CN116600915A - 用于合成球化金属粉末的系统和方法 - Google Patents
用于合成球化金属粉末的系统和方法 Download PDFInfo
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- CN116600915A CN116600915A CN202180082753.XA CN202180082753A CN116600915A CN 116600915 A CN116600915 A CN 116600915A CN 202180082753 A CN202180082753 A CN 202180082753A CN 116600915 A CN116600915 A CN 116600915A
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- titanium
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- microwave plasma
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- 239000000843 powder Substances 0.000 title claims abstract description 211
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 113
- 239000002184 metal Substances 0.000 title claims abstract description 113
- 238000000034 method Methods 0.000 title claims abstract description 110
- 230000002194 synthesizing effect Effects 0.000 title description 3
- 150000004767 nitrides Chemical class 0.000 claims abstract description 39
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 238000009832 plasma treatment Methods 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims description 84
- 239000007789 gas Substances 0.000 claims description 80
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 73
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 56
- 239000010936 titanium Substances 0.000 claims description 35
- 238000004519 manufacturing process Methods 0.000 claims description 34
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 27
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 24
- 229910052799 carbon Inorganic materials 0.000 claims description 24
- 229910052719 titanium Inorganic materials 0.000 claims description 23
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 20
- 238000009826 distribution Methods 0.000 claims description 19
- 238000002844 melting Methods 0.000 claims description 19
- 230000008018 melting Effects 0.000 claims description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 239000000654 additive Substances 0.000 claims description 12
- 230000000996 additive effect Effects 0.000 claims description 12
- 230000000977 initiatory effect Effects 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 239000001307 helium Substances 0.000 claims description 8
- 229910052734 helium Inorganic materials 0.000 claims description 8
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 8
- 229910052743 krypton Inorganic materials 0.000 claims description 8
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052724 xenon Inorganic materials 0.000 claims description 8
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 8
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 7
- 229910052754 neon Inorganic materials 0.000 claims description 7
