CN101194344A - 用于预金属和/或浅槽隔离应用中所用的旋涂介电材料的uv固化方法 - Google Patents

用于预金属和/或浅槽隔离应用中所用的旋涂介电材料的uv固化方法 Download PDF

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CN101194344A
CN101194344A CNA2005800500603A CN200580050060A CN101194344A CN 101194344 A CN101194344 A CN 101194344A CN A2005800500603 A CNA2005800500603 A CN A2005800500603A CN 200580050060 A CN200580050060 A CN 200580050060A CN 101194344 A CN101194344 A CN 101194344A
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dielectric material
exposed
metal
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violet radiation
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C·沃尔弗里德
O·埃斯科尔恰
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Axcelis Technologies Inc
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Abstract

一种用于预金属和浅槽隔离应用中所用的介电材料的紫外固化方法，包括：涂布合适的介电材料到底物上；和使介电材料暴露于有效量的紫外辐射以降低介电材料的有机物含量和/或增加介电材料的密度和/或增加介电材料的耐湿法蚀刻性能。任选地，紫外固化的介电材料可暴露于多种紫外辐射模式。

Description

用于预金属和/或浅槽隔离应用中所用的旋涂介电材料的UV固化方法
相关申请的交叉引用
本申请涉及提交于2004年6月7日的美国临时申请60/577,679且要求对其的优先权，在此全文引入该申请作为参考。
背景
本发明一般来说涉及半导体器件中的介电薄膜，更具体地，涉及用于预金属(pre-metal)和浅槽隔离(shallow trench isolation)应用的旋涂(spin-on)低k介电薄膜的紫外(UV)固化方法。
在先进的半导体制造领域中，器件的尺寸和形成的间距持续被降低，以提高集成电路性能。制造经常要求将介电材料沉积到特征中，所述特征被图案化于硅底物上的材料层中。在大多数情况下，介电材料完全填充这些特征且不形成任何空穴是重要的。填充这种窄小的特征，其也被称为间隙填充，对所用材料，例如用于预金属介电(PMD)或者浅槽隔离(STI)应用的介电材料，提出了严格的要求。集成电路上的预金属介电层使结构与金属互连层电绝缘，并且使其与降低电性能的污染移动离子电绝缘。根据2003年版的International Technology Roadmap forSemiconductors，在2005年对于DRAM器件，要求被预金属介电材料填充的纵横比(aspect ratio)可高达16∶1，转化成深度为大于300纳米(nm)。在间隙填充以后，介电材料需要能够承受后续的加工步骤，例如高温退火、蚀刻和清洁步骤。
