射频等离子体制备增材制造用球形钛钽合金粉末

应真鸿; 谭冲; 施麒; 李贵发; 郑海忠; 刘辛

doi:10.7513/j.issn.1004-7638.2021.03.010

射频等离子体制备增材制造用球形钛钽合金粉末

doi: 10.7513/j.issn.1004-7638.2021.03.010

应真鸿^{1, 2,},
谭冲²,
施麒²,
李贵发¹,
郑海忠¹,
刘辛^2, ,

1.
南昌航空大学材料科学与工程学院，江西南昌 330063
2.
广东省科学院材料与加工研究所，广东广州 510650

基金项目: 国家外国专家项目（G20200130024）；广东省重点领域研发计划（2018B0909040004-5）；广州市重点领域研发计划（202007020008）；广州市对外科技合作（201907010030）

详细信息

作者简介:
应真鸿（1996—），男，汉，江西南昌人，硕士研究生，主要从事金属粉体制备及其近净成形制造研究，E-mail：804270370@qq.com；

通讯作者:
刘辛，男，汉，教授级高级工程师，主要从事金属粉体制备及其近净成形制造研究。E-mail：liuxin@gimp.gd.cn

中图分类号: TF823
计量
- 文章访问数: 449
- HTML全文浏览量: 67
- PDF下载量: 29
- 被引次数: 0
出版历程
- 收稿日期: 2021-04-07
- 刊出日期: 2021-06-10

Preparation of spherical titanium-tantalum alloy powder for additive manufacturing by radio frequency plasma

Ying Zhenhong^{1, 2
,},
Tan Chong²,
Shi Qi²,
Li Guifa¹,
Zheng Haizhong¹,
Liu Xin^{2
, ,}

1.
School of Materials Science and Engineering, Nanchang Hangkong University, Nanchang 330063, Jiangxi, China
2.
Institute of Materials and Processing, Guangdong Academy of Sciences, Guangzhou 510650, Guangdong, China

摘要

摘要: 采用射频等离子体球化技术对氢化破碎不规则形貌的钛钽合金粉末进行球化处理，研究了送粉速率、载气流量和鞘气中氦气流量等工艺参数对钛钽合金粉末球化率、粉体性能和显微结构的影响，并开展了球化后钛钽合金粉末选区激光熔化成形适用性评价。结果表明：经过射频等离子体球化处理后，粉末截面组织由板条状α″-Ti和胞状β-Ti组成，球化率在98%以上，粒度分布变宽，平均粒径由球化前21.41 μm增大至32.3 μm。粉末球化率受送粉速率、载气流量和鞘气中氦气流量等因素影响，当送粉速率为35 g/min，载气流量为5.5 L/min，鞘气中氦气流量为40 L/min，球化效果最好。与原料粉末相比，球化后粉末的霍尔流速(50 g计)为6.27 s，松装密度由1.38 g/cm³提高至3.11 g/cm³，振实密度由2.54 g/cm³提高至3.48 g/cm³。此外，球化后的钛钽合金粉末具有良好的选区激光熔化适用性，成形后制件致密度大于99%，微观组织为针状α″-Ti和胞状β-Ti，钛、钽元素分布均匀，无未熔融的钽颗粒，显微硬度（HV）达到725。
- 钛钽合金粉末 /
- 射频等离子体球化 /
- 粉体特性 /
- 选区激光熔化 /
- 显微结构
Abstract: The titanium-tantalum alloy powder prepared by hydrogen decrepitation process with irregular morphology was spheroidized by radio frequency (RF) plasma. The effects of feeding rate, carrier gas flow rate and sheath gas (He) flow rate on the spheroidization efficiency, powder characteristics and microstructure were studied. The selective laser melting (SLM) process of the spherical titanium-tantalum alloy powder was also explored. The results show that the cross-sectional microstructure of the powder is lamellar α″-Ti and cellular β-Ti after spheroidization, with the spheroidization efficiency over 98%. The particle size distribution becomes wider and the average particle size increases from 21.41 μm to 32.30 μm. The spheroidization efficiency is influenced by the feeding rate, carrier gas flow rate, sheath gas (He) flow rate. The best spheroidization efficiency can be obtained at 35 g/min of feeding rate, 5.5 L/min of carrier gas flow rate and 40 L/min of sheath gas (He) flow rate, respectively. Compared with the raw powder, the hall velocity of the spherical titanium-tantalum alloy powder reaches 6.27 s/50 g, with the apparent density and tap density increased from 1.38 g/cm³ to 3.11 g/cm³, 2.54 g/cm³ to 3.48 g/cm³, respectively. The spherical titanium-tantalum alloy powder is compatible with the selective laser melting process. The relative density of the formed parts is over 99%, with the microstructure of acicular α″-Ti and cellular β-Ti. No unmelted tantalum particles can be found in the samples and the vickers hardness of the samples reaches 725 HV.
- titanium-tantalum alloy powder /
- RF plasma spheroidization /
- powder characteristics /
- selected laser melting /
- microstructure

