CN101065837A - 用于去除蚀刻后残留物的水溶液 - Google Patents
用于去除蚀刻后残留物的水溶液 Download PDFInfo
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- CN101065837A CN101065837A CNA2005800106005A CN200580010600A CN101065837A CN 101065837 A CN101065837 A CN 101065837A CN A2005800106005 A CNA2005800106005 A CN A2005800106005A CN 200580010600 A CN200580010600 A CN 200580010600A CN 101065837 A CN101065837 A CN 101065837A
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- acid
- aqueous solution
- described aqueous
- solution
- 1ppm
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- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
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Abstract
本发明涉及具有改进性能的用于去除蚀刻后残留物的新型溶液及其在半导体生产中的应用。本发明还涉及在半导体生产过程中,对于必须无蚀刻后残留物和颗粒的金属层和表面具有降低的蚀刻速率的水溶液。
Description
本发明涉及具有改进性能的用于去除蚀刻后残留物的新型溶液及其在生产半导体中的应用。本发明尤其涉及在半导体生产过程中,在必须没有蚀刻后残留物和颗粒的金属层和表面上具有降低的蚀刻速率的水溶液。
现有技术:
半导体组件上的后段制程(BEOL)金属层(导电带)基本上由通过溅射施加的铜含量<0.5%的铝/铜层构成。用于铝工艺的BEOL金属层通过光刻法产生。所用电介质为介于各金属层之间的SiO2层,其通过通孔螺栓(钨或铝)垂直连接。这些结构体(导电带和通孔)由反应性离子蚀刻法产生。BEOL金属层通常由下列工艺步骤(1)至(6)产生:
产生Al/Cu导电带的工艺顺序:
1.将下列各层全面积溅射于SiO2绝缘层上:
a.作为扩散膜的薄Ti/TiN层
b.AlCu金属层
c.作为抗反射涂层(ARC)的薄Ti/TiN层
2.通过旋涂施加正性光致抗蚀剂,随后暴露并形成结构体
3.蚀刻:使用含卤素的蚀刻气体进行反应性离子蚀刻(RIE)
4.在任选添加有CF4的氧气或H2O等离子体中灰化光致抗蚀剂
5.去离子水喷雾工艺(冷,热)
6.利用湿法去除PER。
在第3步骤过程中,在铝导电带的侧壁上优先形成所谓的蚀刻后残留物。它们在进行第4和第5步骤过程中化学组成改变。必须在进行随后的的工艺之前,在第6步骤中完全去除PER。
金属层之间的垂直电连接为SiO2绝缘层中的孔(所谓的通孔),其中填充有钨或铝。在通孔的干蚀刻期间,也会形成蚀刻后残留物。但是,它们的化学组成由于所用蚀刻气体而与AlCu蚀刻情况下的不同。
如前所述,进一步加工之前,必须由导电带以及通孔完全去除PER。
该PER通常通过湿清洁方法去除。此处可使用包含配合剂和水的有机溶液。目前最常用的产品EKC265包含组分羟基胺、单乙醇胺、儿茶酚和水。
与去除这些聚合物残留物相关的问题源自于它们与AlCu基础材料相比较的耐化学性。目的是要去除这些聚合物而不腐蚀AlCu层。目前,通过湿清洁方法(浸渍或喷雾法)去除这些聚合物。此二种机理之间的差别在于:
