CN113474108A - 用于制造物理气相沉积(pvd)用靶的方法 - Google Patents
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Abstract
一种用于构建和/或最终形成PVD靶的方法，其中，该方法包括使用增材法来累加靶材的工艺步骤。
Description
本发明涉及一种用于制造要在涂覆机内用于PVD的靶的方法。
PVD靶被用于许多不同的物理气相沉积工艺中，以将薄膜沉积到基材上。这些工艺中最常见的是电弧沉积和溅射。在这两种工艺中，靶都被用作阴极。在这两种情况下，靶都被放入涂覆室中并且涂覆室在沉积过程中被抽真空。
为了电弧沉积，电子产生在阴极(＝靶)处的电弧斑中并被吸引到阳极。在靶面以基本随机的方式移动的电弧斑加热靶面上的斑区且靶材几乎以爆炸方式被蒸发。在涂覆过程中，待涂覆基材与靶面对置，使得蒸发粒子被沉积到待涂覆基材表面。由于大部分蒸发粒子被电离，故施加于基材的(相对于靶而言的)负偏电压甚至会使粒子加速到达基材，由此获得高密度的涂层，这构成这种涂覆方法的其中一个优势。但相当常见的是，不仅粒子/离子从靶面蒸发，靶面材料也因为高温冲击而熔化形成液滴，这些液滴也被喷射且沉积到待涂覆基材表面。对某些应用而言这是一个缺点，因为这种液滴在基材表面形成断点，其有时易破裂且由此在涂层中形成孔洞。
有多种不同的有效方法来避免液滴问题例如过滤和/或脉冲化。但这影响到涂覆工艺的经济性，例如降低沉积速率。
为了溅射，在靶材表面前方产生来自工作气体(如氩气)的正离子。当靶被施以高的负电压时，离子朝着靶面被加速、撞击靶面并通过其撞击来气化/轰离靶面材料。但这种基于电离工作气体的气化过程在标准溅射情况下实际上形成仅少量的电离金属蒸气(与阴极电弧蒸发相比)。在涂覆过程中，待涂覆基材与溅射靶面相对放置，使得蒸发靶材沉积在待涂覆基材表面。
溅射工艺的一个优点是，如果该工艺以适当的方式进行且由此避免过多电弧，则不会形成液滴并且涂层将是均质光滑的。但一个缺点是，如果使用传统的溅射功率，大部分蒸发粒子不会被电离。因此，通过用负电位对基材施加偏电压，只会增大工作气体离子的能量，而不会改变或增加蒸发靶材的原子。工作气体(如氩气)能量的增大可能有助于增大涂层密度，但也可能导致基材表面和在基材表面处的合成涂层被溅射。
为了通过溅射获得高比例的电离粒子，已知可以使用非常高的溅射功率。不幸的是，在此过程中输入到靶中的能量也很高且靶温急速升高，由此在短时间内毁坏靶。为了避免这种情况，功率被脉冲化，由此中断能量输入并给靶提供再次冷却的时间。但这也对涂覆经济性(如沉积速率)产生负面影响。
因此，所有这些方法的关键点在于，在设置用于承载靶材的板与“安装”靶的支座“板”之间有极好的接触。就此而言的接触是指机械接触和/或热接触和/或电接触。就此而言的出色机械接触是指：在载有靶材的板与可供靶因使用而附接的靶座表面之间没有间隙，并且该靶座被相应构造，使得靶无法被弯曲。
就此而言，出色的热接触意味着，在设置用于承载靶材的板和可供靶附接的且被冷却的支座板之间，在这两个表面之间的接触区内只能测量到可忽略不计的温差。][RJ(L1]可以通过施加附加外部压力来增大靶板与支座之间的接触压力以改善热接触。
就此而言，出色的电接触意味着在设置用于承载靶材的板和可供靶附接的支座之间有小于1欧姆、更优选小于0.1欧姆，更优选小于0.05欧姆的电阻I。][RJ(L2]
-机械接触应该是良好的，以便在例如因在电弧蒸发期间集中于局部的能量冲击而使得温度梯度作用于靶面的情况下不允许靶面变形。
-热接触应该良好，以保证靶的快速有效冷却，靶是因在例如高功率脉冲磁控管溅射期间的极端能量冲击而变热的。
-在任何情况下，电接触都应良好，以便在沉积过程中将靶用作阴极表面。
为了生产PVD靶，采用了不同的技术。已知的方法基本可被分为粉末冶金方法和基于金属熔化的方法。对于粉末冶金方法，有许多不同的可能方式，对此在考虑要加入的元素特性的情况下，根据所期望的靶的组成来使用和按需选择。例子是压制(例如热等静压)或烧结、焊接、轧制、热压和放电等离子体烧结或其组合。
所有这些PVD靶制造方法的一个问题是，靶材本身与供其安装的且尤其要处于良好的机械接触、热接触和电接触的基板是分开生产的。该安装需要费力地两步完成，这使得整个过程复杂、昂贵且有时(尤其在涉及脆性靶材时)显著降低产量。
另一个问题是，至少如果靶被用于磁控溅射，则材料主要沿所谓的“跑道”从靶脱离。在一段时间后，沿该跑道形成凹槽，一旦所述凹槽变得太深，则使得靶无法使用，尽管在所述凹槽外仍有大量材料。由于靶材相当昂贵，故靶材使用率至关重要。
因此需要一种至少部分克服前述的现有技术缺陷的靶制造方法。
因此，本发明的目的是至少部分克服这些问题。
根据本发明，该制造方法包括使用增材法来添加靶材的工艺步骤：
根据本发明的一方面，靶材通过热喷涂法来添加。
根据本发明的第二方面，靶材通过传统的激光熔覆来添加。