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 7
- -1 titanium hydride Chemical compound 0.000 claims description 7
- 229910000048 titanium hydride Inorganic materials 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 239000004215 Carbon black (E152) Substances 0.000 claims description 3
- 229930195733 hydrocarbon Natural products 0.000 claims description 3
- 150000002430 hydrocarbons Chemical class 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 239000010937 tungsten Substances 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 3
- 239000000463 material Substances 0.000 abstract description 18
- 238000012545 processing Methods 0.000 abstract description 6
- 230000008569 process Effects 0.000 description 24
- 239000007943 implant Substances 0.000 description 11
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- 150000002431 hydrogen Chemical class 0.000 description 7
- 229910001092 metal group alloy Inorganic materials 0.000 description 7
- 238000012986 modification Methods 0.000 description 7
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- 239000011248 coating agent Substances 0.000 description 6
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- 238000005275 alloying Methods 0.000 description 2
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- 239000010410 layer Substances 0.000 description 2
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- 230000000704 physical effect Effects 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
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- 238000010146 3D printing Methods 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000002296 dynamic light scattering Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
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- 230000006870 function Effects 0.000 description 1
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- 239000011261 inert gas Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
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- 239000011148 porous material Substances 0.000 description 1
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- 239000002243 precursor Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
- 230000008467 tissue growth Effects 0.000 description 1
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Abstract
本文公开了使用微波等离子体处理来处理原料材料的系统和方法的实施方案。具体而言,本文公开的原料材料属于金属粉末。微波等离子体处理可用于将金属粉末球化并形成金属氮化物或金属碳化物粉末。金属氮化物或金属碳化物粉末的化学计量可通过改变等离子体气体的组成和等离子体处理过程中原料材料的停留时间来控制。
Description
通过引用任何优先权申请而并入
根据35 U.S.C.§119(e),本申请要求2020年10月30日提交的美国临时申请号63/108118的优先权权益,其全部公开通过引用并入本文。
背景
领域
本公开的一些实施方案涉及用于从原料材料生产金属球形或类球体粉末产品的系统和方法。
描述
制备一些形式的工业粉末的一个重要方面是球化过程,其将通过常规粉末碎方法产生的不规则形状或有棱角的粉末转变成球形低孔隙率颗粒。球形粉末形状均匀、致密、孔隙少、具有高且一致的流动性和高振实密度。这样的粉末在诸如注塑成型、热喷涂和增材制造等的应用中表现出优异的性能。