·将该聚合物转变为可溶形式,随后经溶解而由表面去除。在某些情况下的暴露时间长至1/2小时且温度高至约90℃,以支持溶解法。基本上是有机溶剂、胺、乙醇胺、儿茶酚和还原剂如羟基胺(HDA)用于此方法(专利EP 4 85 161-A)中。尽管这些化合物具良好清洁作用,但其主要缺点在于其毒性。此外,羟基胺被分类为致癌物。因此,该溶液必须单独处置。在溶液能用水冲掉之前,还需要用水溶性醇,通常是异丙醇进行中间冲洗步骤。这些溶液的处理需要相关保护措施来维护健康和环境。
·还可以通过用无机水溶液处理去除聚合物。这些无机水溶液是可包含硫酸、过氧化氢、氟化铵或发色酸(专利EP 0 068 277)的稀溶液。少量氟化合物如HF加速蚀刻过程,因此这些混合物优选用于单晶片加工的旋转蚀刻剂中。也可在这些溶液中使用其它酸,如硝酸(专利EP 1 139 401 A1)或磷酸或磷酸氢铵(专利EP 1 063 689 A1)。对于所有的这些溶液来说,在聚合物之下的AlCu金属层被轻微蚀刻,使其能够在第1步骤中机械地去除(剥离)。随后聚合物溶解。该方法仅允许AlAu金属层的完全清洁和初蚀刻之间有较短的处理时限。在许多情况下,因为处理时间短通常不足以使聚合物完全溶解,且如AlCu情况下的下层SiO2无法被溶液蚀刻,所以通孔的清洁尤其无法令人满意。
为了说明,图4显示具有AlCu导电带和通孔的晶片在较不利条件下用DSP溶液(稀硫酸/过氧化物)于45℃下清洁5分钟之后的情况。相当多的AlCu金属层的初蚀刻和某些聚合物残留物清晰可见。此外,在通孔底部,通孔呈现相当多的AlCu金属层初蚀刻。
因此,本发明的目的是提供不昂贵的、易于制备的用于去除聚合物残留物或蚀刻后残留物的溶液,其具有改进的清洁作用,在金属层、金属表面或导电带上的蚀刻速率降低。具体地,该目的在于提供在由Al、Cu、Al/Cu、Ti、TiN、SiO2或W构成的表面或线上具有降低的蚀刻速率而对由不锈钢构成的表面也呈惰性的清洁溶液。
发明:
该目的通过基于在合适添加剂存在下包含至少一种羟基羧酸的水溶液的组合物实现,该组合物在半导体产品的生产方法的BEOL工艺中,非常有效地由通孔和导电带去除侧壁残留物。
诸如润湿剂和缓蚀剂的添加剂有助于在宽范围内使用或对工艺时间和工艺温度而言开启了宽的工艺范围。根据本发明所添加的缓蚀剂在应用期间大大降低尤其是AlCu和钨的蚀刻速率。图5的曲线图显示了AlCu(nm)去除与60℃下暴露于溶液的时间之间的关系。即使添加几ppm的合适缓蚀剂,金属层通过蚀刻的去除可降至0nm。如图6所示,通过使用本发明的清洁溶液在60℃暴露20分钟,钨的去除可以此方式容易地由160nm降至10nm。通过其中添加剂以下文所述尤其优选的量存在的组合物获得了特别好的结果。
详细地,可获得的结果取决于之前的工艺步骤的条件和所形成的聚合物最终组成。但是,本领域技术人员可容易地通过几个实验将组合物组分的最佳混合比例设定于所述的混合范围内。
可以可变地使工艺时间和温度适应使用本发明组合物的清洁方法的要求而不侵蚀金属层或表面。
在使用通常使用的无机水溶液,如DSP或DSP+时,在铝/铜金属层的轻微底蚀(underetch)被有意地用于去除PER(剥离)情况下,会有金属结构体因过度蚀刻而被侵蚀的危险。这可以导致点状腐蚀的发生。因此,
a)在这些已知组合物的情况下,暴露时间必须保持非常短(约1分钟,至多几分钟),但是
b)清洁方法要求最低暴露时间,以便完全去除或溶解PER。
初蚀刻和完全清洁作用之间的该狭窄工艺范围通常仅在之前的反应性离子蚀刻法已相应地优化的情况下才能实现。由于这里SiO2电介质的底蚀是不可能的,所以特别困难之处在于通孔清洁。
通过实验,现惊人地发现通常用于此目的的组合物的这些缺点可通过使用含水配制剂而避免,该含水制剂包含至少一种羟基羧酸、过氧化氢和用于改进晶片表面的润湿和防止腐蚀的添加剂。
已经证实,本发明溶液的改进性能在去除所谓的“蚀刻后残留物”中尤其有利。蚀刻后残留物为在干蚀刻期间由正性光致抗蚀剂、蚀刻气体和蚀刻材料组分形成的反应产物。如图1可以看出的那样,这些反应产物优先沉积于金属化区域,尤其是Al/Cu导电带的侧壁和SiO2通孔内部。本发明溶液的一个特别的优点在于特别有效地清洁通孔和金属导电带而不会侵蚀位于下方的Al/Cu金属层。
