WO2020103582A1 - 一种3d打印用低成本钛粉的流化整形制备方法 - Google Patents
一种3d打印用低成本钛粉的流化整形制备方法Info
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- WO2020103582A1 WO2020103582A1 PCT/CN2019/109538 CN2019109538W WO2020103582A1 WO 2020103582 A1 WO2020103582 A1 WO 2020103582A1 CN 2019109538 W CN2019109538 W CN 2019109538W WO 2020103582 A1 WO2020103582 A1 WO 2020103582A1
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- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
- C22C1/0458—Alloys based on titanium, zirconium or hafnium
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- 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
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- 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
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
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- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C14/00—Alloys based on titanium
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- 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
- B22F2009/042—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling using a particular milling fluid
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- B22F2201/00—Treatment under specific atmosphere
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- B22F2201/013—Hydrogen
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- B22F2201/00—Treatment under specific atmosphere
- B22F2201/10—Inert gases
- B22F2201/11—Argon
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- B22—CASTING; POWDER METALLURGY
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- B22F2201/00—Treatment under specific atmosphere
- B22F2201/20—Use of vacuum
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2202/00—Treatment under specific physical conditions
- B22F2202/15—Use of fluidised beds
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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
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/20—Refractory metals
- B22F2301/205—Titanium, zirconium or hafnium
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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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Definitions
- the invention belongs to the technical field of metal powder metallurgy preparation, and provides a low-cost fluidized preparation method of titanium powder for 3D printing.
- Titanium is a metal with low density, good corrosion resistance, high specific strength, and excellent biocompatibility. It is mainly used in aerospace, petrochemical, energy, biomedical and other fields. In recent years, the use of 3D printing and injection molding and other powder metallurgy near-net forming processes to prepare high-performance and complex-shaped titanium products has become a hot research topic at home and abroad.
- the powder metallurgy process has high requirements for the performance of titanium powder raw materials. In addition to the particle size and its composition and oxygen content performance, it particularly puts forward higher requirements for powder fluidity.
- the purpose of the present invention is to provide a method for preparing titanium powder with low sphericity and fluidity, which can meet the requirements of powder metallurgy processes such as 3D printing and injection molding at a low cost, and to solve the current high requirements for spherical titanium powder production equipment and complex processes , High cost and other issues.
- the present invention applies fluidization technology to the shaping process of irregularly shaped powder for the first time.
- Fluidization technology is through solid particles and gas or liquid fluid medium moving and contacting with each other in the container, so as to achieve the purpose of surface treatment, drying or mass and heat transfer, etc., has been widely used in chemical, light industry, medicine, food and other fields .
- the present invention uses low-cost hydrogenated dehydrogenated titanium powder as a raw material, puts the titanium powder into a fluidized reactor, and achieves the purpose of shaping the titanium powder through collision and friction between powder particles at a certain temperature in a protective atmosphere, thereby improving
- the powder sphericity can obtain titanium powder with good fluidity, which can meet the requirements of powder metallurgy processes such as 3D printing and injection molding.
- the method has the advantages of low cost, simple equipment and process, high efficiency, controllable impurity content, and obvious effect of improving powder fluidity. It can also be used as a reshaping treatment for other metal powders.
- the titanium powder is added to the fluidized reactor, and a certain flow of gas (Ar or H 2 ) is introduced into the fluidized bed reactor from top to bottom to eliminate The air in the fluidized reactor provides a gas-protected environment for the powder.
- a certain flow of gas Ar or H 2
- the fluidized bed reactor is removed from the heating system, and the protective gas is continuously vented. After the reactor is cooled in the air, the ventilation is stopped and the processed titanium powder is collected with a vacuum package.
- the protective atmosphere is used in the fluidization process, which effectively reduces the pollution risk of titanium powder in a high-temperature fluidized environment, and the content of impurities such as oxygen content of titanium powder after plastic treatment is effectively controlled.