HTML全文

图 1 钛钽合金粉末球化处理前后形貌

(a)球化前；(b)球化后；(c)球化后粉末截面；(d)球化后粉末开裂缺陷

Figure 1. SEM images of titanium-tantalum alloy powder

下载: 全尺寸图片幻灯片

图 2 粉末EDS能谱

(a)扫描电子显微镜图像；(b)钛元素分布；(c)钽元素分布

Figure 2. EDS of powders

下载: 全尺寸图片幻灯片

图 3 钛钽合金粉末球化前后XRD图谱

Figure 3. XRD patterns of titanium-tantalum alloy powder before and after spheroidization

下载: 全尺寸图片幻灯片

图 4 钛钽合金粉末球化前后粒度分布

Figure 4. Particle size distribution of titanium-tantalum alloy powder before and after spheroidization

下载: 全尺寸图片幻灯片

图 5 不同送粉速率下球化钛钽合金粉末的SEM形貌

Figure 5. SEM images of titanium-tantalum alloy powder prepared at different powder feeding rates

(a) 28 g/min; (b) 35 g/min; (c) 42 g/min

下载: 全尺寸图片幻灯片

图 6 不同载气流量下球化钛钽合金粉末的SEM形貌

Figure 6. SEM images of titanium-tantalum alloy powder prepared at different carrier gas flow rates

(a) 3.0 L/min; (b) 5.5 L/min; (c) 7.0 L/min

下载: 全尺寸图片幻灯片

图 7 不同载气流量下球化钛钽合金粉末的截面组织

(a) 3.0 L/min；(b) 7.0 L/min；(c) 为(a)的局部区域放大；(d)为(b)的局部区域放大

Figure 7. Cross-section microstructure of titanium-tantalum alloy powder prepared at different carrier gas flow rates

下载: 全尺寸图片幻灯片

图 8 不同氦气流量下球化钛钽合金粉末的SEM形貌

Figure 8. SEM images of titanium-tantalum alloy powder prepared at different sheath gas (He) flow rates

(a) 0 L/min; (b) 20 L/min; (c) 40 L/min

下载: 全尺寸图片幻灯片

图 9 选区激光熔化制备钛钽合金的密度随激光能量密度的变化曲线

Figure 9. Relative density of SLM-processed Ti-Ta alloys fabricated by different laser energy densities

下载: 全尺寸图片幻灯片

图 10 SLM打印钛钽合金试样的XRD谱图

Figure 10. XRD patterns of SLM-processed Ti-Ta alloys

下载: 全尺寸图片幻灯片

图 11 SLM打印钛钽合金试样的组织结构

(a)本试验；(b)其他文献^[23]

Figure 11. Microstructure of SLM-processed Ti-Ta alloys

下载: 全尺寸图片幻灯片

图 12 SLM打印钛钽合金试样的电子显微镜形貌

Figure 12. SEM morphology of SLM-processed Ti-Ta alloys

下载: 全尺寸图片幻灯片

图 13 打印试样表面EDS能谱

(a)扫描电镜图像；(b)钽元素分布；(c)钛元素分布

Figure 13. EDS of SLM-processed Ti-Ta alloys

下载: 全尺寸图片幻灯片

图 14 SLM成形钛钽合金试样的维氏硬度随激光能量密度变化曲线

Figure 14. Vickers hardness of SLM processed Ti-Ta alloys fabricated by different laser energy densities