产生球状金属粉末,尤其是含有材料如钛(Ti)的金属粉末,可能会带来许多挑战。实现所需的球体形状、所需水平的孔隙率(例如,无孔隙率到非常多孔)以及所需的组成和微观结构可能是困难的。
氮化钛粉末是特别受关注的。氮化钛已用于多种应用,包括在医疗植入物中作为保护性耐磨涂层。目前许多由例如CoCr或钛合金(例如Ti-64)制成的骨科植入物耐磨性差,且需要氮化钛涂层以防止体内植入物最终失效。氮化钛是一种具有优异的耐磨和耐腐蚀性的陶瓷且与人体相容。该涂层通常通过化学气相沉积(CVD)施加于植入物,其中Ti蒸气与氮气反应以形成氮化钛涂层。这个过程形成了非常薄的、一致的氮化钛层。
然而,随着增材制造(AM)的出现,植入物的设计也发生了变化。现在可以设计具有内腔的植入物,以减轻植入物的重量,并为植入物内部的组织生长提供位置。然而,对于复杂的内腔,在植入物内部的表面上均匀地涂覆氮化钛层变得具有挑战性。
因此,需要生产用于增材制造和其它应用的含金属球形粉末的新颖系统和方法。
概述
出于该概述的目的,本文描述了本发明的某些方面、优点和新颖特征。应当理解,根据本发明的任何特定实施方案,并非所有这样的优点都必然可以实现。因此,例如,本领域技术人员将认识到,可以以实现如本文中教导的一个优点或一组优点的方式实施或进行本发明,而不必实现如本文中教导或建议的其它优点。
本文的一些实施方案涉及制造球化金属氮化物粉末的方法,所述方法包括:提供金属粉末作为微波等离子体焰炬的原料;将原料引入由微波等离子体焰炬产生的微波等离子体中,所述微波等离子体通过使含氮气体经受来自微波电源的微波而产生;以及形成球化金属氮化物粉末,所述球化金属氮化物粉末通过至少部分熔融原料并在微波等离子体焰炬内引发原料和含氮气体之间的化学反应而形成。
在一些实施方案中,所述方法还包括选择球化金属氮化物粉末的所需孔隙率、组成或微观结构,并且其中球化金属氮化物粉末具有所需孔隙率、组成或微观结构。在一些实施方案中,球化金属氮化物粉末具有15-106微米之间的粒度分布。在一些实施方案中,金属粉末包括钛粉末。在一些实施方案中,钛粉末包括商业纯钛(cpTi)粉末。在一些实施方案中,钛粉末包括气雾化钛粉末、氢化-脱氢(HDH)钛粉末或氢化钛粉末。在一些实施方案中,含氮气体包括氢气、氦气、氖气、氩气、氪气或氙气中的一种或多种。在一些实施方案中,含氮气体包括氮气(N2)。在一些实施方案中,球化金属氮化物粉末包括球化氮化钛粉末。在一些实施方案中,球化氮化钛粉末包括TiN、Ti2N或TiN2相中的一种或多种。在一些实施方案中,球化金属氮化物粉末的化学计量通过改变含氮气体中氮的摩尔浓度和/或原料在微波等离子体中的停留时间来控制。在一些实施方案中,化学反应包括:2Ti+N2→2TiN;或4Ti+N2→2Ti2N。在一些实施方案中,球化金属氮化物粉末包括氧、铁和碳中的一种或多种。
本文的一些实施方案涉及增材制造的方法,包括使用使用制造球化金属氮化物粉末的方法合成的球化金属氮化物粉末,所述方法包括:提供金属粉末作为微波等离子体焰炬的原料;将原料引入由微波等离子体焰炬产生的微波等离子体中,所述微波等离子体通过使含氮气体经受来自微波电源的微波而产生;以及形成球化金属氮化物粉末,球化金属氮化物粉末通过至少部分熔融原料并在微波等离子体焰炬内引发原料和含氮气体之间的化学反应而形成。
本文的一些实施方案涉及根据用于制造球化金属氮化物粉末的方法合成的球化金属氮化物粉末,所述方法包括:提供金属粉末作为微波等离子体焰炬的原料;将原料引入由微波等离子体焰炬产生的微波等离子体中,所述微波等离子体通过使含氮气体经受来自微波电源的微波而产生;以及形成球化金属氮化物粉末,球化金属氮化物粉末通过至少部分熔融原料并在微波等离子体焰炬内引发原料和含氮气体之间的化学反应而形成。
本文的一些实施方案涉及制造球化金属碳化物粉末的方法,所述方法包括:提供金属粉末作为微波等离子体焰炬的原料;将原料引入由微波等离子体焰炬产生的微波等离子体中,所述微波等离子体通过使含碳气体经受来自微波电源的微波而产生;以及形成球化金属碳化物粉末,球化金属碳化物粉末通过至少部分熔融原料并在微波等离子体焰炬内引发原料和含碳气体之间的化学反应而形成,球化金属碳化物粉末具有15-106微米的粒度。
在一些实施方案中,金属粉末包括硅、铝、钛、钨或粉末。在一些实施方案中,钛粉末包括商业纯钛(cpTi)粉末。在一些实施方案中,钛粉末包括气雾化钛粉末、氢化-脱氢(HDH)钛粉末或氢化钛粉末。在一些实施方案中,含碳气体包括氢气、氦气、氖气、氩气、氪气或氙气中的一种或多种。在一些实施方案中,含碳气体包括碳氢化合物气体。在一些实施方案中,球化金属氮化物粉末的化学计量通过改变含碳气体中的碳量或原料在微波等离子体中的停留时间来控制。
本文的一些实施方案涉及增材制造的方法,包括使用使用制造球化金属碳化物粉末的方法制造的球化金属碳化物粉末,所述方法包括:提供金属粉末作为微波等离子体焰炬的原料;将原料引入由微波等离子体焰炬产生的微波等离子体中,所述微波等离子体通过使含碳气体经受来自微波电源的微波而产生;以及形成球化金属碳化物粉末,球化金属碳化物粉末通过至少部分熔融原料并在微波等离子体焰炬内引发原料和含碳气体之间的化学反应而形成,球化金属碳化物粉末具有15-106微米的粒度。
本文的一些实施方案涉及根据用于制造球化金属碳化物粉末的方法制造的球化金属碳化物粉末,所述方法包括:提供金属粉末作为微波等离子体焰炬的原料;将原料引入由微波等离子体焰炬产生的微波等离子体中,所述微波等离子体通过使含碳气体经受来自微波电源的微波而产生;以及形成球化金属碳化物粉末,球化金属碳化物粉末通过至少部分熔融原料并在微波等离子体焰炬内引发原料和含碳气体之间的化学反应而形成,球化金属碳化物粉末具有15-106微米的粒度。
本文的一些实施方案涉及用于制造球化粉末的方法,所述方法包括:向微波等离子体焰炬提供原料;将原料引入由微波等离子体焰炬产生的微波等离子体中,所述微波等离子体通过使反应性等离子体气体经受来自微波电源的微波而产生;以及形成球化粉末,球化粉末通过至少部分熔融原料并在微波等离子体焰炬内引发原料与反应性等离子体气体之间的化学反应而形成。在一些实施方案中,所述方法还包括选择球化粉末的所需孔隙率、组成或微观结构,并且其中球化粉末具有所需孔隙率、组成或微观结构。在一些实施方案中,球化粉末具有15-106微米的粒度分布。在一些实施方案中,原料包含钛粉末。在一些实施方案中,钛粉末包括商业纯钛(cpTi)粉末。在一些实施方案中,钛粉末包括气雾化钛粉末、氢化-脱氢(HDH)钛粉末或氢化钛粉末。在一些实施方案中,反应性等离子体气体包括含氮气体,其中含氮气体包括氢气、氦气、氖气、氩气、氪气或氙气中的一种或多种。在一些实施方案中,反应性等离子体气体包括氮气(N2)。在一些实施方案中,球化粉末包括球化氮化钛粉末。在一些实施方案中,球化氮化钛粉末包括TiN、Ti2N或TiN2相中的一种或多种。在一些实施方案中,化学反应包括:2Ti+N2→2TiN;或4Ti+N2→2Ti2N。本文的一些实施方案涉及增材制造的方法,包括使用使用制造球化粉末的方法合成的球化粉末。
