CN1852772A - 制备高密度低介电常数材料的紫外线固化方法 - Google Patents

制备高密度低介电常数材料的紫外线固化方法 Download PDF

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CN1852772A
CN1852772A CNA2004800265492A CN200480026549A CN1852772A CN 1852772 A CN1852772 A CN 1852772A CN A2004800265492 A CNA2004800265492 A CN A2004800265492A CN 200480026549 A CN200480026549 A CN 200480026549A CN 1852772 A CN1852772 A CN 1852772A
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dielectric material
ultraviolet curing
dielectric
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C·沃尔德弗里德
Q·韩
O·埃斯科尔西亚
I·L·伯里三世
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Axcelis Technologies Inc
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Abstract

具有提高的弹性模量和材料硬度的低介电常数材料。制备所述材料的方法，包括：提供介电材料，用紫外线固化所述介电材料，由此得到紫外线固化的介电材料。紫外线固化得到了具有提高的弹性模量和材料硬度的材料，各自的提高率分别大于或等于约50％。对此紫外线固化的介电材料可进行任选的后紫外线处理。与LIV固化介电材料相比，后紫外线处理减小了材料的介电常数同时保持弹性模量和材料硬度的提高。与加热炉固化相比，紫外线固化的介电材料在固化过程中的总热预算少。

Description

制备高密度低介电常数材料的紫外线固化方法
本发明涉及半导体芯片的制备方法。更具体地讲，本发明涉及用于改善用作集成电路(IC)电介质的某些材料的结构性质和可靠性的方法。
人们正在研究一些具有低介电常数的新材料(称为“低k电介质”)，使得它们可在半导体芯片的设计中作为绝缘体使用。低介电常数材料有助于进一步减小集成电路尺寸。在常规的集成电路制备方法中，二氧化硅作为介电材料的基础材料，产生的介电常数大约为3.9。此外，高密度低介电常数材料的介电常数小于大约2.8。空气的介电常数最小(k＝1.0)。由于多孔的电介质可提供极低的介电常数，因此它们是非常好的候选物质。然而，遗憾的是，这种高密度(advanced)低介电常数材料通常存在机械强度不够以及沉积温度超过了允许的热预算的问题。
电器设备用的薄膜电介质涂层在本领域为众所周知。例如，在美国专利4,749,631和4,756,977中，Haluska等人公开了以二氧化硅为基体的涂层制备，该涂层通过分别将烷氧基硅或氢倍半硅氧烷(hydrogen silsesquioxane)的溶液涂布于基体上，然后在200-1000℃的温度下加热所述经涂布的基体得到。但这些涂层的介电常数对某些电子设备和电路来说太高了。
美国专利4,847,162和4,842,888中，Haluska等人提到了在氨的存在下，分别在200-1000℃的温度下加热氢倍半硅氧烷树脂和硅酸酯，由此形成氮化的二氧化硅涂层。
Glasser等人在Jounal of Non-Crystalline Solids，63(1984)，209-221页中等提到了在氨存在下，加热四乙氧基硅烷可得到陶瓷涂层。该文献提到了无水氨的使用以及所得的二氧化硅涂层被氮化。
美国专利4,636,440中，Jada公开了缩短带溶胶-凝胶涂层的基体的干燥时间的方法，所述方法包括把该基体暴露在氢氧化季铵盐和/或者链烷醇胺化合物的水溶液中。Jada要求在加热前将涂层干燥，此方法特别限定于使用水解或部分水解的烷氧基硅。
Chandra等人的美国专利5,262,201及Baney等人的美国专利第5,116,637提到使用碱性催化剂来降低各种可形成陶瓷的材料(preceramic materials)(均包含氢倍半硅氧烷)向陶瓷涂层转化时所需的温度。这些专利还提到在将涂层暴露在碱性催化剂之前将溶剂移除。
Camilletti等人的美国专利5,547,703提到了一种在基体上形成低介电常数的含Si-O键的涂层的方法，该方法包括依次在湿氨、干氨、氧气中加热氢倍半硅氧烷树脂的步骤。所得涂层的介电常数低至在1MHz下为2.42。该文献提到在将涂层转化成陶瓷之前把溶剂移除。
Balance等人的美国专利5,523,163提到了一种在基体上形成含Si-O键涂层的方法，该方法包括加热一种氢倍半硅氧烷树脂使其转化成含Si-O键的陶瓷涂层，然后把该涂层暴露于含氢气的退火气氛中。所得涂层的介电常数低至2.773。该文献提到在将涂层转化成陶瓷之前把溶剂移除。