- the product particles have good fluidity.
- the fluid shaping method is used to grind the sharp corners of irregularly shaped titanium powder through collision and friction between powder particles.
- the fluidity of the obtained titanium powder is effectively improved and better than 30s / 50g, which can meet 3D printing and The requirements of powder metallurgy near-net forming technology such as injection molding.
- Figure 2 is a scanning electron micrograph of the original titanium powder
- FIG. 3 is a scanning electron micrograph of titanium powder after fluidization treatment in Example 1,
- FIG. 4 Example 3 Scanning electron micrograph of titanium powder after fluidization treatment.
- Hydrogenated dehydrogenated irregularly shaped titanium powder with an average particle size of 30 ⁇ m was weighed into 20 g, added to the fluidized reactor, and Ar gas was introduced from the gas inlet at the lower end of the fluidized reactor.
- the flow rate is 0.5L / min, and the air in the fluidized reactor is removed in 30 minutes to prevent the oxidation of titanium powder. It was heated to 450 ° C, the flow rate was 1 L / min, fluidized and kept warm for 10 min, and the reactor was taken out to cool for 10 min, and then the powder was taken out and vacuum-encapsulated.
- the fluidized hydrogenated dehydrogenated titanium powder was subjected to microscopic morphology observation (see Figure 3) and the test of fluidity and oxygen content.
- the oxygen content of the powder was the difference between the oxygen content of the treated powder and the untreated powder.
- Table 1 the flowability test uses a Hall flowmeter funnel (diameter of 5mm), and the oxygen content is tested using an inert gas pulse infrared thermal conductivity method.
- the titanium powder after fluidization and shaping treatment has extremely low oxygen increase, and the fluidity meets the requirements of powder metallurgy near net forming processes such as 3D printing and injection molding.
- Hydrogenated dehydrogenated irregularly shaped titanium powder with an average particle size of 80 ⁇ m was weighed into 50 g, added to the fluidized reactor, and Ar gas was introduced from the gas inlet at the lower end of the fluidized reactor, the flow rate was 1 L / min, and the fluidized reaction was removed in 10 min The air in the device prevents the oxidation of titanium powder. It was heated to 500 ° C, the flow rate was 2L / min, fluidized and held for 20min, and the reactor was taken out to cool for 30min, and then the powder was taken out and vacuum encapsulated.
- the hydrodehydrogenated titanium powder subjected to fluidization treatment was subjected to microscopic morphology observation and fluidity and oxygen content tests, in which the oxygen content of the powder was the difference between the oxygen content of the treated powder and the untreated powder.
- the results are shown in Table 1. .
- the flowability test uses a Hall flowmeter funnel (diameter of 5mm), and the oxygen content is tested using an inert gas pulse infrared thermal conductivity method. Titanium powder after fluid shaping
- the titanium powder after fluid shaping is only 0.16wt.%, And the fluidity meets the requirements of powder metallurgy near net forming processes such as 3D printing and injection molding.
- Hydrogenated dehydrogenated irregularly shaped titanium powder with an average particle size of 40 ⁇ m was weighed into 200 g, added to the fluidized reactor, H 2 gas was introduced from the gas inlet at the lower end of the fluidized reactor, the flow rate was 0.8 L / min, and the flow was removed in 40 min Air in the reactor to prevent oxidation of titanium powder. It was heated to 550 ° C, the flow rate was 5 L / min, fluidized and kept warm for 60 min, and the reactor was taken out to cool for 25 min, and then the powder was taken out and vacuum-encapsulated. The fluidized hydrogenated dehydrogenated titanium powder was subjected to microscopic morphology observation (see Figure 4) and the test of fluidity and oxygen content.