本文的一些实施方案涉及球化氮化钛粉末,其包含:多个呈现基本球形形状的氮化钛颗粒,多个氮化钛颗粒具有15-106微米的粒度分布,以及多个氮化钛包含以下相中的至少一种:α-Ti、TiN、Ti2N或TiN2。
在一些实施方案中,球化氮化钛粉末通过钛原料的微波等离子体处理而合成。在一些实施方案中,多个颗粒包括通过使钛原料与含氮等离子体气体反应形成的微观结构。在一些实施方案中,多个颗粒具有大于0.75或0.91的平均球度。在一些实施方案中,多个颗粒具有大于0.75或0.91的中值球度。在一些实施方案中,多个颗粒包括与cpTi核一起形成的氮化钛壳。在一些实施方案中,多个颗粒包括遍布整个颗粒的氮化钛。
附图简述
提供附图以说明示例性实施方案,而不意在限制本公开的范围。在结合附图参考以下描述时将领会对本文描述的系统和方法的更好理解,其中:
图1图示了根据本文描述的一些实施方案的用于生产球化的含金属粉末的方法的示例流程图。
图2图示了根据本文描述的一些实施方案的微波等离子体焰炬的示例图。
图3图示了根据本文描述的一些实施方案生产的氮化钛粉末的示例形态。
图4图示了根据本文描述的一些实施方案生产的氮化钛粉末的示例微观结构。
图5图示了根据本文描述的一些实施方案生产的钛粉末的示例X射线粉末衍射。
图6图示了根据本文描述的一些实施方案生产的钛粉末的示例粒度分布。
详述
尽管下文公开了某些优选实施方案和实例,但发明主题超出具体公开的实施方案而延伸到其它替代性实施方案和/或使用及其修改和等同方案。因此,对此所附权利要求的范围不受下文描述的任何特定实施方案的限制。例如,在本文公开的任何方法或过程中,方法或过程的动作或操作可以以任何合适的顺序执行并且不一定限于任何特定公开的顺序。可以以有助于理解某些实施方案的方式将各种操作依次描述为多个离散操作;然而,描述的顺序不应被解释为暗示这些操作是次序相关的。此外,本文描述的结构、系统和/或设备可以体现为集成组件或分离组件。为了比较各种实施方案的目的,描述了这些实施方案的某些方面和优点。不一定所有这些方面或优点都由任何特定实施方案实现。因此,例如,可以以实现或优化如本文所教导的一个优点或一组优点的方式来执行各种实施方案,而不必实现如本文也可教导或建议的其它方面或优点。
现在将描述某些示例性实施方案以提供对本文公开的装置和方法的结构、功能、制造和使用的原理的全面理解。这些实施方案中的一个或多个实例在附图中示出。本领域技术人员将理解,本文具体描述和附图中所示的装置和方法是非限制性的示例性实施方案,并且本发明的范围仅由权利要求限定。结合一个示例性实施方案说明或描述的特征可以与其它实施方案的特征组合。这样的修改和变型意在被包括在本技术的范围内。
本文公开了用于制造球化粉末的方法和系统的实施方案。本文的一些实施方案涉及包括金属、金属合金、碳化物、氮化物或可能难以球化的其它材料的金属粉末的生产。实现所需的类球体形状、所需水平的孔隙率(例如,无孔隙率到非常多孔)以及所需的组成和微观结构可能是困难的。本文的一些实施方案涉及金属氮化物或金属碳化物粉末的生产。氮化钛是一种熔融温度为约2,930℃的陶瓷。当使用等离子体处理时,等离子体中达到的温度和氮化钛原料的停留时间的组合可能无法提供氮化钛熔融所需的热通量。只有当通过等离子体的颗粒完全熔融、部分熔融或表面熔融时才可以球化。因此,可能难以使用等离子体处理对氮化钛原料进行球化。然而,球化粉末可用于多种应用,包括增材制造,例如激光床系统、电子束系统和粘合剂喷射系统。例如,使用AM-相容的氮化钛粉末来3维打印医用植入物将消除昂贵、耗时且不必要的植入物加工(例如CVD),并缩短制造的交付周期。由于氮化钛的耐磨性和耐腐蚀性,可不需要其它涂层。
在一些实施方案中,增材制造的基本材料要求是球形形式且在指定粒度(通常在微米范围内)内的金属合金、金属碳化物或金属氮化物粉末。要控制的最关键属性之一是粉末的粒度,因为这是AM过程中的关键参数。粒度分布对粉末流动性和提供均匀粉末床密度的能力具有直接影响。这转而又决定了加工粉末粒子所需的能量输入,并且也影响表面光洁度(finish)。例如,可用于AM过程的球化粉末可具有约15-45微米、约20-63微米或约45-106微米的粒度分布。然而,根据本文所述的一些方法和系统,除了AM过程通常需要的微米范围之外,球化粉末还可以具有纳米范围至毫米范围的粒度分布。例如,根据本文实施方案的球化粉末可具有约0.1微米至约1000微米的粒度分布。在一些实施方案中,根据本文实施方案的球化粉末可具有约0.1微米至约1微米、约1微米至约15微米、约15微米至约45微米、约20微米至约63微米、约45微米至约106微米,约106微米至约200微米、约200微米至约300微米、约300微米至约400微米、约400微米至约500微米、约500微米至约600微米、约600微米至约700微米、约700微米至约800微米、约800微米至约900微米和约900微米至约1000微米,或任何上述范围之间的粒度分布。
此外,为了在需要高粉末流量的增材制造或粉末冶金(PM)应用中有用,金属粉末颗粒应该呈现球形形状,这可以通过等离子体球化过程实现。该过程涉及颗粒在高温环境中的完全熔融、表面熔融或部分熔融,由此液态金属的表面张力将每个颗粒成形为球形几何形状,然后冷却并重新凝固。
在一些实施方案中,通过等离子体处理获得的最终颗粒可以是球形、球化或类球体的,这些术语可以互换使用。有利地,通过使用与所公开的不同原料中的每一种相关的关键和具体公开,所有原料都可以转化为球形粉末。
本公开的实施方案涉及生产基本球化或已经经历显著球化的颗粒。在一些实施方案中,球形、类球体或球化颗粒是指具有大于特定阈值的球度的颗粒。颗粒球度可以通过使用以下等式计算颗粒的球体表面积A表面积,理想以及与之匹配的体积V来计算:
A表面积,理想=4πr理想 2
可以将颗粒的理想表面积与测量表面积A表面积,实际进行比较:
