CN1669122A - 向接收基板转移碳化硅薄层的优化方法 - Google Patents

向接收基板转移碳化硅薄层的优化方法 Download PDF

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CN1669122A
CN1669122A CNA038046911A CN03804691A CN1669122A CN 1669122 A CN1669122 A CN 1669122A CN A038046911 A CNA038046911 A CN A038046911A CN 03804691 A CN03804691 A CN 03804691A CN 1669122 A CN1669122 A CN 1669122A
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B·吉瑟兰
F·勒特尔特
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Abstract

本发明涉及从源基板(1)向接收基板(4)转移单晶碳化硅薄层(100)的优化方法，包括由以下组成的步骤：用大多数的H+离子轰击所述源基板(1)的正面以形成脆化带(5)；沿所述脆化带(5)从所述源基板(1)的剩余部分(10)分离所述薄层(100)。其特征在于，根据以下不等式进行H+离子的注入，其中注入计量D用每平方厘米的H+离子数目来表示，且用keV表示注入能量E，其大于或等于95keV：[(E×1·1014+5·1016)/1.1]≤D≤[(E×1·1014+5·1016)/0.9]且其特征在于，在粘合步骤之后，施加足够的热量束以完整地或几乎完整地剥落未转移到所述接收基板(4)的源基板(1)的所述薄层(100)的带(12)。

Description

向接收基板转移碳化硅薄层的优化方法
本发明涉及向接收基板或增强基板转移得自相同材料源基板的单晶碳化硅薄层的优化方法，特别地，该方法允许在转移该薄层后再循环所述基板。
例如，已知的商标为“Smart Cut”的方法能够从源基板向氧化硅或多晶碳化硅型的接收基板转移薄层。该方法同样能够再利用已移除该薄层的源基板。
然而，在每个层转移操作之后，源基板的上表面会有一定数量的表面不规则。
将参考图1-5描述这些表面不规则的形成，图1-5示出了进行“Smart Cut”方法的具体示例。该方法是本领域技术人员已知的并不再详细描述。
图1示出了源基板1，其具有称为“正面”的平坦面2，在其上已完成注入气体种类的步骤。通过离子轰击进行注入，例如用H+离子(在图1上标记为B)并使用注入器。
在特定能量、注入剂量和温度下进行注入，以便在离子的平均注入深度p的附近产生标记为3的脆化区域。
脆化区域3在所述的源基板1中限定两个部分，即，一方面，在正面2与所述脆化区域3之间延伸的上薄层100，而另一方面为基板的剩余部分，标记为10。
如图2所示，然后，在源基板1的正面2上施加增强或接收基板4。
由本领域技术人员根据最终的应用预计选择增强件。在已知方式中，可以如下方式施加增强件，例如，通过蒸发、溅射、化学气相淀积，或可以使用粘接剂粘合，或通过英文术语为“wafer bonding”的已知的“分子附着粘合(bonding bymolecular adhesion)”技术。
如图3所示，然后进行从基板1的剩余部分10分离薄层100的步骤。通过向增强件4施加机械应力或通过向增强件4和基板1的组合施加热能进行用箭头S表示的分离步骤。
由于所进行的倒角操作，例如在它们的制造期间，用于分子附着的构成源基板1的胶片具有有下陷边缘。结果，增强件4与正面2之间的粘着力在所述源基板1的基本为环形的外围区域中较弱。
因此，在剥去增强件4的期间，只有与增强件4牢固粘着的薄层100的中心部分被分离，而薄层100基本为环形的外围与源基板1的剩余部分10保持为整体。
由此，源基板1上在其中心部分同时存在由脆化区域3区域中的断裂引起的表面粗糙11和在其外围的额外厚度12或表面拓扑，该额外厚度或表面拓扑是与未转移到接收基板或增强件4上的区域相对应的起泡区域。
