CN1537325A - Msq-基多孔低-k薄膜材料的等离子体固化 - Google Patents

Msq-基多孔低-k薄膜材料的等离子体固化 Download PDF

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CN1537325A
CN1537325A CNA028142888A CN02814288A CN1537325A CN 1537325 A CN1537325 A CN 1537325A CN A028142888 A CNA028142888 A CN A028142888A CN 02814288 A CN02814288 A CN 02814288A CN 1537325 A CN1537325 A CN 1537325A
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film material
porous film
plasma
plasma curing
modulus
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Q·韩
¸
C·瓦尔德弗里德
O·埃斯科西亚
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R·阿巴诺
I·L·贝里三世
J·詹格
I·巴尔
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Axcelis Technologies Inc
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Abstract

弹性模量提高的低介电常数薄膜材料。制造这类薄膜材料的方法包含：提供一种由一种含至少2个Si－CH3基团的树脂制成的多孔甲基倍半硅氧烷－基介电薄膜材料并等离子体固化该多孔薄膜材料，以使该薄膜转化为多孔二氧化硅。多孔薄膜材料的等离子体固化产生一种模量与脱气性提高的薄膜。弹性模量的提高一般大于或约为100％，更典型地，大于或约为200％。该薄膜在低于或约为350℃的一个温度下等离子体固化约15～约120秒钟。该等离子体固化的多孔薄膜材料可任选地进行退火处理。与等离子体固化多孔薄膜材料相比，等离子体固化薄膜的退火可减小薄膜的介电常数，同时保持提高的弹性模量。退火温度一般低于或约为450℃。退火等离子体固化薄膜的介电常数范围为约1.1～约2.4，且弹性模量有所提高。

Description

MSQ-基多孔低-K薄膜材料的等离子体固化
本发明一般地涉及用于电子和半导体器件如集成电路的多孔介电薄膜材料。更具体地，本发明涉及具有更高弹性模量和低介电常数的等离子体固化多孔甲基倍半硅氧烷(MSQ)-基介电薄膜材料以及制造这种薄膜的方法。
随半导体工业引进新一代性能更高、功能更强的集成电路(IC)，构成这些集成电路的元件密度也提高了，而各部件或元件的尺寸、大小和部件或元件之间的间距则缩小了。虽然在过去这种缩小仅受光刻技术上确定结构的能力所限制，但尺寸小至0.25μm或更小的器件几何形状已产生了新的限制因素，如金属元件的导电率或元件之间所用绝缘材料的介电常数等。例如，对于任何2个相邻导电路径，随导体之间距离的缩短，所产生的电容(被导电路径间距离分隔的绝缘材料的介电常数(k)的函数)提高了。该电容增量又会增加导体之间的电容耦合增加、提高功耗并增加阻容(RC)时间常数。因此，半导体IC性能与功能性的继续改进取决于开发如下材料：这种材料形成的介电薄膜的介电常数(k)低于大多数常用材料，即二氧化硅的介电常数(k)，由此减小电容。随这类器件尺寸变得越来越小，将要求电容大幅度减小到所谓的“超低-k”范围(例如，k＜2.5)。
