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CN109881162A - 一种基于等离子喷涂技术的溅射用靶材制备工艺 - Google Patents

一种基于等离子喷涂技术的溅射用靶材制备工艺 Download PDF

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CN109881162A
CN109881162A CN201811447256.1A CN201811447256A CN109881162A CN 109881162 A CN109881162 A CN 109881162A CN 201811447256 A CN201811447256 A CN 201811447256A CN 109881162 A CN109881162 A CN 109881162A
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芮瑛
吉和林
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Abstract

本发明公开了一种基于等离子喷涂技术的溅射用靶材制备工艺，步骤包括：将待喷涂粉体加工到用于等离子喷涂的粒度范围；对底板的表面进行满足等离子喷涂的表面处理；利用等离子体喷涂机将制备的待喷涂粉体喷涂在表面处理后的底板表面；对喷涂后的底板进行清洁和检测。该溅射用靶材制备工艺利用等离子喷涂技术进行靶材制备，具有较高的致密度(>93％的相对密度)和与初始粉末材料相当的高纯度；与热压或烧结方法相比，本发明的制备工艺既能够满足薄膜电池生产需要的大尺寸靶材制备要求，又能够用于电极材料的靶材制作。

Description

一种基于等离子喷涂技术的溅射用靶材制备工艺
技术领域
本发明涉及一种溅射用靶材制备工艺，尤其是一种基于等离子喷涂技术的溅射用靶材制备工艺。
背景技术
与传统的锂电池相比，薄膜锂电池具有一些优势。最明显的是尺寸小，能量密度高，循环寿命长。薄膜锂电池是由阴极和阳极两个电极和电解质组成。例如，阴极材料可以是LiCoO2、LiMn2O4、LiFePO4或其他材料。阳极可以是C、Si、Ge、Sn或各种氧化物、氮化物或氧氮化物。锂磷氧氮化物(LiPON)是薄膜锂电池中最常用的电解质材料之一，通常用物理气相淀积手段在氮气氛围下用磷酸锂靶镀膜产生。现有技术表明电解质对电池性能至关重要，因此溅射靶的制作也很重要。适用于溅射靶的高密度Li3PO4材料，常用有烧结和热压两种制造方法，这两种制造方法有一些共同的困难：(1)靶材尺寸难以做大，这里有两个关键因素，一是Li3PO4是脆性陶瓷材料，机械和热应力会导致开裂，二是随着所需炉膛尺寸的增大，炉膛压力、温度均匀性越来越难以控制，再加上相图复杂，想要得到密度高、纯度高的这种陶瓷材料，温度窗口相对较小；(2)接缝，如上所述，一个大尺寸的靶很难做成一块，需要把几块连接起来做成更大的一块，然而，接缝可能是靶材提早失效的原因之一。靶材与背板之间需要焊接/粘结，通常用铟焊或用耐高温的导电胶，这样接缝处容易造成污染；(3)相纯度，高密度和纯相很难同时存在，高温高压下常见的杂质是Li4P2O7，这是由磷酸锂失LiO2造成的，不同的相可能会有不同的溅射速率，最终导致靶材颗粒脱落；(4)工作气体通常仅限于惰性气体和其他不腐蚀气室部件的气体，否则会加速损耗或损坏反应炉里的部件，特别是石墨热场，这样没有喷涂法的灵活性。
发明内容
发明要解决的技术问题是：现有的工艺难以满足磷酸锂材料的溅射用靶材的制备要求。
技术方案：本发明所述的基于等离子喷涂技术的溅射用靶材制备工艺，包括如下步骤：
步骤1，将待喷涂粉体加工到用于等离子喷涂的粒度范围；
步骤2，对底板的表面进行满足等离子喷涂的表面处理；