该溶液为环境友好的、无毒性且易于被中和处置。该组合物具有低蒸气压、未显示爆炸风险且在清洁操作期间不需吸取烟雾。
此外,本发明组合物可根据半导体工业的质量要求,由半导体工业常用的高纯度市售物质高纯度地制备。
使用本发明溶液清洁通孔可得到特别有利的结果。在喷雾器和槽式处理器中,在60℃处理仅5分钟,就可完全清洁通孔,如图2所示的那样。向溶液中加入适合的表面活性剂确保晶片表面最佳润湿并且促进清洁作用。工艺时间为5至20分钟,温度为45至75℃、尤其是50至70℃、非常特别优选55至65℃下得到最佳结果,如图2和3所示的那样。
本发明提供了在其应用中导致显著改进的组合物。这些改进例如在于,在金属层上,例如在Al/Cu金属层或包含Al、Cu、Ti或W的金属层或在TiN或SiO2层上的蚀刻速率非常低。这有助于在50至70℃、优选60℃下暴露时间长达30分钟。图4显示相应的清洁结果。本发明溶液可成功地用于喷雾工具和旋转处理器以及槽装置中。经清洁的晶片可直接用超纯水冲洗并且随后使用氮气干燥。如有机溶液(如异丙醇)情况下的中间冲洗步骤是不必要的。
如前所述,这些改进的结果可通过参照图1至3中的SEM显微图非常清楚地看出。根据本发明,添加添加剂,如表面活性剂和NMP可显著改进清洁作用。所用缓蚀剂一方面降低钨的蚀刻速率,另一方面也降低Al/Cu的蚀刻速率,如图4和5所示。
用于去除PER的本发明合适溶液优选是包含至少一种选自羟基羧酸和/或二羧酸和三羧酸的有机酸的水溶液。适合的羟基羧酸为乙醇酸、乳酸、羟基丁酸、甘油酸、苹果酸、酒石酸、柠檬酸。适合的二羧酸是丙二酸、琥珀酸、戊二酸、马来酸。除至少一种有机酸之外,本发明组合物还包含至少一种氧化剂。多种氧化剂都适用,但优选过氧化氢和过二硫酸铵,其可单独或组合存在于溶液中。
此外,为了改进清洁作用和保护不欲侵蚀的表面,本发明溶液可包含宽范围的添加剂。因此,已经证实有利的是溶液包含缓蚀剂。优选添加咪唑啉化合物作为缓蚀剂用于处理具有例如钨和铝金属层的晶片表面。适合的咪唑啉化合物是苯并咪唑(烷基取代的咪唑啉或1,2-二烷基咪唑啉)、氨基苯并咪唑和2-烷基苯并咪唑。使用包含油酸羟乙基咪唑啉作为缓蚀剂的溶液得到特别好的清洁结果。
为支持清洁作用并保护晶片表面,有利的是将非质子极性溶剂添加至溶液中。适于此目的的非质子极性溶剂为N-甲基吡咯烷酮(NMP)、乙二醇、丙二醇、二甲亚砜(DMSO)、乙酸1-甲氧基-2-丙酯(PGMEA)。这些有机溶剂可单独或以混合物形式存在于溶液中。
另外还证实有利的是,清洁溶液另外包含界面活性物质。已证实适合的界面活性物质为阴离子表面活性剂。特别适合的表面活性剂选自脂族羧酸和/或选自烷基苯磺酸。适合的脂族羧酸例如为庚酸和辛酸。可采用的烷基苯磺酸尤其是十二烷基苯磺酸。
阴离子表面活性剂可以与非离子表面活性剂同时使用或以后者代替。可采用的非离子表面活性剂选自烷基烷氧基化物和/或烷基酚乙氧基化物。适用于此目的的烷基烷氧基化物例如为脂肪醇烷氧基化物。可添加的烷基酚乙氧基化物尤其是辛基酚乙氧基化物。此外,脱水山梨糖醇化物,例如聚氧乙烯脱水山梨糖醇脂肪酸酯也适合在本发明溶液中作为表面活性剂。这些包括例如为名称为Tween的市售产品的表面活性剂。
进行的实验已显示,与目前已知的清洁溶液比较,在40至70℃的温度下,本发明溶液具有显著改进的清洁结果。
令人吃惊地是,与目前已知的组合物比较,在1分钟至60分钟的清洁时间(清除时间)内,本发明溶液可达到显著改进的清洁结果。有利的是,在清洁操作期间可完全去除PER,而金属化的导电带或其它例如包含TiN或SiO2的表面未察觉到被腐蚀。
具有改进清洁作用的本发明清洁溶液,具有如下表所示的组成:
表1:
1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | |
有机酸 | × | × | × | × | × | × | × | × |