Syktich等人的美国专利5,618,878提到含溶解于饱和烷烃中的氢倍半硅氧烷树脂的涂料组合物，这种组合物可用于形成厚的陶瓷涂层。上述烷烃为最高为十二烷的烷烃。文献中没有提到在移除溶剂之前将经涂布的基体暴露于碱性催化剂中。
Chung等人的美国专利6,231,989公开了一种制造低介电常数的多孔网络状涂层的方法。此方法包括用包含含至少2个Si-H基团的树脂和溶剂的溶液在基体上沉积涂层，其中沉积后至少有5体积％的溶剂残留在涂层中。然后把涂层置于含碱性催化剂和水的环境中。最后，从涂层中蒸发出溶剂形成多孔网络。如果需要可以把涂层加热固化形成陶瓷。这个方法所制备的薄膜的介电常数在1.5-2.4之间，弹性模量为约2-约3GPa。
用旋涂和化学蒸气沉积法或通过自组装(self-assembly)方法产生的低介电常数材料，在沉积后需要进行固化。通常固化低介电常数薄膜的工艺条件包括：将用氮气吹扫的加热炉在约350-约450℃的温度下退火30-180分钟。如美国专利申请系列号09/681,332(美国专利6,558,755)、09/952,649、09/906,276和10/627,894提到代替热固化或等离子体处理，采用低介电常数薄膜可在明显更短的时间或较低温度下经紫外线固化，这样消除了以往加热炉固化的需要，由此减少了总的热预算。上述专利文献通过引用结合到本文中。
此外，仍然存在对制备具有改进的结构特性，如提高的弹性模量和材料硬度，同时不危害或恶化材料电性能的其它低介电常数材料的方法的需要。
本发明通过提供高密度低介电常数材料的紫外线固化方法满足了上述需求。
尽管本发明不受特殊的优点或功能的限定，但值得注意的是，本发明方法得到了具有低介电常数、提高的弹性模量和材料硬度的材料，或得到了具有相当模量和硬度的材料，同时与加热炉固化相比减少总热预算。
本发明的一个实施方案提供了制备紫外线固化材料的方法，所述方法包括提供具有第一介电常数、第一弹性模量和第一材料硬度的介电材料。用紫外线固化此介电材料得到紫外线固化材料紫外线固化的介电材料，所得介电材料具有与第一介电常数相当的第二介电常数，还具有分别大于第一弹性模量和第一材料硬度的第二弹性模量和第二材料硬度。这里所说的″相当”是指在第一介电常数约±20％范围之内。弹性模量和材料硬度的增量通常大于或等于大约50％。
可任选经后紫外线处理所述紫外线固化材料，得到具有第三介电常数、第三弹性模量和第三材料硬度的后紫外线处理的紫外线固化的介电材料。与进行后紫外线处理前相比，对紫外线固化的介电材料的后紫外线处理可在保持弹性模量和材料硬度升高的同时减小介电常数。更具体地讲，第三弹性模量和第三材料硬度分别大于第二弹性模量和第二材料硬度或分别在第二弹性模量和第二材料硬度约±20％范围内。
制备紫外线固化材料的方法还包括把介电材料置于加工室中，抽真空或吹扫加工室以排出室内空气，向加工室内通入加工气体，加热介电材料以及将介电材料暴露在紫外线中。
本发明的另一个实施方案为制备紫外线固化材料的方法，所述方法包括提供未固化的低介电常数材料，在不超过约5分钟或温度不超过约450℃的条件下，对这种介电材料进行紫外线固化，得到紫外固化的介电材料，所述紫外线固化的总热预算与加热炉固化相比减少了约50％以上。
因此，本发明的一个目的在于制造具有低介电常数、提高的弹性模量和材料硬度的介电材料。
本发明的另一个目的在于制造介电材料，其中形成工艺和固化工艺在缩短时间或降低温度或者两者下完成，从而减少方法的热预算。
参照附图和本发明的详细说明，以便完全了解本发明的上述以及其它特点和优点。值得注意的是，权利要求的范围由每项权利要求的叙述所限定，而不是由说明书中所阐述的特点和优点的具体讨论所限定。
参照附图来阅读以下对本发明实施方案的详细描述，将有助于最佳理解这些本发明的实施方案，附图中的相同的结构由相同的编号标记。
图1图示了基于MSQ的旋涂低介电常数薄膜的FTIR光谱(傅立叶变换红外光谱图)，其中所述薄膜分别经过热固化、在O2中经热固化和紫外线固化、以及在N2中经热固化和紫外线固化。
图2图示了基于HSQ的旋涂低介电常数薄膜的FTIR光谱，其中所述薄膜未经固化、在O2中经紫外线固化和在N2中经紫外线固化。
图3图示了基于5％MSQ/95％HSQ的旋涂低介电常数薄膜的FTIR光谱，其中所述薄膜未经固化、在O2中经紫外线固化和在N2中经紫外线固化。
图4图示了CVD低介电常数薄膜的FTIR光谱，其中所述薄膜未经固化和经紫外线固化。
本领域技术人员应理解在图中示例的各要素是为了简化和明了化，并没有按比例进行绘制。比如，为了有助于理解本发明的实施方案，图中一些要素的尺寸相对于其他要素来说被放大了。
