CN1793274A - 化学机械抛光用的选择性浆料 - Google Patents
化学机械抛光用的选择性浆料 Download PDFInfo
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- CN1793274A CN1793274A CNA2005101361633A CN200510136163A CN1793274A CN 1793274 A CN1793274 A CN 1793274A CN A2005101361633 A CNA2005101361633 A CN A2005101361633A CN 200510136163 A CN200510136163 A CN 200510136163A CN 1793274 A CN1793274 A CN 1793274A
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- 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
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- 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
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
- H01L21/31051—Planarisation of the insulating layers
- H01L21/31053—Planarisation of the insulating layers involving a dielectric removal step
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- 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
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
- H01L21/321—After treatment
- H01L21/32115—Planarisation
- H01L21/3212—Planarisation by chemical mechanical polishing [CMP]
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
一种用来在低-k介电体存在情况下进行选择性除去的水溶液。该溶液包含0-25重量%氧化剂;0.00002-5重量%多组分表面活性剂,该多组分表面活性剂具有疏水性尾部、非离子亲水性部分和阴离子亲水性部分,疏水性尾部具有6-30个碳原子,非离子亲水性部分具有10-300个碳原子;0-15重量%对非铁金属的抑制剂;0-50重量%磨料;0-20重量%非铁金属的络合剂;以及水。
Description
技术领域
本发明涉及抛光半导体晶片,具体地说,涉及存在如低k-介电层的另一层的情况下除去晶片层如阻挡材料的组合物及方法。
背景技术
通常,半导体基板具有硅基片和有许多凹槽的介电层,所述凹槽在介电层内排列形成电路互连的图案。这些凹槽图案具有波纹结构或双重波纹结构。此外,通常一层至三层或更多层遮盖层涂布在具有凹槽图案的介电层上,又有阻挡层覆盖在这些遮盖层上面。最后,又有金属层覆盖着阻挡层并填充形成图案的凹槽。金属层形成电路互连,而电路互连部位连接各介电区域并形成集成电路。