下载: 全尺寸图片幻灯片

表 1 原料钛钽合金粉末化学成分

Table 1. Chemical composition of raw titanium-tantalum alloy powder %

Ti	Ta	H	O	C
Bal.	28.24	2.84	0.85	0.024

下载: 导出CSV

表 2 射频等离子体球化工艺参数

Table 2. Experimental parameters for RF plasma spheroidization

功率/kW	鞘气流量1(Ar)/(L·min⁻¹)	鞘气流量2(He)/(L·min⁻¹)	载气流量(Ar)/(L·min⁻¹)	送粉速率/(g·min⁻¹)
20～40	30～50	20～40	3～7	28～42

下载: 导出CSV

表 3 选区激光熔化成形参数

Table 3. SLM process parameters used for this study

编号	激光功率/W	扫描速度/(mm·s⁻¹)	层厚/μm	扫描间距/μm	激光能量密度/(J·mm⁻³)
1	80	400	30	60	111.11
2	120	400	30	60	166.66
3	160	400	30	60	222.22
4	80	500	30	60	88.88
5	120	500	30	60	133.33
6	160	500	30	60	177.78
7	80	600	30	60	74.00
8	120	600	30	60	111.11
9	160	600	30	60	148.15

下载: 导出CSV

表 4 球化后钛钽合金粉末化学成分

Table 4. Chemical composition of titanium-tantalum alloy powder after spheroidization %

Ti	Ta	H	O	C
Bal.	29.62	2.28	0.8	0.024

下载: 导出CSV

表 5 钛钽合金粉末球化前后的粉末特征

Table 5. Particle characteristics of titanium-tantalum alloy powder before and after spheroidization

粉末	流动性(50 g计)/s	松装密度/(g·cm⁻³)	振实密度/(g·cm⁻³)	氧含量/%
原料粉末		1.375	2.542	0.85
球化粉末	6.27	3.113	3.478	0.8

下载: 导出CSV

参考文献(23)