在一些实施方案中,颗粒可具有大于0.5、0.6、0.7、0.75、0.8、0.9、0.91、0.95或0.99(或大于约0.5、约0.6、约0.7、约0.75、约0.8、约0.8、约0.91、约0.95或约0.99)的平均球度。在一些实施方案中,颗粒可具有0.75或更大或0.91或更大(或约0.75或更大或约0.91或更大)的球度。在一些实施方案中,颗粒可具有小于0.5、0.6、0.7、0.75、0.8、0.9、0.91、0.95或0.99(或小于约0.5、约0.6、约0.7、约0.75、约0.8、约0.8、约0.91、约0.95或约0.99)的球度。在一些实施方案中,如果颗粒具有等于或高于任何上述球度值的球度,则颗粒被认为是球形的、类球体的或球化的,并且在一些优选的实施方案中,如果颗粒的球度等于或约为0.75或更大或等于或约为0.91或更大,则颗粒被认为是球形的。
在一些实施方案中,给定粉末内所有颗粒的中值球度可以为大于0.5、0.6、0.7、0.75、0.8、0.9、0.91、0.95或0.99(或大于约0.5、约0.6、约0.7、约0.75、约0.8、约0.8、约0.91、约0.95或约0.99)。在一些实施方案中,给定粉末内所有颗粒的中值球度可以为小于0.5、0.6、0.7、0.75、0.8、0.9、0.91、0.95或0.99(或小于约0.5、约0.6、约0.7、约0.75、约0.8、约0.8、约0.91、约0.95或约0.99)。在一些实施方案中,如果针对给定粉末测量的所有或阈值百分比(如以下任何分数所述)的颗粒具有大于或等于任何上述球度值的中值球度,则粉末被认为是球化的,并且在一些优选的实施方案中,如果所有或阈值百分比的颗粒具有等于或约为0.75或更大或者等于或约为0.91或更大的中值球度,则粉末被认为是球化的。
在一些实施方案中,粉末内可高于给定球度阈值(例如如上所述)的颗粒分数可以为大于50%、60%、70%、80%、90%、95%、或99%(或大于约50%、约60%、约70%、约80%、约90%、约95%或约99%)。在一些实施方案中,粉末内可高于给定球度阈值(例如如上所述)的颗粒分数可以为小于50%、60%、70%、80%、90%、95%或99%(或小于约50%、约60%、约70%、约80%、约90%、约95%或约99%)。
粒度分布和球度可以通过任何合适的已知技术来确定,例如通过SEM、光学显微镜、动态光散射、激光衍射、使用图像分析软件手动测量尺寸,例如在同一材料切片或样品的至少三幅图像上进行约15-30次测量/图像,以及任何其它技术。
落在上述规格内的氮化钛粉末目前是未知的,且因此,使用氮化钛的AM过程目前是未知的。因此,本文的一些实施方案涉及用于大规模制造金属氮化物和金属碳化物粉末的系统和方法,包括在AM所需规格内的氮化钛粉末。然而,应当注意,本文所述的方法和系统可广泛应用于范围广泛的材料,特别是那些难以球化的材料。特别参考氮化钛,现有的氮化钛生产包括使用CVD在基材上进行氮化钛薄涂层。然而,本文的一些实施方案涉及使用等离子体处理合成例如微米尺寸的球形氮化钛粉末。在一些实施方案中,主要合金化元素是氮。从氮化钛粉末的组成来看,在不同的氮浓度下,形成不同的氮化物相,包括TiN、Ti2N和TiN2。这些相具有不同的物理性质。例如,TiN是一种非常硬的相,具有高耐磨性,而Ti2N可能是一种相对较软的相。因此,基于应用和所需的功能性质,将需要不同的组成和不同的微观结构。本文的实施方案可涉及具有任何所需相的氮化钛的合成,其中相可通过控制反应性等离子体气体的化学计量来控制。
在一些实施方案中,用于制造球化的含金属粉末(例如,金属氮化物粉末)的方法可以包括使用金属粉末(例如,Ti粉末)作为前体或原料,以及反应性等离子体气体(例如,N2)作为反应性气体物类以合成球化含金属粉末。例如,在一些实施方案中,制造球化金属氮化物或碳化物粉末的方法涉及使用商业纯金属粉末,例如商业纯钛粉末(cpTi)作为原料,以及使用含氮或含碳气体作为反应性等离子体气体来分别合成金属氮化物或金属碳化物粉末。在一些实施方案中,原料可以改为包括液体金属。在一些实施方案中,金属粉末原料可以在引入等离子体之前进行预处理。在一些实施方案中,原料可以是大致球形的或大致非球形的粉末。虽然这里的原料一般是关于钛粉末描述的,但是原料也可以包括其它金属粉末,例如B、Al或Si,以分别形成例如氮化硼、氮化铝、氮化硅。
在一些实施方案中,金属粉末原料中的金属可与反应性气体物类反应以在等离子体内形成球化的含金属粉末。例如,钛对间隙元素(interstitial)如氮、氢、碳和氧具有强亲和力。当这些物类存在于等离子体气体中时,它们处于电离状态且被认为更具“反应性”。通过有目的地选择可包含氮气和不同量的其它气体(例如氢气、氩气、氦气、氙气、氪气或其它“非反应性”气体)的反应性等离子体气体,并使cpTi粉末基本瞬时地通过反应性等离子体气体,反应性等离子体气体可以与Ti反应来形成球化粉末,例如氮化钛粉末。在一些实施方案中,通过控制等离子体中反应性气体(例如,N2)的量和金属粉末颗粒在等离子体中的停留时间,可以控制所产生的含金属的球化粉末的化学计量(例如,化合物中N的百分比)。在使用等离子处理处理钛原料的传统方法中,通常不使用含氮等离子体气体。这是由于Ti对N的亲和力非常高,N被认为在钛颗粒上形成氮化物表面层。然而,使用本文的实施方案,出乎意料地发现含氮等离子体气体可通过钛颗粒的全部质量与钛原料反应,导致的出乎意料的结果是产生球化氮化钛粉末。因此,本文的实施方案不同于涉及钛和类似原料的等离子体处理的常规方法。
图1示出了根据本文所述的一些实施方案的用于生产球化的含金属粉末的方法的示例流程图。在一些实施方案中,用于制造球化的含金属粉末的方法可包括在100处,提供金属粉末作为原料。例如,金属粉末可包括钛粉末,例如商业纯钛(cpTi)粉末、气雾化钛粉末、氢化-脱氢(HDH)钛粉末或氢化钛粉末。在一些实施方案中,所述方法还可包括在102处,将原料引入微波等离子体中以形成球化的含金属粉末。在一些实施方案中,微波等离子体可以通过使反应性等离子体气体例如含氮(例如,N2)或含碳(例如,碳氢化合物)气体经受由微波电源产生的微波而产生。在一些实施方案中,反应性等离子体气体还可以包括氢气、氦气、氖气、氩气、氪气或氙气中的一种或多种。在一些实施方案中,在104处,球化的含金属粉末可通过原料与反应性等离子体气体之间的化学反应形成。在一些实施方案中,球化的含金属粉末具有15-106微米的粒度分布。在一些实施方案中,球化的含金属粉末包括球化氮化钛粉末。在一些实施方案中,球化氮化钛粉末包括一种或多种氮化钛相,例如TiN、Ti2N或TiN2。