根据本发明的第三方面，靶材通过极高速激光熔覆(EHLA)来添加。如果需要生产盘状靶，因为它们实际上具有旋转对称性，因此这是非常有效的。
根据本发明的第四方面，靶材通过3D打印方法来添加。如果靶材需要具有内部结构如微间隙，则这是尤其有效的。这种间隙可被用于使靶更耐温。在WO20151971696中描述了该原理本身。但在WO20151971696中使用了随机分布的微间隙，而增材方法且特别是3D打印方法允许靶中有预先规定的微间隙。另一个优点是，借助于3D打印，在靶材本身可预见用于水冷或空冷的冷却通道，其允许很高效的冷却方法。
本发明的另一方面是靶修复和/或靶填补：除了用增材方法来完全构建该材料外，还可以通过这些方法中的一种或多种来部分添加材料。也可以将传统的靶制造方法如烧结和/或热等静压与这些增材方法中的一种或多种相结合。
例如可行的是通过增材方法来局部填补跑道凹槽。因此可以修复用过的靶，使其能够被再用。没有必要启用从基板开始构建的全新靶。也没有必要从基板上剥离剩余靶材以修补它。就此而言，传统的激光熔覆、热喷涂或3D打印是特别有效的。
在电弧靶的情况下，有时会因某些工艺缺陷而在靶板中烧出孔洞。根据本发明的增材步骤允许修复这样的靶。
根据本发明的另一方面，可以使用迄今为止难以或甚至无法组合的材料组合。如果增材方法基于粉末材料，则可以使用粉末混合物来执行增材步骤，用以构建或最终形成靶板。
现在将基于非限制性例子并在所示附图的帮助下详述本发明。
图1示出该过程之前的靶。
图2示出该过程之后的靶。
图3示出涂覆层的表面。
图4示出另一张具有更高放大倍数的涂覆层表面照片。
图5示出EDX，其示出涂覆层的表面化学成分。
图6示出在高放大倍数下的利用根据本发明的靶来涂覆的层的断口横截面的SEM。
图7示出在与图6相比较低放大倍数下的利用根据本发明的靶来涂覆的层的另一个SEM。
图8示出通过涂覆层的球痕研磨所获得的所谓的圆顶坑轮廓。
图9示出沿涂覆层横截面的EDX线扫描。
根据以下示例，靶基板通过激光熔覆方法被涂覆。熔覆材料包含21.5％的Ni、8.5％的Cr、3.5％的Mo、3％的Nb且余量为Fe。它是一种标准规格的粉末。欧瑞康美科以商品名MetcoClad 625F销售这种粉末。
MetcoClad 625F被添加到适于固定在卡口夹具中的底板表面。将材料添加至表面的方法是激光熔覆。
图1示出所生成的未用的靶。在制造后，靶是略弯的。但它能够容易地以机械方式被充分压平，从而适合被插入到电弧蒸发镀膜机中。这已经表明激光熔覆涂层在金属基板上的出色附着性。靶被插入到涂覆机中，并且约10微米的涂层被沉积而没有出现任何问题。为了测试在非反应性和反应性电弧蒸发中的可靠操作，靶在开始时在没有氧气情况下操作，然后连续在电弧蒸发中加入氧气流，从而在朝着层表面的生长过程中产生连续氧化层。
图2示出被用于沉积之后的靶。靶面也未显示出任何问题。
于是，发明人分析了该涂层。图3和图4示出涂层表面。可以看到该涂覆过程产生粗糙表面，其涂层含大量液滴。但这未必是一个缺点。
进行用于测量所涂覆的层表面的化学成分的EDX。它在图5中被示出。EDX显示氧化层表面。氧化层中的金属组成的化学成分与用于激光熔覆的MetcoClad625F粉末大体上一致。如前所述，为了测试在非反应性(无氧气)和反应性(具有不同氧流量)气氛中的工艺稳定性，以递增氧的方式生产该层。在图8中，圆顶坑轮廓通过朝着近表面层区(3.5微米)的颜色变化来表明在7.2微米之后的形貌变化，这种颜色变化是由在沉积过程中氧渐变所导致的。
为了显示所沉积的涂层的形貌，拍摄所沉积的层的两个横截面的SEM照片。它们在图6和图7中被示出。形貌的变化也能在此横截面显微照片中被简要说明(图6，在约7微米后)。
图9示出在整个涂层范围的EDX线扫描，并且清楚表明层中的氧渐变。
Claims (11)
1.一种用于构建和/或最终形成PVD靶的方法，其特征在于，该方法包括使用增材方法来累加靶材的工艺步骤。
2.根据权利要求1所述的方法，其特征在于，所述增材方法是一种选自如下组成的方法组的方法：热喷涂法、传统激光熔覆法、极高速激光熔覆法或3D打印法，或者是其中两种或更多种所述方法的组合。
3.根据权利要求1至2中任一项所述的方法，其特征在于，在所述增材方法的至少一部分过程中，材料组合被用来构建和/或最终形成该PVD靶。
4.根据前述权利要求中任一项所述的方法，其特征在于，所述增材方法基于粉末材料，所述粉末优选为粉末混合物。
5.根据前述权利要求之一的方法，其特征在于，在所述增材方法期间实现预先规定的微间隙。
6.根据前述权利要求之一的方法，其特征在于，该方法是用于修复和/或重新填补该靶的方法。
7.根据权利要求1至5中任一项所述的方法，其特征在于，用该增材法来涂覆靶基板，以完全实现新靶。
8.根据权利要求1至6中任一项所述的方法，其特征在于，所述靶包括靶基板和靶材，其中，所述靶材被添加到所述基板。
9.根据权利要求1至8中任一项所述的方法，其特征在于，在该靶材已被加入后，该靶被压平，特别是该靶以机械方式被压平。