用于PMD和STI应用的介电材料通常通过化学气相沉积或旋涂方法来沉积。这些方法的每一种对于填充非常窄小的缝隙都有某些局限性，而这需要被克服以便成功集成。旋涂玻璃和旋涂聚合物例如硅酸盐、硅氧烷、硅氮烷或硅倍半氧烷通常具有好的间隙填充性能。这些材料的薄膜典型地通过施涂包含聚合物的涂层溶液然后热固化方法形成。通常进行热固化方法以完成化学键的形成、去除残余成分的气体和降低薄膜的介电常数。这种固化方法通常在炉中使用间歇方式进行或利用单晶片方式在加热板上进行。在任何一种情况下，传统的固化方法不期望地使晶片受到升高的温度达一段延长的时间(例如超过一个小时至数个小时并且处于高于约300℃的温度)。这些温度可能超过要求制造商满足的可允许的热预算。而且，可包括超过800℃的加工温度的热固化方法能引起收缩。大量收缩能导致不可接受的薄膜破裂和/或多孔材料的形成，尤其是在窄间隙里面。破裂或多孔材料在接下来的方法步骤中可具不期望的高湿法蚀刻率。
在涉及旋涂预金属介电材料的现有技术中，至少因为提到的这些问题，将期望实施替代的低k预金属介电材料固化方法，其使收缩最小化且提供改善的耐湿法蚀刻性能。更加期望的是获得具有成功集成所期望性能的旋涂预金属电介质。
简述
本文所公开的是用于UV固化涂布到底物表面上的旋涂预金属介电材料的方法。在一个实施方案中，用于预金属和浅槽隔离应用中所用的介电材料的UV固化方法包括涂布介电材料到底物上；和使介电材料暴露于有效量的紫外辐射以降低介电材料中的有机物含量。
在另一个实施方案中，用于预金属和浅槽隔离应用中所用的介电材料的UV固化方法包括涂布介电材料到底物上；和使介电材料暴露于有效量的紫外辐射以增加介电材料的密度。
在另一个实施方案中，用于预金属和浅槽隔离应用中所用的介电材料的UV固化方法包括涂布介电材料到底物上；和使介电材料暴露于有效量的紫外辐射以增加介电材料的耐湿法蚀刻性能，其中相对于暴露之前的介电材料的湿法蚀刻率，耐湿法蚀刻性能提高。
在又一个实施方案中，用于固化涂布到底物表面上的旋涂预金属介电材料的方法包括涂布旋涂预金属介电材料到底物上；使旋涂预金属介电材料暴露于第一紫外辐射模式(ultraviolet radiation pattern)达一段时间和强度以有效增加预金属介电材料的弹性模量性能和/或硬度性能；和使旋涂预金属介电材料暴露于第二紫外辐射模式达一段时间和强度以有效进一步地增加预金属介电材料的弹性模量性能和/或硬度性能，其中第一和第二紫外辐射模式不同。
上述的和其他的特点由以下的附图和详细说明举例说明。
附图简述
现在参看附图，其为示范性实施方案且其中相同的元件以相同的附图标记表示：
图1图示了各个I型无电极微波驱动灯泡的宽带光谱输出，该灯泡来自Axcelis Technologies，Inc.，其适用于UV固化介电材料；
图2图示了各个II型无电极微波驱动灯泡的宽带光谱输出，该灯泡适用于UV固化介电材料；
图3图示了根据一个实施方案未固化和UV固化的预金属介电薄膜的FTIR光谱；
图4-5是说明相对于化学气相沉积法沉积的TEOS介电材料，在不同稀释的氢氟酸溶液(DHF)中非UV固化和UV固化的旋涂低k介电材料的耐湿法蚀刻性能的图表；
图6-7是说明相对于化学气相沉积法沉积的TEOS介电材料，在不同稀释的氢氟酸溶液(DHF)中非UV固化和UV固化的旋涂低k介电材料的耐湿法蚀刻性能随时间变化的图表；
图8是说明UV暴露之前和之后旋涂预金属低k介电材料的介电常数的图表，其中工艺室(process chamber)使用了不同的惰性气体；和
图9是说明UV暴露之前和之后旋涂预金属低k介电材料的击穿电压(breakdown voltage)的图表，其中工艺室使用了不同的惰性气体。
详述
本发明涉及用于旋涂预金属介电材料的UV固化方法。如本文所用的，提到的术语“预金属”介电材料意指包括浅槽介电材料应用，因为这些介电材料通常是相同的并且为间隙填充而优化。应用本文描述的UV固化方法对PMD和STI应用来说将具有相似的优势。UV固化方法通常包括在集成电路中沉积任何金属层之前旋转涂布预金属介电材料到合适的底物上，并使介电材料在低于约450℃的温度下暴露于具有一个或多个大于150纳米至小于400纳米波长的紫外辐射。