额外厚度12的区域深度等于所转移的薄层100的厚度。其典型地从几十纳米变化到大于一微米。该深度决定于氢离子的注入能量。
在这些图中，为了简化和图解，对于源基板的剩余部分10有意使用直角和显著的厚度以截面示出了额外厚度的区域12。实际上，其具有更加不规则的形状和按比例更小的厚度。
在进行以下薄层的转移之前，再循环源基板的剩余部分10是必不可少的。
这种再循环包括，一方面，表面平面化步骤(箭头P)，即，额外厚度12和下陷区域的消除，以及另一方面，进行消除表面粗糙11的特定修整步骤(箭头F)以获得具有新正面2’的基板。
这些再循环步骤通常通过机械和/或机械化学抛光技术来完成。
在源基板1为碳化硅的具体情况中，由于材料非常硬，发现这些抛光步骤进行得非常长并且昂贵。
现有技术文献：“The effect of damage onhydrogen-implant-induced thin-film separation from bulksilicon carbide”，R.B.Gregory，Material Research SocietySymp.，Vol.572，1999，示出了可以改变剥落的区域的百分比来选择向碳化硅中注入氢的条件，即，碳化硅自由表面的百分比，其在基板热退火期间被自发地消除。
在该文献中，在60keV注入能量下，作为剥落区域百分比的函数，表示H+离子注入剂量的结果曲线具有圆锥形，对于5.5·1016H+/cm2的注入剂量来说，剥落区域的最大值为33％。离开该值，即注入剂量增大或降低，则剥落百分比降低。
文献“Complete surface exfoliation of 4H-SiC by H+and Si+co-implantation”，J.A.Bennett，Applied Physics Letters，Vol.76，No.22，pp.3265-3267，2000年5月29日，示出了可以通过共同注入H+和Si+离子完成碳化硅基板表面的完整剥落。
更具体地，该文献描述了在4H-SiC碳化硅上完成的试验，其通过在不同剂量和190keV能量下注入Si+离子，然后在6·1016H+/cm2的注入剂量和60keV能量下注入H+离子。Si+的注入剂量大于或等于5·105Si+/cm2而使碳化硅表面100％剥落。
然而，整个剥落SiC层所必需的Si离子注入剂量同样足够高而使碳化硅变成非晶形态。因此，该方法不适宜转移具有良好晶体质量的碳化硅薄膜，这是由于无法回收用于在微电子或光电子中使用的以后形成的器件的该薄膜。
本发明的目的是纠正所述缺点，特别地是优化注入条件以利于碳化硅源基板的再循环。
该目的通过向接收基板转移得自相同材料源基板的单晶碳化硅薄层的方法来实现，该方法倾向利于源基板剩余部分的循环再利用，其包括以下步骤：
-用大多数的H+离子轰击所述源基板的称为“正面”的平坦面，以便在所述离子的平均注入深度p附近的深度上形成脆化区域，该区域在所述薄层和所述基板的剩余部分之间形成界限，用注入能量E和注入剂量D完成使用所述H+离子的轰击。
-将所述接收基板粘合到所述正面，
-沿所述脆化区域从源基板的剩余部分分离所述薄层。
根据本发明的特征，H+离子的注入根据以下不等式完成，其中注入剂量D用每平方厘米的H+离子数目来表示，且用keV表示注入能量E，其大于或等于95keV：
[(E×1·1014+5·1016)/1.1]≤D≤[(E×1·1014+5·1016)/0.9]
以便以优化方式使所述脆化区域脆化，并在粘合步骤后，施加足够的热量束以便于完整地或几乎完整地剥落未转移到所述接收基板的、源基板的所述薄层区域。
根据本发明的其它优点，但不限于该特征，单独或组合进行：
-所注入的离子为专用H+离子；
-在离子束曝光期间，在不故意加热源基板的情况下完成H+离子的注入；
-源基板是非定向单晶碳化硅；
-首先通过施加外部机械应力沿所述优化的脆化区域完成分离，然后施加足够的热量束用于完整地或几乎完整地剥落未转移到接收基板的薄层区域，否则：
-通过施加适当的热量束同时完成沿优化的脆化区域分离并完整地-或几乎完整地-剥落未转移到接收基板的薄层区域；