为提供k值降低的绝缘薄膜，最初的方法是用能降低k值的其它组分掺杂氧化硅材料(k～3.9)。例如，用氟掺杂的氧化硅材料一般能降低k值，但只能降到约3.5～3.9。这些掺杂薄膜的成型工艺常优选采用与成型未掺杂氧化硅薄膜相同或类似的方法。因此一般易将氟掺杂薄膜整合进典型的工艺流程。但是，由于这类氟掺杂薄膜仅造成k值的少量降低，还需要有降低介电常数的其它解决方案。最后，这类含氟薄膜的湿稳定性仍未解决。
许多类有机聚合物是提供低-k介电薄膜的另一个初步解决办法。一般而言，有机聚合物能形成k值可能在2.5或更高范围内的介电薄膜。一般地说，形成这类介电薄膜的方法首先要在一个基体上涂布适当预聚体的溶液。然后加热该基体直到预聚体交联并聚合到所要求的程度，形成固体薄膜。由于有机材料以液体形式施涂，能获得一定程度的表面平面化且常常无需另外的平面化工艺。但是，与由化学蒸气沉积之类的方法形成的氧化硅薄膜相比，虽然这类有机聚合物薄膜兼具较低的介电常数和提高的平面化程度，但就薄膜的其它性能而言，这类氧化硅薄膜仍具有缺点。例如，有机材料在450℃以上的热稳定性一般都有限；它们与常用金属如钨(W)和铝(Al)的粘结性往往较差；以及这类有机薄膜的机械性能比氧化硅的低得多。最后，这类有机薄膜一般具有仅在“低-k”范围内的k值(例如，k＝2.7-3.0)。
电器上的介电薄膜涂层在本领域内是熟知的。例如，授予Haluska等的美国专利号4,749,631和4,756,977公开了由下述方法制备的二氧化硅基涂层：分别在基体上涂布硅醇盐或氢倍半硅氧烷溶液，然后将带涂层基体加热到200～1000℃之间的一个温度下。对于某些电子器件与电路，这类涂层的介电常数往往太高。
授予Haluska等的美国专利号4,847,162和4,842,888提出，分别将氢倍半硅氧烷树脂和硅酸酯树脂在有氨存在下加热到200～1000℃之间的一个温度下，形成氮化二氧化硅涂层。这些文献提出使用无水氨，使所形成涂层中的含氮量约为1～2重量％。
Glasser等在Journal of Non-Crystalline Solids，64(1984)，209-221页一文中提出，通过在有氨存在下加热四乙氧基硅烷，形成陶瓷涂层。该文献提出使用无水氨以及所形成的二氧化硅涂层已被氮化了。
授予Jada的美国专利号4,636,440公开了一种缩短带溶胶-凝胶涂层的基体干燥时间的方法，该方法包含将基体暴露在含水氢氧化季铵和/或链烷醇胺化合物中。Jada要求在加热前先干燥涂层。该方法特别限于水解或部分水解的硅醇盐。
授予Chandra的美国专利号5,262,201和授予Baney等的美国专利号5,116,637提出使用碱催化剂，以降低要使包含氢倍半硅氧烷的各种前陶瓷材料转化成陶瓷涂层所必要的温度。这些文献提出，在涂层暴露于碱性催化剂之前，要先除去溶剂。
授予Camilletti等的美国专利5,547,703提出一种在基体上形成低介电常数含Si-O涂层的方法，该方法包含相继在湿氨、干氨和氧中加热氢倍半硅氧烷树脂。所形成的涂层在1MHz的介电常数低达2.42。该文献提出，在将涂层转化为陶瓷之前，要先除去溶剂。
授予Balance等的美国专利5,523,163提出一种在基体上形成含Si-O涂层的方法，该方法包含加热氢倍半硅氧烷树脂，使之转化为含Si-O的陶瓷涂层，然后将该涂层暴露在含氢气的退火气氛中。所得涂层的介电常数低达2.773。该文献提出，在将涂层转化为陶瓷之前，要先除去溶剂。
授予Syktich等的美国专利号5,618,878公开了适合于形成厚陶瓷涂层的含氢倍半硅氧烷树脂溶于饱和烷烃中的涂层组合物。所公开的烷烃是最长为十二烷的那些。该文献未提出在除去溶剂前要将带涂层基体暴露于碱性催化剂中。
授予Chung等的美国专利6,231,989题为“形成涂层的方法”，该专利公开了一种制备低介电常数多孔网络涂层的方法。该方法包含用一种溶液在基体上沉积涂层的方法，溶液包含一种含至少2个Si-CH3基团的树脂和一种溶剂，沉积方式要使沉积后涂层内保留至少5体积％的溶剂。然后将该涂层暴露于包含碱性催化剂与水的环境中。最后，让溶剂从涂层中蒸发出去，形成多孔网络。如果需要，可将该涂层加热固化成陶瓷。由该方法制得薄膜的介电常数为1.5～2.4，弹性模量约为2～3GPa。
