CN111054914A - 一种电子束选区熔化成形用tc4钛合金粉末及其制备方法和应用 - Google Patents
一种电子束选区熔化成形用tc4钛合金粉末及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种电子束选区熔化成形用TC4钛合金粉末及其制备方法和应用，属于增材制造技术领域。本发明的目的是提供一种能够适用于电子束选区熔化成形，且具有良好的流动性、球形度和颗粒度的TC4钛合金粉末，来满足航空航天领域对电子束选区熔化成形航空航天精密结构件的应用需求。本发明采用真空感应熔炼气体雾化工艺，在惰性气体的冲击下合金溶液破碎，冷却凝固得到钛合金粉末，然后采用旋风分离技术对制得球形TC4钛合金粉末进行筛分处理。本发明制备得到的TC4钛合金粉末，具有粒径范围广，细粉收得率高，球形度好等优点。且该粉末在电子束成形舱中铺粉效果良好，打印性能均一，表面质量优良。
Description
技术领域
本发明涉及一种电子束选区熔化成形用TC4钛合金粉末及其制备方法和应用，属于增材制造技术领域。
背景技术
随着国内金属增材制造技术的不断发展，多种采用增材制造技术生产的钛合金件已经完成了在航天型号产品中的工程化验证，使金属增材制造技术的应用优势更加明显。作为金属增材制造的原材料，电子束选区熔化成形使用的TC4钛合金粉末由于其具有的熔点高、活性高等化学性质，是制备难度很大的耗材粉末。并且粉末的流动性、成分均一性、粒径均匀度、球形度等对电子束选区熔化成形质量具有显著的影响。因此提供一种能够适用于电子束选区熔化成形，且具有良好的流动性、球形度和颗粒度的TC4钛合金粉末，来满足航空航天领域对电子束选区熔化成形航空航天精密结构件的应用需求是十分必要的。
发明内容
本发明目的在于提供一种电子束选区熔化成形用TC4钛合金粉末制备优化方法，通过该方法批量制备出成分均一、流动性好、粒径均匀、球形度好、低杂质含量的TC4基合金粉末，满足航空航天领域对电子束选区熔化成形航空航天精密结构件的应用需求。
本发明的技术方案：
一种电子束选区熔化成形用TC4钛合金粉末，该粉末为球状颗粒，粒径为15μm～500μm，流动性30s/50g以下，松装密度为2.25g/cm3以下。
一种电子束选区熔化成形用TC4钛合金粉末的制备方法，该方法包括以下步骤：
步骤一，雾化制粉：对TC4钛合金锭清洗后，使用雾化制粉设备对TC4钛合金锭进行感应熔炼和雾化制粉处理，获得粒径为53μm～106μm的TC4钛合金粉末；
步骤二，筛分处理：采用旋风分离技术对粒径为15μm～500μm的TC4钛合金粉末的进行筛分处理，获得粒径范围为53μm～106μm的电子束选区熔化成形用TC4钛合金粉末。其中，通过旋风分离技术能获得粒径范围在15μm～52μm，53μm～106μm，107μm～250μm和251μm～500μm等粒径尺寸范围内的钛合金粉末，本发明选取53μm～106μm粒径尺寸范围内的钛合金粉末用于电子束选区熔化成形。
进一步限定，TC4钛合金锭化学成分按质量百分比为：Al：5.50％～6.75％，V：3.50％～4.50％，Fe：≤0.3％，C：≤0.3％，H：≤0.12％，O：≤0.18％，N：≤0.04％，余量为Ti。
进一步限定，步骤一中对TC4钛合金锭清洗的具体操作过程为：使用酸洗液对TC4钛合金锭进行酸洗后，使用去离子水清洗，并用无水乙醇擦拭；其中酸洗液由HF、HNO3和蒸馏水组成，其中HF、HNO3和H2O的质量比为2:5:93。
进一步限定，步骤一的雾化制粉过程中使用分瓣水冷铜坩埚进行感应熔炼，感应熔炼工艺过程为：100KW保温1min～2min后，升至200KW后保温2min～3min，然后升至250KW保温1min～2min，然后升至300KW保温2min～3min，最后升至370KW保温2min～3min。