-施加完整地或几乎完整地剥落所述薄层区域的所述区域所必需的热量束在700℃以上进行；
-以随机方式实现离子轰击；
-在离子轰击步骤之前，用厚度小于或等于约50纳米(50nm)的非晶形材料层覆盖源基板；
-通过分子粘着完成接收基板向源基板正面的粘合；
-在接收基板的正面和接触面中，至少一个面是用中间粘合层覆盖的；
-所述非晶形材料层和/或所述中间粘合层由选自二氧化硅(SiO2)或氮化硅(Si3N4)的材料构成；
-接收基板选自硅、碳化硅、氮化镓、氮化铝、蓝宝石、磷化铟、砷化镓或锗；
-接收基板是通过区域熔融生长获得的低氧含量的硅；
-该方法还包括修整分离后获得的源基板正面的步骤。
现在将参考本发明的仅作为说明性示例给出的实施例描述本发明，该描述基于附图，其中：
图1-5是表示根据技术状况的转移薄碳化硅层方法的不同步骤的示意图；
图6-18是表示根据本发明的方法及其可替代选择方案的不同步骤的示意图；
图19是表示在不同注入能量下，作为H+离子注入剂量D的函数的剥落区域百分比的曲线图；以及
图20是表示为获得注入层100％剥落的作为H+离子注入剂量D的函数的H+离子注入能量E的值的曲线图。
现在将参考图6-18描述根据本发明的方法。
图6-18非常类似图1-5，且同一元件具有相同的参考数字。
在图6中可以看出本发明的目的是优化单晶碳化硅源基板1中原子种类的注入条件B，以便在离子注入平均深度p的附近产生称为“优化脆化区域”的区域5，从而在层100分离后并在已施加适当的热量束之后，在以后能够100％或约100％剥落起泡的额外厚度区域12，该起泡的额外厚度区域12在现有技术的方法中(参见图3)与基板的剩余部分10保持为整体。
术语“优化脆化”意味着，为了以最佳方式活化所使用的脆化机制，以精确且受控的方式向晶体引入原子种。
在本发明的范围内，原子种的注入包括使用H+离子的基板1的正面2的离子轰击，且可能用H+离子和氦或硼离子联合轰击，而H+离子保持占大多数。
优选使用离子束注入器在单晶碳化硅源基板1的表面中进行这些离子的注入。
为了确定最好的操作条件，在碳化硅源基板1中使用不同的注入轨迹。
如图7和8所示，其示出了碳化硅的晶体结构，通常对源基板1的平坦表面垂直进行离子的注入B。
在图7所示的情况中，相应于定向的碳化硅晶体(以英文术语“on axis”为本领域技术人员所知)，使硅和碳原子的堆叠处于平行于上平坦表面或正面2的平面中。然后离子平行于所述晶体的晶体生长轴C穿透。
与之相反，在图8所示的情况中，相应于不定向的碳化硅晶体(以英文术语“off axis”为本领域技术人员所知)，使硅和碳原子的堆叠处于与正面2不平行而是与其形成角度α的平面中。然后离子沿垂直于所述正面2的轴穿透而以角度α的值从所述晶体生长轴C有角度地偏移。
在两种所述情况中，由离子注入产生的微腔50主要在垂直于晶体生长轴C的平面中形成。
因此，在定向晶体中，微腔50平行于正面2，且形成与所述正面2的平面平行的并产生实际上连续的断裂线的优化脆化区域5，而在不定向晶体中，这些微腔50对于正面2的平面倾斜且不形成连续的线。
实验上已经观测到，对于给定的注入剂量D和能量E来说，当在不定向晶体上进行注入时，获得更大的脆化区域5并在以后获得更好的额外厚度12的剥落百分比。
在有利的意义上，在本发明的方法中，以随机方式进行该离子注入，以避免称为“沟道效应(channeling)”的现象。
当沿特定沟道或结晶轴注入离子时发生沟道效应现象。由此，引入的离子在它们的轨道上遇到较少的原子，结果所述离子的相互作用较少且减速更少。因此这些离子将注入地更深。
在根据本发明的工艺中，由于沟道注入不是工业上可行的技术，而寻求相反地避免了由于工业原因引起的沟道效应现象。
而且，为了在分离期间提高最终获得的剥落百分比并在随机注入模式中操作，优选的是(但不是必需的)通过在基板1的正面2上形成的非晶材料20的层进行离子注入。该可选实施例在图9中示出。
该非晶材料20的层有利的是由二氧化硅(SiO2)或氮化硅(Si3N4)构成的层。然而，由于将在以后确定的连接注入能量E和注入剂量D关系有被改变的危险，该层不应超过约50nm(5·10-9)的厚度。