尽管不想受理论约束，据信UV固化方法去除了可能已在旋涂预金属介电材料中形成的类似有机物的杂质或部分。术语旋涂(spin-on)介电材料，如本文所用的，包括但不意味局限于硅酸盐、氢硅倍半氧烷、有机硅倍半氧烷、有机硅氧烷、有机氢化硅氧烷(organhydridosiloxane)、硅倍半氧烷-硅酸盐共聚物、硅氮烷基材料、聚碳硅烷(polycarbosilane)和乙酸基硅烷(acetoxysilane)。UV固化方法去除和/或化学改性了介电材料的一部分。例如，根据具体的旋涂预金属介电材料，减少了在涂布的介电材料中，尤其，Si-H、Si-CH3、SixCyHz的量，其中x、y、z通常是0-12之间的整数，条件是x＝1且y+z等于或大于1。结果，UV固化方法有利地增加介电材料的密度和/或降低有机物含量，和/或增加介电材料的耐湿法蚀刻性能。
本文描述的用于形成旋涂预金属介电材料的单体、单体混合物和聚合物能够并且以多种方式被设计成被溶剂化或溶解于任何合适的溶剂，只要产生的溶液可以旋转涂布或机械铺设在底物、晶片或层状材料上即可。优选的溶液被设计且预期以被旋转涂布、辊涂、滴涂(drip)或喷洒在晶片、底物或层状材料上。最优选的溶液被设计为旋转涂布在晶片、底物或层状材料上。典型的溶剂是介电材料、层状元件或电子元件领域的技术人员易于获得的那些溶剂。
典型的溶剂也是能使单体、同分异构单体混合物和聚合物溶剂化的溶剂。预期的溶剂包括任何合适的在期望温度挥发的有机、有机金属或无机分子的纯物质或混合物。溶剂也可包括任何合适的极性和非极性化合物的纯物质或混合物。在优选的实施方案中，溶剂包括水、乙醇、丙醇、丙酮、甲苯、醚、环己酮、丁内酯、甲基乙基酮、甲基异丁基酮、N-甲基吡咯烷酮、聚乙二醇甲醚、均三甲基苯和苯甲醚。
在一个实施方案中，UV固化方法包括旋转涂布合适的预金属介电材料到底物上；和使预金属介电材料在低于约450℃的温度暴露于紫外辐射模式达一段时间以有效地在介电材料中增加密度和/或增加耐湿法蚀刻性能和/或降低有机物含量。本领域周知的，涂布旋涂介电材料有很多方法，所有周知的方法都认为是合适的。本文预期的合适的底物可包括任何期望的基本上实心的(solid)材料，对其来说，包括旋涂介电材料在内的预金属介电或浅槽隔离结构可能是所期望的。例如，合适的底物包括但不局限于硅、二氧化硅、玻璃、氮化硅、陶瓷和砷化镓。术语底物还通常指任何平面化的或具有构形(topography)的层，包括半导体晶片、介电层、栅、隔离层、蚀刻停止层和集成电路器件中存在的金属线。
任选地，退火过程可在UV固化方法之后使用。退火过程可包括使含有UV固化的预金属介电材料的底物暴露于升高的温度达一段时间以有效地在介电材料中增加密度和/或增加耐湿法蚀刻性能和/或降低有机物含量。例如，退火温度可高达约1100℃达约2小时或更短。
如前所述，已经发现，所得的UV固化的预金属介电材料对后续的如在集成电路制造过程中通常使用的湿法化学处理方法是更稳定的。例如，光刻(lithography)后，可使用湿法蚀刻方法以选择性地去除底物和/或沉积层的部分。典型地，底物浸没在剥离剂如稀释的含水氢氟酸浴中。其他湿法剥离剂包括酸、碱和本领域技术人员周知的溶剂。所用的具体的湿法剥离剂为本领域技术人员所理解。例如，硝酸、硫酸、氨水、氢氟酸是通常使用的湿法剥离剂。在操作中，湿法剥离剂以浸没、搅混、流淌、喷洒等方式作用于底物上，然后用去离子水漂洗。如同将在下文中更加详细讨论的那样，相对于未暴露到UV固化方法的相同材料，UV固化的旋涂介电材料提高了耐湿法蚀刻性能。
在UV固化方法中，使用UV辐照器工具。合适的UV辐照器工具是RapidCureTM工具，由Axcelis Technologies，Incorporated商业化可得。在使用过程中，光源室可以被惰性气体如氮、氦或氩吹扫，使得UV辐射以最小的光谱吸收进入相邻的工艺室。预金属介电材料置于被单独吹扫的工艺室内，且在不同的应用中可使用工艺气体如N2、H2、Ar、He、Ne、H2O蒸气、COz、Oz、CxHy、CxFy、CxHzFy及其混合物，其中x是1-6的整数，y是4-14的整数，z是1-3的整数。在这点上，UV固化可在真空条件下发生，或在氧气不存在的情况下，或在氧化气体下发生。在一个实施方案中，工艺室由氢气和氦气吹扫。
