CN1376740A - 硅基组合物、低介电常数膜、半导体器件以及制造低介电常数膜的方法 - Google Patents
硅基组合物、低介电常数膜、半导体器件以及制造低介电常数膜的方法 Download PDFInfo
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- CN1376740A CN1376740A CN01133846A CN01133846A CN1376740A CN 1376740 A CN1376740 A CN 1376740A CN 01133846 A CN01133846 A CN 01133846A CN 01133846 A CN01133846 A CN 01133846A CN 1376740 A CN1376740 A CN 1376740A
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- silicone resin
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- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
- H01L21/76801—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing
- H01L21/76802—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing by forming openings in dielectrics
- H01L21/76807—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing by forming openings in dielectrics for dual damascene structures
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/14—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
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Abstract
一种组合物,包含硅氧烷树脂、基本上由硅、碳和氢构成的硅化合物,其中在一分子的主链中形成-X-键的碳与硅原子数之比范围为2∶1~12∶1,其中X是(C)m,其中m是1~3的整数,或者9个或更少碳原子的取代或未取代的芳香族基团和溶剂,对该组合物进行热处理以形成低介电常数膜。因此,提供了一种具有优异的耐化学品性和优异的耐潮性的低介电常数膜。通过采用该膜可制造出能快速响应的半导体集成电路。
Description
本申请基于并要求2001年3月23日提交的日本专利申请2001-84475的优先权,其内容在此参考引用。
技术领域
本发明涉及采用低介电常数膜的半导体器件、该膜所用的硅基组合物、低介电常数膜和制造低介电常数膜的方法。
背景技术
降低半导体集成电路的多层布线工艺中布线之间产生的寄生电容和降低信号传播速率的延迟(即布线延迟),对半导体的集成化和小型化而言很重要。
虽然很早就认识到信号传播速率因绝缘膜的寄生电容而降低,布线延迟对整个器件的影响在布线间隙大于1μm的那一代半导体器件中还未如此明显过。
但是在布线间隙为1μm或更小的情况下,对器件速率的影响就变得严重起来。特别是当所形成的电路其布线间隙是不久的将来所要求的0.5μm或更小时,布线之间的寄生电容对器件速率的影响会更大。因此这可能是半导体集成化和小型化的一大障碍。
换句话说,当信号传播速率的降低很大程度上依赖于半导体集成电路的多层布线中布线之间的布线电阻和寄生电容时,提高器件的集成度使布线和布线间隙的宽度更窄,导致布线之间布线电阻和寄生电容的增加。
绝缘膜的电容可通过使布线厚度更薄以降低横截面积的方式实现降低。但是,使布线更薄会导致更大的布线电阻,并因此而无法实现更高的信号传播速率。
因此,要实现更高的信号传播速率,就必须使布线的电阻和绝缘膜的介电常数更低,并且希望未来它们会在决定器件性能方面扮演非常重要的角色。
布线延迟(T)取决于布线电阻(R)和布线间的电容(C),如方程式1所示。
T∝CR (1)在方程式1中,ε(介电常数)和C之间的关系表示为方程式1’。
C=ε0εr·S/d (1′)其中S是电极的表面积;ε0是真空的介电常数;εr是绝缘膜的相对介电常数;而d是布线间隙。
因此,通过使绝缘膜的介电常数更低可有效地降低布线延迟。
迄今为止已采用过无机膜如二氧化硅(SiO2)、氮化硅(SiN)和磷硅酸盐玻璃(PSG)以及有机聚合物如聚酰亚胺作为绝缘材料。
但是,半导体器件最常用的CVD-SiO2膜的介电常数约为4左右。虽然SiOF膜,它是目前备受关注的低介电常数CVD膜,其介电常数约为3.3~3.5,但是它是吸湿性的,因此存在介电常数因吸水而增加的问题。