最后，优选地在不提供外部热量的情况下进行完成所示离子注入的试验，即，在最大温度约200℃下，该注入能够使碳化硅基板到达该温度。
如果在注入期间加热基板，例如到显著大于650℃的温度，则观察到大范围剥落现象的退化或抑制。这可以由扩散注入和参与在工艺中的再结晶机制期间的活化来解释。这种不受控的原位活化退化了对所期望的剥落效应的控制。
此外，为了确定所使用的最好的注入剂量D和注入能量E数值对，进行补充试验。这些试验将在以后详细描述。
然后，将接收基板4粘合到源基板1的正面2。
该基板4的粘合有利地通过分子粘着来实现，因为这种粘合模式最适于电子应用，特别是归因于使用的粘合力的均匀性和不同种类的众多材料粘合在一起的可能性。然而，同样可以通过其它已知的现有技术来完成。
通过将接收基板4的称为“接触面”的一个面40加到源基板1的正面2上，并直接(参见图10)或通过一个或多个中间粘合层6(如图11所示)完成该粘合，其中该中间粘合层6设置在基板4的接触面40上，或源基板1的正面2上，或在这两个面上。
这些中间粘合层6是绝缘层，例如，由二氧化硅(SiO2)或氮化硅(Si3N4)构成，或者另一方面，这些中间粘合层6为导电层。
应该注意到，当通过由非晶材料20构成的层进行注入B时，则该层可以作为部分中间粘合层6。
分别如图12和13所示得到层的组合。
接收基板有利地(但不是必须的)选自硅、碳化硅、氮化镓(GaN)、氮化铝(AlN)、蓝宝石、磷化铟(InP)、砷化镓(GaAs)或锗(Ge)。同样可以使用其它材料。
同样，接收基板可以是易碎基板，例如通过区域熔融生长获得的低氧含量的硅，即，由多晶硅通过区域熔融得到的单晶硅。
然后进行接收基板4的分离并从基板1的剩余部分10分离薄层100(箭头S)。
可以通过施加外部机械应力(如图14所示)或通过具有适当热量束的热处理(参见图17)进行该分离S。
在本领域技术人员所知的方式中，这些外部机械应力可以是例如施加剪切力、牵引力或压力，或施加超声波、静电场或电磁场。
如果采用外部机械应力进行分离S，则随后进行退火处理，该退火处理根据适当的热量束完整地或几乎完整地将薄层100的区域12从未与接收基板4粘合的源基板1上剥落(参见图15)。热量束等于处理持续时间与退火处理温度的乘积。
然而，该处理比技术状况中用于进行这种操作所使用的抛光更简单且更快。
此时，仅剩下源基板1的合适修整步骤F(参见图16)。
该修整步骤的目的在于消除表面粗糙11。通常通过机械化学抛光来进行。
同样可以进行薄层100的自由表面的修整步骤。
如果薄层100从源基板1的剩余部分10的分离S通过热退火处理进行(参见图17)，则同时进行区域12的完整或几乎完整的剥落(参见图18)。实际上，热的施加使缺陷或微腔50生长直到它们形成微裂纹51，它们连接起来，结果形成解理面并沿所述优化的脆化区域5的裂开。
然后进行合适的修整步骤F，如图16所示。
现在将描述确定H+离子最佳注入剂量D和注入能量E的数值对的试验。
操作条件：
在8°不定向的单晶碳化硅SiC4H基板(以“SiC4H 8°off-axis”为本领域技术人员所知)的正面上进行H+离子注入，该基板覆盖有约50纳米(50nm)厚的二氧化硅非晶层。
注入温度为200℃以下。
分别在50keV、95keV、140keV和180keV的注入能量E下进行四组试验。
对每个能量E的数值来说，注入剂量D在5.25·1016H+/cm2到8·1016H+/cm2之间变化。
然后将由硅构成的接收基板4加到源基板1上，然后在900℃下进行1小时退火。
然后测量外围区域12的剥落百分比，该外围区域12在现有技术中与基板的剩余部分保持为整体。
获得的结果在下表中给出。
数值100％意味着未与接收基板4密切接触(即，未粘着)的这个区域12被整体剥落。例如，数值30％意味着只有30％的额外厚度区域12被剥落，而70％的区域12与基板1的剩余部分10保持为整体。
                                  注入剂量D(1016H+/cm2)
 注入能量E(keV) 5.25 5.5 5.75 6 6.5 6.75 7 7.25 7.5 8