UV光源可以是微波驱动、弧光放电、电介质隔离放电(dielectricbarrier discharge)或电子碰撞产生的。而且，可以根据应用选择具有不同光谱分布的UV发生灯泡如，例如，被称为I型或II型的微波无电极灯泡，其可由Axcelis Technologies(Beverly，MA)获得。由I型和II型灯泡获得的光谱以及适用于UV固化方法的光谱分别在图1和2中给出。
底物(晶片)温度可控制为室温至450℃，任选地被红外光源、光学光源、热表面或光源本身控制。工艺压力可小于、大于或等于大气压。典型地，对UV固化的介电材料进行UV处理不超过或约为600秒，且优选地不超过约300秒，更具体地，在约60和约180秒之间。同时，UV处理介电材料可在如下条件下进行：温度为约室温至约450℃；过程压力为小于、大于或约等于大气压；UV能量为约0.1-约2000mW/cm2；UV波长谱为约100-约400nm。
本发明由下面的非限制性实施例进一步阐述。
实施例1
预金属介电材料的耐湿法蚀刻性能
在本实施例中，获自Honeywell Company的名为HoneywellElectronic Material A(HEMA)的预金属介电材料被旋转涂布在裸硅晶片上。根据厂商的推荐，晶片经过一个传统的旋涂方法。每个晶片经历完全一样的处理。经涂布的晶片在425℃暴露于UV固化方法5分钟。UV固化方法在Rapid Cure Exposure工具中使用多种微波无电极灯泡，上述工具自Axcelis Technologies，Incorporated商业化可得。图3中显示的FTIR数据没有显示低k介电材料在UV固化之后任何可探测的吸收变化。然后使UV固化晶片暴露于湿法蚀刻方法，其包括浸没该晶片于40∶1和100∶1稀释的氢氟酸水溶液2分钟、5分钟和10分钟。上述的比例代表水与氢氟酸的重量比。结果显示在图4、5中且相对于使用等离子增强化学气相沉积法(PECVD)沉积的四原硅酸盐(TEOS，tetraorthosilicate)薄膜给出，后者以其耐湿法蚀刻性能众所周知，但不适合用作预金属介电材料用于高级设计规则，如小于90纳米。
如图所示，UV固化方法明显降低了预金属介电材料在40∶1氢氟酸溶液中的耐湿法蚀刻性能。未固化材料的蚀刻率约为820埃/分钟，其降低到约350埃/分钟，取决于预金属介电材料的组成。时间变量具有非常小的影响。比较结果在更加稀释的HF溶液(100∶1)中观察到。然而，结果从视觉上看不很明显，因为稀释导致观察到相对弱的蚀刻行为。
实施例2
基于HEMA的旋涂介电材料的耐湿法蚀刻性能
在本实施例中，如同实施例1中的那样，HEMA预金属旋涂介电材料被旋转涂布到空白晶片上。另外，由Honeywell Corporation可得的称为NGX的纳米玻璃旋涂介电材料被旋转涂布到空白晶片上。晶片在惰性气体混合物中在425℃暴露于使用III型无电极灯泡的Rapidcure工具中产生的UV辐射达10分钟。旋涂介电材料在后烘烤后以及在UV固化方法之后，测量厚度和折射率(RI)。有些晶片进一步在900℃或1000℃暴露于炉退火过程达1小时。基于UV固化方法和退火(如果可应用的话)前后的厚度计算收缩百分数。在本实施例中，晶片组1指HEMA旋涂介电材料，晶片组2和3指旋涂NGX低k介电材料，其中每个晶片组代表三个加工的晶片的平均值。数据在表1中给出。
表1
    晶片组号   炉退火     后烘烤[PB]厚度(nm)   PB-RI   后固化[PC]厚度(nm)   PC-RI   收缩(％)   后退火[PA]厚度(nm)   PA-RI     收缩(％)
    1   无     5789   1.49   5756   1.5   0.57
