CN103796425B - 用于使在低温基底上的薄膜高速反应的方法和装置 - Google Patents
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Abstract
公开了一种用于使低温基底上的薄膜在反应气氛内反应的方法。所述薄膜包含可还原的金属氧化物,并且所述反应气氛包含诸如氢或甲烷的还原气体。所述低温基底可以为聚合物、塑料或纸。使用来自高强度频闪系统的多个光脉冲将所述金属氧化物还原成金属并且如果适用则烧结所述金属。
Description
本申请是申请日为2009年10月19日、国际申请号为PCT/US2009/061172、中国国家申请号为200980145384.3、名称为“用于使在低温基底上的薄膜高速反应的方法和装置”的PCT专利申请的分案申请。
相关申请的交叉引用
本申请基于35U.S.C.§119(e)(1)要求2008年10月17日提交的临时申请61/196,531的优先权,通过参考将其内容并入到这里。
技术领域
本发明一般而言涉及固化方法,具体而言,涉及用于使低温基底上的薄膜高速反应的方法和装置。
背景技术
在电路上形成电导体的一种方法是将包含金属的墨印刷到基底上,然后加热基底以烧结包含金属的墨中的颗粒,从而形成导电路径。通常,适合电传导的大多数金属需要被加热到非常高的温度,该温度通常在其熔点的两百摄氏度的范围内。例如,银是用于形成导电迹线的良好金属,这是因为其可以在空气中被加热,并且电导率相对低的其氧化物在相对低的温度下分解。另外,当在选择用于形成导电迹线的金属时,银是导电性最好的金属的事实经常胜过其高成本。
由于其低成本,在制造导电迹线时一直使用的另一种金属是铜。铜具有约为银的电导率的90%的电导率,但通常比银便宜50到100倍(基于质量)。然而,由于制造和处理铜墨以避免氧化的附加成本通常高于体材料的成本差异,因此银墨仍支配着印刷电子市场。基本上,当在空气中加热铜颗粒时,它们在烧结之前氧化,这导致非导体。
因此,希望提供一种用于使用诸如铜的相对低成本金属制造导电迹线的改进的方法。
发明内容
根据本发明的优选实施例,最初提供气态气氛。然后将位于低温基底顶上的薄膜层输送通过所述气态气氛。在所述薄膜层被输送通过所述气态气氛时,将所述薄膜层暴露到多个脉冲电磁发射,以使所述薄膜层与所述气态气氛化学反应。
本发明的所有特征和优点将在下面详细的描述中变得显而易见。
附图说明
通过参考对示例性实施例的以下详细描述并结合附图阅读,本发明本身以及优选使用模式、其他目的及其优点将得到最好的理解,在附图中:
图1为根据本发明的优选实施例的固化装置的图;以及
图2为根据本发明的优选实施例的用于使低温基底上的薄膜反应的方法的高级逻辑流程图。
具体实施方式
公知如果某些金属氧化物具有正还原势,则这些金属氧化物可被氢或烃还原。实例包括铜、金、铂和钯的氧化物。可以通过利用加热工艺使含有铜氧化物的矿石与木炭反应而制成铜。当在还原气氛中加热氧化的铜颗粒或者甚至纯铜氧化物时,颗粒可烧结而形成导体。
当通过印刷铜颗粒而制造薄膜导体时,如果在惰性或还原气氛中将颗粒加热到其烧结温度,则可以形成导电优良的迹线。由于铜的熔点接近1085℃,因此烧结所需的温度要求仅仅可以采用高温基底,例如玻璃或陶瓷。对基底的该相对高温度要求阻止了诸如纸或塑料的便宜基底的使用。
备选地,如果将铜氧化物置于低温基底上,铜氧化物可被加热到接近基底的分解温度并可将低温基底置于还原气氛中。然而,依赖于基底厚度,低温基底使所需的时间量大幅增加到数分钟或甚至数小时。并且,在这些低温度下,烧结非常有限。如果利用强而短的光脉冲来固化基底,则基底温度和气体气氛要求可被克服。不幸地,这些方法对于在铜膜中解决剩余氧化物的问题没有作用。可还原的金属氧化物可在氢气氛中被置于两个电接触之间,并且电流可被反复地脉冲通过氧化物以加热氧化物并还原氧化物。然而,该技术需要电接触,并且其吞吐量相对有限。由此,需要以高吞吐量在低温基底上还原金属氧化物。