在一种产生具有平面化表面的氧化硅层的方法中，已用聚有机倍半硅氧烷制备了旋涂玻璃(SOG)组合物；例如，见授予Fukuyama等的美国专利号4,670,299(Fukuyama’299)。Fukuyama’299的SOG组合物是甲硅烷基化聚有机倍半硅氧烷。该组合物以一种类似于前述有机聚合物所用的方法施涂，然后加热成固体聚合薄膜。这类薄膜，即形式为聚有机倍半硅氧烷(POSQ)的有机聚二氧化硅薄膜的优点在于：(1)它们使薄膜具有低介电常数(k＝2.6-3.0)，以及(2)它们保留了氧化硅型材料较高的机械强度。
但是，优选有一种如下的最终介电薄膜：既具有从有机聚二氧化硅如聚有机倍半硅氧烷形成的薄膜的优点，介电常数又更低(k＜2.5)。为达到这一目标，最可能的方法是将POSQ与另一种介电常数较低的物质进行共混。介电常数最低的物质是空气(k＝1.0)。因此，为达到较低的介电常数，可以在POSQ材料中引进孔隙率。
已采用过几种方法在低介电材料如有机低-k聚合物或有机聚二氧化硅低-k聚合物中引入孔隙率。方法之一是合成一种由一种高热稳定性、高Tg低-k聚合物与一种更易热降解的第二(有机)聚合物组成的嵌段共聚物。据称该方法的优点在于：在材料热固化时形成闭孔多孔结构。见Iledrick等，(1993)聚合物34：4717和Hendrick等，(1995)聚合物36：4855。但是，该方法因控制合成与加工步骤上的困难而受阻，也受聚合物材料热稳定性的限制。另一种方法使用一种由成孔(即孔隙率-引进)有机侧链聚合物接枝到高热稳定性、高Tg低k聚合物上的接枝聚合，以便在热处理后形成多孔材料；见授予Hawker等的美国专利号6,107,357和5,767,014。但该方法也将合成与加工复杂性引进了孔隙率-引入方法。
但是，多孔薄膜的机械性能不好。在芯片制造过程中弱膜会在为平面化晶片表面所用的化学机械抛光(CMP)工艺中失效。多孔薄膜的机械性能随薄膜的孔隙率而变。自然而然，较高的孔隙率导致较低的介电常数而较差的机械性能。因此，需要一种兼具低介电常数与良好机械性能的多孔薄膜。
本发明通过提供一种具有低介电常数与弹性模量提高的多孔介电薄膜材料来满足上述需要。这种薄膜材料的制造方法包含：提供一种具有第一介电常数和第一弹性模量的多孔MSQ-基介电薄膜材料，其中多孔薄膜材料由一种含至少2个Si-CH3基团的树脂制成。将该薄膜进行等离子体固化，以减少一定量的Si-CH3键并产生一种具有第二介电常数和第二弹性模量的含SiOx等离子体固化多孔薄膜材料，第二介电常数与第一介电常数相当，第二弹性模量大于第一弹性模量，以及其中，x是一个介于1-2的数字。弹性模量的提高一般大于或约为100％，更典型地，大于或约为200％。
等离子体固化多孔薄膜材料可任选地进行退火处理，以获得一种具有第三介电常数和第三弹性模量的退火等离子体固化多孔薄膜材料。等离子体固化多孔膜材料的热退火会保持或降低薄膜的介电常数，同时保持较退火前弹性模量提高的弹性模量。退火等离子体固化多孔薄膜材料的介电常数在约1.1～约3.5范围内。退火温度一般都低于或约为450℃，退火时间一般不超过或约为60分钟。
因此，本发明的一个目的是要生产具有提高的弹性模量、低介电常数、提高的热稳定性、提高的脱气性和非常优良的集成性能的介电薄膜材料。
本发明基于以下发现：等离子体固化多孔MSQ-基薄膜会提高薄膜的弹性模量而无需热固化薄膜。等离子体固化会减少一定量的Si-CH3键而不会失去薄膜的低密度结构。
等离子体固化会在膜内产生可观量的极性成分，它们在某些应用中是不希望存在的。本发明还基于以下发现：对等离子体固化多孔MSQ-基介电薄膜进行热退火处理会产生一种低介电常数和模量提高的薄膜材料。