    2   900℃     7804   1.41   7510   1.40   3.77   5826   1.50     22.42
    3   1000℃     7788   1.41   7549   1.40   3.07   5623   1.50     25.51
结果表明，UV固化方法显示出很小的收缩和很小的折射率变化。然而，后退火过程确实引起薄膜密度增加和/或损失以及折射率的增加。从FTIR数据得到的与介电材料关联的相关峰在表2中给出。PB指旋涂和后烘烤过程之后的介电材料；PC指UV固化之后的PB介电材料；PA指在PB和PC和暴露于炉退火过程之后的介电材料。
表2
 晶片组号  炉退火(℃) OH/SiO  SiC/SiO  CH/SiO  C+C/SiO
PB  PC  PA  PB  PC  PA  PB  PC  PA  PB  PC  PA
 1  无 0.06  0.103  0  0  0  0  0  0.0156  0.0071
 2  900 0.026  0  0.0606  0.031  0.028  0  0.008  0.008  0  0  0  0.0159
 3  1000 0.028  0  0.1131  0.031  0.029  0  0.008  0.009  0  0  0  0.0181
FTIR数据表明UV固化方法导致C＝C峰的减少，且展示了对预金属介电材料的Si-OH含量很小的影响。
实施例3
在本实施例中，如同实施例1一样，介电常数和击穿电压在UV固化方法前后被测量。称为HEMA(m1)、(m2)和(m3)的旋涂低k介电材料按照制造商针对具体的低k介电材料推荐的那样以传统的旋转涂布方法被涂布。结果在下列表3中给出。
表3
        HEMA(m1)        HEMA(m2)     HEMA(m3)
UV固化前 UV固化后  UV固化前  UV固化后  UV固化前  UV固化后
介电常数 7.84  6.91  6.27  6.19  7.6  6.7
击穿电压 0.58  1.88  1.99  2.04  1.24  2.27
每个例子中，使旋涂介电材料暴露于UV固化方法有利地降低了介电常数。随同介电常数的降低，观察到伴随着击穿电压的增加。
实施例4
在本实施例中，观察工艺室中使用不同的吹扫气体产生的影响。晶片按照实施例1中那样被处理。NR(I)指用氦作为惰性气体而NR(2)指使用氢/氦气体混合物。如图6、7所示，UV固化方法显著地提高了在40∶1和100∶1的稀释氢氟酸溶液中的耐湿法蚀刻性能。在某些例子中，耐湿法蚀刻性能比TEOS PECVD沉积薄膜更优异。图8和9图示了各个薄膜的介电常数和击穿电压。UV固化方法显著改善介电常数和击穿电压。
虽然本公开内容参照示例性实施方案进行了描述，但本领域的技术人员将理解，不脱离本公开内容的范围可以进行多种变化，且其要素可被等价物替代。另外，不脱离本公开内容的范围，为了使具体的情况或材料适于本公开的教导，可以做很多修改。因此，意图是本公开内容不局限于作为最好模式的、预期用来实施本公开内容的具体实施方案，而是本公开内容将包括落在所附权利要求范围内的所有实施方案。

Claims (24)

1.一种用于预金属和浅槽隔离应用中所用的介电材料的紫外固化方法，包括：
涂布介电材料到底物上；和
使所述介电材料暴露于有效量的紫外辐射，以降低所述介电材料中有机物的含量。
2.权利要求1的方法，其中使所述介电材料暴露于紫外辐射包括在介电材料周围形成一种环境，其中该环境包括N2、H2、Ar、He、Ne、H2O蒸气、COz、Oz、CxHy、CxFy、CxHzFy和其混合物，其中x是1-6的整数，y是4-14的整数，z是1-3的整数。
3.权利要求1的方法，其中所述紫外辐射模式包括大于150纳米至小于400纳米的波长。
4.权利要求1的方法，进一步包括在所述暴露期间加热底物。