所公开的方法的一些实施方案可以包括使用粉末进料器将粉末原料进料到微波产生的反应性等离子体中,其中控制粉末原料的功率密度、气体流量和停留时间。所需的工艺参数,如功率密度、流速和粉末在反应性等离子体中的停留时间,可取决于原料金属的物理特性,如熔点和热导率。
本文的一些实施方案涉及使用微波产生的等离子体对金属或金属合金进行球化的方法。在一些实施方案中,粉末原料被夹带在惰性和/或还原性气体环境中并注入到微波等离子体环境中。在注入热等离子体(其可能包括等离子体羽流或等离子体焰炬的排气)中后,原料被球化并释放到填充有惰性气体的腔室中,并被导入气密密封的桶中以将其储存。在一些实施方案中,将原料注入等离子体中包括将原料注入等离子体羽流或等离子体排气中。该过程可以在大气压、部分真空或略高于大气压的压力下进行。在替代性实施方案中,该过程可以在低、中或高真空环境中进行。该过程可以连续运行或以间歇过程运行,并且可以在收集容器充满球化金属或金属合金颗粒时更换收集容器。可以控制球化金属和金属合金的冷却速率以战略性地影响球化粉末的微观结构。通过控制工艺参数例如冷却气体流速、停留时间、冷却气体组成等,可以控制金属和金属合金的微观结构。形成这些结构所需的精确冷却速率在很大程度上取决于材料中合金化元素的类型和数量。
在一些实施方案中,在等离子体、等离子体羽流或等离子体焰炬的排气内,熔融金属由于液体表面张力而一致地球化。由于微波产生的等离子体表现出基本均匀的温度分布,因此可以实现超过90%的颗粒球化(例如,91%、93%、95%、97%、99%、100%)。离开等离子体后,颗粒在进入收集箱之前被冷却。当收集箱充满时,可以根据需要将它们移除并用空箱替换,而无需停止该过程。
图2示出了根据本文的一些实施方案的可用于生产球状金属或金属合金粉末的示例性微波等离子体焰炬。如上所述,可以将金属进料材料9、10引入到维持微波产生的等离子体11的微波等离子体焰炬2中。在一些实施方案中,微波等离子体焰炬可以包括侧进料料斗而不是图2的实施方案中所示的顶部进料料斗3,从而允许下游进料。因此,在该实施方式中,原料在微波等离子体焰炬施加器之后注入以在微波等离子体焰炬的“羽流”或“排气”6中进行处理。因此,微波等离子体焰炬的等离子体在等离子体焰炬的出口端接合以允许原料的下游进料,这与关于图2所讨论的顶部进料(或上游进料)相反。其它进料配置可包括一个或多个围绕等离子体羽流的单独进料喷嘴。原料粉末可从任何方向进入等离子体,并可围绕等离子体以360°进料。原料粉末可以在沿等离子体羽流长度的特定位置处进入等离子体,在该特定位置处已经测量了特定温度并且估计了用于颗粒充分熔融的停留时间。熔融的颗粒离开等离子体进入密封腔室,在那里它们被急冷然后收集。
在一些实施方案中,可以通过入口5注入夹带气流和鞘流(向下箭头)以在经由微波辐射源1点燃等离子体11之前在等离子体焰炬内产生流动条件。在一些实施方案中,夹带流和鞘流都是轴对称的和层流的,而在其它实施方案中,气流是涡流的。可以将进料9轴向地或以其它方式引入微波等离子体焰炬中,在那里它们被将材料引向等离子体的气流夹带。在微波产生的等离子体中,进料材料被熔融以使材料球化,并且可发生进料与反应性等离子体气体之间的化学反应。入口5可用于引入工艺气体以沿轴12向等离子体11夹带并加速颗粒9、10。首先,颗粒9使用通过等离子体焰炬内的环形间隙产生的核心层流气流(上箭头组)通过夹带而被加速。可以通过第二环形间隙产生第二层流(下组箭头)以为介电焰炬2的内壁提供层流鞘流以防止其因来自等离子体11的热辐射而熔融。在一些实施方案中,层流沿尽可能靠近轴12的路径将颗粒9、10引向等离子体11,使它们暴露于等离子体11内的基本均匀的温度。在一些实施方案中,存在合适的流动条件以防止颗粒10到达其中可能发生等离子体附着的等离子体焰炬2的内壁。颗粒9、10被气流导向微波等离子体11,每个颗粒都经历均匀的热处理。可以调整微波产生的等离子体的各种参数以及颗粒参数以实现期望的结果。这些参数可包括微波功率、原料材料尺寸、原料材料插入速率、气体流速、等离子体温度、停留时间和冷却速率。在一些实施方案中,气流是层流的;然而,在替代性实施方案中,旋流或湍流可用于将进料材料引向等离子体。
实施例
使用氮气作为反应性等离子体气体,在微波等离子体中由cpTi粉末合成氮化钛粉末。氮化钛粉末表现出45-106微米的粒度分布(PSD),并且是使用使用氮气(N2)作为等离子体气体产生的微波等离子合成的。通过HDH方法制造的cpTi在包含氮气(N2)和氢气(H2)混合物的反应性等离子体中进行处理。在反应性氮气中引入少量氢气(~10%)以防止cpTi粉末在等离子体处理过程中氧化。等离子处理将不规则形状的HDH cpTi粉末转变为球形氮化钛粉末。在球化过程中,由于高温以及等离子体中电离氮物类与完全熔融、表面熔融或部分熔融的cpTi颗粒之间的接触,Ti和N之间开始发生反应,生成氮化钛TixNy。示例反应如下所示:
2Ti(s)+N2(g)→2TiN(s)
4Ti(s)+N2(g)→2Ti2N(s)
合成的氮化钛具有以下元素组成:12重量%的氮、0.34重量%的氧、0.034重量%的铁、0.0068重量%的碳和85.9重量%的钛。合成的氮化钛具有其中D10为50.35微米、D50为68.5微米和D90为97.73微米的粒度分布。合成的氮化钛具有以下物理性质:霍尔流量为27s/50g、表观密度(AD)为2.54g/cm3、真实密度为4.9g/cm3以及振实密度(TD)为2.91g/cm3。
图3图示了根据本文所述的一些实施方案合成的氮化钛粉末的示例形态。如图所示,氮化钛粉末的颗粒为基本球形,因此可以在AM过程中使用该粉末。
图4图示了根据本文所述的一些实施方案合成的氮化钛粉末的示例微观结构。在一些实施方案中,氮化钛粉末的微观结构可包括一个或多个单独相。例如,在一些实施方案中,相可以包括α-Ti、TiN、Ti2N或TiN2。在一些实施方案中,氮化钛壳将与cpTi核一起形成。是否形成氮化钛壳或粉末包含遍布整个颗粒的氮化钛取决于等离子体焰炬内的处理条件。在图4的所示显微观结构中,微观结构表示Ti基体,其中TiN和Ti2N相分散在该基体中。
图5图示了根据本文所述的一些实施方案合成的氮化钛粉末的示例X射线粉末衍射。如图所示,粉末通常由TiN与TiO、Ti和Ti2N形成。
图6图示了根据本文所述的一些实施方案合成的氮化钛粉末的示例粒度分布。在一些实施方案中,氮化钛粉末可具有约15微米至约150微米的粒度分布。