除此之外,作为低介电常数膜,由带SiH键的硅氧烷树脂制造的多孔膜是已知的。但是,当半导体器件用碱溶液进行清洗时,会产生一个问题,即,由于水解而形成吸湿性高的SiOH基团,导致介电常数升高,还有对半导体部件造成机械损伤的问题,比如因清洗产生裂纹。为了解决这些问题,按常规方法形成一层保护膜比如SiO2膜。但是,这会使半导体器件中低介电常数膜的速率降得更低,并因此在形成多层布线时增大有效介电常数。
为了进行比较,可采用有机聚合物膜来获得低介电常数。但是,玻璃化转变温度低达200-350℃而热膨胀系数却很大,因此存在对布线造成损伤的问题。
发明内容
因此,本发明的目的是解决上述几个问题以形成优异的膜,以及提供同常规的绝缘膜相比有较低的介电常数的绝缘膜,并且提供快速且可靠的半导体器件。
除此之外,本发明在许多情况下改进了硅基膜的耐化学品性,特别是耐碱溶液性能,并且可解决由硅氧烷树脂制造的常规多孔膜所表现出来的高吸湿性问题。
根据本发明的一个方面,提供了一种组合物,它包含硅氧烷树脂、基本上由硅、碳和氢构成的硅化合物,其中在一分子的主链中形成-X-键(其中X是(C)m(其中m是1~3的整数),或者碳原子不超过9的取代或未取代的芳香族基团)的碳与硅原子数之比为2∶1~12∶1,以及溶剂。在这里要注意(C)m中的‘C’表示碳原子。
本发明的其它方面,提供了一种通过将组合物进行热处理而获得的低介电常数膜、一种以低介电常数膜作层间绝缘膜的半导体器件,以及制造该低介电常数膜的方法。
发现通过对硅氧烷树脂添加骨架链(主链)中带硅-碳键的硅化合物而获得的膜具有耐受化学品如碱的特性。
也发现当对硅氧烷树脂添加该化合物时,因为其相容性高所以该化合物均匀地分散到硅氧烷树脂中,并改进耐酸和碱溶液的能力而且即使以基于100重量份硅氧烷树脂向硅氧烷树脂中添加重量比为0.1重量份的化合物还能保持该效果。
也发现骨架上带硅-碳键的硅化合物有高的耐潮性,并且因此根据本发明的组合物即使是在形成如果不采用本发明的组合物就存在耐潮性低问题的多孔膜时也是有效的。
也发现硅氧烷树脂和这种硅化合物的并用可防止在碱性溶液中对硅氧烷基低介电常数膜造成的损伤(机械损伤比如裂纹),这一直是带SiH键的低介电常数膜的一个问题,并且由吸湿性所造成的介电常数的提高在许多情况下均可解决,这也一直是低介电常数多孔膜的另一个问题。
这种硅化合物的特点是硅化合物主链中带-X-键(其中X是(C)m(其中m=1~3),或者9个或更少碳原子的取代或未取代的芳香族基团)。
通过采用主链中带上述-X-键(其中X是(C)m(其中m=1~3),或者9个或更少碳原子的取代或未取代的芳香族基团)的硅化合物,连同硅氧烷树脂,形成含有二者的涂膜,并加热得到的膜,可制造出水解和/或遭化学处理损伤现象均下降的低介电常数膜,同时抑制了半导体制造方法中介电常数的增大。
上述硅化合物优选具有以下结构式2所示的结构:其中R4和R5彼此相同或不同,是H或1~3个碳原子的脂族烃基团或者取代或未取代的6~9个碳原子的芳族烃基团;R6是1~3个碳原子的脂族烃基团或者取代或未取代的亚苯基;而p是20~1,000的整数。
有必要限制R4、R5以及聚合度,以使组合物的粘度在形成膜之前保持在适当的范围之内,同时对R6的限制对确保所形成的低介电常数膜的耐热性而言很重要。
R1、R2或R3不太优选除了氢、氟或甲基以外的脂族烃基团,因为会加强氢的消除反应,从而促进交联键的形成。已发现虽然-O-键也促进交联反应,但它们不会造成有实效的问题。
本文所用的-X-键(其中X是(C)m(其中m=1~3),或者9个或更少碳原子的取代或未取代的芳香族基团),以m=3情况为例,表示3个碳原子顺序键合成C-C-C的状态,其中每个碳可带有除氢以外的取代基。m=3情况的一个简单例子是亚丙基。m限制在1~3,因为当m为4或更大时可观察到耐热性降低。亚苯基是9个或更少碳原子的取代或未取代的芳香族基团的例子。
试验表明,优选基本上由硅、碳和氢构成的硅化合物,其中在一分子的主链中形成-X-键(其中X是(C)m(其中m是1~3的整数),或者9个或更少碳原子的取代或未取代的芳香族基团)的碳与硅原子数之比为2∶1~12∶1,因为它给出一种就低介电常数、对酸和碱的耐化学品性以及耐潮性取得了良好平衡的低介电常数膜。
从制造方法的角度出发,上述硅氧烷树脂优选通过热处理含有(a∶b)摩尔比为0∶1~1∶0的四烷氧基硅烷(a)和烷基三烷氧基硅烷和/或三烷氧基硅烷(b)的混合物而获得的硅氧烷树脂。
为了获得质量稳定的硅氧烷树脂,优选通过在上述的热处理过程中从100mol的(a+b),即四烷氧基硅烷(a)和烷基三烷氧基硅烷和/或三烷氧基硅烷(b)的总量中释放出100~400mol醇的方法制造树脂。
也发现优选硅氧烷树脂中的碳含量范围是硅氧烷树脂中总原子数的1~80原子%,以实现稳定的低介电常数。据推断在低介电常数膜的形成过程中抑制了水解。
也发现同样优选直接键合在硅氧烷树脂中的硅上的氢原子含量范围是硅氧烷树脂中总原子数的1~25原子%。
两种条件均满足的情况也是优选实施方案之一。
上述硅化合物与上述硅氧烷树脂的重量比优选为0.001~2,即,0.1~200重量份的前者基于100重量份的后者。
根据本发明的组合物也优选含有选自酚醛清漆树脂、环氧树脂、丙烯酸类树脂、聚酯、聚丙烯、酚化合物、咪唑化合物和金刚烷化合物的物质。
已发现在上述物质中特别优选丙烯酸树脂。