为了本发明,将固化限定为热处理,其包括使薄膜与气态气氛反应。薄膜被限定为小于100微米厚的涂层。低温基底可以由纸、塑料或聚合物构成。电磁发射可包括电磁辐射,其包括γ-射线、x-射线、紫外、可见光、红外光、毫米波、微波、或无线电波。电磁发射源包括激光器、感应加热器、微波发生器、闪光灯、发光二极管等等。
下面参考附图,特别地,参考图1,其描述了根据本发明的优选实施例的固化装置的图。如图所示,固化装置100包括传送带系统110、频闪头120、继电器架(relay rack)130和卷到卷(reel-to-reel)供应系统140。固化装置100能够固化被安装在位于以相对高的速度跨传送带移动的毛网(web)上的低温基底103上的薄膜102。传送带系统110可以以例如0到1000ft/min的速度工作以移动基底103。固化装置100可收纳6英寸增量的任何宽度的毛网。可通过现有技术的一种或组合,将薄膜102附加到基底103上,这些现有技术为例如丝网印刷、喷墨印刷、凹版印刷、激光印刷、静电复印、移印(pad printing)、涂抹、蘸水笔(dippen)、注射(syringe)、气刷、橡皮版印刷、化学气相沉积(CVD)、蒸发、溅射等等。
频闪头120包括用于固化位于基底103上的薄膜102的高强度脉冲氙闪光灯121,该频闪头120优选为水冷的。脉冲氙闪光灯121可提供不同的强度、脉冲长度和脉冲重复频率的脉冲。例如,脉冲氙闪光灯121可提供脉冲重复速率最高为1kHz的具有3’’乘6’’宽度束的10微秒到50毫秒脉冲。来自脉冲氙闪光灯121的发射的光谱含量的范围为200nm到2500nm。可以通过用铈掺杂的石英灯替代石英灯而调整光谱以去除低于350nm的大多数发射。还可以用蓝宝石灯替代石英灯以使发射从约140nm延伸到约4500nm。还可以添加滤光器以去除光谱的其他部分。闪光灯121还可以是有时被称为定向等离子弧(DPA)灯的水冷壁闪光灯。
继电器架130包括可调电源131、传送控制模块132和频闪控制模块134。可调电源131可产生具有最高为4千焦耳每脉冲的能量的脉冲。可调电源131被连接到脉冲氙闪光灯121,并且可以通过控制流过脉冲氙闪光灯121的电流的量来改变来自脉冲氙闪光灯121的发射的强度。
可调电源131控制脉冲氙闪光灯121的发射强度。依赖于薄膜102和基底103的光学、热学和几何特性,来自脉冲氙闪光灯121的发射的功率、脉冲持续时间和脉冲重复频率被电子地调整和同步到毛网速度,以允许对薄膜102的最优固化而不损伤基底103。
在固化操作期间,基底103以及薄膜102被移动到传送带系统110上。传送带系统110使薄膜102在频闪头120下方移动,在那里薄膜102被来自脉冲氙闪光灯121的快速脉冲所固化。通过频闪控制模块134控制来自脉冲氙闪光灯121的发射的功率、持续时间和重复速率,并且由传送控制模块132确定基底103移动经过频闪头120的速度。
利用传感器150来感测传送带系统110的速度,该传感器150可以是机械的、电学的或光学的传感器。例如,可以通过检测来自被连接到与移动的传送带接触的轮的轴端编码器的信号来感测传送带系统110的传送带速度。反过来,可以相应地用传送带系统110的传送带速度来同步脉冲重复速率。由下式给出频闪脉冲速率f的同步:
其中f=频闪脉冲速率[Hz]
S=毛网速度[ft/min]
O=重叠因子
W=固化头宽度[in]
重叠因子O为由基底接收到的频闪脉冲的平均数目。例如,当毛网速度为200ft/min,重叠因子为5,固化头宽度为2.75英寸时,频闪灯的脉冲速率为72.7Hz。
外壳160包围基底103并包含还原气氛161。透明窗口162使来自闪光灯121的光通过。当闪光灯121被脉冲时,膜102被瞬时加热并与气氛161化学反应。当快速脉冲串与移动基底103组合时,可以在薄膜102的每个部分被暴露于多个脉冲时在任意大的面积内获得均匀的固化,这近似于诸如炉的连续固化系统。