[1]	Niinomi M. Recent metallic materials for biomedical applications[J]. Metallurgical & Materials Transactions A, 2002,33(3):477.
[2]	Laheurte P, Prima F, Eberhardt A, et al. Mechanical properties of low modulus β titanium alloys designed from the electronic approach[J]. J Mech Behav Biomed Mater, 2010,3(8):565−573. doi: 10.1016/j.jmbbm.2010.07.001
[3]	Xu Lijuan, Xiao S L, Tian J, et al. Microstructure, mechanical properties and dry wear resistance of β-type Ti-15Mo-xNb alloys for biomedical applications[J]. Transactions of Nonferrous Metals Society of China, 2013,23(3):692−698. doi: 10.1016/S1003-6326(13)62518-2
[4]	Taekyung, Lee, Yoon-Uk, et al. Microstructure tailoring to enhance strength and ductility in Ti–13Nb–13Zr for biomedical applications[J]. Scripta Materialia, 2013,69(11−12):785−788. doi: 10.1016/j.scriptamat.2013.08.028
[5]	Pokluda J. Theoretical strength of solids: recent results and applications[J]. Materials Science, 2012,47(5):492−495.
[6]	Ying L Z, Niinomi M, Akahori T. Effects of Ta content on Young’s modulus and tensile properties of binary Ti–Ta alloys for biomedical applications[J]. Mater Sci Eng A, 2004,371(1/2):283−290.
[7]	Zhou Y L, Niinomi M, Akahori T, et al. Corrosion resistance and biocompatibility of Ti-Ta alloys for biomedical applications[J]. Materials Science & Engineering A, 2005,398(1−2):28−36.
[8]	Yang Xuechun, Jiang Wenjun, Cao Ming, et al. Organization and mechanical properties of selected laser melting aluminum alloys[J]. Machine Tools and Hydraulics, 2021,49(1):21−25, 41. (杨雪春, 江文俊, 曹铭, 等. 选区激光熔化铝合金的组织和力学性能[J]. 机床与液压, 2021,49(1):21−25, 41. doi: 10.3969/j.issn.1001-3881.2021.01.005
[9]	Sing, Leong S, Yeong, et al. Selective laser melting of titanium alloy with 50 % tantalum: Microstructure and mechanical properties[J]. Journal of Alloys and Compounds: An Interdisciplinary Journal of Materials Science and Solid-state Chemistry and Physics, 2016,660(5):263−265.
[10]	Egba B, Aema C, Jef A, et al. Remelt processing and microstructure of selective laser melted Ti25Ta-science direct[J]. Journal of Alloys and Compounds, 2020,820(6):363−366.
[11]	Dz A, Ch B, Yan L A, et al. Improvement on mechanical properties and corrosion resistance of titanium-tantalum alloys in-situ fabricated via selective laser melting[J]. Journal of Alloys and Compounds, 2019,804:288−298. doi: 10.1016/j.jallcom.2019.06.307
[12]	Gou Y J, Chen G, Zhao S Y, et al. Titanium-tantalum alloy powder produced by the plasma rotating electrode process (PREP)[J]. Key Engineering Materials, 2018,770:18−22. doi: 10.4028/www.scientific.net/KEM.770.18
[13]	Bai L, Fan J, Peng H, et al. RF plasma synthesis of nickel nanopowders via hydrogen reduction of nickel hydroxide/carbonate[J]. Journal of Alloys & Compounds, 2009,481(1−2):563−567.
[14]	Kumar R, Cheang P, Khor K A. Radio frequency (RF) suspension plasma sprayed ultra-fine hydroxyapatite (HA)/zirconia composite powders[J]. Biomaterials, 2003,24(15):2611−2621. doi: 10.1016/S0142-9612(03)00066-8
[15]	A Y Y, A M M H, A T W, et al. Effects of feed rate and particle size on the in-flight melting behavior of granulated powders in induction thermal plasmas[J]. Thin Solid Films, 2008,516(19):6622−6627. doi: 10.1016/j.tsf.2007.11.084
[16]	Wang J J, Hao J J, Guo Z M, et al. Preparation of spherical tungsten and titanium powders by RF induction plasma processing[J]. Rare Metals, 2015,34(6):431−435. doi: 10.1007/s12598-014-0293-4
[17]	Jiang X L, Boulos M. Induction plasma spheroidization of tungsten and molybdenum powders[J]. Transactions of Nonferrous Metals Society of China, 2006,16(1):13−17. doi: 10.1016/S1003-6326(06)60003-4
[18]	Gu Zhongtao, Ye Gaoying, Jin Yuping. Component analysis of spherical titanium powder prepared by radio frequency induction plasma[J]. Intense Laser and Particle Beam, 2012,24(6):1409−1413. (古忠涛, 叶高英, 金玉萍. 射频感应等离子体制备球形钛粉的成分分析[J]. 强激光与粒子束, 2012,24(6):1409−1413. doi: 10.3788/HPLPB20122406.1409
[19]	Hou Y B, Zeng K L, Yue-Guang Y U, et al. Plasma spheroidization of tungsten powder[J]. Nonferrous Metals, 2008,(1):41−43.
[20]	Harbec D, Gitzhofer F, Tagnit-Hamou A. Induction plasma synthesis of nanometric spheroidized glass powder for use in cementitious materials[J]. Powder Technology, 2011,214(3):356−364. doi: 10.1016/j.powtec.2011.08.031
[21]	Zhang Ge, Wang Jianhong, Zhang Hao. Study on spheroidization phenomenon of laser melting in selected areas of metal powder[J]. Casting Technology, 2017,38(2):262−265. (张格, 王建宏, 张浩. 金属粉末选区激光熔化球化现象研究[J]. 铸造技术, 2017,38(2):262−265.
[22]	Leong S S, Edith W F, Yee Y W. Selective laser melting of titanium alloy with 50 % tantalum: Effect of laser process parameters on part quality[J]. International Journal of Refractory Metals and Hard Materials, 2018,77:120−127. doi: 10.1016/j.ijrmhm.2018.08.006
[23]	Soro N, Attar H, Brodie E, et al. Evaluation of the mechanical compatibility of additively manufactured porous Ti–25Ta alloy for load-bearing implant applications[J]. Journal of the Mechanical Behavior of Biomedical Materials, 2019,97(3):326−329.