有各种在聚合度、共聚程度等方面有区别的丙烯酸树脂。可通过试配法从其中选择一个合适的。
添加这些物质,通过其在低介电常数膜形成过程中的汽化和散逸(dissipation)而形成孔。即,它们是脱离剂(dissipating agent)(成孔物质)。
虽然可通过成孔而制造介电常数更低的低介电常数膜,可是机械性能比如强度同时受损。因此,希望尺寸适当的孔以适当的方式分布。
优选向100重量份的硅氧烷树脂中添加5~200重量份的脱离剂。这是因为当用量少于5重量份时,介电常数降得不够,而当超过200重量份时膜的强度降低。
也发现热失重系数处于特定范围的物质适合作为上述物质。即,希望物质在以10℃/min的速率从常温加热到150℃时损失5wt%或更高的重量而在400℃则损失90wt%或更高的重量。这可能是因为上述孔的形成得到了适当的控制。
希望上述孔的孔隙率为低介电常数膜总体积的10%~70vol%。当孔隙率低于10vol%时,成孔效果很小。当孔隙率超过70vol%时,机械性能受损。希望的平均孔尺寸(直径)范围为50~200nm。
上述检测表明,具有SiO4键、C-SiO3-键以及-X-键(其中X是(C)m(其中m是1~3的整数),或者9个或更少碳原子的取代或未取代的芳香族基团)并且具有10%~70vol%的孔隙率和1.4~2.5的相对介电常数的低介电常数膜可实现低介电常数、抑制水解并具有良好的机械性能。通过膜,其具有包含硅氧烷树脂和其骨架链上带硅-碳键的硅化合物的组合物,与孔的结合,就可得到具备这些性能的低介电常数膜。
作为代表性的机械强度,希望Stud Pull法测得的拉伸断裂强度是30~80MPa。小于30MPa的拉伸断裂强度在机械性能上是不够的。当超过80MPa时,从机械性能角度而言并不是不好,但是在许多情况下会使介电常数受损。
通过研究具有SiO4键、C-SiO3-键以及-X-键(X是(C)m(其中m是1~3的整数),或者9个或更少碳原子的取代或未取代的芳香族基团)的体系而实现了本发明。然而,仅从物理性能角度观察所得到的结果时,可认为,具有孔隙率10%~70vol%、相对介电常数1.4~2.5以及Stud Pull法测定的拉伸断裂强度30~80MPa并且基本上由硅、碳、氢和氧构成的低介电常数膜提供了上述的各种效果。
附图说明
图1是具有铝(Al)布线的半导体器件的横截面图;
图2是具有铜(Cu)布线的半导体器件的横截面图;和
图3表示通过稍微修改图2的半导体器件而获得的半导体器件。
具体实施方式
采用图、表和以下的实施例对本发明的实施方案进行示范性说明。本发明并不限于这些实施例、图和表。其它实施方案只要处于本发明的范围和精神之内,就属于本发明的范畴。
本发明的实施方案之一是一种组合物,其包含硅氧烷树脂、基本上由硅、碳和氢构成并且在其中碳原子与硅原子数之比为2∶1~12∶1的一分子主链中具有-X-键(其中X是(C)m(其中m是1~3的整数),或者9个或更少碳原子的取代或未取代的芳香族基团)的硅化合物,还有溶剂。
这种硅氧烷树脂的制备方法通常是,加热含有四烷氧基硅烷、烷基三烷氧基硅烷和/或三烷氧基硅烷以及溶剂的混合物,然后蒸发出预设量的醇。
虽然硅化合物通常在上述加热之后才添加,但如果可能的话,也可在加热之前添加。
根据本发明骨架上含有硅-碳键并有待添加到硅氧烷树脂中的硅化合物包括聚二甲基碳硅烷、聚氢甲基碳硅烷、聚二乙基碳硅烷、聚氢乙基碳硅烷、聚碳硅杂苯乙烯(polycarbosila styrene)、聚苯基甲基碳硅烷、聚二苯基碳硅烷、聚二甲基硅亚苯基硅氧烷、聚甲基硅亚苯基硅氧烷、聚二乙基硅亚苯基硅氧烷、聚乙基硅亚苯基硅氧烷、聚二丙基硅亚苯基硅氧烷、聚丙基硅亚苯基硅氧烷、聚苯基硅亚苯基硅氧烷、聚二苯基硅亚苯基硅氧烷、聚苯基甲基硅亚苯基硅氧烷、聚苯基乙基硅亚苯基硅氧烷、聚苯基丙基硅亚苯基硅氧烷、聚乙基甲基硅亚苯基硅氧烷、聚甲基丙基硅亚苯基硅氧烷和聚乙基丙基硅亚苯基硅氧烷。
优选添加0.1~200重量份的硅化合物到100重量份的硅氧烷树脂中。如果硅化合物的添加量低于0.1重量份,无法获得足够的耐化学品性。如果硅化合物的添加量大于200重量份,所获得的膜的强度降低。
本发明所用的硅氧烷树脂没有特别限制,只要能用溶剂稀释即可。这种硅氧烷树脂包括四烷氧基硅烷的溶胶-凝胶型聚合物、三烷氧基硅烷的溶胶-凝胶型聚合物、甲基三烷氧基硅烷的溶胶-凝胶型聚合物、四烷氧基硅烷和三烷氧基硅烷的溶胶-凝胶型聚合物、四烷氧基硅烷和甲基三烷氧基硅烷的溶胶-凝胶型聚合物、甲基三烷氧基硅烷和三烷氧基硅烷的溶胶-凝胶型聚合物、四烷氧基硅烷和二甲基烷氧基硅烷的溶胶-凝胶型聚合物、氢倍半硅氧烷、甲基倍半硅氧烷和含氟的氢倍半硅氧烷。
当按化学结构定义例如上述的硅化合物时,优选化学结构如上述结构式2所示的硅化合物。当按化学结构定义例如上述的硅氧烷树脂时,优选化学结构如结构式3所示的硅氧烷树脂。
通过涂布根据本发明的组合物就可形成膜,比如采用旋转涂布法。对稀释溶剂没有特别的限制,只要它能溶解本发明所用的硅氧烷树脂和骨架上带硅-碳键的硅化合物即可。这种溶剂包括环己酮、甲基异丁基酮、甲乙酮、甲基溶纤剂、乙基溶纤剂、辛烷、癸烷、丙二醇、丙二醇单甲基醚、丙二醇单甲基醚乙酸酯、二甘醇、丙二醇、丙二醇单甲基醚、丙二醇单乙基醚和丙二醇单丙基醚。