- the oxygen content of the powder was the difference between the oxygen content of the treated powder and the untreated powder. As shown in Table 1. Among them, the flowability test uses a Hall flowmeter funnel (diameter of 5mm), and the oxygen content is tested using an inert gas pulse infrared thermal conductivity method. Titanium powder after fluid shaping The titanium powder after fluid shaping has a high oxygen content, but the fluidity meets the requirements of powder metallurgy near-net forming processes such as 3D printing and injection molding.
- Hydrogenated dehydrogenated irregularly shaped titanium powder with an average particle size of 120 ⁇ m was weighed into 200 g, added to the fluidized reactor, H 2 gas was introduced from the gas inlet at the lower end of the fluidized reactor, the flow rate was 1 L / min, and fluidization was removed in 40 min The air in the reactor prevents the oxidation of titanium powder. It was heated to 600 ° C, the flow rate was 3L / min, fluidized and kept warm for 70min, the reactor was taken out to cool for 30min, and then the powder was taken out and vacuum-encapsulated. The hydrodehydrogenated titanium powder subjected to fluidization treatment was subjected to microscopic morphology observation and testing of fluidity and oxygen content.
- the oxygen content of the powder was the difference between the oxygen content of the treated powder and the untreated powder.
- the flowability test uses a Hall flowmeter funnel (diameter of 5mm), and the oxygen content is tested using an inert gas pulse infrared thermal conductivity method. Titanium powder after fluid shaping The titanium powder after fluid shaping is too high in oxygen, but the fluidity meets the requirements of powder metallurgy near net forming processes such as 3D printing and injection molding.
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Abstract
