Application of ultrafine metal powder injection moulding on tungsten components in fusion devices
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摘要: 从超细粉末制备、喂料准备、注射工艺、烧结工艺和热等静压处理等方面研究了超细纯钨粉以及超细稀土氧化物弥散增强钨粉的金属注射成形技术，利用该技术制备了聚变装置中的钨零部件，并对这种超细金属粉末注射成形钨零件的微观组织和热力学性能进行了分析。结果表明：超细纯钨粉零件相对密度可达98%以上，平均晶粒尺寸10~15 μm，500℃以上的热导率与锻造钨零件相当；超细稀土氧化物弥散增强钨粉零件相对密度可达99%以上，平均晶粒尺寸3~5 μm，抗热冲击性能优良。Abstract: Metal injection moulding (MIM) technology used for ultrafine pure W powders and rare earth oxides dispersion strengthened-W (ODS-W) powders was investigated, including ultrafine powders preparation, feedstock preparation, injection molding technology, sintering technology, and hot isostatic pressing treatment. This technology was applied to manufacture the tungsten components in fusion devices. Microstructures and thermodynamic performances of the tungsten components prepared by this ultrafine metal powder injection moulding technology were analyzed. The results show that, the MIM tungsten components used with ultrafine pure W powders (MIM-W) can achieve the relative density more than 98%, the average grain size is about 10~15 μm, and the thermal conductivity (above 500℃) of MIM-W is close to that of the wrought tungsten components. The MIM tungsten components used with rare earth oxides dispersion strengthened-W powders (MIM-ODS-W) can achieve the relative density more than 99%, the average grain size is 3~5 μm, and the thermal shock resistance of MIM-ODS-W shows excellent.
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图 1 实验用超细粉末显微组织形貌：（a）W粉；（b）W–1.2Y2O3粉
Figure 1. SEM images of ultrafine powders used in the experiment: (a) W powders; (b) W–1.2Y2O3 powders
图 2 喂料装载量与转矩关系曲线：（a）超细纯W粉；（b）超细W–1.2Y2O3粉
Figure 2. Relationship of loading capacity and torque: (a) ultrafine W powders; (b) ultrafine W–1.2Y2O3 powders
图 3 金属注射成形样品：（a）朗缪尔探针纯W本体和热屏；（b）氦冷却偏滤器W–1.2Y2O3套筒
Figure 3. Fabricated samples by MIM: (a) main body and shielding by MIM–W powders for Langmiur probe; (b) thimble parts by MIM–W–1.2Y2O3 powders for helium cooling divertor
图 4 MIM–W和MIM–W–1.2Y2O3零件微观组织：（a）MIM–W烧结；（b）MIM–W–1.2Y2O3烧结；（c）MIM–W烧结+热等静压；（d）MIM–W–1.2Y2O3烧结+热等静压
Figure 4. Microstructures of MIM–W and MIM–W–1.2Y2O3 components: (a) sintered MIM–W; (b) sintered MIM–W–1.2Y2O3; (c) sintered + HIP MIM–W; (d) sintered + HIP MIM–W–1.2Y2O3
图 5 MIM–W零件、MIM–W–1.2Y2O3零件和锻造W零件的热导率
Figure 5. Thermal conductivity of MIM–W, MIM–W–1.2Y2O3, and wrought W components
图 6 室温下未经热等静压处理的MIM–W和W–1.2Y2O3样品初步热冲击测试结果：（a）MIM–W，160 MW·m-2；（b）MIM–W，220 MW·m-2；（c）MIM–W，330 MW·m-2；（d）MIM–W–1.2Y2O3，220 MW·m-2；（e）MIM–W–1.2Y2O3，330 MW·m-2
Figure 6. Preliminary thermal shock test results at room temperature of MIM–W and W–1.2Y2O3 samples without HIP treatment: (a) MIM–W, 160 MW·m-2; (b) MIM–W, 220 MW·m-2; (c) MIM–W, 330 MW·m-2; (d) MIM–W–1.2Y2O3, 220 MW·m-2; (e) MIM–W–1.2Y2O3, 330 MW·m-2
表 1 超细W粉和W–1.2Y2O3粉中气体元素成分（质量分数）
Table 1. Composition of gaseous elements in ultrafine W and W–1.2Y2O3 powders
% 粉末 N O C W 0.0151 0.1500 0.0048 W–1.2Y2O3 0.0150 0.0820（排除Y2O3中的O元素） 0.0035 
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表 2 超细W粉和W–1.2Y2O3粉末物理性能
Table 2. Physical properties of ultrafine W and W–1.2Y2O3 powders
粉末 粒度分布/ μm 平均粒度/ μm 松装密度/ (g·cm-3) 振实密度/ (g·cm-3) 理论密度/ (g·cm-3) D10 D50 D90 W 1.422 3.145 5.738 0.70 2.47 4.81 19.23 W–1.2Y2O3 2.264 4.846 9.711 0.82 2.04 4.08 18.61
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表 3 超细纯W粉生坯注射工艺
Table 3. Injection molding parameters of green prepared by ultrafine W powders
温度/ ℃ 注射参数 保压参数 喷嘴 料筒温区2 料筒温区3 料筒温区4 料筒温区5 模温 速度/ (cm3·s-1) 压力/ MPa 进料量/ cm3 料垫/ cm3 背压/ MPa 冷却时间/ s 速度/ (cm3·s-1) 压力/ MPa 时间/ s 153 157 157 157 153 40 14 160 9.2 2.1 2.5 10 15 50 0.5
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表 4 超细W–1.2Y2O3粉生坯注射工艺
Table 4. Injection molding parameters of green prepared by ultrafine W–1.2Y2O3 powders
温度/ ℃ 注射参数 保压参数 喷嘴 料筒温区2 料筒温区3 料筒温区4 料筒温区5 模温 速度/ (cm3·s-1) 压力/ MPa 进料量/ cm3 料垫/ cm3 背压/ MPa 冷却时间/ s 速度/ (cm3·s-1) 压力/ MPa 时间/ s 155 158 158 158 155 25 12 100 5.3 2.1 2.5 10 12 50 0.3
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表 5 超细金属粉末注射成形钨材化学成分（质量分数）
Table 5. Chemical composition of MIM–W materials
×10-6 C O N Ta Th Al S Ca Hg U Cr Fe Ti Re Ni Zn Co F 其他 W < 5 < 10 < 5 < 1 < 0.0001 0.03 0.02 0.03 < 0.1 < 0.0001 0.08 0.01 0.02 < 0.05 0.02 0.02 0.008 < 0.01 < 0.38 基体
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表 6 MIM–W粉和MIM–W–1.2Y2O3粉烧结后物理性能
Table 6. Physical properties of W powders and W–1.2Y2O3 powders after sintering
加工参数和物理性能 W粉 W–1.2Y2O3粉 烧结 烧结+ 热等静压 烧结 烧结+ 热等静压 烧结参数 1950 ℃，4 h 1700 ℃，2 h 1950 ℃，4 h 1700 ℃，2 h 热等静压参数 — 1700 ℃，180 MPa，1 h — 1700 ℃，180 MPa，1 h 密度/ (g·cm-3) 18.95 18.97 18.35 18.47 相对密度/ % 98.2 98.5 98.6 99.2 硬度，HV30 388 403 450 447 晶粒尺寸/ μm 20~30 10~15 3~5 3~5
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