本发明建立在以下发现的基础上，即事实上紫外线固化任何介电材料都要远快于加热炉固化，并且一般来说还能在保持低介电常数性质的同时提高弹性模量(杨氏模量)和材料硬度。介电材料可包括有机材料、无机材料或它们的组合物，但并不限定于这些。更具体地讲，介电材料可包括氢倍半硅氧烷(HSQ)介电材料、甲基倍半硅氧烷(MSQ)介电材料、碳掺杂的氧化物(CDO)介电材料、氢化的氧碳化硅(SiCOH)介电材料、苯并环丁烯(BCB)介电材料、基于芳基环丁烯的介电材料、基于聚亚苯基的介电材料和它们的组合等，但并不限定于这些材料。这些材料可以通过使用旋涂、化学蒸气沉积(CVD)、等离子体辅助CVD、蒸发、反应性蒸发、或自组装方法在基体上沉积介电涂层而得到。该介电材料可以是多孔的也可以是紧密的材料。多孔的介电材料可具有由成孔剂产生的、溶剂形成的或由分子工程(molecular engineered)形成的孔，这些细孔可以是相连或密闭的孔，可随机或有序地分散，如垂直孔(vertical pore)。
对于一些低介电常数的材料，采用后紫外线法，以不同的波长和温度处理紫外固化的介电材料，得到具有更低介电常数、相等或是提高的弹性模量和材料硬度的材料。
本发明的方法特别适用于在电子设备或电子电路上沉积涂层，所述涂层可用作生产晶体管类设备的层间介电层、掺杂介电层，用作生产电容和类电容设备、多层设备、3-D设备、绝缘体设备上的硅层、多层芯片设备等的装载有颜料的含硅粘合剂等。然而，对采用本发明方法涂布的基体和设备的选择的限制仅是要求基体在本发明方法所使用的温度和压力下对热和化学品稳定，基体。同样地，本发明的介电材料可用在诸如塑料的基体上，例如聚亚酰胺、环氧树脂、聚四氟乙烯树脂和它们的共聚物、聚碳酸酯、丙烯酸类、聚酯、陶瓷、皮革、纺织品、金属、半导体等。
本发明中的“陶瓷”包括无定形二氧化硅等陶瓷材料以及无定形二氧化硅类材料等类陶瓷材料，它们不是完全不含碳和/或氢，而是具有陶瓷的特性。“电子设备”或“电子电路”包括基于硅的设备、基于砷化镓的设备、基于碳化硅的设备、焦平面阵列、光电子设备、光伏特电池或光学设备等，但不限于这些。
在本发明中，以介电材料作为原材料使用。一种这样的介电材料是高密度CVD低介电常数薄膜，如可得自ASM InternationalN.V.(Bilthoven，the Netherlands)的AURORA，它是一种氢化的氧碳化硅(SiCOH)介电材料。这种高密度低介电材料通过使用等离子体增强的化学蒸气沉积法得到，其介电常数值通常为小于或等于约2.5。其它的CVD低介电常数材料的例子包括可得自Applied MaterialsInc.(Santa Clara，CA)的Black Diamond薄膜、可得自Novellus SystemInc.(San Jose，CA)的Coral低介电常数材料、可得自TrikonTechnologies Inc.(Newport，South Wales，UK)的Orion材料。可用于本发明的典型的基于旋涂的介电材料包括：1)Dow CorningCorporation(Midland，MI)生产的基于FOx HSQ的介电材料和基于HSQ的XLK多孔介电材料，和2)可得自Chemat Technology，Inc.(Northridge，CA)和JSR Corporation(Tokyo，Japan)的基于MSQ的低介电常数多孔介电材料。
本发明所用的典型的高密度低介电常数材料的生产方法为本领域所熟知。一种生产这样的介电材料的方法是美国专利6,231,989中公开的多孔网络涂布法制备，其教导了如何生产具有超低介电常数的多孔介电材料，在此通过引用结合到本文中。该专利描述了制备介电常数介于约1.5-约2.4的超低介电常数涂层的方法，其中在HSQ基薄膜中引入孔。HSQ基薄膜按照美国专利6,231,989的教导生产，在热条件下固化，含有约20％-约60％的Si-H键密度。当此涂层的介电常数在约2.0时，其弹性模量为约2-约3GPa。
美国专利6,558,747公开了制备高密度低介电材料的第二种方法，该方法形成了介电常数低至2.5-3.0的有机硅氧化物介电薄膜。美国专利6,475,564描述了另一种方法，其中在化学蒸气沉积体系中通过使含硅气体与过氧化物反应形成高密度低介电材料。美国专利6,383,955描述了通过等离子体CVD方法形成SiCOH基高密度低介电常数材料的方法。
另一种制备高密度低介电常数材料的方法为热固化含有较大烷基的硅氧烷树脂，然后热分解这些烷基以在涂层上形成孔隙。如Zhong的美国专利6,143,360和6,184,260所公开，在含有铂族金属的硅氢化催化剂的存在下，使含氢化硅的树脂与含约8-约28个碳原子的1-烯烃接触，形成烷基氢化硅氧烷树脂，其中至少大约5％的硅原子被至少一个氢原子取代；在足以固化所得树脂和将烷基从硅原子上热解的温度下加热所得树脂，由此形成具有纳米微孔的硅树脂。这些专利通过引用结合到文本中。
在Zhong等人的美国专利6,232,424、6,359,096、6,313,045、6,541,107中公开了硅树脂和由这些硅树脂制得的多孔涂层。硅树脂由包含以下组分的混合物构成：15-70摩尔％的四烷氧基甲硅烷、12-60摩尔％的式R′SiX3有机硅烷，其中R′是氢原子或是含有1-6个碳原子的烷基、15-70摩尔％的式R″Si(OR″)3的有机三烷氧基甲硅烷，其中R″是含有约8-24个碳原子的烃基或是含有约8-24个碳原子的烃基链的取代烃基；所述专利通过引用结合到文本中。