附加实施方案
在前述说明书中,本发明已经参考其具体实施方案进行了描述。然而,很明显,在不脱离本发明的更广泛的精神和范围的情况下,可以对其进行各种修改和改变。相应地,说明书和附图应以举例说明而非限制性含义加以考虑。
实际上,虽然本发明已经在某些实施方案和实施例的上下文中公开,但是本领域技术人员将理解,本发明超出具体公开的实施方案延伸到本发明的其它替代性实施方案和/或使用及其明显的修改和等同方案。此外,虽然已经详细示出和描述了本发明的实施方案的若干变型,但是基于本公开,本领域的技术人员将容易地明白在本发明的范围内的其它修改。还设想可以对实施方案的具体特征和方面进行各种组合或子组合,并且这些组合仍然落在本发明的范围内。应当理解,所公开的实施方案的各种特征和方面可以相互组合或替代,以形成所公开的发明的实施方案的不同模式。本文中公开的任何方法不需要以所述次序执行。因此,意在本文公开的本发明的范围不应受到上述特定实施方案的限制。
应当理解,本公开的系统和方法各自具有多个创新方面,其中没有任何一个单独负责本文公开的期望属性或为其所需要。上述各种特征和过程可以彼此独立地使用或者可以以各种方式组合。所有可能的组合和子组合旨在落入本公开的范围内。
本说明书中在单独实施方案的上下文中描述的某些特征也可以在单个实施方案中组合实施。相反,在单个实施方案的上下文中描述的各种特征也可以单独地或以任何合适的子组合在多个实施方案中实施。此外,尽管特征可能在上面被描述为在某些组合中起作用,并且甚至最初也如此要求保护,但在某些情况下,可能会从所要求保护的组合中删除该组合的一个或多个特征,并且所要求保护的组合可能涉及子组合或子组合的变型。没有单个特征或特征组对于各个和每个实施方案都是必要的或必不可少的。
还应当理解,本文使用的条件性语言,例如“可以”、“可”、“可能”、“会”、“例如”等,除非另有明确说明,或者在所使用的上下文中以其它方式理解,通常旨在传达某些实施方案包括但其它实施方案不包括某些特征、要素和/或步骤。因此,这样的条件性语言通常并不意在暗示一个或多个实施方案以任何方式需要特征、要素和/或步骤,或者该一个或多个实施方案必须包括用于在有或没有作者输入或提示的情况下决定是否这些特征、要素和/或步骤包括在任何特定实施方案中或要在任何特定实施方案中执行的逻辑。术语“包含”、“包括”、“具有”等是同义词,并且以开放式方式包容性地使用,并且不排除额外的要素、特征、动作、操作等。此外,术语“或”在其包容性含义(而非排他性含义)中使用,使得例如当用于连接要素列表时,术语“或”表示一个、一些或全部列表中的要素。此外,除非另有说明,否则本申请和所附权利要求中使用的冠词“一个”、“一种”知“该”应被解释为表示“一个或多个”或“至少一个”。类似地,虽然操作可能以特定次序在附图中描绘,但应认识到这样的操作不需要以所示的特定次序或顺序次序执行,或者执行所有图示的操作以获得期望的结果。此外,附图可以流程图的形式示意性地描绘一个或多个示例过程。然而,未描绘的其它操作可并入示意性说明的示例方法和过程中。例如,可以在任何所示操作之前、之后、同时或之间执行一个或多个附加操作。另外,在其它实施方案中可以重新排列或重新排序操作。在某些情况下,多任务处理和并行处理可能是有利的。另外,上述实施方案中各个系统组件的分离不应理解为所有实施方案中都需要这样分离,并且应当理解,所描述的程序组件和系统一般可以集成在单一软件产品中,或者打包成多个软件产品。此外,其它实施方案也在所附权利要求的范围内。在某些情况下,权利要求中记载的动作可以以不同的次序执行并且仍然实现期望的结果。
此外,虽然本文描述的方法和装置可能易受各种修改和替代形式的影响,但是其具体实例已经在附图中示出并且在本文中被详细描述。然而,应当理解,本发明不限于所公开的特定形式或方法,但相反,本发明涵盖落入所描述的各种实施方式和所附的权利要求的精神和范围内的所有修改、等同方案和替代方案。此外,与实施方式或实施方案相关的任何特定特征、方面、方法、性质、特征、质量、属性、要素等的本文公开可用于本文阐述的所有其它实施方式或实施方案。本文中公开的任何方法不需要以所述次序执行。本文公开的方法可包括实践者采取的某些行动;但是,这些方法还可以包括任何第三方对这些行动的明示或暗示指示。本文公开的范围还涵盖任何和所有重叠、子范围及其组合。诸如“至多”、“至少”、“大于”、“小于”、“之间”等的语言包括所列举的数字。以术语例如“约”或“大约”开头的数字包括引用的数字,并且应根据情况进行解释(例如,在这种情况下尽可能合理准确,例如±5%、±10%、±15%等)。例如,“约3.5毫米”包括“3.5毫米”。以术语如“基本”开头的短语包括所引用的短语,并且应该根据情况进行解释(例如,在这种情况下尽可能合理)。例如,“基本恒定”包括“恒定”。除非另有说明,否则所有测量均在包括温度和压力的标准条件下进行。
如本文所用,提及项目列表中的“至少一个”的短语是指那些项目的任何组合,包括单个成员。例如,“A、B或C中的至少一个”旨在涵盖:A、B、C、A和B、A和C、B和C,以及A、B和C。连词例如短语“X、Y和Z中的至少一个”,除非另有明确说明,否则在上下文中被理解为通常用于传达项目、术语等可以是X、Y或Z中的至少一个。因此,这样的连词通常并不意在暗示某些实施方案需要X中的至少一个、Y中的至少一个和Z中的至少一个各自存在。本文提供的标题(如果有的话)仅为方便起见,并且不一定影响本文公开的装置和方法的范围或含义。
因此,权利要求不旨在限于本文所示的实施方案,而是要符合与本文公开的本公开、原理和新颖特征一致的最宽范围。
Claims (43)
1.一种制造球化金属氮化物粉末的方法,所述方法包括:
提供金属粉末作为微波等离子体焰炬的原料;
将所述原料引入由所述微波等离子体焰炬产生的微波等离子体中,所述微波等离子体通过使含氮气体经受来自微波电源的微波而产生;和
形成球化金属氮化物粉末,所述球化金属氮化物粉末通过至少部分熔融所述原料并在所述微波等离子体焰炬内引发所述原料和所述含氮气体之间的化学反应而形成。
2.根据权利要求1所述的方法,还包括选择所述球化金属氮化物粉末的所需孔隙率、组成或微观结构,并且其中所述球化金属氮化物粉末具有所需孔隙率、组成或微观结构。
3.根据权利要求1所述的方法,其中所述球化金属氮化物粉末具有15-106微米的粒度分布。
4.根据权利要求1所述的方法,其中所述金属粉末包括钛粉末。