5.权利要求1的方法，其中所述预金属介电材料包括氢硅倍半氧烷、烷基硅倍半氧烷、碳掺杂的氧化物、氢化碳氧化硅、乙阶聚合物、芳基环丁烯基聚合物、基于聚亚苯基的聚合物、聚亚芳醚、聚酰亚胺、多孔硅石和包括至少一种上述介电材料的结合。
6.权利要求1的方法，其中所述旋涂预金属介电材料在暴露于所述紫外辐射前后具有基本上相同的介电常数。
7.权利要求1的方法，其中在所述暴露过程中，预金属介电材料的弹性模量性能和/或硬度性能增加至少约50％。
8.权利要求1的方法，其中使所述旋涂预金属介电材料暴露于所述紫外辐射模式达一段时间和强度以有效降低介电常数。
9.权利要求1的方法，进一步包括：在使所述旋涂预金属介电材料暴露于紫外辐射模式后，使所述旋涂预金属介电材料暴露于炉固化过程或热位置固化过程。
10.一种用于预金属和浅槽隔离应用中所用的介电材料的紫外固化方法，包括：
涂布介电材料到底物上；和
使所述介电材料暴露于有效量的紫外辐射，以增加所述介电材料的密度。
11.权利要求10的方法，其中使所述介电材料暴露于紫外辐射包括在所述介电材料周围形成一种环境，其中该环境包括N2、H2、Ar、He、Ne、H2O蒸气、COz、Oz、CxHy、CxFy、CxHzFy和其混合物，其中x是1-6的整数，y是4-14的整数，z是1-3的整数。
12.权利要求10的方法，其中所述紫外辐射模式包括大于150纳米至小于400纳米的波长。
13.权利要求10的方法，进一步包括在暴露期间加热所述底物。
14.权利要求10的方法，其中所述预金属介电材料包括氢硅倍半氧烷、烷基硅倍半氧烷、碳掺杂的氧化物、氢化碳氧化硅、乙阶聚合物、芳基环丁烯基聚合物、基于聚亚苯基的聚合物、聚亚芳醚、聚酰亚胺、多孔硅石和包括至少一种上述介电材料的结合。
15.权利要求10的方法，其中所述旋涂预金属介电材料在暴露于紫外辐射前后具有基本上相同的介电常数。
16.权利要求10的方法，其中在暴露过程中，所述预金属介电材料的弹性模量性能和/或硬度性能增加至少约50％。
17.权利要求10的方法，其中使所述旋涂预金属介电材料暴露于紫外辐射模式达一段时间和强度以有效降低介电常数。
18.权利要求10的方法，进一步包括在使所述旋涂预金属介电材料暴露于紫外辐射模式之后，使所述旋涂预金属介电材料暴露于炉固化过程或热位置固化过程。
19.一种用于预金属和浅槽隔离应用中所用的介电材料的紫外固化方法，包括：
涂布介电材料到底物上；和
使所述介电材料暴露于有效量的紫外辐射，以增加所述介电材料的耐湿法蚀刻性能，其中相对于暴露前的所述介电材料的湿法蚀刻率，耐湿法蚀刻性能提高。
20.一种涂布到底物表面上的旋涂预金属介电材料的固化方法，包括：
涂布旋涂预金属介电材料到底物上；
使所述旋涂预金属介电材料暴露于第一紫外辐射模式达一段时间和强度以有效增加所述预金属介电材料的弹性模量性能和/或硬度性能；和
使所述旋涂预金属介电材料暴露于第二紫外辐射模式达一段时间和强度以有效进一步地增加所述预金属介电材料的弹性模量性能和/或硬度性能，其中第一和第二紫外辐射模式不同。
21.权利要求20的方法，其中所述第一和第二紫外辐射模式包括大于150纳米至小于400纳米的波长。
22.权利要求20的方法，进一步包括在暴露期间加热所述底物。
23.权利要求20的方法，其中所述预金属介电材料包括氢硅倍半氧烷、烷基硅倍半氧烷、碳掺杂的氧化物、氢化碳氧化硅、乙阶聚合物、芳基环丁烯基聚合物、基于聚亚苯基的聚合物、聚亚芳醚、聚酰亚胺、多孔硅石和包括至少一种上述介电材料的结合。
24.权利要求20的方法，其中以大于300纳米的纵横比涂布所述旋涂预金属介电材料到所述底物上。
CNA2005800500603A 2005-06-09 2005-06-09 用于预金属和/或浅槽隔离应用中所用的旋涂介电材料的uv固化方法 Pending CN101194344A (zh)

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