剥落区域(％)     50     5   50    15
    95   10   100   60   30
    140   40   80    100   60   40
    180   30   90   100   80   40
注入能量低于50keV进行的试验未给出良好的剥落结果。
获得的结果已转换成图19的曲线。可以看出，对于大于或等于95keV的各个注入能量E的数值来说，可以获得能够100％剥落的注入剂量数值D(获得圆锥形曲线)。
图20是表示作为这些相同离子的注入能量E的函数的为获得100％剥落区域的H+离子注入剂量D的曲线图。
获得的直线与以下等式相对应：
       D＝E×1·1014+5·1016        (1)
其中E≥95keV，
其中H+离子的注入能量E用keV表示，并用H+离子/cm2表示注入这些离子的剂量D。
考虑到与可能的微小的实验变化和制造公差以及使用的注入设备的控制相关的D和E数值的波动，认为D和E的数值对应遵循以下不等式：
-ε×D≤D-(E×1·1014+5·1016)≤ε×D     (2)
其中D和E具有前述意义，且ε×D表示对于给定的E的数值来说，根据以上等式(1)获得的D的理论值和D的允许值之间的绝对公差，且其中ε表示相对公差。
试验后，认为该相对公差ε等于10％。
由此得到以下不等式(3)：
-0.1×D≤D-(E×1·1014+5·1016)≤0.1×D        (3)
其还可以表示为以下不等式(4)
[(E×1·1014+5·1016)/1.1]≤D≤[(E×1·1014+5·1016)/0.9]
遵循以上不等式的D和E的数值对能够获得优化的脆化区域5的脆化，且在施加足够的热量束后，能够完整地或几乎完整地剥落未转移到接收基板4上的薄层100的区域12。
然后进行补充试验以确定适当的热量束。
在700℃以下，SiC中的氢扩散机制几乎不起作用。
由此可以确定，完整地或几乎完整地剥落区域12所必需的热量束必须在700℃以上且优选地在800℃以上。
另一方面，由此获得具有良好结晶质量的SiC薄层100，且另一方面，源基板1的正面不具有表面拓扑12。

Claims (15)

1.一种转移单晶碳化硅薄层(100)的方法，其从相同材料的源基板(1)向接收基板(4)转移，该方法意图利于源基板(1)的剩余部分(10)的再循环，包括由以下组成的步骤：
-用大多数的H+离子轰击所述源基板(1)的称为“正面”的平坦面(2)，以便在所述离子的平均注入深度p附近的深度上形成脆化区域(5)，该区域(5)在所述薄层(100)和所述基板(1)的剩余部分(10)之间形成界限，用注入能量E和注入剂量D完成该使用H+离子的轰击。
-将所述接收基板(4)粘合到所述正面(2)，
-沿所述脆化区域(5)从源基板(1)的剩余部分(10)分离所述薄层(100)，
其特征在于，H+离子的注入根据以下不等式完成，其中注入计量D用每平方厘米的H+离子数目来表示，且用keV表示注入能量E，其大于或等于95keV：[(E×1·1014+5·1016)/1.1]≤D≤[(E×1·1014+5·1016)/0.9]
以便以优化方式使所述脆化区域(5)脆化，并在粘合步骤后，施加足够的热量束以便于完整地或几乎完整地剥落未转移到所述接收基板(4)的源基板(1)的所述薄层(100)的区域(12)。
2.根据权利要求1所述的方法，其特征在于，注入的离子是专用H+离子。
3.根据权利要求1或2所述的方法，其特征在于，在离子束曝光期间，在不故意加热源基板(1)的情况下完成H+离子的注入。
4.根据前述任一项权利要求的方法，其特征在于，源基板(1)是不定向单晶碳化硅。
5.根据前述任一项权利要求的方法，其特征在于，首先通过施加外部机械应力沿所述优化的脆化区域(5)完成分离，且在于然后施加足够的热量束用于完整地或几乎完整地剥落未转移到接收基板(4)的薄层(100)的区域(12)。
6.根据前述权利要求1-4中任一项的方法，其特征在于，通过施加适当的热量束同时完成沿优化的脆化区域(5)的分离以及完整地-或几乎完整地-剥落未转移到接收基板(4)的薄层(100)的区域(12)。