一种3D打印用低成本钛粉的流化整形制备方法,具体制备方法为:使用低成本氢化脱氢不规则形状钛粉为粉末原料,将钛粉置于流化床反应器中,并通入Ar或H 2,气流流速为0.5~1.5L/min,将反应器加热至300~700℃,流化处理时间为5~90min,对钛粉进行流化整形处理,在流动高纯氩气及高温加热的状态下,通过粉末颗粒之间的碰撞和摩擦,对不规则形状钛粉的尖锐棱角进行打磨处理,使所得钛粉的流动性得到有效改善,其杂质含量也得到了有效控制,具有设备工艺简单、效率高、杂质含量可控、制备成本低等优点,所得低成本钛粉原料满足3D打印和注射成形等粉末冶金工艺要求。
Description
本发明属于金属粉末冶金制备技术领域,提供一种3D打印用低成本钛粉的流化整形制备方法。
钛是一种密度低、耐腐蚀好、比强度高、生物相容性优异的金属,主要应用于航空航天、石油化工、能源、生物医用等领域。近年来,利用3D打印和注射成形等粉末冶金近净成形工艺制备高性能且形状复杂的钛制品成为了国内外争相研究的热点。粉末冶金工艺对于钛粉末原料的性能要求较高,除了粒度及其组成、氧含量性能之外,特别对粉末流动性提出了较高的要求。因为,粉末流动性直接影响到粉末成形质量,比如3D打印过程中的粉末铺展均匀性或注射成形喂料中的粉末装载率(量)等,从而关乎最终制品的综合性能。因此,3D打印和注射成形等粉末冶金工艺通常使用粉末流动性较好的球形钛粉作为原料。球形钛粉主要采用惰性气体雾化、等离子旋转电极雾化、等离子熔丝雾化和等离子球化等方法制得,这些工艺所制钛粉的球形度较高,杂质含量较低,流动性较好。然而,上述球形钛粉的制备方法设备复杂、工艺繁琐,生产成本高(目前3D打印或注射成形用球形钛及钛合金粉末每公斤价格超过2000元),高昂的价格成为限制了粉末冶金钛制品的广泛应用的关键因素。因此,开发一种成本低、工艺过程简单、杂质含量可控、流动性好,且能满足粉末冶金工艺要求的钛粉制备或加工技术迫在眉睫。
发明内容
本发明的目的在于提供一种低成本制备球形度和流动性好,且能满足3D打印和注射成形等粉末冶金工艺要求的钛粉的方法,解决目前球形钛粉的生产设备要求高、工艺复杂、成本高等问题。
本发明首次将流化技术应用于不规则形状粉末的整形处理。流化技术是通过固体颗粒与气体或液体流体介质在容器中相互运动和接触,从而达到表面处理、 干燥或传质传热等目的,已被广泛用于化工、轻工、医药、食品等领域。本发明采用低成本氢化脱氢钛粉为原料,将钛粉至于流化反应器中,在保护气氛中于一定温度下通过粉末颗粒之间的碰撞和摩擦,达到钛粉整形的目的,从而改善粉末球形度,获得流动性好的钛粉,满足3D打印和注射成形等粉末冶金工艺的要求。该方法具有成本低、设备和工艺简单、效率高、杂质含量可控、粉末流动性改善效果明显等优点,也可用作其他金属粉末的整形处理。
一种3D打印用低成本钛粉的流化整形制备方法(示意图见图1),包括如下具体步骤:
(1)采用氢化脱氢不规则形状钛粉为原料,将钛粉加入流化反应器中,自上而下地往流化床反应器通入一定流量的气体(Ar或者H
2),以排除流化反应器内的空气,为粉末提供气体保护环境。
(2)待流化床反应器内部空气排完之后,将其移至加热系统中,流化过程中连续通入稳定流量的气体(Ar或者H
2),气流流速为0.5~1.5L/min,并加热温度至300~700℃,在恒温下流化5~90min。流化过程中,由于气流的作用,钛粉颗粒漂浮于反应器中,并发生颗粒间的相互碰撞和摩擦,使其表面形貌和粒度组成发生变化。
(3)流化结束后,将流化床反应器移出加热系统,持续通保护气体,待反应器待在空气中冷却,停止通气并用真空封装收集处理后的钛粉。
本发明首次采用流化技术对钛粉进行整形处理,具有成本低、氧含量可控、粉末整形效果好等优势,具体如下:
(1)成本低。采用氢化脱氢不规则形状钛粉作为原料,降低了粉末原料的成本;采用流化床工艺对不规则形状钛粉进行整形处理,设备简易,工艺简单,效率高,工艺成本低;钛粉收得率接近100%,同样也降低了生产成本。
(2)无污染,氧含量易控。在流化过程中采用保护气氛,有效降低了钛粉在高温流化环境中的污染风险,整形处理后的钛粉氧元素等杂质含量得到有效控制。
(3)产物颗粒流动性好。采用流化整形方法通过粉末颗粒之间的碰撞和摩擦,对不规则形状钛粉的尖锐棱角进行打磨处理,所得钛粉的流动性 得到了有效改善且优于30s/50g,能够满足3D打印和注射成形等粉末冶金近净成形工艺的要求。