在Zhong的美国专利6,596,834 B2中公开了由通式为(R1SiO3/2)x(HSiO3/2)y的硅树脂制备的多孔涂层，其中R1是含8-24个碳原子的烷基。此涂层的介电常数为1.5-2.3，该专利通过引用结合到本文中。上述专利中进一步描述了通过以下将描述的两步骤从式(R1SiO3/2)x(HSiO3/2)y的树脂制备多孔低介电常数涂层，其中R1是3，7，11，15-四甲基-3-羟基-十六烷基，该专利通过引用结合到本文中。
在美国专利申请09/951,899中(Zhong，发明名称“硅树脂及由其制得的多孔材料”，2001年9月12号提交，通过引用结合到本文中)公开了由通式(R1SiO3/2)u(HSiO3/2)v(SiO4/2)w(HOSiO3/2)z的硅树脂制得的多孔涂层，其中R1是含8-24个碳原子的支链烷基，在烷基链上含至少一个拉电子侧基；u值为0.1-0.7；v值为0.12-0.6；z≥0.5；w+z的值为0.15-0.7；且u+v+w+z＝1。
第一步通过混合以下描述的组分(A)、(B)、(C)、(D)、(E)和(F)(其量在如上引用的美国专利申请的表1所述)制备树脂样品。
(A)0.45摩尔份(mole parts)的三乙氧基甲硅烷，
(B)0.25摩尔份的有机三乙氧基甲硅烷，RSi(OR’)3，R是3，7，11，15-四甲基-3-羟基-十六烷基，
(C)0.30摩尔份的四乙氧基甲硅烷，和
(D)甲基异丁基酮(MIBK)和异丁酸异丁酯的混合物(重量比：6∶4)，其量足以使所得的树脂浓度为9％。
参照上面引用的申请的表1中的量，在混合物中加入水(E)和氯化氢(F)的混合物。在60℃减压条件下，汽提出所得的反应物的挥发份，直到固含量为14-21％。加入异丁酸异丁酯使得固含量变为14％。加热回流溶液2小时，连续排出所生成的水。通过汽提除去异丁酸异丁酯并加入环己酮，使溶剂转变成环己酮。
第二步在硅晶片上旋涂所得的树脂溶液，使其适合介电常数测量，并在440℃的氮气流中固化1小时。测定的介电常数为1.9。或者，使用等离子体和/或紫外线辅助方法可加速旋涂薄膜的固化。
在Albaugh等人的美国专利申请09/915,899中公开了从含(RSiO3/2)(R’SiO3/2)(R”SiO3/2)树脂的树脂得到的多孔涂层，其中R是含1-5个碳原子或氢原子的烷基，R’是带支链的烷氧基，R”是含6-30个碳原子的取代或未取代的直链、支链、环状的单价有机基团，所述专利通过引用结合到本文中。
Boisvert等人的美国专利申请09/915,903和Albaugh等人的美国专利申请09/915,902公开了由式TRTR’的树脂制备的多孔涂层，其中R可以是甲基也可以是氢，R’是带支链的烷氧基，所述专利通过引用结合到本文中。
尽管具有低介电常数的介电材料符合要求，但更加优选具有更高弹性模量和材料硬度的介电材料。
为了提高介电材料的弹性模量，将其进行紫外线固化加工。紫外线固化方法提高了低介电常数材料的力学性质，在维持介电材料孔隙率、结构、密度和电学性能的同时提高材料的硬度。
在典型的紫外线固化方法中，利用了一个紫外线辐射工具，首先将所述工具经氮气、氦气、氩气吹扫，使得紫外线以最小的光吸收进入加工室。把介电材料放入加工室，所述介电材料已经被单独吹扫，并且根据应用的不同可使用不同的加工气体，如N2、H2、Ar、He、Ne、水蒸气、COz、Oz、CxHy、CxFy、CxHzFy和它们的混合物等，其中x为1-6的整数，y为4-14的整数，z为1-3的整数。在这种情况下，紫外线固化可在真空或者在不存在氧或氧化气体的条件下进行。依照不同的应用可选择有不同光谱分布的紫外线发光灯，如可得自Axcelis Technologies(Beverly，MA)的HL或是HL-bulbs。这样，紫外线光源可以是由微波驱动的光源、电弧放电的光源、介质阻挡放电(dielectric barrier discharge)的光源或是电子碰撞而形成的光源。通过红外光源、光学光源、热表面或紫外线光源本身将晶片的温度控制在大约室温至大约450℃之间。加工压力可大于、大约等于或小于环境压力。
200mm晶片的典型紫外线固化条件示例如下：
紫外线强度：          0.1mW-2000mW/cm2
紫外线波长：          从100-600nm之间的连续光谱分布
晶片温度：            室温-450℃
加工压力：            ＜、＞或者＝环境压力
紫外线固化时间：      小于300秒
加工气体：           He/Ne/Ar/H2/N2/H2O/CO/CO2/CxHy/O2/CxHzFy
与加热炉(热)固化或未固化的介电材料相比，紫外线固化的介电材料的弹性模量和材料硬度都有所提高。经加热炉固化或未经固化的高密度低介电常数材料在介电常数为约1.6-约2.7时的代表性弹性模量为约0.5GPa-约0.8GPa。紫外线固化的介电材料的典型弹性模量大于或等于约2.5，更典型地为约4GPa-约12GPa。经加热炉固化或未经固化的薄膜的材料硬度为大约0.1GPa，紫外线固化的介电材料的材料硬度通常大于或等于约0.25GPa，更通常为约0.25GPa-约1.2GPa。
另外，紫外线固化方法优选在约420℃或更低的温度下进行约20秒到约5分钟，而加热炉固化优选在约420℃下操作30分钟到3小时。因此，紫外线固化方法相对于加热炉固化来说降低了总热预算。