现在参考图2,其描述了根据本发明的优选实施例的用于使低温基底上的薄膜反应的方法的高级逻辑流程图。最初,如块221中所示,提供包含还原气体的气态气氛,例如图1的还原气氛161。优选地,气态气氛包含氢或烃,例如甲烷、丙烷等等。
接下来,如块222中所示,将位于低温基底顶上的薄膜层输送通过该气态气氛。该薄膜优选包含可还原的金属氧化物,例如铜氧化物(CuO)、金氧化物(Ag2O)、铂氧化物(PtO)和钯氧化物(PdO)等等。为了经济,希望铜作为用于印刷电子设备的导体。印刷的铜膜通常包含作为电子传导的阻挡层的铜氧化物。低温基底可以由聚合物或纸构成。
然后,如块223中所示,在薄膜层被输送通过气态气氛的同时,将每段(即,固化头宽度)薄膜层暴露到来自闪光灯(例如图1中的闪光灯121)的至少一个脉冲,以使薄膜层与气态气氛化学反应。基本上,来自频闪系统的脉冲在还原位于低温基底上的诸如铜氧化物的金属氧化物的薄膜,以在小于一秒内形成诸如铜膜的导电金属膜而不损伤低温基底。
当在氢环境中将金属氧化物还原为金属时,反应进行的速度是受到扩散限制的。扩散速率与固化系统的温度有关。当利用炉子时,温度受到低温基底的分解温度的限制。脉冲光将金属氧化物加热到极高的温度而不分解低温基底。这大幅地缩短了用于还原金属氧化物的时间。
如上所述,本发明提供了一种用于使低温基底上的薄膜反应的方法和装置。本发明的一个优点在于,即使在最初沉积纯金属氧化物时也可以获得金属薄膜。沉积金属氧化物颗粒的动机之一是,它们比其金属对应部分更容易得到,当它们处于纳米颗粒形式时尤其如此。在保持其纯度的同时形成极微细(几十nm)金属颗粒是尤其困难的。极微细金属颗粒通常被氧化物和/或帽盖基团覆盖。此外,金属氧化物颗粒更容易被分散,并且更容易被印刷在各种基底上。
本发明的另一优点在于其不需要配准(registration)。如果薄膜是印刷图形,则仅仅那个图形反应,而低温基底的通常较不吸收光脉冲的未印刷部分保持冷却。
虽然金属氧化物的还原被示出为在还原气氛中以形成金属膜,但其他膜/反应气体组合也是可能的。其他实例包括:
(1)利用H2进行还原(或者产生氢化物用于H2存储材料)
(2)利用O2进行氧化(用于电介质)
(3)利用含碳气体进行渗碳(carburization)以形成碳化物。在含碳气体流内的O2分压以形成氧碳化物。
(4)利用氨或胺进行氮化以形成氮化物。在氨或胺气体流内的O2分压以形成氧氮化物。
(5)由各种前体气体形成硫属化物。硫属化物为硫化物(S2-)、硒化物(Se2-)以及碲化物(Te2-)。这覆盖了一大类半导体(II-VI半导体),例如,ZnS、ZnSe、CdS、CdSe、CdTe等等。
(6)由各种前体气体形成磷属化物(pnictide)。磷属化物为磷化物(P3-)、砷化物(As3-)和锑化物(Sb3-)。这也覆盖了一大类半导体的合成(III-V族半导体),例如,GaP、GaAs、InP、InAs、InSb等等。
虽然已经参考优选实施例具体示出并描述了本发明,但本领域技术人员将理解,在不脱离本发明的精神和范围的情况下,可以在其中进行形式和细节上的各种变化。
Claims (17)
1.一种用于使低温基底上的薄膜反应的方法,所述方法包括:
提供还原气态气氛;
将安装在低温基底上的金属氧化物薄膜层移动通过所述还原气态气氛;以及
将所述金属氧化物薄膜层暴露到脉冲电磁发射,同时使所述金属氧化物薄膜层在所述还原气态气氛内相对于所述脉冲电磁发射的源移动,以使所述金属氧化物薄膜层与所述还原气态气氛化学反应,从而还原所述金属氧化物薄膜层而形成导电金属膜,
其中所述低温基底以与所述脉冲电磁发射的重复速率同步的速度移动,
其中,由下式给出频闪脉冲速率f的同步:
<mrow>
<mi>f</mi>
<mo>=</mo>
<mfrac>
<mrow>
<mn>0.2</mn>
<mo>*</mo>
<mi>S</mi>
<mo>*</mo>
<mi>O</mi>
</mrow>
<mi>W</mi>
</mfrac>
</mrow>
其中f=频闪脉冲速率[Hz]
S=毛网速度[ft/min]
O=重叠因子
W=固化头宽度[in],