根据本发明,当从上述的组合物形成多孔膜或诸如此类时,就可得到足够的耐碱性(耐碱腐蚀性)和耐潮性。
采用用于形成根据本发明的低介电常数膜的材料就可形成膜,方法比如是通过旋转涂布法在底材上涂布上述的组合物,在温度120℃~250℃蒸发溶剂,然后在温度300℃或更高热处理涂布的组合物以使硅氧烷树脂交联。根据本发明,可形成多孔膜的方法也可比如是,通过旋转涂布法在底材上涂布上述的组合物并在温度120℃~250℃对溶剂进行蒸发处理和对脱离剂进行散逸处理,或者以UV线照射进行汽化处理和散逸处理,然后在温度300℃或更高热处理涂布的组合物以使硅氧烷树脂交联。
实施例
以下说明本发明的实施例。
采用以下方法进行分析。
硅氧烷树脂或硅化合物的分子量通过凝胶渗透色谱进行测定,以四氢呋喃为溶剂,并表达为按聚苯乙烯换算(polystyrene-converted)的分子量。
硅化合物的一分子主链中形成-X-键(其中X是(C)m(其中m是1~3的整数),或者9个或更少碳原子的取代或未取代的芳香族基团)的碳与硅原子数之比通过XPS(X射线光电子光谱法)进行测定。
碳在硅氧烷树脂总原子数中的含量以XPS(X射线光电子光谱法)测定。
直接键合在硅上的氢原子在硅氧烷树脂总原子数中的含量从原料的IR测试结果计算得到。
通过约10mg样品在热重量分析仪器中以10℃/min的速率从常温加热至500℃时的重量损失来测定热失重。
通过氮吸附法测定孔隙率。
通过在光学显微镜下进行观察来确定出现或不出现裂纹。
实施例1
在反应器中于搅拌下向由20.8g(0.1mol)四乙氧基硅烷、17.8g(0.1mol)甲基三乙氧基硅烷和39.6g甲基异丁基酮构成的混合物中滴加16.2g(0.9mol)含400ppm硝酸的硝酸水溶液。该添加持续10min。添加结束之后,反应再继续进行以熟化另外2h。反应在搅拌下进行。
然后添加5g硫酸镁以除去过量的水,并且通过旋转蒸发仪除去熟化中形成的乙醇以使反应混合物的体积变为50ml。形成0.7mol量的乙醇。
向所获得的反应混合物中添加20ml甲基异丁基酮。然后,在烘箱中于200℃除去甲基异丁基酮。发现反应混合物含有17.4wt%的固体。向反应混合物中添加1.74g甲基氢聚碳硅烷以制备成膜用的涂布液。
上述反应以及旋转蒸发仪处理在常温和常压下进行。
分析表明,成膜用涂布液中硅氧烷树脂和甲基氢聚碳硅烷的分子量分别为3,500和1,800。
甲基氢聚碳硅烷的一分子主链中形成-X-键(其中X是(C)m(其中m是1~3的整数),或者9个或更少碳原子的取代或未取代的芳香族基团)的碳与硅原子数之比为3∶1。
碳浓度为13原子%,基于上述硅氧烷树脂的总原子数。
直接键合在硅上的氢原子的浓度为1原子%,基于上述硅氧烷树脂的总原子数。
实施例2
以与实施例1类似的方式进行处理,只是采用20.8g(0.1mol)四乙氧基硅烷、16.4g(0.1mol)三乙氧基硅烷和37.2g甲基异丁基酮,而不是20.8g(0.1mol)四乙氧基硅烷、17.8g(0.1mol)甲基三乙氧基硅烷和39.6g甲基异丁基酮,并且在烘箱中于200℃除去甲基异丁基酮,结果表明溶液含有固体16.8wt%。形成0.7mol量的乙醇。
以与实施例1类似的方式向反应混合物中添加1.68g甲基氢聚碳硅烷以制备成膜用涂布液。
分析表明,成膜用涂布液中硅氧烷树脂的分子量是2,800。
碳浓度为2原子%,基于上述硅氧烷树脂的总原子数。
直接键合在硅上的氢原子的浓度为11原子%,基于上述硅氧烷树脂的总原子数。
实施例3
以与实施例1类似的方式进行处理,只是采用17.8g(0.1mol)甲基三乙氧基硅烷、16.4g(0.1mol)三乙氧基硅烷和37.2g甲基异丁基酮,而不是20.8g(0.1mol)四乙氧基硅烷、17.8g(0.1mol)甲基三乙氧基硅烷和39.6g甲基异丁基酮,并且在烘箱中于200℃除去甲基异丁基酮,结果表明溶液含有固体15.8wt%。形成0.7mol量的乙醇。
以与实施例1类似的方式向反应混合物中添加1.58g甲基氢聚碳硅烷以制备成膜用涂布液。
分析表明,成膜用涂布液中硅氧烷树脂的分子量是4,500。
碳浓度为11原子%,基于上述硅氧烷树脂的总原子数。
直接键合在硅上的氢原子的浓度为12原子%,基于上述硅氧烷树脂的总原子数。
实施例4
向实施例1制备的成膜用涂布液中添加1.74g丙烯酸树脂,以制备成多孔膜用涂布液。
上述的丙烯酸树脂在150℃损失10wt%的自身重量而在400℃则损失100wt%的自身重量。
实施例5
向实施例2制备的成膜用涂布液中添加1.68g聚酯基树脂,以制备成多孔膜用涂布液。
上述的聚酯基树脂在150℃损失10wt%的自身重量而在400℃则损失95wt%的自身重量。
实施例6
向实施例3制备的成膜用涂布液中添加1.58g金刚烷单酚(adamantane monophenol),以制备成多孔膜用涂布液。
上述的金刚烷单酚在150℃损失60wt%的自身重量而在400℃则损失100wt%的自身重量。
实施例7
将实施例1~6制备的成膜用涂布液和成多孔膜用涂布液以3,000rpm在Si底材上旋转涂布20s,并在200℃蒸发溶剂,然后所获得的膜在氮中含氧量为100ppm或更低的氮气氛下于400℃退火30min,以形成低介电常数的绝缘膜。