本发明的紫外线固化的介电材料具有改进的化学稳定性和尺度稳定性，改进的“化学稳定性”是指这种介电材料更能耐化学品，比如清洁剂和化学抛光剂，以及在光致抗蚀剂灰烬和干蚀刻过程中抵抗等离子体破坏。
但是，由于一些低介电常数材料和加工气体结合，紫外线固化方法会在介电材料中产生一些不合要求的极性物质。在这样的情况下，如果需要，可任选使用热、UV或等离子体暴露方法对这些紫外线固化的介电材料进行后紫外线处理，以此来降低介电常数和/或提高弹性模量和材料硬度。例如，把紫外线固化的介电材料放入常规的烘箱中进行退火，直到极性物质被除去，如在约400℃-约450℃的温度下退火约30-约60分钟。一种作为选择的退火所述材料的方法是在快速退火加工(Rapid Anneal Processing，RAP)室里退火所述紫外线固化的介电材料，以减少介电常数。将所述紫外线固化的介电材料在常规的温度下退火足够的时间，然后冷却到大约100℃。但在大多数应用中并不需要进行RAP。
RAP方法的典型操作条件如下：
升温速率：    15-150℃/sec
晶片温度：    150-450℃
退火时间：    ＜120秒
加工压力：    环境压力
加工气氛：   N2
后紫外线处理也可通过把紫外线固化的介电材料暴露在另一种紫外线环境下进行。通常，将紫外线固化的介电材料经紫外线处理时间不超过或约等于300秒，优选大约60-大约180秒，或者，可下如下条件下进行紫外线处理：温度，大约室温至约450℃；压力，大于、小于或约等于环境压力；紫外线强度，约0.1-约2000mW/cm2；紫外线波长，约100-约400nm。而且，可以在使用加工气体吹扫的条件下，对紫外线固化的介电材料进行紫外线处理，所述加工气体如N2、Oz、Ar、He、H2、水蒸气、COz、CxHy、CxFy、CxHzFy、空气和它们的混合物，其中x为1-6的整数，y为4-14的整数，z为1-3的整数。
另一种类型的后紫外线处理是在高温条件下把紫外线固化的介电材料暴露在等离子体环境中。在典型的等离子体辅助后紫外线处理方法中，根据应用的不同，可使用如O2、N2、H2、Ar、He、CxHy、含氟气体和它们的混合物等加工气体，其中x为1-6的整数，y为4-14的整数。晶片温度可控制在大约室温至大约450℃。通常，所述紫外线固化的介电材料在大约1托-约10托的加工压力进行等离子体处理。
对200mm和300mm晶片的典型的等离子体辅助后紫外线处理的示例性条件如下所示。
条件                   200mm系统                                    300mm系统
微波等离子体功率：     500W-3000W                                   500W-3000W
晶片温度：             80℃-350℃                                   80℃-350℃
加工压力：             1.0托-3.0托                                  1.0托-4.0托
等离子体处理时间：     ＜90秒                                       ＜90秒
加工气体：            H2/N2/CF4/O2/Ar/He/CxHy     H2/N2/CF/O2/Ar/He/CxHy
N2H2流速：          ＞0-4000sccm                                 ＞0-10,000sccm
O2流速               ＞0-4000sccm                                 ＞0-10,000sccm
CF4流速              ＞0-400sccm                                  ＞0-1000sccm
Ar流速               ＞0-4000sccm                                 ＞0-10,000sccm
He流速               ＞0-4000sccm                                 ＞0-10,000sccm
经后紫外线处理的紫外线固化的介电材料的介电常数要比紫外线固化的介电材料的介电常数小。经后紫外线处理的紫外线固化的介电材料的介电常数通常为约1.1-约3.5，更通常为约1.6-约2.4。
下表1中列举了经过紫外线固化的多孔低介电常数薄膜的典型材料性质。
                表1  紫外线固化的多孔低介电常数材料特性
材料性质 基于MSQ的介电材料 基于HSQ的介电材料
介电常数的改变 ＜0.1 ＜0.2
模量增加 ≥50％ ≥50％
孔隙率 不变 不变
合适的紫外线固化气体 真空、Ar、He、Ne、H2、NH3、CO2、CO、N2/H2 真空、N2/H2、Ar、He、Ne、NH3、O2、H2、H2O
密度 不变 不变
厚度损失 ＜10％ ＜10％
折光率改变 ＜0.01 ＜0.03