所述重叠因子O为由所述基底接收到的频闪脉冲的平均数目。
2.根据权利要求1的方法,其中所述还原气态气氛包含氢。
3.根据权利要求1的方法,其中所述还原气态气氛包含烃气体。
4.根据权利要求1的方法,其中所述还原气态气氛包含多于一种气态物类。
5.根据权利要求1的方法,其中所述金属氧化物薄膜为包含具有正还原势的金属的金属氧化物。
6.根据权利要求5的方法,其中所述金属氧化物为铜氧化物。
7.根据权利要求5的方法,其中所述金属氧化物为铂氧化物。
8.根据权利要求5的方法,其中所述金属氧化物为钯氧化物。
9.根据权利要求1的方法,其中所述低温基底由塑料制成。
10.根据权利要求1的方法,其中所述低温基底由纸制成。
11.根据权利要求1的方法,其中所述低温基底由聚合物制成。
12.一种固化装置,包括:
外壳,用于提供还原气态气氛;
频闪头,具有闪光灯,用于向安装在低温基底上的金属氧化物薄膜层提供脉冲电磁发射,以使所述金属氧化物薄膜层与所述还原气态气氛化学反应,从而还原所述金属氧化物薄膜层而形成导电金属膜;
传送系统,用于使所述金属氧化物薄膜层在所述还原气态气氛内相对于所述频闪头移动;以及
频闪控制模块,用于控制由所述闪光灯产生的所述脉冲电磁发射的功率、持续时间、重复速率和数目,
其中所述低温基底以与所述脉冲电磁发射的所述重复速率同步的速度移动,
其中,由下式给出频闪脉冲速率f的同步:
<mrow>
<mi>f</mi>
<mo>=</mo>
<mfrac>
<mrow>
<mn>0.2</mn>
<mo>*</mo>
<mi>S</mi>
<mo>*</mo>
<mi>O</mi>
</mrow>
<mi>W</mi>
</mfrac>
</mrow>
其中f=频闪脉冲速率[Hz]
S=毛网速度[ft/min]
O=重叠因子
W=固化头宽度[in],
所述重叠因子O为由所述基底接收到的频闪脉冲的平均数目。
13.根据权利要求12的固化装置,其中所述闪光灯为氙闪光灯。
14.根据权利要求12的固化装置,其中通过卷到卷系统传送所述低温基底。
15.根据权利要求12的固化装置,其中所述还原气态气氛包含氢。
16.根据权利要求12的固化装置,其中所述还原气态气氛包含烃气体。
17.根据权利要求12的固化装置,其中所述金属氧化物薄膜为包含具有正还原势的金属的金属氧化物。
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- 2016-08-09 JP JP2016156258A patent/JP6328702B2/ja active Active
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2018
- 2018-04-18 JP JP2018079858A patent/JP2018131691A/ja active Pending
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2019
- 2019-08-09 JP JP2019147583A patent/JP2019189947A/ja not_active Withdrawn
Non-Patent Citations (1)
Title |
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Reduction of Copper Oxide Thin Films with Hydrogen Plasma Generated by a Dielectric-Barrier Glow Discharge;Yasushi Sawada, et al;《Japanese Journal of Applied Physics》;19991115;第38卷(第11期);第6506-6511页 * |
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