氧化剂 | × | × | × | × | × | × | × | × |
溶剂 | × | × | × | × | ||||
表面活性剂 | × | × | × | × | ||||
缓蚀剂 | × | × | × | × |
本发明的清洁水溶液可包含如下的各个组分:
-有机酸,选自羟基羧酸和/或二羧酸和三羧酸,其量为0.1至30%
-氧化剂,其量为0.1至10%
-用于钨和铝的缓蚀剂,例如选自咪唑啉化合物,其量为1ppm至1%
-非质子极性溶剂,其量为0.1至10%
-阴离子表面活性剂,选自脂族羧酸和烷基苯磺酸,其量为1ppm至1%
和/或
-非离子表面活性剂,选自烷基烷氧基化物、烷基酚乙氧基化物和脱水山梨糖醇化合物,其量为1ppm至1%。
因此,具改进性能的适合清洁溶液可以包含如下量的各组分:
二羧酸、三羧酸或羟基羧酸 0.1至30%
过氧化氢 0.1至30%
N-甲基吡咯烷酮和/或DMSO 0.1至10%
缓蚀剂 1ppm至1%
阴离子或非离子表面活性剂 1ppm至1%
由下列组分组成的组合物可获得尤其好的清洁结果:
酸(柠檬酸、马来酸、酒石酸) 5(+/-2)%
过氧化氢 2(+/-0.5)%
溶剂(NMP、DMSO、PGMEA) 1(+/-0.5)%
缓蚀剂(油酸羟乙基咪唑啉) 100至1000ppm
润湿剂(庚酸、Triton X100、Tween 20、 100至1000ppm
十二烷基苯磺酸、Plurafac 120)
尤其适合的是例如以如下量包含所述组分的溶液:
柠檬酸 0.1至30%
过氧化氢 0.1至10%
N-甲基吡咯烷酮NMP 0.1至10%
缓蚀剂 1至1000ppm
润湿剂 1至1000ppm
就此而言,以所述量包含下列组分的组合物显示非常特别有利的性能:
柠檬酸 5(+/-2)%
过氧化氢 2(+/-1)%
N-甲基吡咯烷酮NMP 1(+/-0.5)%
缓蚀剂(油酸羟乙基咪唑啉) 50至1000ppm
润湿剂 100至1000ppm
已经证实前述混合物尤其在难清洁的通孔的情况下非常有效,见图2。
用本发明水溶液处理晶片表面,不仅从表面去除PER,还同时使得表面无附着的干扰颗粒。这具有的优点是使得去除PER之后的复杂清洁步骤不再必要。
有利的是,本发明组合物是稳定的组合物,即使长时间储存之后也不会分解。如前所述,该组合物环境友好且容易处置。它们可用于喷雾单元和槽处理器中。如果需要,它们也可被回收。
本说明书中所有的百分数数据为基于溶液总量的重量百分数。不言而喻的是,组合物中添加的组分的量总和为100%。
实施例
为更好地理解和说明本发明,以下还以显示清洁结果的照片形式再现了实施例。所用组合物属于本发明保护的范围之内。因此,实施例也用于说明本发明。但是,由于所述的本发明的原理的通用性,实施例并不是将本申请保护的范围仅限于此。
实施例中所用的温度单位总是℃。
实施例1
清洁前参照(灰化后残留物)
通孔 AlCu线
用包含下列组份的清洁水溶液进行清洁:
柠檬酸 5%
过氧化氢 2%
NMP 1%
Tween 20 1000ppm
用于Semitool SAT喷雾工具的工艺参数:
步骤 | 名称 | 时间 | RPM | 温度 | 排放 | |
1 | 聚合物去除 | 5分钟 | 50rpm | 60℃ | 槽 | |
2 | 吹洗 | 10秒钟 | 50rpm | N2 | 槽 | |
3 | DI冲洗1 | 5分钟 | 50rpm | RT | H2O | 流出 |
4 | DI冲洗2 | 2分钟 | 300rpm | RT | ||
4 | 吹洗 | 10秒钟 | 300rpm | N2 | 流出 | |
5 | 干燥1 | 2分钟 | 750rpm | 热 | N2 | |
6 | 干燥2 | 8分钟 | 300rpm | 热 | N2 |
AlCu线 通孔
实施例2
用包含下列组分的清洁水溶液进行清洁:
柠檬酸 5%
过氧化氢 2%
油酸羟乙基咪唑啉 1000ppm
用于Arias湿清洗台的工艺参数
步骤 | 名称 | 时间 | 温度 | 排放 | |