下表2列举了经过紫外线固化的高密度低介电常数薄膜的典型材料性质。
                    表2  紫外线固化的高密度低介电常数材料的特性
          平均         提高率％
样品     灯   时间(秒)   温度(℃)    模量     硬度     模量     硬度   模量  硬度
作为对照的SiCOH低介电常数材料     6.36.16.4     0.810.800.80 6.27 0.80 N/A N/A
N2加工气体 1 HL- 30 360     6.76.66.6     0.850.870.86 6.63 0.86 5.9 7.1
2 Hmod 180 360     7.37.07.2     0.990.950.96 7.17 0.97 14.4 20.3
3 Dmod 180 360     6.66.26.4     0.930.860.91 6.40 0.90 2.1 12.0
He加工气体 A HL- 180 360     9.39.19.0     1.000.971.03 9.13 1.00 45.7 24.5
B HL- 120 360     8.28.58.4     1.071.011.04 8.37 1.04 33.5 29.5
为了更容易理解本发明，给出了以下实施例。这些实施例只是用于解释本发明而不是用于限定本发明。
附图给出了紫外线固化的特征。各实施例分别为i)基于MSQ的低介电常数薄膜，ii)基于HSQ的低介电常数薄膜，iii)MSQ/HSQ混合的低介电常数薄膜，和iv)等离子体增强CVD沉积SiCOH低介电常数薄膜，厚度均为大约5000。
实施例1：基于MSQ的低介电常数薄膜
基于MSQ的低介电常数薄膜的傅立叶变换红外光谱(FTIR)的特征为：在1280cm-1和3000cm-1附近具有Si-CH3特征谱带，在1100cm-1附近具有两个Si-O峰。紫外线固化这些薄膜通常使模量增加100％或以上，在FITR光谱中表现为Si-CH3谱带部分消失以及笼形Si-O键(高波数)和网络状Si-O键(低波数)的比例发生改变。
紫外线处理可成功地固化基于MSQ的多孔低介电常数薄膜。图1显示了三条基于MSQ的多孔低介电常数薄膜的FTIR光谱：热固化(底部)、在O2中进行热固化+紫外线固化1分钟(中间)、在N2中进行热固化+紫外线固化5分钟(顶部)。固化效果极大地依赖于室内吹扫气体的组成。可观察到在O2中的紫外线固化比在N2中的更有效。
实施例2：基于HSQ的低介电常数薄膜
基于HSQ的低介电常数薄膜的FTIR光谱的特征为：在2200cm-1附近具有Si-H谱带，在850cm-1附近具有SiO-H伸缩振动谱带和在1100cm-1附近具有两个Si-O峰。这些薄膜的固化通常使模量增加100％或以上，在FTIR光谱中表现为Si-H谱带完全消失以及笼形Si-O键和网络状Si-O键的比例发生改变。
紫外线处理可成功地固化基于HSQ的低介电常数薄膜。图2显示了三条基于HSQ的低介电常数薄膜的FTIR光谱：未经固化(点线)、在O2中进行紫外线固化60秒(虚线)和在N2中进行紫外线固化60秒(实线)。固化效果取决于室内吹扫气体的组成。可观察到在O2中的紫外线固化比在N2中的更有效。
实施例3：HSQ/MSQ混合的低介电常数薄膜
HSQ/MSQ混合的低介电常数薄膜的FTIR光谱的特征为：在2200cm-1附近具有Si-H谱带，在850cm-1附近具有SiO-H伸缩振动谱带，在1100cm-1附近具有两个Si-O峰。另外在1280cm-1附近也有Si-CH3特征谱带。本实施例研究了5％MSQ/95％HSQ混合薄膜。与单纯的基于HSQ的薄膜相比，这些薄膜的紫外线处理更依赖于紫外线吹扫气体混合物。然而，O2吹扫的紫外线处理也能有效且成功地固化这些低介电常数薄膜。
图3显示了三条基于5％MSQ/95％HSQ的低介电常数薄膜的FTIR光谱：未经固化(点线)、在O2中进行紫外线固化60秒(虚线)、在N2中进行紫外线固化60秒(实线)。在所有的情况下，为了除去通常在紫外线固化过程中产生的Si-OH键，需要一个继起的或可能的(possibly)退火步骤。
例4：SiCOH CVD低介电常数薄膜
SiCOH CVD低介电常数薄膜FTIR光谱的特征为：在1230cm-1附近具有Si-CH3谱带，在2950cm-1附近具有C-H谱带和在1100cm-1附近具有两个Si-O峰。薄膜的固化通常使弹性模量和材料硬度增加约50％或以上，在FTIR光谱表现为两个Si-O谱带的比率发生改变，这种改变表明网络型的增加。虽然通常也可见Si-CH3和C-H谱带减少，但是这些特定谱带的减少最好是最小程度地减少或不发生这样的减少。
紫外线处理可成功地固化SiCOH CVD低介电常数薄膜。图4显示了两条CVD低介电常数薄膜的FTIR光谱：未经固化(实线)和在He中紫外线固化120秒(点线)。紫外线固化处理在加工室压力为环境压力、晶片温度为约380℃的条件下，使用HL-灯、He吹扫气进行。