本发明的方法特别适用于在电子器件或电路板上沉积涂层，它们在生产晶体管之类的器件中起层内介电层、掺杂介电层的作用，在生产电容器和电容器类的器件、多层器件、三维器件、绝缘体器件上的硅、超晶格器件等中，起含硅带颜料粘结剂体系的作用。但是，拟用本发明涂布的基体和器件的选择仅受基体在本发明所用温度与压力下的热稳定性和化学稳定性所限制。因此，本发明的涂层能用于下列基体上：包括如聚酰亚胺、环氧、聚四氟乙烯及其共聚物、聚碳酸酯、丙烯酸类和聚酯之类的塑料、陶瓷、皮革、织物、金属等。
如本发明所用，术语“陶瓷”包括无定形二氧化硅之类的陶瓷和类陶瓷材料如并非完全没有碳原子和/或氢原子、但呈陶瓷特性的类无定形二氧化硅材料。术语“电子器件”或“电路板”包括，但不限于，二氧化硅-基器件、砷化镓-基器件、碳化硅-基器件、聚焦平面阵列、光电子器件、光伏电池和光学器件。
作为本发明的起始材料，需要一种多孔MSQ-基介电薄膜。这种包含硅、氧和碳的薄膜涂层可以由多孔有机取代聚二氧化硅和一种有机成孔剂形成。由旋涂工艺制成并用于本发明的典型超低-k多孔介电MSQ-基材料可购自Chemat Technologies公司(Northridge，CA)和JSR公司(Tokyo，Japan)。制造这类多孔介电薄膜的方法如下文所述。
生产多孔MSQ-基介电薄膜材料的一种方法始于在基体上沉积一薄层多孔有机取代聚二氧化硅涂层。该多孔聚二氧化硅薄膜涂层是通过用一种共混溶液旋涂一薄层多孔有机取代聚二氧化硅薄膜而制成。该共混溶液是在合适的溶剂(即醇)中包含下列组分：(1)一种含至少2个Si-CH3基团的热稳定、低介电常数、有机-无机混杂主体聚合物；(2)一种可热降解的有机聚合物，起成孔剂(即一种孔隙率-诱导材料)作用；和选择性地包括(3)其它添加剂(如表面活性剂)。
热稳定低介电常数主体聚合物是一种有机-无机混杂聚合物(即有机聚二氧化硅，具体地说，是(RSiOx)n型聚有机倍半硅氧烷(POSQ)，其中R是一个有机取代基，如甲基、乙基或苯基，以及其中，x是一个介于1与2之间的数字。
成孔剂或孔隙率-诱导材料是一种可热降解的有机聚合物，热固化时，它在主体聚合物交联温度以上的温度下完全降解为非反应性气态小分子物。然后这些非反应性气态小分子降解物扩散出主体材料，在主体聚合物中留下孔洞(即孔隙率)。主体聚合物(如MSQ等)的交联温度通常在100-200℃量级，所以有机成孔剂的降解温度需大大超过该温度(如250-350℃)。
降解温度达300℃或更高的适用有机成孔剂必须足够大(如＞10)才能在主体材料中形成轮廓分明的孔洞，但不能大到(例如，＜100)孔尺寸在低-k材料薄膜总宽度中占一个可观的百分数。进一步，优选在主体材料中产生的孔洞具有规则与重现性几何形状(例如，直径和体积都相同的球形孔)。一般而言，有机树状聚合物或超支化有机聚合物是具有上述特性的最佳侯选成孔剂，比线形聚合物的重现性好得多。线形聚合物可能具有较高的分子量与尺寸分布，在材料中产生规则(即球状)与可重现的孔洞与孔尺寸要难得多。
这类薄膜能通过热固化除去成孔剂。其结果形成一种多孔超低-k材料的薄膜。也可用涉及其它方法的另一些实施方案来产生多孔聚二氧化硅。
虽然这类具有低介电常数的多孔MSQ-基介电材料在生产某些电子或半导体器件中是理想的，但优选有一种弹性模量更高的薄膜。
为提高多孔MSQ-基介电薄膜材料的弹性模量，要将它进行等离子体固化。等离子体固化可通过射频(RF)、感应耦合、RF电容耦合、螺旋形谐振器、微波顺流和微波电子回旋加速共振(ECR)等离子体进行。等离子体固化会提高多孔MSQ-基介电薄膜材料的机械性能、增加材料硬度，同时保持介电、孔结构、密度和电性能。
在一个典型的等离子体固化工艺中，以快速等速升温步骤将晶片迅速加热到所要求的温度并等离子体固化该晶片。
等离子体固化的精确条件取决于所用的等离子体类型。对于一个200mm晶片，典型的微波等离子体固化条件的实例如下所示：
微波等离子体功率：      500W-3000W
晶片温度：              80℃-350℃
加工压力：              1.0乇-4.0乇
等离子体固化时间：      ＜120秒