1 | 聚合物去除 | 20分钟 | 60℃ | ||
2 | DI冲洗1 | 10分钟 | RT | H2O | |
3 | 干燥1 | 2分钟 | 热 | N2 | |
4 | 干燥2 | 8分钟 | 热 | N2 |
AlCu线 通孔
实施例3
与市售有机聚合物去除剂比较
1.聚合物去除剂(包含羟基胺、儿茶酚、单乙醇胺)
75℃,20分钟(烧杯)
2.IPA RT,3分钟
3.DI水 RT,5分钟
4.N2吹干
1.柠檬酸5%/过氧化氢2%/NMP 1%/Tween 20 1000ppm60℃,20分钟(烧杯)
2.DI水10分钟
3.N2吹干
附图说明
图5:溅射的Al/Cu层的物质去除与暴露时间的关系图。所用溶液由5%柠檬酸、2%过氧化物、1%NMP的水溶液组成。深色曲线显示无缓蚀剂的去除。浅色线显示添加了缓蚀剂的去除。
图6:CVO沉积的钨层的物质去除与暴露时间的关系图。所用溶液(见图5)。
图13:向或未向溶液(见图5)中添加缓蚀剂时,多种涂层的蚀刻速率(去除/时间)图。
Claims (22)
1.具有降低的蚀刻速率的用于蚀刻后残留物去除的水溶液,其在氧化剂以及任选的用于改进清洁作用和对Al、Cu、Ti、W、Al/Cu、TiN和SiO2表面的惰性的添加剂存在下,包含选自羟基羧酸和/或选自单羧酸、二羧酸和三羧酸的有机酸。
2.如权利要求1所述的水溶液,包含选自咪唑啉化合物的缓蚀剂。
3.如权利要求1或2所述的水溶液,包含作为缓蚀剂的一种或多种选自苯并咪唑、氨基苯并咪唑和2-烷基苯并咪唑的化合物,包括烷基取代的咪唑啉和1,2-二烷基咪唑啉和油酸羟乙基咪唑啉。
4.如权利要求1所述的水溶液,包含至少一种非质子极性溶剂。
5.如权利要求1或4所述的水溶液,包含至少一种选自N-甲基吡咯烷酮(NMP)、乙二醇、丙二醇、二甲亚砜(DMSO)和乙酸1-甲氧基-2-丙酯(PGMEA)的非质子极性溶剂。
6.如权利要求1所述的水溶液,包含至少一种表面活性物质。
7.如权利要求1或6所述的水溶液,包含作为表面活性物质的至少一种阴离子表面活性剂和/或非离子表面活性剂。
8.如权利要求7所述的水溶液,包含至少一种选自脂族羧酸和烷基苯磺酸的阴离子表面活性剂和/或至少一种选自烷基烷氧基化物和烷基酚乙氧基化物的非离子表面活性剂。
9.如权利要求8所述的水溶液,包含至少一种选自庚酸、辛酸和十二烷基苯磺酸的阴离子表面活性剂和/或至少一种选自脂肪醇烷氧基化物、辛基酚乙氧基化物和聚氧乙烯脱水山梨糖醇脂肪酸酯(Tween)的非离子表面活性剂。
10.如权利要求1-9中任一项所述的水溶液,包含至少一种选自乙醇酸、乳酸、羟基丁酸、甘油酸、苹果酸、酒石酸、柠檬酸、丙二酸、琥珀酸、戊二酸和马来酸的有机酸。
11.如权利要求1-9中任一项所述的水溶液,包含至少一种选自过氧化氢和过二硫酸铵的氧化剂。
12.如权利要求1-11中任一项所述的水溶液,基于总重量包含0.1至30%的选自羟基羧酸和/或选自单羧酸、二羧酸和三羧酸的有机酸。
13.如权利要求1-11中任一项所述的水溶液,基于总重量包含0.1至10%的氧化剂。
14.如权利要求1-11中任一项所述的水溶液,基于总重量包含1ppm至1%的至少一种缓蚀剂。
15.如权利要求1-11中任一项所述的水溶液,基于总重量包含0.1至10%的至少一种非质子极性溶剂。
16.如权利要求1-11中任一项所述的水溶液,基于总重量包含0.1至10%的至少一种非质子极性溶剂。
17.如权利要求1-11中任一项所述的水溶液,基于重量包含1ppm至1%的至少一种阴离子表面活性剂,和/或基于重量包含1ppm至1%的至少一种非离子表面活性剂。
18.如权利要求1-11中任一项所述的水溶液,以100至1000ppm的量包含至少一种选自庚酸、TritonX100、Tween20、十二烷基苯磺酸和Plurafac120的润湿剂。
19.如权利要求1-11中任一项所述的水溶液,包含柠檬酸、过氧化氢、N-甲基吡咯烷酮(NMP)和任选的添加剂。