虽然给出了一些具有代表性的实施方案和详细描述来举例说明本发明，但对于本领域技术人员来说，只要不脱离本发明的范围，可以对本发明公开的组成和方法进行各种改变。因此，本发明不限于所公开的实施方案，而是受下述权利要求的限定。

Claims (66)

1.一种紫外线固化的材料的制备方法，所述方法包括：
提供具有第一介电常数、第一弹性模量和第一材料硬度的介电材料；和
用紫外线固化所述介电材料得到具有第二介电常数、第二弹性模量和第二材料硬度的紫外线固化的介电材料，其中所述第二介电常数在第一介电常数的大约±20％的范围内、所述第二弹性模量和第二材料硬度分别大于第一弹性模量和第一材料硬度。
2.权利要求1的方法，其中所述介电材料选自有机材料、无机材料或它们的组合物。
3.权利要求1的方法，其中所述介电材料选自氢倍半硅氧烷(HSQ)介电材料、甲基倍半硅氧烷(MSQ)介电材料、碳掺杂的氧化物(CDO)介电材料、氢化的氧碳化硅(SiCOH)介电材料、苯并环丁烯(BCB)介电材料、基于芳基环丁烯的介电材料、基于聚亚苯基的介电材料或它们的组合物。
4.权利要求1的方法，其中所述介电材料通过使用如下方法在基体上沉积介电涂层制备：旋涂方法、化学蒸气沉积方法、等离子体辅助化学蒸气沉积方法、蒸发方法、活性蒸发方法或自组装沉积方法。
5.权利要求1的方法，其中所述介电材料选自紧密的介电材料、成孔剂形成的多孔介电材料、溶剂形成的多孔介电材料或分子工程产生的多孔介电材料或它们的组合物。
6.权利要求1的方法，其中所述介电材料的紫外线固化时间短于或等于大约300秒。
7.权利要求1的方法，其中所述介电材料的紫外线固化时间为约60-约180秒。
8.权利要求1的方法，其中在紫外线固化过程中所述介电材料的晶片温度高于或等于大约80℃。
9.权利要求1的方法，其中在紫外线固化过程中所述介电材料的晶片温度为大约室温至大约450℃。
10.权利要求1的方法，其中所述介电材料在低于或大约等于环境压力的加工压力下进行紫外线固化。
11.权利要求1的方法，其中所述介电材料在高于或大约等于环境压力的加工压力下进行紫外线固化。
12.权利要求1的方法，其中所述介电材料在约0.1-约2000mW/cm2的紫外线强度下进行紫外线固化。
13.权利要求1的方法，其中所述介电材料在加工气体吹扫下进行紫外线固化，其中所述吹扫气体选自N2、Oz、Ar、He、H2、水蒸气、COz、CxHy、CxFy、CxHzFy、空气和它们的组合物，其中x为1-6的整数，y为4-14的整数，和z为1-3的整数。
14.权利要求1的方法，其中所述介电材料在约100nm-约400nm的紫外线波长下进行紫外线固化。
15.权利要求1的方法，其中所述介电材料的第一弹性模量和紫外线固化的介电材料的第二弹性模量之间的弹性模量增量大于或等于大约50％。
16.权利要求1的方法，其中所述紫外线固化的介电材料的第二弹性模量大于或等于大约2.5GPa。
17.权利要求1的方法，其中所述紫外线固化的介电材料的第二弹性模量为约4GPa-约12GPa。
18.权利要求1的方法，其中所述介电材料的第一材料硬度和所述紫外线固化的介电材料的第二材料硬度之间的材料硬度增量大于或等于大约50％。
19.权利要求1的方法，其中所述紫外线固化的介电材料的第二材料硬度大于或等于大约0.25GPa。
20.权利要求1的方法，其中所述紫外线固化的介电材料的第二材料硬度为大约0.25-大约1.2GPa。
21.权利要求1的方法，所述方法进一步包括对所述紫外线固化的介电材料进行后紫外线处理，得到具有第三介电常数、第三弹性模量和第三材料硬度的经后紫外线处理的紫外线固化的介电材料，所述第三介电常数小于第二介电常数，第三弹性模量和第三材料硬度分别大于第二弹性模量和第二材料硬度、或者分别在第二弹性模量和第二材料硬度的大约±20％的范围内。
22.权利要求21的方法，其中所述经后紫外线处理的紫外线固化的介电材料的第三介电常数为约1.1-约3.5。
23.权利要求21的方法，其中所述经后紫外线处理的紫外线固化的介电材料的第三介电常数为约1.6-约2.4。
24.权利要求21的方法，其中所述后紫外线处理为热退火处理。
25.权利要求24的方法，其中所述紫外线固化的介电材料的退火温度低于或等于大约450℃。
26.权利要求24的方法，其中所述紫外线固化的介电材料的退火温度为大约150℃-大约450℃。
27.权利要求24的方法，其中所述紫外线固化的介电材料的退火时间不超过或等于大约60秒。
28.权利要求21的方法，其中所述后紫外线处理是等离子体处理，通过在高温下把紫外线固化的介电材料暴露在等离子体环境中进行。
29.权利要求28的方法，其中所述紫外线固化的介电材料在约500-约3000W的等离子功率下进行等离子体处理。
30.权利要求28的方法，其中所述紫外线固化的介电材料在约100-约450℃的温度进行等离子体处理。
31.权利要求28的方法，其中所述紫外线固化的介电材料的等离子体处理时间不超过或等于大约90秒。
32.权利要求28的方法，其中所述紫外线固化的介电材料在约1托-约10托的加工压力下进行等离子体处理。
33.权利要求28的方法，其中所述紫外线固化的介电材料使用等离子气体进行等离子体处理，其中所述等离子气体选自N2、O2、Ar、He、H2、CxHy、含氟气体或它们的组合物，其中x为1-6的整数，y为1-14的整数。