遮盖层可以用作不同目的。例如,遮盖层如碳氮化硅(silicon carbide nitrde)涂层介电材料可以用作停止抛光层(polishing stop),防止下面的介电层在抛光时被除去。碳化氮化硅中的氮浓度可随制造厂家变化;可以包含至多约50原子%氮,如果氮含量为0,则停止层在化学上就只是碳化硅。此外,二氧化硅层、氮化硅层或两层的组合可以修正停止层上面的形貌。通常,阻挡层如钽或氮化钽阻挡层涂布在遮盖层上,导电性金属层覆盖在阻挡层上,形成互连金属。
化学机械平面化即CMP方法通常包括多个抛光步骤。例如,最初的平面化步骤从下面的阻挡介电层除去金属,使晶片平面化。这第一步抛光除去了金属层,同时在有金属填充了凹槽的晶片上留下光滑的平坦表面,金属填充的凹槽在平坦的抛光表面上形成电路互连。第一步抛光步骤会以相对较高速率除去过量的互连金属如铜。第一步抛光之后,第二步抛光步骤通常除去留在半导体晶片上的阻挡层。这一第二步抛光从其下面的介电层上除去阻挡层,在该介电层上形成平坦的抛光表面。第二步抛光可以在遮盖层上停止,可以除去所有的遮盖层或者可以下面介电层的一部分。
不幸的是,CMP过程经常导致从电路互连过多除去不需要的金属或产生“凹陷(dishing)”。这种凹陷在第一步抛光和第二步抛光都会产生。超出可接受程度的凹陷会引起电路互连的尺寸损失。在电路互连中的这些薄区域会削弱电信号并且可能影响双重波纹结构的连续制造。除了凹陷外,CMP法经常在称作“磨蚀”的作用下除去过量的介电层。在邻近互连金属处发生的磨蚀可能引起电路互连的尺寸缺陷。此外,磨蚀对低k-和超低k介电层特别成为问题。象凹陷一样,这些缺陷会导致削弱电信号并影响双重波纹结构的随后生产。
除去阻挡层和所有不需要的遮盖层后,第一停止抛光遮盖层如碳化氮化硅的停止层常常可以防止CMP过程损害介电层。通过控制除去速率,这种停止层通常能保护下面的介电层,避免或减轻介电层的磨蚀。阻挡层和其它遮盖层(如氮化硅和二氧化硅)的除去速率与停止层的除去速率之比是选择率的例子。对本申请目的,选择率指以/分钟测定的除去速率的比例。
Singh等人在WO专利公报No.03/072670中公开了任选使用非离子、阴离子、阳离子和两性离子表面活性剂来提高选择性。然而,此专利公报未揭示对限制低k-介电体磨蚀有用的具体配方。
需要能够选择性除去阻挡材料和遮盖材料(如,氮化硅和二氧化硅),不会除去过量介电层如低-k介电层和超低-k介电层的组合物。此外,需要一种能如下抛光半导体晶片的浆料:除去阻挡材料;减少互连的凹陷现象,降低介电体磨蚀;避免介电层剥离;用或不用碳化硅-氮化硅停止层进行操作。
发明内容
一个方面,本发明提供一种用于在低-k介电体存在下进行选择性除去的水溶液,该溶液包含0-25重量%氧化剂;0.00002-5重量%多组分表面活性剂,该多组分表面活性剂具有疏水性尾部、非离子亲水性部分和阴离子亲水性部分,疏水性尾部具有6-30个碳原子,非离子亲水性部分具有10-300个碳原子;0-15重量%对非铁金属的抑制剂;0-50重量%磨料;0-20重量%对非铁金属的络合剂;以及水。
另一方面,本发明提供一种用于在低-k介电体存在下进行选择性除去的水溶液,该溶液包含0-20重量%氧化剂;0.00005-2重量%多组分表面活性剂,该多组分表面活性剂具有疏水性尾部、非离子亲水性部分和阴离子亲水性部分,疏水性尾部具有8-20个碳原子,非离子亲水性部分具有20-200个碳原子;0.001-15重量%对非铁金属的抑制剂;0-40重量%磨料;0-10重量%对非铁金属的络合剂;以及水。