10.一种靶，包括靶基板和靶材，其中，该靶材直接位于该靶基板上，其中，该靶基板尤其具有与该靶材不同的材料，并且其中，尤其是该靶材是通过使用根据权利要求1至9之一所述的方法被添加到该靶基板的。
11.3D打印方法的用途，用于改善在构建和/或最终形成和/或修复和/或重新填补由基板和该基板所载的靶材组成的靶的过程中所达成的热接触和/或电接触，做法是所需要的靶材被3D打印到该基板和/或已由该基板所载的靶材上，优选甚至是在其上完成所述3D打印的靶材本身并非是3D打印而成的。
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| PCT/EP2020/054779 WO2020169847A1 (en) | 2019-02-22 | 2020-02-24 | Method for producing targets for physical vapor deposition (pvd) |
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| CN113523298B (zh) * | 2021-06-30 | 2023-07-07 | 洛阳科威钨钼有限公司 | 一种平面锂靶材的制备方法 |
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| US7794554B2 (en) * | 2001-02-14 | 2010-09-14 | H.C. Starck Inc. | Rejuvenation of refractory metal products |
| DE102014009419B4 (de) | 2014-06-25 | 2023-06-07 | Zf Cv Systems Hannover Gmbh | Druckluftversorgungsanlage, pneumatisches System und Verfahren zum Steuern einer Druckluftversorgungssanlage |
| AT14346U1 (de) * | 2014-07-08 | 2015-09-15 | Plansee Se | Target und Verfahren zur Herstellung eines Targets |
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| WO2002064287A2 (en) * | 2001-02-14 | 2002-08-22 | H. C. Starck, Inc. | Rejuvenation of refractory metal products |
| WO2004074540A1 (en) * | 2003-02-24 | 2004-09-02 | Tekna Plasma Systems Inc. | Process and apparatus for the maufacture of a sputtering target |
| CN1918320A (zh) * | 2004-03-15 | 2007-02-21 | 贝卡尔特先进涂层公司 | 减小溅射靶中热应力的方法 |
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| US20180323047A1 (en) * | 2015-11-12 | 2018-11-08 | Honeywell International Inc. | Sputter target backing plate assemblies with cooling structures |
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| US20170287685A1 (en) * | 2016-04-01 | 2017-10-05 | Honeywell International Inc. | Sputtering target assembly having a graded interlayer and methods of making |
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| KR20210130178A (ko) | 2021-10-29 |
| US20220145446A1 (en) | 2022-05-12 |
| CA3130828A1 (en) | 2020-08-27 |
| EP3927485A1 (en) | 2021-12-29 |
| WO2020169847A1 (en) | 2020-08-27 |
| JP2022523357A (ja) | 2022-04-22 |
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