34.权利要求21的方法，其中所述后紫外线处理是将所述紫外线固化的介电材料暴露在紫外线环境中进行紫外线处理。
35.权利要求34的方法，其中所述紫外线固化的介电材料的紫外线处理时间不超过或等于大约300秒。
36.权利要求34的方法，其中所述紫外线固化的介电材料的紫外线处理时间为约60-约180秒。
37.权利要求34的方法，其中所述所述紫外线固化的介电材料在大约室温至大约450℃的温度下进行紫外线处理。
38.权利要求34的方法，其中所述紫外线固化的介电材料在小于或等于大约环境压力的加工压力下进行紫外线处理。
39.权利要求34的方法，其中所述紫外线固化的介电材料在大于或等于大约环境压力的加工压力下进行紫外线处理。
40.权利要求34的方法，其中所述紫外线固化的介电材料在约0.1-约2000mW/cm2的紫外线强度下进行紫外线处理。
41.权利要求34的方法，其中所述紫外线固化的介电材料在加工气体吹扫下进行紫外线处理，其中所述吹扫气体选自N2、Oz、Ar、He、H2、水蒸气、COz、CxHy、CxFy、CxHzFy、空气和它们的组合物，其中x为1-6的整数，y为4-14的整数，z为1-3的整数。
42.权利要求34的方法，其中所述紫外线固化的介电材料在约100nm-约400nm的紫外线波长下进行紫外线处理。
43.权利要求1的方法，其中所述紫外线固化可在真空或者不存在氧或氧化气体的条件下进行。
44.一种通过权利要求1的方法制得的紫外线固化的介电材料。
45.一种通过权利要求21的方法制得的经后紫外线处理的紫外线固化的介电材料。
46.一种通过权利要求1的方法制得的含紫外线固化的介电材料的电子设备。
47.一种通过权利要求21的方法制得的含经后紫外线处理的紫外线固化的介电材料的电子设备。
48.一种通过权利要求1的方法制得的具有紫外线固化涂层的基体。
49.一种通过权利要求21的方法制得的具有经后紫外线处理的紫外线固化涂层的基体。
50.权利要求1的方法，所述方法还包括：
将介电材料放入加工室内；
对加工室进行抽真空或吹扫，除去室内的空气；
向加工室内通入加工气体；
将所述介电材料加热至大约450℃或以下的加工温度；并
将所述介电材料暴露在约100nm-约400nm波长的紫外线辐射下。
51.权利要求50的方法，其中所述紫外线辐射由选自以下的紫外线光源提供：微波驱动的光源、电弧放电光源、介质阻挡放电光源或电子碰撞产生的光源。
52.权利要求50的方法，其中加热所述介电材料的加热源选自红外光源、光学光源、热表面光源或紫外线光源。
53.一种紫外线固化的介电材料，所述介电材料的介电常数为约1.1-约3.5，弹性模量和材料硬度分别大于未经紫外线固化的介电材料的弹性模量和材料硬度约50％。
54.一种紫外线固化的介电材料，所述介电材料的介电常数为约2.0-约2.9，弹性模量和材料硬度分别大于未经紫外线固化的介电材料的弹性模量和材料硬度约50％。
55.一种制备紫外线固化材料的方法，所述方法包括：
提供未经固化的高密度低介电常数材料；和
在不超过大约5分钟、不超过大约450℃下将所述介电材料进行紫外线固化，得到紫外线固化的介电材料，其中紫外线固化比加热炉固化方法的总热预算减少大于约50％。
56.权利要求55的方法，其中所述介电材料选自有机材料、无机材料或它们的组合物。
57.权利要求55的方法，其中所述介电材料选自氢倍半硅氧烷(HSQ)介电材料、甲基倍半硅氧烷(MSQ)介电材料、碳掺杂氧化物(CDO)介电材料、氢化的氧碳化硅(SiCOH)介电材料、苯并环丁烯(BCB)介电材料、基于芳基环丁烯的介电材料、基于聚亚苯基的介电材料或它们的组合物。
58.权利要求55的方法，其中所述介电材料通过使用以下方法，在基体上沉积介电涂层制备：旋涂方法、化学蒸气沉积方法、等离子辅助化学蒸气沉积方法、蒸发方法、活性蒸发方法或自组装沉积方法。
59.权利要求55的方法，其中所述介电材料选自紧密介电材料、成孔剂形成的多孔介电材料、溶剂形成的多孔介电材料或分子工程产生的多孔介电材料或它们的组合物。
60.权利要求55的方法，其中所述介电材料的紫外线固化时间为约60-约180秒。
61.权利要求55的方法，其中所述介电材料在紫外线固化过程中的晶片温度为约室温至约450℃。
62.权利要求55的方法，其中所述介电材料在小于或约等于环境压力的加工压力下进行紫外线固化。
63.权利要求55的方法，其中所述介电材料在大于或大约等于环境压力的加工压力下进行紫外线固化。
64.权利要求55的方法，其中所述介电材料在约0.1-约2000mW/cm2的紫外线强度下进行紫外线固化。
65.权利要求55的方法，其中所述介电材料在加工气体吹扫下进行紫外线固化，其中所述吹扫气体选自N2、Oz、Ar、He、H2、水蒸气、COz、CxHy、CxFy、CxHzFy、空气和它们的组合物，其中x为1-6的整数，y为4-14的整数，z为1-3的整数。
66.权利要求55的方法，其中所述介电材料在约100nm-约400nm的波长下进行紫外线固化。
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