另一方面,本发明提供从半导体晶片除去一层的至少一部分的方法,该方法包括用抛光溶液对半导体基板进行抛光的步骤,该溶液包含0-25重量%氧化剂;0.00002-5重量%多组分表面活性剂,该多组分表面活性剂具有疏水性尾部、非离子亲水性部分和阴离子亲水性部分,疏水性尾部具有6-30个碳原子,非离子亲水性部分具有10-300个碳原子;0-15重量%对非铁金属的抑制剂;0-50重量%磨料;0-20重量%对非铁金属的络合剂;以及水。
具体实施方式
所述溶液和方法提供了意想不到的除去多种层材料如碳化硅、碳化氮化硅、TEOS、钽、氮化钽和其它含钽材料的选择性,同时不会除去过量低k-材料如(硅)碳掺杂的氧化物(CDO)。所述浆料依靠多组分表面活性剂来选择性除去非低k-层,而不抛光低k-层或仅除去一部分的低k-层。这种选择性促进了减少互连金属的凹陷以及低k-介电层的磨蚀。此外,浆料能除去阻挡材料和遮盖层如氮化硅,有机遮盖物和介电体,脆性低k-介电层如碳掺杂氧化物不致从半导体晶片上剥离或分层。这些抛光溶液的另一个好处是能对碳掺杂的氧化物层停止除去的能力。
本说明书中使用的表面活性剂是指存在时具有吸附到晶片基板表面或界面上的性质或能改变晶片基板表面或界面的表面自由能的物质。术语“界面”是任何两个不混溶相之间的边界。术语“表面”指一相是气体通常是空气时的界面。表面活性剂通常用来降低界面的自由能。
多组分表面活性剂的分子结构具有对水的吸引力很小,被称作疏水性尾部的第一结构部分、具有对水吸引力的非离子亲水性部分的第二结构部分和对水具有强吸引力的阴离子亲水基团,所述阴离子亲水基团在溶液中离子化时具有负离子电荷。
疏水性基团通常是具有适合于水溶性长度的长链烃、碳氟化合物或硅烷的链。具体地,疏水性基团总共具有6-30个碳原子。疏水性基团较好具有8-20个碳原子,最好具有12-16个碳原子。疏水性部分可以是直链、支链或环状链。疏水性部分可以是饱和链、不饱和链或含有芳族基团。一个具体例子是源自脂肪醇的直链聚合物。
非离子亲水性部分含有10-300个碳原子。非离子亲水性部分较好含有20-200个碳原子;最好含有25-150个碳原子。非离子亲水性部分可以是直链、支链或环状链。非离子亲水性部分可以是饱和链、不饱和链或含有芳族基团。合适的非亲水性部分的一个具体例子是聚环氧乙烷的直链。
阴离子部分的例子包括羧酸、磺酸、硫酸、膦酸、它们的盐或它们的混合物中至少一种的阴离子部分。优选的阴离子部分含有选自羧酸根(羧酸盐)、磺酸根(磺酸盐)、硫酸根(硫酸盐)或磷酸根(磷酸或多磷酸酯)的至少一个化学基团。表面活性剂的亲水性部分可含有一个或多个氮原子或者一个或多个氧原子或它们的混合物,但优选含有至少一个可离子化的基团,提供溶解性和对负电荷表面如二氧化硅表面的排斥力。
通常,加入0.00002-5重量%的多组分表面活性剂可以达到高选择性。本发明所指的所有浓度均以重量%表示,除非另外特别指出。此外,所揭示的范围包括合并和部分合并的范围以及范围的两个端值。较好的是,表面活性剂为0.00005-2重量%,最好是0.0001-1重量%。
通常,这些表面活性剂以铵盐、钾盐、季铵盐或钠盐加入。对高纯度制剂,表面活性剂最好以铵盐形式加入。