在所得到的膜上形成厚度为1mm的Au电极,而从测得的电容计算得到的膜的相对介电常数汇总在表1中。
在上述退火步骤过程中除去脱离剂,形成孔。
在采用实施例4的涂布液时,其孔的孔隙率为48%,在采用实施例5的涂布液时为42%而在采用实施例6的涂布液时为45%。
通过FT-IR和XPS分析这些膜证实存在着SiO4键、C-SiO3-键和-X-键(其中X是(C)m(其中m是1~3的整数),或者9个或更少碳原子的取代或未取代的芳香族基团)。
Stud Pull法测得的拉伸断裂强度为64MPa。
实施例8
对于实施例1~6中的每一个,如表2和3所示改变聚碳硅烷的添加量,并且以与实施例7类似的方式制备膜,所获得的膜分别在2.38wt%四甲基氢化铵水溶液和5wt%氢氧化铵水溶液中浸泡1min。然后观察裂纹,并测定膜厚度和介电常数的变化。如表2所示,当添加了0.1重量份或更多的聚甲基氢碳硅烷后,浸泡处理之后与浸泡处理之前,所有的评价项目都没有什么变化。
实施例9
然后在以下描述采用根据上述实施例1~6的涂布液制造的半导体器件结构及其制造方法。
要注意的是,以下在与实施例7类似的条件下形成低介电常数膜。
图1表示有铝(Al)布线的半导体器件的横截面图。有源区以硅底材1表面上形成的场氧化膜2为界。金属氧化物半导体场效应晶体管(MOSFET)3在有源区中形成。MOSFET 3包含源区3S、漏区3D、栅电极3G和栅氧化膜3I。
在底材上形成由SiO2构成的层间绝缘膜10和由SiN构成的阻断(stopper)膜11,以覆盖MOSFET 3。在层间绝缘膜10中在相当于漏区3D位置处形成接触孔12。由TiN构成的势垒层13覆盖在接触孔12的侧壁和底表面上。除此之外,由钨(W)构成的插塞14填充接触孔12。
势垒层13和插塞14是在TiN膜和W膜淀积在整个底材表面上之后通过化学-机械抛光(CMP)而形成的。TiN膜是通过溅射淀积的。W膜是采用六氟化钨和氢通过化学汽相淀积(CVD)而淀积的。
在阻断膜11的表面上形成第一层布线20。第一层布线20具有三层结构,按厚度为50nm的TiN膜21(底)、厚度为450nm的含Cu的Al膜22以及厚度为50nm的TiN膜23(顶)的顺序构成。通过等离子体刻蚀采用氯化氢气体将TiN膜和Al膜刻出图案。第一层布线20有多个部分以导电的方式连接到钨插塞14上。
第一层的布线20和阻断膜11的表面以由SiO2构成并且厚度为50nm的衬底(liner)膜25覆盖。衬底膜25是采用原硅酸四乙酯(TEOS)和氧通过CVD而形成的。
在衬底膜25上形成低介电常数膜26。低介电常数膜26可通过旋转涂布根据上述实施例4~6的涂布液而形成。形成低介电常数膜26要使得在从硅底材的平坦表面进行测定时其厚度为500nm。
为了更详细说明,布线20是通过包括以下步骤而形成的:形成由低介电常数层包围的金属图案,然后金属图案的表面与低介电常数层的表面一起进行化学-机械抛光(CMP)处理,以形成布线20的一个层(或膜21、22或23)。在布线的形成过程中,通过层压比如上述的介电常数层而形成低介电常数膜26。
在低介电常数膜26上形成由SiO2构成并且厚度为1,000nm的罩面(cap)层27。罩面层27是采用TEOS和氧通过CVD而形成的。利用CMP将罩面层27的上表面平坦化。进行该抛光要使得当在未配置第一层的布线20的位置处进行测定时,衬底膜25、低介电常数膜26和罩面层27的总膜厚为1,200nm。
在衬底膜25、低介电常数膜26和罩面层27的三个层中形成通孔28。通孔28是采用CF4和CHF3通过等离子体刻蚀而形成的。通孔28的侧壁和底表面用由TiN构成的势垒层29涂布。钨(W)插塞30填充在通孔28中。势垒层29和W插塞30是以与形成其下面的势垒层13和插塞14类似的方式形成的。
在罩面层27上形成第二层的布线40。层合第二层的衬底膜41、低介电常数膜42和罩面层43,以覆盖第二层的布线40。这些是以与形成第一层的对应部分类似的方式形成的。
在图1所示的多层布线结构中,以根据本发明的低介电常数膜填充同一布线层中相邻的布线之间的间隙,从而可降低布线之间的寄生电容。除此之外,膜的耐潮性并不下降而且即使是在用碱溶液处理之后也保持了低的介电常数。
图2表示有铜(Cu)布线的半导体器件的横截面图。从硅底材1一直到阻断层11的各个组件其结构与图1所示半导体器件的对应组件的结构相同。因此,图2中的这些组件与图1中的对应组件有着相同的参考数字和符号。
在阻断膜11上形成低介电常数膜50。采用根据上述实施例的成膜材料形成低介电常数膜50,使得当从硅底材的平坦表面进行测定时,其厚度为450nm。在低介电常数膜50上形成由SiO2构成并且厚度为50nm的罩面层51。罩面层51是采用TEOS和氧通过CVD而形成的。
穿过低介电常数膜50和罩面层51形成第一层的布线槽52。第一层的布线槽52是采用CF4和CHF3通过等离子体刻蚀而形成的。在第一层布线槽52的底表面上露出插塞14的上表面。
第一层的布线槽52的侧壁和底表面以由TaN构成并且厚度为50nm的势垒层53覆盖。由Cu构成的第一层的布线54填充在布线槽52中。
以下描述了形成势垒层53和第一层的布线54的方法。