步骤3，利用等离子体喷涂机将步骤1制备的待喷涂粉体喷涂在步骤2表面处理后的底板表面；
步骤4，对步骤3喷涂后的底板进行清洁和检测。
进一步地，步骤3中，利用等离子体喷涂机进行喷涂的具体步骤为：
步骤3.1，在常压或减压条件下，将工作气体吹入等离子体产生区；
步骤3.2，设定等离子体喷涂机的电弧直流功率，并在电弧稳定后利用载体气体将待喷涂粉体送入等离子体流中；
步骤3.3，调整等离子体喷涂机的喷枪头部与底板之间的喷射距离，移动等离子体喷涂机的喷枪将待喷涂粉体均匀喷涂在底板的指定区域上。
进一步地，步骤3.1中，工作气体为Ar、N2、O2、NH3、空气或其他惰性气体，工作气体吹入等离子体产生区的流速为1-100L/min。
进一步地，步骤3.1中，在将工作气体吹入等离子体产生区时，同时加入H2作为辅助工作气体。
进一步地，步骤3.2中，载体气体将待喷涂粉体送入等离子体流中的速率为1-100g/min。
进一步地，步骤3.2中，等离子体喷涂机的电弧直流功率为1-400kW。
进一步地，步骤3.3中，喷射距离为20-200mm，等离子体喷涂机的喷枪移动速度为2-500cm/s。
进一步地，步骤3.3中，在喷枪将待喷涂粉体均匀喷涂在底板的指定区域上时，在吹送冷却气流围绕在喷涂火焰周围以控制底板温度。
进一步地，步骤3.3中，在喷枪将待喷涂粉体均匀喷涂在底板的指定区域上时，在底板的背面通冷却水以控制底板温度。
进一步地，底板的温度控制在小于等于90％待喷涂粉体的熔点。
进一步地，步骤1中，待喷涂粉体加工后的粒度范围为5-500um。
进一步地，步骤2中，满足等离子喷涂的表面处理包括增强附着力处理、调整热膨胀系数差值处理、污染物减少处理、表面粗糙度处理以及表面过渡层增设处理，在进行表面处理时，根据需要选择实施其中的一种处理或多种处理组合。
进一步地，步骤2中，底板为浮地、接地或另加直流偏置。
进一步地，底板为纯金属、合金或导电型非金属材质。
进一步地，待喷涂粉体为用于制备固态电池电解质的粉体中的单一粉体或几种粉体的混合粉体，或者为用于制备钠离子电池正负极材料的粉体中的单一粉体或几种粉体的混合粉体。
进一步地，用于制备固态电池电解质的粉体包括磷酸锂、硅酸锂、氮化硅、磷酸铁锂、Li(NiCoSl)O2、Li(Mn2O4)、硅、石墨、LiTiO3、LLTO、LLZO以及钴酸锂；用于制备钠离子电池正负极材料的粉体包括钠-过渡金属氧化物、钠-过渡金属磷酸盐及变种、钠-过渡金属硫酸盐、钠-过渡金属普鲁士蓝类化合物、硬碳、软碳以及过渡金属氧化物。
本发明与现有技术相比，其有益效果是：与热压和烧结工艺的一个很大的区别是，靶材材料是直接喷到基体上，不需要额外的键合步骤；利用等离子喷涂方法制备溅射用靶材，具有较高的密度(>93％的相对密度)和与初始粉末材料相当的高纯度；与热压或烧结方法相比具有一定的优越性，能够满足大尺寸薄膜锂电池生产需要的靶材的制备要求。
附图说明
图1为本发明的制备工艺流程图；
图2为本发明工艺制作的一种溅射靶材的截面扫描电子显微镜(SEM)图；
图3为本发明工艺制作的一种溅射靶材的X射线衍射(XRD)图。
具体实施方式
下面结合附图对本发明技术方案进行详细说明，但是本发明的保护范围不局限于所述实施例。
实施例1：
如图1所示，本发明公开的基于等离子喷涂技术的溅射用靶材制备工艺，包括如下步骤：
步骤1，将待喷涂粉体加工到用于等离子喷涂的粒度范围；
步骤2，对底板的表面进行满足等离子喷涂的表面处理；
步骤3，利用等离子体喷涂机将步骤1制备的待喷涂粉体喷涂在步骤2表面处理后的底板表面；
步骤4，对步骤3喷涂后的底板进行清洁和检测。
进一步地，步骤3中，利用等离子体喷涂机进行喷涂的具体步骤为：
步骤3.1，在常压或减压条件下，将工作气体吹入等离子体产生区；
步骤3.2，设定等离子体喷涂机的电弧直流功率，并在电弧稳定后利用载体气体将待喷涂粉体送入等离子体流中；