表1不同温度流化处理后钛粉的流动性和增氧量(相对于原始未处理钛粉)
图1为流化处理钛粉装置及工艺过程示意图,
图2为原始钛粉扫描电镜照片,
图3为实例1流化处理后钛粉扫描电镜照片,
图4实例3流化处理后钛粉扫描电镜照片。
实施例1
将平均粒径30μm的氢化脱氢不规则形状钛粉(显微形貌如图2所示)称量20g、加入流化反应器中,从流化反应器下端进气口通入Ar气,流量为0.5L/min,30min除去流化反应器内的空气,防止钛粉氧化。加热至450℃,流量为1L/min,流化并保温10min,取出反应器冷却10min,随后将粉末取出并进行真空封装。将经过流化处理的氢化脱氢钛粉进行显微形貌观察(见图3)及流动性和氧含量的测试,其中粉末增氧量为处理粉末与未处理粉末的氧含量之差,结果如表1所示。其中,流动性测试采用霍尔流速计漏斗(直径为5mm)、氧含量采用惰气脉冲红外热导法测试。流化整形处理后的钛粉增氧量极低,且流动性满足3D打印和注射成形等粉末冶金近净成形工艺的要求。
实施例2
将平均粒径80μm的氢化脱氢不规则形状钛粉称量50g、加入流化反应器中,从流化反应器下端进气口通入Ar气,流量为1L/min,10min除去流化反应器内的空气,防止钛粉氧化。加热至500℃,流量为2L/min,流化并保温20min,取出反应器冷却30min,随后将粉末取出并进行真空封装。将经过流化处理的氢化脱氢钛粉进行显微形貌观察及流动性和氧含量的测试,其中粉末增氧量为处理粉末与未处理粉末的氧含量之差,结果如表1所示。其中,流动性测试采用霍尔流速计漏斗(直径为5mm)、氧含量采用惰气脉冲红外热导法测试。流化整形处理后的钛粉流化整形处理后的钛粉增氧量仅为0.16wt.%,且流动性满足3D打印和注射成形等粉末冶金近净成形工艺的要求。
实施例3
将平均粒径40μm的氢化脱氢不规则形状钛粉称量200g、加入流化反应器中,从流化反应器下端进气口通入H
2气,流量为0.8L/min,40min除去流化反应器内的空气,防止钛粉氧化。加热至550℃,流量为5L/min,流化并保温60min,取出反应器冷却25min,随后将粉末取出并进行真空封装。将经过流化处理的氢化脱氢钛粉进行显微形貌观察(见图4)及流动性和氧含量的测试,其中粉末增氧量为处理粉末与未处理粉末的氧含量之差,结果如表1所示。其中,流动性测试采用霍尔流速计漏斗(直径为5mm)、氧含量采用惰气脉冲红外热导法测试。流化整形处理后的钛粉流化整形处理后的钛粉增氧量偏高,但流动性满足3D打印和注射成形等粉末冶金近净成形工艺的要求。
实施例4
将平均粒径120μm的氢化脱氢不规则形状钛粉称量200g、加入流化反应器中,从流化反应器下端进气口通入H
2气,流量为1L/min,40min除去流化反应器内的空气,防止钛粉氧化。加热至600℃,流量为3L/min,流化并保温70min,取出反应器冷却30min,随后将粉末取出并进行真空封装。将经过流化处理的氢化脱氢钛粉进行显微形貌观察及流动性和氧含量的测试,其中粉末增氧量为处理粉末与未处理粉末的氧含量之差,结果如表1所示。其中,流动性测试采用霍尔流速计漏斗(直径为5mm)、氧含量采用惰气脉冲红外热导法测试。流化整形处理后的钛粉流化整形处理后的钛粉增氧量过高,但流动性满足3D打印和注射成形等粉末冶金近净成形工艺的要求。
Claims (3)
- 一种3D打印用低成本钛粉的流化整形制备方法,其特征在于制备步骤如下:(1)采用氢化脱氢不规则形状钛粉为原料,将钛粉加入流化反应器中,自上而下地往流化床反应器通入一定流量的Ar或者H 2,以排除流化反应器内的空气,为粉末提供气体保护环境;(2)待流化床反应器内部空气排完之后,将其移至加热系统中,流化过程中连续通入稳定流量的Ar或者H 2,并加热至一定温度下恒温流化;流化过程中,由于气流的作用,钛粉颗粒漂浮于反应器中,并发生颗粒间的相互碰撞和摩擦,使其表面形貌和粒度组成发生变化;(3)流化结束后,将流化床反应器移出加热系统,持续通保护气体,待反应器待在空气中冷却,停止通气并用真空封装收集处理后的钛粉。
- 如权利要求1所述3D打印用低成本钛粉的流化整形制备方法,其特征在于Ar或者H 2气流流速为0.5~1.5L/min。
- 如权利要求1所述3D打印用低成本钛粉的流化整形制备方法,其特征在于加热温度为300~700℃,恒温流化时间为5~90min。
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