在整个底材上,包括第一层的布线槽52的内表面,通过溅射法形成TaN膜。在所形成的膜上,通过溅射法进一步形成厚度为50nm的Cu膜。使用所形成的Cu膜作为电极,通过电解电镀形成厚度为600nm的Cu膜。Cu和TaN膜的多余部分通过CMP除去,而在第一层的布线槽52中留下势垒层53和第一层的布线54。
在罩面层51上层合由SiN构成并且厚度为50nm的防扩散膜60、低介电常数膜61、由SiN构成并且厚度为50nm的阻断膜62、低介电常数膜63以及由SiN构成并且厚度为50nm的罩面层64。防扩散膜60和阻断膜62是采用硅烷和氨气通过等离子体CVD而形成的。低介电常数膜61和63是采用根据本发明的硅基组合物而形成的。低介电常数膜61和63的形成要使得当从硅底材的平坦表面进行测定时,其厚度分别为650nm和400nm。
在防扩散膜60和低介电常数膜61的包围下形成通孔68。在阻断膜62、低介电常数膜63和罩面层64的包围下形成第二层的布线槽69。通孔68和第二层布线槽69的内表面用由TaN构成并且厚度为50nm的势垒层70覆盖。由Cu构成的第二层布线72填充在通孔68和第二层布线槽69中。第二层的布线72是通过双金属镶嵌法形成的。
以下简要说明双金属镶嵌法。首先,形成从罩面层64延伸至第一层的布线54上表面的通孔68。然后,形成从罩面层64延伸至低介电常数膜61上表面的第二层的布线槽69。势垒层70和第二层的布线72以与其下势垒层53和第一层布线54的形成类似的方式形成。
第一层的布线54和第二层的布线72被低介电常数膜50、61和63所包围,以实现布线之间寄生电容的降低。除此之外,这些低介电常数膜50、61和63是使用根据本发明的硅基组合物形成的,从而可在不降低耐潮性的情况下使介电常数保持低值,即使是在以碱处理液处理之后。
图3表示通过稍微更改图2所示半导体器件而制造的半导体器件。
在图2所示的半导体器件中,由氮化硅构成的阻断膜62放在低介电常数膜61与其上的低介电常数膜63之间,而阻断膜62在图3中不存在,并且在半导体器件中低介电常数膜63与低介电常数膜61接触。
这种结构可通过选择低介电常数膜用材料实现,其使得上面的低介电常数膜63的刻蚀速率在相同的刻蚀条件下比下面的低介电常数膜61的更快。
当在通孔68形成之后通过刻蚀而形成第二层的布线槽时,如果上面的低介电常数膜63的刻蚀速率比下面的介电常数膜61的更快,那么在通过刻蚀除去上面的低介电常数膜63之后暴露出的下面的低介电常数膜61被刻蚀得更慢,结果是上面的低介电常数膜63可在没有除去下面的低介电常数膜61的情况下除去。
表1涂层的相对介电常数
实施例1 | 2.92 |
实施例2 | 2.88 |
实施例3 | 2.79 |
实施例4 | 2.12 |
实施例5 | 2.16 |
实施例6 | 2.14 |
表2在2.38%四甲基氢化铵水溶液中浸泡的结果
添加的聚碳硅烷(重量份) | 出现或不出现裂纹 | 膜厚度变化 | 相对介电常数变化 | |||||||||||||||
实施例 | 实施例 | 实施例 | ||||||||||||||||
1 | 2 | 3 | 4 | 5 | 6 | 1 | 2 | 3 | 4 | 5 | 6 | 1 | 2 | 3 | 4 | 5 | 6 | |
0 | - | + | + | - | + | + | -54nm | -34nm | -38nm | -45nm | -39nm | -52nm | +0.8 | +0.4 | +1.2 | +0.6 | +0.8 | +0.5 |
0.05 | - | - | + | - | + | + | -12nm | -18nm | -23nm | -21nm | -22nm | -19nm | +0.2 | +0.3 | +0.4 | +0.4 | +0.5 | +0.4 |
0.1 | - | - | - | - | - | - | <-1nm | <-1n m | <-1nm | <-1nm | <-1nm | <-1nm | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 |
10 | - | - | - | - | - | - | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 |
50 | - | - | - | - | - | - | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 |
100 | - | - | - | - | - | - | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 |
180 | - | - | - | - | - | - | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 |
200 | - | - | - | - | - | - | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 |
250 | - | - | - | - | - | - | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 |