步骤3.3，调整等离子体喷涂机的喷枪头部与底板之间的喷射距离，移动等离子体喷涂机的喷枪将待喷涂粉体均匀喷涂在底板的指定区域上。
进一步地，步骤3.1中，工作气体为Ar、N2、O2、NH3、空气或其他惰性气体，工作气体吹入等离子体产生区的流速为1-100L/min。
进一步地，步骤3.1中，在将工作气体吹入等离子体产生区时，同时加入H2作为辅助工作气体。辅助工作气体H2的作用在于一方面可以控制失氧/氧化，一方面提供熵。
进一步地，步骤3.2中，载体气体将待喷涂粉体送入等离子体流中的速率为1-100g/min。载体气体可以为空气和/或N2，主要用于将待喷涂粉体送入等离子体流中。
进一步地，步骤3.2中，等离子体喷涂机的电弧直流功率为1-400kW。
进一步地，步骤3.3中，喷射距离为20-200mm，等离子体喷涂机的喷枪移动速度为2-500cm/s。
进一步地，步骤3.3中，在喷枪将待喷涂粉体均匀喷涂在底板的指定区域上时，在吹送冷却气流围绕在喷涂火焰周围以控制底板温度。冷却气体可以采用氮气或空气，对底板的温度控制能够有利于控制变形并提高粉体的利用率。
进一步地，步骤3.3中，在喷枪将待喷涂粉体均匀喷涂在底板的指定区域上时，在底板，背面通冷却水以控制底板温度。对底板的温度控制能够有利于控制变形并提高粉体的利用率。
进一步地，底板的温度控制在小于等于90％待喷涂粉体的熔点。
进一步地，步骤1中，待喷涂粉体加工后的粒度范围为5-500um。
进一步地，步骤2中，满足等离子喷涂的表面处理包括增强附着力处理、调整热膨胀系数差值处理、污染物减少处理、表面粗糙度处理以及表面过渡层增设处理，在进行表面处理时，根据需要选择实施其中的一种处理或多种处理组合。
进一步地，步骤2中，底板为浮地、接地或另加直流偏置。
进一步地，底板为纯金属、合金或导电型非金属材质。例如铜、钛、钼或不锈钢。
进一步地，待喷涂粉体为用于制备固态电池电解质的粉体中的单一粉体或几种粉体的混合粉体，或者为用于制备钠离子电池正负极材料的粉体中的单一粉体或几种粉体的混合粉体。
进一步地，用于制备固态电池电解质的粉体包括磷酸锂、硅酸锂、氮化硅、磷酸铁锂、Li(NiCoSl)O2、Li(Mn2O4)、硅、石墨、LiTiO3、LLTO、LLZO以及钴酸锂；用于制备钠离子电池正负极材料的粉体包括钠-过渡金属氧化物、钠-过渡金属磷酸盐及变种、钠-过渡金属硫酸盐、钠-过渡金属普鲁士蓝类化合物、硬碳、软碳、合金以及过渡金属氧化物。
如图2和3所示，以Li3PO4粉体为例，利用本发明公开的等离子喷涂方法制备的Li3PO4靶在SEM和XRD的分析下显示接近纯Li3PO4相，与起始的Li3PO4粉末组成一致。本发明公开的制备工艺不仅适用于电解质选材Li3PO4及其类似陶瓷材料，也适用于电极，如LiCoO2等。等离子喷涂适用于大批量生产和低成本生产。
与现有的工艺方法相比：(1)不需要焊接，靶材直接喷在底板上；(2)可以根据不同的大小进行调整，并且不存在基本的尺寸限制；(3)对靶材厚度没有基本的限制，特别是薄的靶材，这是很难用其他方法制备而成的，特别是大尺寸薄靶材；(4)对靶材形状没限制，比如平面式、滚筒式都可以；(5)用过的靶材可以重新喷涂以重复使用，而不需要去掉全部剩余的材料；(6)喷涂过程可以集成到PVD工艺流水线中，以保持每次PVD处理的厚度相同；(7)与各种底板材料附着力强；(8)可用于直接形成薄膜，而不只是制造靶材；(9)可用于纯粉或混合粉的非反应性、甚至反应性沉积；(10)具备循环沉积/等离子表面处理工艺的能力；(11)用同一个靶能够分层或图案化沉积不同的材料。
如上所述，尽管参照特定的优选实施例已经表示和表述了本发明，但其不得解释为对本发明自身的限制。在不脱离所附权利要求定义的本发明的精神和范围前提下，可对其在形式上和细节上作出各种变化。