进一步限定，感应熔炼的熔炼室真空度为10Pa以下，熔炼室充气压力为90KPa～93KPa，熔炼室漏率为150Pa/h以下，雾化舱真空度为10Pa以下，雾化舱充气压力为90KPa～93KPa，雾化舱漏率为150Pa/h以下，储气罐压力为6.5MPa以上。
进一步限定，步骤一的雾化制粉过程中在钛液温度为1750℃～1800℃，开启惰性气体喷嘴，喷气压力为4.5MPa～5.5MPa。
进一步限定，步骤一雾化制粉过程中采用环形辅气促进雾化液滴冷却，并在雾化舱底部实施反喷氩气，反喷气压力为0.4MPa。
进一步限定，步骤二的筛分过程中旋风分离的气流分级压力为0.5MPa，引风频率为13Hz。
应用上述方法制得的TC4钛合金粉末通过电子束选区熔化成形打印方法，该方法的电子束选区熔化成形的工艺参数为：偏焦电流为25mA，扫描线间距为0.20mm，扫描速度指数为18。
本发明具有以下有益效果：本发明制备的应用于电子束选区熔化成形，粒径为53μm～106μm规格的TC4钛合金粉收得率为20％～40％。本发明制备得到的TC4钛合金粉末，具有粒径范围广，细粉收得率高，球形度好。在电子束成形舱中铺粉效果良好，打印性能均一，表面质量优良等优点。此外，使用本发明制得的TC4钛合金粉通过电子束选区熔化成形得到的打印构件具有力学性能优良，强度高等优点。
附图说明
图1为TC4钛合金粉末的形貌图以及局部放大图；
图2为图1的局部放大图；
图3为使用TC4钛合金粉末采用电子束3D打印获得的测试构件示意图。
具体实施方式
下述实施例中所使用的实验方法如无特殊说明均为常规方法。
具体实施方式1：
电子束选区熔化成形用TC4钛合金粉末的制备
步骤一，制粉：首先，使用酸洗液对TC4钛合金锭进行酸洗，然后使用去离子水清洗，并用无水乙醇擦拭。其中，酸洗液由HF、HNO3和蒸馏水组成，其中HF、HNO3和H2O的质量比为2:5:93；TC4钛合金锭的化学成分按质量百分比为：Al：5.50％～6.75％，V：3.50％～4.50％，Fe：≤0.3％，C：≤0.3％，H：≤0.12％，O：≤0.18％，N：≤0.04％，余量为Ti。然后，使用分瓣水冷铜坩埚对TC4钛合金锭进行感应熔炼，感应熔炼的熔炼室真空度为4±0.2Pa，熔炼室充气压力为92±0.2KPa，熔炼室漏率为120±0.2Pa/h，雾化舱真空度为4±0.2Pa，雾化舱充气压力为92±0.2KPa，雾化舱漏率为120±0.2Pa/h，储气罐压力为8.5±0.2MPa，感应熔炼工艺过程见下表。
| 加载功率 | 100KW | 200KW | 250KW | 300KW | 370KW |
| 保温时间 | 12min | 2min | 2min | 3min | 3min |
在钛液实际温度达到1780±10℃时，开启高压惰性气体喷嘴，喷气压力为5.0±0.2MPa。并采用环形辅气促进雾化液滴冷却，在雾化舱底部实施反喷氩气，反喷气压压力0.4MPa。获得粒径为15μm～500μm的TC4钛合金粉末。其中在雾化舱底部实施反喷氩气除可以避免粉末粘连团聚外，还可以在降低液滴喷射速度的同时，又对合金液滴起冷却作用，从而避免粉末粘连团聚减少卫星球数量。
步骤二，筛分处理：采用旋风分离技术对粒径为15μm～500μm的TC4钛合金粉末的进行筛分处理，其中气流分级压力为0.5MPa，引风频率为13Hz，分级次数为3次，获得粒径范围为53μm～106μm的电子束选区熔化成形用TC4钛合金粉末，收得率为38.8％，粉末流动性为25s/50g，松装密度为2.3g/cm3。
具体实施方式2：
使用具体实施方式1制得的钛合金粉末进行电子束选区熔化成形打印测试