20.如权利要求19所述的溶液,包含0.1至30%的柠檬酸、0.1至10%的过氧化氢和0.1至10%的N-甲基吡咯烷酮。
21.如权利要求19或20所述的溶液,包含1ppm至1%的缓蚀剂和1ppm至1%的润湿剂。
22.如权利要求1-21中任一项所述的水溶液在喷雾工具上或在槽装置中生产半导体的用途。
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US (1) | US7919445B2 (zh) |
EP (1) | EP1733421B1 (zh) |
JP (1) | JP2007531992A (zh) |
KR (1) | KR20070015558A (zh) |
CN (1) | CN101065837A (zh) |
IL (1) | IL178187A (zh) |
MY (1) | MY148396A (zh) |
TW (1) | TWI375988B (zh) |
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- 2005-03-10 JP JP2007505411A patent/JP2007531992A/ja active Pending
- 2005-03-10 WO PCT/EP2005/002511 patent/WO2005098920A2/de active Application Filing
- 2005-03-10 US US10/594,767 patent/US7919445B2/en not_active Expired - Fee Related
- 2005-03-10 KR KR1020067022651A patent/KR20070015558A/ko not_active Application Discontinuation
- 2005-03-10 EP EP05707734.9A patent/EP1733421B1/de active Active
- 2005-03-24 MY MYPI20051281A patent/MY148396A/en unknown
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CN110777021A (zh) * | 2018-07-24 | 2020-02-11 | 弗萨姆材料美国有限责任公司 | 蚀刻后残留物清洁组合物及其使用方法 |
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Also Published As
Publication number | Publication date |
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MY148396A (en) | 2013-04-15 |
TW200539342A (en) | 2005-12-01 |
US7919445B2 (en) | 2011-04-05 |
WO2005098920A3 (de) | 2007-07-05 |
TWI375988B (en) | 2012-11-01 |
IL178187A0 (en) | 2006-12-31 |
JP2007531992A (ja) | 2007-11-08 |
KR20070015558A (ko) | 2007-02-05 |
WO2005098920A2 (de) | 2005-10-20 |
US20070161243A1 (en) | 2007-07-12 |
EP1733421B1 (de) | 2016-08-10 |
EP1733421A2 (de) | 2006-12-20 |
IL178187A (en) | 2012-10-31 |
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