多组分表面活性剂较好其抑制阻挡膜如钽(Ta)或氮化钽(TaN)的除去速率与抑制碳掺杂氧化物(CDO)的除去速率(以/分钟测定)不同。如果定义膜X的除去速率的相对抑制(ΔX)为ΔX=(X0-X)/X0,其中,X0和X代表加入表面活性剂之前和之后,以/分钟测定的X膜的除去速率。本发明揭示的表面活性剂较好满足了下面式子中的至少一个(用TaN作为例子):Δ(CDO)>Δ(TaN),测定的垂直于晶片的微孔聚氨酯抛光垫的压力为13.8kPa(2psi)并用实施例的条件。例如,当在13.8kPa压力和实施例条件下,用IC1010TM抛光垫抛光时,不含表面活性剂的组合物对碳掺杂氧化物提供500/分钟和对氮化钽提供500/分钟的对照抛光速率(X0)。而加入多组分表面活性剂后,在同样条件下,对碳掺杂氧化物的抛光速率降低至300/分钟,而对TaN的除去速率必须大于300/分钟,以满足上述的选择性的式子。
调节pH水平以及氧化剂浓度能促进含亚胺和肼衍生化合物的抛光溶液提高阻挡物的除去速率。此外,该溶液和方法提供了意想不到的选择性并且能控制阻挡材料的去除。任选地,该溶液依靠选自亚胺和肼衍生的化合物以及它们的混合物的阻挡层去除剂来选择性除去阻挡材料。该溶液除去阻挡材料时,能减小介电层磨蚀,还减小金属互连如铜的凹陷、磨蚀和划痕。而且,溶液除去钽阻挡材料时,没有低k-介电层从半导体晶片上剥离或分层的现象。此外,溶液对从原硅酸四乙酯(TEOS)前体沉积的二氧化硅所形成的硬掩模具有受控制的TEOS除去速率。
具体地,溶液包含阻挡层除去剂,用来除去阻挡材料如钽、氮化钽、钽-硅氮化物和其它含钽的阻挡材料。虽然该溶液在酸性pH范围对含钛阻挡材料有效,但是该溶液对含钽材料特别有效。在本说明书中,含钽材料包括钽、钽基合金和钽的金属互化物如钽的碳化物、氮化物和氧化物。该浆料对从有图案的半导体晶片上除去含钽阻挡层最有效。
优选的亚胺衍生物包括下面结构式(I)的化合物:
式中,R1是-H或-NH2,R2是-H、-NH2、烃基、氨基、羰基、酰亚胺基、偶氮基、氰基、硫代基或硒基和OR7,其中R7是烃基。
优选的肼衍生物包括下面结构式(II)的化合物:
R3R4N-NR5R6 (II)
式中,R3、R4、R5和R6各自独立地是-H、-OR7、-NH2、烃基、羰基、酰亚胺基、偶氮基、氰基、硫代基或硒基。
亚胺衍生物的例子包括;乙脒、乙脒盐、乙脒衍生物、精氨酸、精氨酸盐、精氨酸衍生物、甲脒、甲脒盐、甲脒衍生物、胍衍生物、胍盐以及它们的混合物。优选的结构式(I)的亚胺衍生物包括例如,盐酸乙脒、盐酸氨基-胍、精氨酸、甲脒、甲脒亚磺酸、乙酸甲脒、1,3-二苯基胍、1-甲基-3-硝基胍、盐酸胍、四甲基胍、2,2-偶氮二(二甲基-丙脒)二-HCl、硫酸胍、胍乙酸、碳酸胍、硝酸胍以及它们的混合物。
优选的结构式(II)的肼衍生物包括例如:碳酰肼、乙酰肼、盐酸半卡巴肼、1,2-二甲酰肼、甲基肼基-羧酸酯、草酸二酰肼、丙酮吖嗪和甲酰肼以及它们的混合物。
结构式(I)的亚胺衍生物较好含有给电子取代基如R1或R2,并不含吸电子基团。更好的是,R1和R2中一个是给电子取代基,另一个取代基是氢或给电子取代基。如果亚胺衍生物中存在两个给电子取代基,这两个取代基可以相同或不同。
结构式(II)的亚胺衍生物较好含有肼官能团(>N-NH2),但含有不超过一个以上的吸电子取代基。当R3和R4都是氢,或R5和R6都是氢时,提供肼官能团。
为本说明书目的,术语“给电子”是指连接在一种物质上将电子密度转移到该物质的化学基团。F.A.Carey和R.J.Sundberg在有机化学进展(AdvancedOrganic Chemistry),Part A:结构和机理(Structure and Mechanisms),3rdEdition New York:Plenum Press(1990),208页和546-561页中,提供对给电子取代基的详细描述。亚胺衍生物具有一个给电子取代基,能将足够的电子密度转移到该物质,在该取代基上形成可观得的部分负电荷。给电子取代基包括例如,氨基、羟基(OH)、烷基、取代的烷基、烃基、取代的烃基、酰胺基和芳基。这些给电子取代基能加速除去含钽的阻挡材料。