等离子体气体：         H2/N2/CF4/O2
N2H2流率：           ＞0-4000sccm
O2流率：              ＞0-4000sccm
CF4流率：             ＞0-400sccm
与炉内(热)固化多孔薄膜材料相比，等离子体固化多孔薄膜材料的弹性模量提高了，当介电常数约为2.0时，弹性模量介于约1.0～约3.5GPa之间。弹性模量的提高一般大于或约为100％，更典型地，大于或约为200％。一般地说，等离子体固化多孔薄膜材料的弹性模量大于或约为3GPa，更典型地，介于约3Gpa到约10GPa之间。
本发明的等离子体固化多孔MSQ-基介电薄膜材料具有提高的化学稳定性和提高的尺寸稳定性。所谓提高的化学稳定性，是指该薄膜更耐化学药品，如清洗液和化学抛光液，且更耐光刻抛光和干刻蚀工艺中的等离子体损伤。
此外，等离子体固化大大减少或消除了齐聚二氧化硅和其它物质从多孔膜中的脱气。但是，等离子体固化会在薄膜中产生可观量的极性成分。
如果需要，等离子体固化薄膜材料可任选地用任何类型的热暴露进行退火处理，以降低介电常数。例如，可以将等离子体固化薄膜放在一个常用烘箱内直到除尽极性成分，例如在400℃处理30分钟。能采用的另一个方法涉及在一个快速热加工(RTP)室内退火处理等离子体固化薄膜材料，以降低介电常数。等离子体固化薄膜要在一个典型的温度下退火足够长的时间，然后冷却到约100℃。
RTP工艺的典型操作条件如下所示：
扫描速率：    15℃/秒
晶片温度：    350-450℃
退火时间：    ＜180秒
加工压力：    大气压
与等离子体固化MSQ-基介电薄膜相比，退火等离子体固化薄膜材料的介电常数会有所下降。退火等离子体固化薄膜的介电常数一般为约1.1～约3.5，更典型地，约1.8～约2.4范围内。
在本发明的又一个实施方案中，将多孔MSQ-基介电薄膜材料等离子体固化到厚度约0.3μm～约0.7μm，并用于大马士革工艺中。或者，也可将该薄膜等离子体固化到厚度约0.7μm～约1.25μm，并用于双大马士革工艺。或者，也可将在带图形晶片上的多孔MSQ-基薄膜等离子体固化到厚度约1.3～约1.5μm，并用作层间介电层或钝化层。
在还有一个实施方案中，将一层或多层等离子体固化的或退火等离子体固化的多孔MSQ-基介电薄膜层成型为一个具有多层互联结构的微电子器件。
为更易理解本发明，参考下列实施例，这些实施例旨在说明本发明而不限制它们的范围。
实施例1
典型MSQ-基介电薄膜材料的不同等离子体条件及所得性能示于下表1。
表1 MSQ-基介电薄膜材料的等离子体条件与性能
工艺 条件 厚度减少(％) R.I提高(％)  等离子体固化后的接触角 弹性模量GPa 介电常数
    He/H2     60s/3乇/350℃   3.25   1.37     50     1    2.30
    Ar/H2     60s/3乇/250℃   2.21   0.98     55
    N2H2     60s/1乇/285℃   7.70   1.60     5     1.6    2.35
    N2H2+CF4     60s/1乇/285℃   14.05   -0.04     60     2.5    2.35
    N2H2+O2+CF4     60s/2.5乇/285℃   29.52   0.49     29     5    6.00
    对比   0.07   0.00     90     1    2.30
虽然为说明本发明已给出了一些代表性实施方案和细节，但对本领域内的技术人员来说，显然在公开于此的组成和方法上都可作各种变化而不偏离本发明的范围，范围规定在所附权利要求中。

Claims (28)

1.一种制造等离子体固化材料的方法，该方法包含：
提供一种具有第一介电常数与第一弹性模量的多孔甲基倍半硅氧烷-基介电薄膜材料，其中，多孔薄膜材料由一种含至少2个Si-CH3基团的树脂制成；以及