表3在3.5%氨水溶液中浸泡的结果
添加的聚碳硅烷(重量份) | 出现或不出现裂纹 | 膜厚度变化 | 相对介电常数变化 | |||||||||||||||
实施例 | 实施例 | 实施例 | ||||||||||||||||
1 | 2 | 3 | 4 | 5 | 6 | 1 | 2 | 3 | 4 | 5 | 6 | 1 | 2 | 3 | 4 | 5 | 6 | |
0 | - | - | + | - | - | + | -32nm | -31nm | -35nm | -36nm | -15nm | -34nm | +0.8 | +0.3 | +0.2 | +0.4 | +0.2 | +0.4 |
0.05 | - | - | + | - | - | + | -5nm | -9nm | -5nm | -8nm | -5nm | -12nm | +0.2 | +0.2 | +0.2 | +0.3 | +0.2 | +0.2 |
0.1 | - | - | - | - | - | - | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 |
10 | - | - | - | - | - | - | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 |
50 | - | - | - | - | - | - | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 |
100 | - | - | - | - | - | - | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 |
180 | - | - | - | - | - | - | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 |
200 | - | - | - | - | - | - | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 |
250 | - | - | - | - | - | - | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <-1nm | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 | <±0.1 |
根据本发明形成的低介电常数膜具有低介电常数。膜也具有相当优异的耐化学品比如酸和碱的能力,以及优异的耐潮性,从而膜的介电常数因吸收潮气而增加得极少。根据本发明形成的膜有效地作为半导体器件的低介电常数层间绝缘膜。采用该绝缘膜可获得快速响应和/或对裂纹或诸如此类的产生有良好抵抗能力(耐化学品性)的优异的半导体集成电路。
Claims (27)
1.一种组合物,包含:
硅氧烷树脂;
基本上由硅、碳和氢构成的硅化合物,其中在一分子的主链中形成-X-键的碳与硅原子数之比为2∶1~12∶1,其中X是(C)m,其中m是1~3的整数,或者9个或更少碳原子的取代或未取代的芳香族基团;和
溶剂。
4.根据权利要求1的组合物,其中所述的硅氧烷树脂通过以下方法获得:
热处理含有摩尔比(a∶b)为0∶1~1∶0的四烷氧基硅烷(a)和烷基三烷氧基硅烷和/或三烷氧基硅烷(b)的混合物;并且
从100mol的(a+b),四烷氧基硅烷(a)和烷基三烷氧基硅烷和/或三烷氧基硅烷(b)的总量中释放出100~400mol的醇。
5.根据权利要求1的组合物,其中所述硅氧烷树脂中的碳浓度为1~80原子%,基于硅氧烷树脂的总原子数。
6.根据权利要求1的组合物,其中直接键合在所述硅氧烷树脂的硅上的氢原子的浓度为1~25原子%,基于硅氧烷树脂的总原子数。
7.根据权利要求1的组合物,其中采用了0.1~200重量份的所述硅树脂,基于100重量份的所述硅氧烷树脂。
8.根据权利要求1、2、3、4、5、6或7的组合物,其中:
组合物含有成孔用的脱离剂;和
脱离剂包含当以10℃/min的速率从常温开始升温加热,在150℃时损失5wt%或更多的自身重量而在400℃时损失90wt%或更多的物质。
9.根据权利要求8的组合物,其中所述的脱离剂包含至少一种选自酚醛清漆树脂、环氧树脂、丙烯酸类树脂、聚酯、聚丙烯、酚化合物、咪唑化合物和金刚烷化合物的物质。
10.根据权利要求8的组合物,其中5~200重量份的所述脱离剂被添加到100重量份的硅氧烷树脂中。
11.根据权利要求8的组合物,其中所述的脱离剂是丙烯酸类树脂。
12.一种通过热处理根据权利要求1、2、3、4、5、6或7的组合物而获得的低介电常数膜。
13.一种根据权利要求12的低介电常数膜,具有孔隙率为10%~70vol%的孔。
14.一种低介电常数膜,
具有SiO4键、C-SiO3-键以及-X-键,其中X是(C)m,其中m是1~3的整数,或者9个或更少碳原子的取代或未取代的芳香族基团;并且
具有10%~70vol%的孔隙率,和1.4~2.5的相对介电常数。
15.一种根据权利要求12的低介电常数膜,具有Stud Pull法测得的拉伸断裂强度为30~80MPa。