Claims (16)

1.一种基于等离子喷涂技术的溅射用靶材制备工艺，其特征在于，包括如下步骤：
步骤1，将待喷涂粉体加工到用于等离子喷涂的粒度范围；
步骤2，对底板的表面进行满足等离子喷涂的表面处理；
步骤3，利用等离子体喷涂机将步骤1制备的待喷涂粉体喷涂在步骤2表面处理后的底板表面；
步骤4，对步骤3喷涂后的底板进行清洁和检测。
2.根据权利要求1所述的基于等离子喷涂技术的溅射用靶材制备工艺，其特征在于，步骤3中，利用等离子体喷涂机进行喷涂的具体步骤为：
步骤3.1，在常压或减压条件下，将工作气体吹入等离子体产生区；
步骤3.2，设定等离子体喷涂机的电弧直流功率，并在电弧稳定后利用载体气体将待喷涂粉体送入等离子体流中；
步骤3.3，调整等离子体喷涂机的喷枪头部与底板之间的喷射距离，移动等离子体喷涂机的喷枪将待喷涂粉体均匀喷涂在底板的指定区域上。
3.根据权利要求2所述的基于等离子喷涂技术的溅射用靶材制备工艺，其特征在于，步骤3.1中，工作气体为Ar、N2、O2、NH3、空气或其他惰性气体，工作气体吹入等离子体产生区的流速为1-100L/min。
4.根据权利要求2所述的基于等离子喷涂技术的溅射用靶材制备工艺，其特征在于，步骤3.1中，在将工作气体吹入等离子体产生区时，同时加入H2作为辅助工作气体。
5.根据权利要求2所述的基于等离子喷涂技术的溅射用靶材制备工艺，其特征在于，步骤3.2中，载体气体将待喷涂粉体送入等离子体流中的速率为1-100g/min。
6.根据权利要求2所述的基于等离子喷涂技术的溅射用靶材制备工艺，其特征在于，步骤3.2中，等离子体喷涂机的电弧直流功率为1-400kW。
7.根据权利要求2所述的基于等离子喷涂技术的溅射用靶材制备工艺，其特征在于，步骤3.3中，喷射距离为20-200mm，等离子体喷涂机的喷枪移动速度为2-500cm/s。
8.根据权利要求2所述的基于等离子喷涂技术的溅射用靶材制备工艺，其特征在于，步骤3.3中，在喷枪将待喷涂粉体均匀喷涂在底板的指定区域上时，在吹送冷却气流围绕在喷涂火焰周围以控制底板温度。
9.根据权利要求2所述的基于等离子喷涂技术的溅射用靶材制备工艺，其特征在于，步骤3.3中，在喷枪将待喷涂粉体均匀喷涂在底板的指定区域上时，在底板的背面通冷却水以控制底板温度。
10.根据权利要求8或9所述的基于等离子喷涂技术的溅射用靶材制备工艺，其特征在于，底板的温度控制在小于等于90％待喷涂粉体的熔点。
11.根据权利要求1所述的基于等离子喷涂技术的溅射用靶材制备工艺，其特征在于，步骤1中，待喷涂粉体加工后的粒度范围为5-500um。
12.根据权利要求1所述的基于等离子喷涂技术的溅射用靶材制备工艺，其特征在于，步骤2中，满足等离子喷涂的表面处理包括增强附着力处理、调整热膨胀系数差值处理、污染物减少处理、表面粗糙度处理以及表面过渡层增设处理，在进行表面处理时，根据需要选择实施其中的一种处理或多种处理组合。
13.根据权利要求1所述的基于等离子喷涂技术的溅射用靶材制备工艺，其特征在于，步骤2中，底板为浮地、接地或另加直流偏置。
14.根据上述任一项权利要求所述的基于等离子喷涂技术的溅射用靶材制备工艺，其特征在于，底板为纯金属、合金或导电型非金属材质。
15.根据上述任一项权利要求所述的基于等离子喷涂技术的溅射用靶材制备工艺，其特征在于，待喷涂粉体为用于制备固态电池电解质的粉体中的单一粉体或几种粉体的混合粉体，或者为用于制备钠离子电池正负极材料的粉体中的单一粉体或几种粉体的混合粉体。
16.根据权利要求15所述的基于等离子喷涂技术的溅射用靶材制备工艺，其特征在于，用于制备固态电池电解质的粉体包括磷酸锂、硅酸锂、氮化硅、磷酸铁锂、Li(NiCoSl)O2、Li(Mn2O4)、硅、石墨、LiTiO3、LLTO、LLZO以及钴酸锂；用于制备钠离子电池正负极材料的粉体包括钠-过渡金属氧化物、钠-过渡金属磷酸盐及变种、钠-过渡金属硫酸盐、钠-过渡金属普鲁士蓝类化合物、硬碳、软碳以及过渡金属氧化物。
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