5.根据权利要求4所述的方法,其中所述钛粉末包括商业纯钛(cpTi)粉末。
6.根据权利要求4所述的方法,其中所述钛粉末包括气雾化钛粉末、氢化-脱氢(HDH)钛粉末或氢化钛粉末。
7.根据权利要求1所述的方法,其中所述含氮气体包括氢气、氦气、氖气、氩气、氪气或氙气中的一种或多种。
8.根据权利要求1所述的方法,其中所述含氮气体包括氮气(N2)。
9.根据权利要求1所述的方法,其中所述球化金属氮化物粉末包括球化氮化钛粉末。
10.根据权利要求9所述的方法,其中所述球化氮化钛粉末包括TiN、Ti2N或TiN2相中的一种或多种。
11.根据权利要求1所述的方法,其中通过改变所述含氮气体中氮的摩尔浓度和/或所述原料在所述微波等离子体中的停留时间来控制所述球化金属氮化物粉末的化学计量。
12.根据权利要求1所述的方法,其中所述化学反应包括:
2Ti+N2→2TiN;或者
4Ti+N2→2Ti2N。
13.根据权利要求1所述的方法,其中所述球化金属氮化物粉末包含氧、铁和碳中的一种或多种。
14.一种增材制造的方法,包括使用使用根据权利要求1所述的方法合成的球化金属氮化物粉末。
15.一种根据以下方法合成的球化金属氮化物粉末:
提供金属粉末作为微波等离子体焰炬的原料;
将所述原料引入由所述微波等离子体焰炬产生的微波等离子体中,所述微波等离子体通过使含氮气体经受来自微波电源的微波而产生;和
形成球化金属氮化物粉末,所述球化金属氮化物粉末通过至少部分熔融所述原料并在所述微波等离子体焰炬内引发所述原料和所述含氮气体之间的化学反应而形成。
16.一种制造球化金属碳化物粉末的方法,所述方法包括:
提供金属粉末作为微波等离子体焰炬的原料;
将所述原料引入由所述微波等离子体焰炬产生的微波等离子体中,所述微波等离子体通过使含碳气体经受来自微波电源的微波而产生;和
形成球化金属碳化物粉末,所述球化金属碳化物粉末通过至少部分熔融所述原料并在所述微波等离子体焰炬内引发所述原料和所述含碳气体之间的化学反应而形成,
所述球化金属碳化物粉末具有15-106微米的粒度。
17.根据权利要求16所述的方法,其中所述金属粉末包括硅、铝、钛、钨或粉末。
18.根据权利要求17所述的方法,其中所述钛粉末包括商业纯钛(cpTi)粉末。
19.根据权利要求17所述的方法,其中所述钛粉末包括气雾化钛粉末、氢化-脱氢(HDH)钛粉末或氢化钛粉末。
20.根据权利要求16所述的方法,其中所述含碳气体包括氢气、氦气、氖气、氩气、氪气或氙气中的一种或多种。
21.根据权利要求16所述的方法,其中所述含碳气体包括碳氢化合物气体。
22.根据权利要求16所述的方法,其中通过改变所述含碳气体中的碳量或所述原料在所述微波等离子体中的停留时间来控制所述球化金属氮化物粉末的化学计量。
23.一种增材制造的方法,包括使用使用根据权利要求16所述的方法制造的球化金属碳化物粉末。
24.一种根据以下方法制造的球化金属碳化物粉末:
提供金属粉末作为微波等离子体焰炬的原料;
将所述原料引入由微波等离子体焰炬产生的微波等离子体中,所述微波等离子体通过使含碳气体经受来自微波电源的微波而产生;和
形成球化金属碳化物粉末,所述球化金属碳化物粉末通过至少部分熔融所述原料并在所述微波等离子体焰炬内引发所述原料和所述含碳气体之间的化学反应而形成,
所述球化金属碳化物粉末具有15-106微米的粒度。
25.一种制造球化粉末的方法,所述方法包括:
向微波等离子体焰炬提供原料;
将所述原料引入由所述微波等离子体焰炬产生的微波等离子体中,所述微波等离子体通过使反应性等离子体气体经受来自微波电源的微波而产生;和
形成球化粉末,所述球化粉末通过至少部分熔融所述原料并在所述微波等离子体焰炬内引发所述原料和所述反应性等离子体气体之间的化学反应而形成。
26.根据权利要求25所述的方法,还包括选择所述球化粉末的所需孔隙率、组成或微观结构,并且其中所述球化粉末具有所需孔隙率、组成或微观结构。
27.根据权利要求25所述的方法,其中所述球化粉末具有15-106微米的粒度分布。
28.根据权利要求25所述的方法,其中所述原料包括钛粉末。
29.根据权利要求28所述的方法,其中所述钛粉末包括商业纯钛(cpTi)粉末。
30.根据权利要求28所述的方法,其中所述钛粉末包括气雾化钛粉末、氢化-脱氢(HDH)钛粉末或氢化钛粉末。
31.根据权利要求25所述的方法,其中所述反应性等离子体气体包括含氮气体,其中所述含氮气体包括氢气、氦气、氖气、氩气、氪气或氙气中的一种或多种。
32.根据权利要求25所述的方法,其中所述反应性等离子体气体包括氮气(N2)。
33.根据权利要求25所述的方法,其中所述球化粉末包括球化氮化钛粉末。
34.根据权利要求33所述的方法,其中所述球化氮化钛粉末包括TiN、Ti2N或TiN2相中的一种或多种。
35.根据权利要求25所述的方法,其中所述化学反应包括:
2Ti+N2→2TiN;或者
4Ti+N2→2Ti2N。
36.一种增材制造的方法,包括使用使用根据权利要求25所述的方法合成的球化粉末。
37.一种球化氮化钛粉末,包括:
呈基本球形形状的多个氮化钛颗粒,
所述多个氮化钛颗粒具有15-106微米的粒度分布,并且
所述多个氮化钛颗粒包括以下相中的至少一种:α-Ti、TiN、Ti2N或TiN2。
38.根据权利要求37所述的球化氮化钛粉末,其中所述球化氮化钛粉末通过钛原料的微波等离子处理而合成。
39.根据权利要求38所述的球化氮化钛粉末,其中所述多个颗粒具有通过使所述钛原料与含氮等离子体气体反应而形成的微观结构。
40.根据权利要求37所述的球化氮化钛粉末,其中所述多个颗粒具有大于0.75或0.91的平均球度。
41.根据权利要求37所述的球化氮化钛粉末,其中所述多个颗粒具有大于0.75或0.91的中值球度。
42.根据权利要求37所述的球化氮化钛粉末,其中所述多个颗粒包括与cpTi核一起形成的氮化钛壳。
43.根据权利要求37所述的球化氮化钛粉末,其中所述多个颗粒包括遍布整个颗粒的氮化钛。
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EP4237174A1 (en) | 2023-09-06 |
US11919071B2 (en) | 2024-03-05 |
CA3196653A1 (en) | 2022-05-05 |
AU2021371051A1 (en) | 2023-03-30 |
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