使用粒径为15μm～500μm的TC4钛合金粉末进行电子束选区熔化成形，打印尺寸为20×20×50mm构件，打印过程的工艺参数为：偏焦电流为25mA，扫描线间距为0.20mm，扫描速度为18。
对获得的尺寸为20×20×50mm构件进行力学性能测试，其屈服强度为1032MPa，抗拉强度为936MPa，延伸率为15.1％。
Claims (10)
1.一种电子束选区熔化成形用TC4钛合金粉末，其特征在于，所述的TC4钛合金粉末为球状颗粒，粒径为53μm～106μm，流动性30s/50g以下，松装密度为2.25g/cm3以下。
2.如权利要求1所述的电子束选区熔化成形用TC4钛合金粉末的制备方法，其特征在于，该方法包括以下步骤：
步骤一，制粉：对TC4钛合金锭清洗后，使用雾化制粉设备对TC4钛合金锭进行感应熔炼和制粉处理，获得粒径为15μm～500μm的TC4钛合金粉末；
步骤二，筛分处理：采用旋风分离技术对粒径为15μm～500μm的TC4钛合金粉末的进行筛分处理，选取粒径范围为53μm～106μm即得到电子束选区熔化成形用TC4钛合金粉末。
3.根据权利要求2所述的一种电子束选区熔化成形用TC4钛合金粉末的制备方法，其特征在于，所述的TC4钛合金锭化学成分按质量百分比为：Al：5.50％～6.75％，V：3.50％～4.50％，Fe：≤0.3％，C：≤0.3％，H：≤0.12％，O：≤0.18％，N：≤0.04％，余量为Ti。
4.根据权利要求2所述的一种电子束选区熔化成形用TC4钛合金粉末的制备方法，其特征在于，所述的步骤一中对TC4钛合金锭清洗的具体操作过程为：使用酸洗液对TC4钛合金锭进行酸洗后，使用去离子水清洗，并用无水乙醇擦拭；其中酸洗液由HF、HNO3和蒸馏水组成，其中HF、HNO3和H2O的质量比为2:5:93。
5.根据权利要求2所述的一种电子束选区熔化成形用TC4钛合金粉末的制备方法，其特征在于，所述的步骤一的感应熔炼其使用分瓣水冷铜坩埚进行感应熔炼，感应熔炼工艺过程为：100KW保温1min～2min后，升至200KW后保温2min～3min，然后升至250KW保温1min～2min，然后升至300KW保温2min～3min，最后升至370KW保温2min～3min。
6.根据权利要求2或5所述的一种电子束选区熔化成形用TC4钛合金粉末的制备方法，其特征在于，所述的感应熔炼的熔炼室真空度为10Pa以下，熔炼室充气压力为90KPa～93KPa，熔炼室漏率为150Pa/h以下，雾化舱真空度为10Pa以下，雾化舱充气压力为90KPa～93KPa，雾化舱漏率为150Pa/h以下，储气罐压力为6.5MPa以上。
7.根据权利要求2所述的一种电子束选区熔化成形用TC4钛合金粉末的制备方法，其特征在于，所述的步骤一的制粉处理过程中在钛液温度为1750℃～1800℃，开启惰性气体喷嘴，喷气压力为4.5MPa～5.5MPa。
8.根据权利要求2所述的一种电子束选区熔化成形用TC4钛合金粉末的制备方法，其特征在于，所述的步骤一雾化制粉过程中采用环形辅气促进雾化液滴冷却，并在雾化舱底部实施反喷氩气，反喷气压力为0.4MPa。
9.根据权利要求2所述的一种电子束选区熔化成形用TC4钛合金粉末的制备方法，其特征在于，所述的步骤二的筛分过程中旋风分离的气流分级压力为0.5MPa，引风频率为13Hz。
10.应用权利要求1所述的TC4钛合金粉末通过电子束选区熔化成形打印方法，其特征在于，该方法的电子束选区熔化成形的工艺参数为：偏焦电流为25mA，扫描线间距为0.20mm，扫描速度指数为18。
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