将该多孔薄膜材料等离子体固化以减少一定量的Si-CH3键并产生具有第二介电常数和第二弹性模量的含SiOx等离子体固化多孔薄膜材料，其第二介电常数与第一介电常数相当，第二弹性模量大于第一弹性模量，以及其中，x是一个介于1-2之间的数字。
2.权利要求1的方法，其中多孔薄膜材料的等离子体固化用约500W～约3000W的等离子体功率进行。
3.权利要求1的方法，其中多孔薄膜材料的等离子体固化在低于或约为350℃的一个温度下进行。
4.权利要求1的方法，其中多孔薄膜材料的等离子体固化在约150℃～约350℃的一个温度下进行。
5.权利要求1的方法，其中多孔薄膜材料的等离子体固化在约270℃～约300℃的一个温度下进行。
6.权利要求1的方法，其中多孔薄膜材料的等离子体固化在约1乇～约4乇的加工压力下进行。
7.权利要求1的方法，其中多孔薄膜材料的等离子体固化时间在约15～约120秒。
8.权利要求1的方法，其中用一种等离子体气体对多孔薄膜材料进行等离子体固化。
9.权利要求8的方法，其中等离子体气体选自H2等离子体气体、N2等离子体气体、CF4等离子体气体或O2等离子体气体，或它们的组合。
10.权利要求1的方法，其中，在多孔薄膜材料的第一弹性模量与等离子体固化多孔薄膜材料的第二弹性模量之间，弹性模量的增量大于或约为100％。
11.权利要求1的方法，其中，在多孔薄膜材料的第一弹性模量与等离子体固化多孔薄膜材料的第二弹性模量之间，弹性模量的增量大于或约为200％。
12.权利要求1的方法，其中等离子体固化多孔薄膜材料的第二弹性模量大于或约为3GPa。
13.权利要求1的方法，其中等离子体固化多孔薄膜材料的第二弹性模量为约3GPa～约10GPa。
14.权利要求1的方法，其中等离子体固化多孔薄膜材料的脱气量已大大降低或消除。
15.权利要求1的方法，该方法还包含将等离子体固化多孔薄膜材料进行退火处理，以获得一种具有第三介电常数与第三弹性模量的退火等离子体固化多孔薄膜材料，第三介电常数与第二介电常数相当或更低，第三弹性模量与第二弹性模量相当。
16.权利要求15的方法，其中等离子体固化多孔薄膜材料在低于或约为450℃的一个温度下进行退火处理。
17.权利要求15的方法，其中等离子体固化多孔薄膜材料在约350℃～约450℃的一个温度下进行退火处理。
18.权利要求15的方法，其中等离子体固化多孔薄膜材料的退火时间不超过或约为60分钟。
19.权利要求15的方法，其中退火等离子体固化多孔薄膜材料的第三介电常数为约1.1～约3.5。
20.权利要求15的方法，其中退火等离子体固化多孔薄膜材料的第三介电常数为约1.8～约2.4。
21.一种由权利要求1的方法制成的等离子体固化多孔薄膜材料。
22.一种由权利要求15的方法制成的退火等离子体固化多孔薄膜材料。
23.一种含有由权利要求1的方法制成的等离子体固化多孔薄膜材料的电子器件。
24.一种含有由权利要求15的方法制成的退火等离子体固化多孔薄膜材料的电子器件。
25.一种带有由权利要求1的方法制成的等离子体固化多孔薄膜材料的基体。
26.一种带有由权利要求15的方法制成的退火等离子体固化多孔薄膜材料的基体。
27.一种含SiOx的多孔等离子体固化薄膜材料，其介电常数为约1.1～约3.5，弹性模量比非等离子体固化的含SiOx多孔薄膜材料的高约100～200％。
28.一种含SiOx的多孔等离子体固化薄膜材料，其介电常数为约1.8～约2.4，弹性模量比非等离子体固化的含SiOx多孔薄膜材料的高约100～200％。
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CN111363183B (zh) * 2020-02-25 2022-09-06 深圳赛兰仕科创有限公司 复合膜及其制备方法

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