粉末；
[0056] 2)高能球磨：将步骤1所选原材料加入高性能球磨装置进行球磨；
[0057] 本实施例中，球磨罐为WC材质，研磨球选用WC球，球料比为10:1，球磨时间为 10h，球磨转速为600r/min ;为了控制球磨的速率和防止氧化，本实施例在球磨过程中以石 油醚作为过程控制剂，同时在球磨罐中封入高纯氩气；
[0058] 3)筛选：筛选研磨所得粉体，若球磨后粉体粒径符合要求，则进入射频等离子体 球化步骤，反之返回球磨步骤；
[0059] 4)射频（RF)等离子体球化：干燥步骤3)筛选得到的不规则铝合金粉末，然后送 入射频RF等离子体球化设备中进行球化处理；
[0060] 本实施例中，球化参数设定为，总气流量60L/min，等离子体输入功率80kW，系统 出气口负压为_ 2000Pa，送粉量为50g/min。
[0061] 图2a为实施例2制得球形粉末的微观形貌图，图2b为实施例2制得球形粉末的 粒径分布图；由图2可以看出，本实施例所制得的不锈钢粉末粒径分布均匀，粒度分布范围 80-300 μ m，呈标准正态分布，球形度> 95%。
[0062] 图3a为实施例3制得球形粉末的微观形貌图，图3b为实施例3制得球形粉末的 粒径分布图；由图3可以看出，本实施例所制得的钛合金粉末粒径分布均匀，粒度分布范围 10-70 μ m，呈标准正态分布，球形度> 95%。
[0063] 图4a为实施例4制得球形粉末的微观形貌图，图4b为实施例4制得球形粉末的 粒径分布图；由图4可以看出，本实施例所制得的镍基合金粉末粒径分布均匀，粒度分布范 围45-150 μ m，呈标准正态分布，球形度> 95%。
[0064] 由此可见，本发明制备粉体材料球形度高，粒度均匀，含氧量低，适用于3D打印。
[0065] 需要说明的是，本发明的处理方法还可以用于处理其他材料，如高分子材料、陶瓷 材料、纳米复合材料以及碳纤维材料等。
[〇〇66] 最后说明的是，以上优选实施例仅用以说明本发明的技术方案而非限制，尽管通 过上述优选实施例已经对本发明进行了详细的描述，但本领域技术人员应当理解，可以在 形式上和细节上对其作出各种各样的改变，而不偏离本发明权利要求书所限定的范围。
Claims (5)
1. 一种制备三维打印用球形粉末材料的方法，其特征在于：包括原料选取，高能球磨 和射频等离子体球化步骤，所述原料选取步骤所选原料为金属或合金粉末，所述高能球磨 步骤在氩气保护下进行，球磨介质为石油醚。
2. 根据权利要求1所述制备三维打印用球形粉末材料的方法，其特征在于：所述金属 或合金粉末为铝合金粉、不锈钢粉、钛合金粉、镍基合金粉、钨合金粉、钴铬合金粉、镁合金 粉或铜粉，其粒径< 100 μ m。
3. 根据权利要求1所述制备三维打印用球形粉末材料的方法，其特征在于：所述高能 球磨步骤球料比为5:1〜10:1，球磨时间为6〜24h，球磨转速为800〜1500r/min。
4. 根据权利要求1所述制备三维打印用球形粉末材料的方法，其特征在于：所述高能 球磨后还包括分级筛选步骤，若球磨后粉体粒径符合要求，则进入射频等离子体球化步骤， 反之返回球磨步骤。
5. 根据权利要求1所述制备三维打印用球形粉末材料的方法，其特征在于：射频等离 子体球化步骤总气流量100〜200L/min，等离子体输入功率50〜100kW，系统出气口负压 为-lOOOPa 〜-2000Pa，送粉量为 50 〜150g/min。
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