16.一种低介电常数膜:
基本上由硅、碳、氢和氧构成;和
具有孔隙率为10%~70vol%、相对介电常数为1.4~2.5和StudPull法测得的拉伸断裂强度为30~80MPa。
17.一种半导体器件,具有作为层间绝缘膜的根据权利要求12的低介电常数膜。
18.一种半导体器件,含有包含含铜材料的布线和根据 12的低介电常数膜,所述的布线按以下方法形成;
形成包含含铜材料并用低介电常数层包围的金属图案;和
将金属图案的表面与所述低介电常数层的表面一起进行化学-机械抛光,以形成所述的布线或所述布线的层,
其中所述的低介电常数膜以层合体的形式形成并包括所述的介电常数层作为所述层合体的一部分。
19.一种制造低介电常数膜的方法,其中一种组合物包含:
基本上由硅、碳和氢构成的硅化合物,并且具有以下式2所示的结构,其中R4和R5彼此相同或不同,是H或具有1~3个碳原子的脂族烃基团或者具有6~9个碳原子的取代或未取代的芳族烃基团;R6是具有1~3个碳原子的脂族烃基团,或者取代或未取代的亚苯基;而p是20~1,000的整数,其中在一分子的主链中形成-X-键的碳与硅原子数之比为2∶1~12∶1,其中X是(C)m,其中m是1~3的整数,或者9个或更少碳原子的取代或未取代的芳香族基团,
溶剂;以及
成孔用脱离剂,
对该组合物进行热处理,使硅氧烷树脂和硅化合物交联,并使溶剂和脱离剂汽化以留下孔。
20.一种制造低介电常数膜的方法,其中一种组合物包含:
通过以下方法获得的硅氧烷树脂:热处理含有摩尔比(a∶b)为0∶1~1∶0的四烷氧基硅烷(a)和烷基三烷氧基硅烷和/或三烷氧基硅烷(b)的混合物,并从100mol(a+b),四烷氧基硅烷(a)和烷基三烷氧基硅烷和/或三烷氧基硅烷(b)的总量中释放出100~400mol的醇;
基本上由硅、碳和氢构成的硅化合物,并且具有以下式2所示的结构,其中R4和R5彼此相同或不同,是H或具有1~3个碳原子的脂族烃基团,或者具有6~9个碳原子的取代或未取代的芳族烃基团;R6是具有1~3个碳原子的脂族烃基团,或者取代或未取代的亚苯基;而p是20~1,000的整数,其中在一分子的主链中形成-X-键的碳与硅原子数之比为2∶1~12∶1,其中X是(C)m,其中m是1~3的整数,或者6~9个碳原子的取代或未取代的芳香族基团;
溶剂;以及
成孔用脱离剂,
对该组合物进行热处理,使硅氧烷树脂和硅化合物交联,并且使溶剂和脱离剂汽化以留下孔。
21.一种根据权利要求19或20的制造低介电常数膜的方法,其中所述的脱离剂包含当以10℃/min的速率从常温加热,在150℃时损失5wt%或更多的自身重量而在400℃时损失90wt%或更多的物质。
22.一种根据权利要求21的制造低介电常数膜的方法,其中所述的脱离剂包含至少一种选自酚醛清漆树脂、环氧树脂、丙烯酸类树脂、聚酯、聚丙烯、酚化合物、咪唑化合物和金刚烷化合物的物质。
23.一种根据权利要求21的制造低介电常数膜的方法,其中5~200重量份的所述脱离剂被添加到100重量份的所述硅氧烷树脂中。
24.一种根据权利要求21的制造低介电常数膜的方法,其中所述的脱离剂是丙烯酸类树脂。
25.一种根据权利要求21的制造低介电常数膜的方法,其中所述硅氧烷树脂中的碳浓度为1~80原子%,基于所述硅氧烷树脂的总原子数。
26.一种根据权利要求21的制造低介电常数膜的方法,其中直接键合在所述硅氧烷树脂的硅上的氢原子的浓度为1~25原子%,基于所述硅氧烷树脂的总原子数。
27.一种根据权利要求21的制造低介电常数膜的方法,其中采用了0.1~200重量份的所述硅化合物,基于100重量份的所述硅氧烷树脂。
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CN110028640B (zh) * | 2019-04-23 | 2021-08-06 | 湘潭大学 | 一种基于三苯基咪唑-间苯三酚的多孔聚合物及其制备方法和用途 |
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TWI238844B (en) | 2005-09-01 |
KR20020075191A (ko) | 2002-10-04 |
JP2002284998A (ja) | 2002-10-03 |
DE10154771B4 (de) | 2013-02-14 |
KR100726269B1 (ko) | 2007-06-08 |
US20040180188A1 (en) | 2004-09-16 |
DE10164943B4 (de) | 2009-02-26 |
DE10154771A1 (de) | 2002-10-10 |
CN1220731C (zh) | 2005-09-28 |
US7358299B2 (en) | 2008-04-15 |
JP4545973B2 (ja) | 2010-09-15 |
US6780498B2 (en) | 2004-08-24 |
US20030003288A1 (en) | 2003-01-02 |
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