7.根据前述任一项权利要求的方法，其特征在于，施加完整地或几乎完整地从薄层(100)剥落所述区域(12)所必需的热量束在700℃以上进行。
8.根据前述任一项权利要求的方法，其特征在于，以随机方式实现离子轰击。
9.根据前述任一项权利要求的方法，其特征在于，在离子轰击步骤之前，用厚度小于或等于约50纳米的由非晶材料(20)构成的层覆盖源基板(1)。
10.根据前述任一项权利要求的方法，其特征在于，通过分子粘着完成接收基板(4)向源基板(1)的正面(2)的粘合。
11.根据权利要求10的方法，其特征在于，在正面(2)和接收基板(4)的接触面(40)中，至少一个面是用中间粘合层(6)覆盖。
12.根据权利要求9或11的方法，其特征在于，所述非晶材料(20)构成的层和/或所述中间粘合层(6)由选自二氧化硅(SiO2)或氮化硅(Si3N4)的材料构成。
13.根据前述任一项权利要求的方法，其特征在于，接收基板(4)选自硅、碳化硅、氮化镓、氮化铝、蓝宝石、磷化铟、砷化镓或锗。
14.根据前述任一项权利要求的方法，其特征在于，接收基板(4)是通过区域熔融生长获得的低氧含量的硅。
15.根据前述任一项权利要求的方法，其特征在于进一步包括分离后获得的源基板(1)剩余部分(10)的正面(11)的修整步骤F。
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CN103632924A (zh) * 2012-08-23 2014-03-12 法国原子能及替代能源委员会 用于将InP薄膜转移到加强基板上的方法
CN103632924B (zh) * 2012-08-23 2017-10-20 法国原子能及替代能源委员会 用于将InP薄膜转移到加强基板上的方法
US9875935B2 (en) 2013-03-08 2018-01-23 Infineon Technologies Austria Ag Semiconductor device and method for producing the same
CN104037070B (zh) * 2013-03-08 2018-05-04 英飞凌科技奥地利有限公司 半导体器件及其生产方法
CN109564891A (zh) * 2016-08-11 2019-04-02 索泰克公司 用于转移有用层的方法
CN109564891B (zh) * 2016-08-11 2023-08-29 索泰克公司 用于转移有用层的方法
CN111902571A (zh) * 2018-03-28 2020-11-06 索泰克公司 AlN材料单晶层的制造方法和外延生长AlN材料单晶膜的衬底

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US20050266659A1 (en) 2005-12-01
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US6974760B2 (en) 2005-12-13
US20050032330A1 (en) 2005-02-10
EP1468445B1 (en) 2006-08-09
WO2003063213A2 (en) 2003-07-31
TWI266362B (en) 2006-11-11
TW200306620A (en) 2003-11-16
KR100767138B1 (ko) 2007-10-15
CN100576448C (zh) 2009-12-30
ATE336077T1 (de) 2006-09-15
EP1468445A2 (en) 2004-10-20
KR20040077795A (ko) 2004-09-06
FR2835097B1 (fr) 2005-10-14
DE60307419T2 (de) 2007-03-29
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