此外,添加磨料能有效给予亚胺衍生物和肼衍生物吸电子取代基。术语“吸电子”指连接在一种物质上从该物质将电子密度转移出去的化学基团。吸电子取代基从该物质转移出去足够的电子密度,在该取代基上形成可观得的正电荷,它不会加速阻挡层的除去。吸电子取代基包括例如,-O-烷基、-卤素、-C(=O)H、-C(=)O-烷基、-C(=O)OH、-C(=O)-烷基、-SO2H、-SO3H和-NO2。不是吸电子基的羰基,不是酰胺基。
钽阻挡物除去剂可以是乙脒、乙脒盐、乙脒衍生物、精氨酸、精氨酸盐、精氨酸衍生物、甲脒、甲脒盐、甲脒衍生物、胍、胍衍生物、胍盐和它们的混合物。这些阻挡物除去剂在酸性pH范围看来对钽阻挡材料和含钽材料具有强的亲合力。这种亲合力看来能用有限的磨料乃至不使用任何磨料时提高阻挡材料的除去速率。但使用有限的磨料可使得抛光除去钽阻挡物的速率大于除去介电层和金属互连的速率。溶液依靠选自甲脒、甲脒盐、甲脒衍生物、如胍、胍衍生物、胍盐以及它们混合物这些钽阻挡物除去剂来选择性除去钽阻挡材料。特别有效的阻挡物除去剂包括胍、盐酸胍、硫酸胍、盐酸氨基-胍、胍乙酸、碳酸胍、硝酸胍、甲脒、甲脒亚磺酸、乙酸甲脒以及它们的混合物。优选溶液最好含有0.1-10重量%阻挡物除去剂,对大多数用途,阻挡物除去剂浓度为0.1-4重量%能提供足够的阻挡物除去速率。
阻挡物除去剂在碱性、中性和酸性抛光水溶液中有效。较好的是,溶液有余量水,pH为2-12。优选溶液为碱性pH。将pH调小的常用试剂包括硝酸、磺酸、盐酸、磷酸和有机酸。最好按照需要用氢氧化钾和硝酸提供最后的pH调节。此外,溶液最好用去离子水,用以限制会偶然带来的杂质。
在pH小于7时,任选的氧化剂能促进阻挡物的除去。所述组合物包含0-25重量%的氧化剂。氧化剂能使浆料在酸性pH情况下特别有效地操作。较好的是,溶液含有0-20重量%的氧化剂。溶液最好含有0.01-5重量%的氧化剂。氧化剂可以在众多氧化性化合物中的至少一种,如过氧化氢、单过硫酸盐、碘酸盐、过氧苯二甲酸镁、过氧乙酸、过硫酸盐、溴酸盐、过溴酸盐、高氯酸盐、过碘酸盐、硝酸铁、铁盐、铈盐、锰(Mn)(III)盐、(Mn)(IV)盐和Mn(VI)盐、银盐、铜盐、铬盐、钴盐、卤素、次氯酸盐,以及它们的混合物。此外,经常优选使用氧化剂化合物的混合物。优选的氧化剂是过氧化氢或碘酸盐。当抛光浆料含有不稳定的氧化剂如过氧化氢时,最好在使用时才将氧化剂混入浆料中。最优选的氧化剂是过氧化氢。
适用于互连金属包括例如,铜、铜合金、金、金合金、镍、镍合金、铂族金属、铂族金属合金、银、银合金、钨和钨合金和含有至少一种上述金属的混合物。优选的互连金属是铜。在使用氧化剂如过氧化氢的酸性抛光组合物和浆料中,铜除去速率和静态腐蚀速率都较高,这主要是由于铜的氧化。为降低互连金属的除去速率,抛光组合物使用一种腐蚀抑制剂。腐蚀抑制剂的功能是降低互连金属的除去速率。这将有利于提供减少互连金属的凹陷现象而改善抛光性能。
所述腐蚀抑制剂任选以0-15重量%存在,腐蚀抑制剂可以是对互连金属的一种腐蚀抑制剂或多种腐蚀抑制剂的混合物。在此范围之内,要求腐蚀抑制剂量等于或大于0.001重量%,较好大于或等于0.05重量%。还要求在此范围内的量小于或等于4重量%,较好,小于或等于1重量%。优选的腐蚀抑制剂是苯并三唑(BTA)。在一个实施方式中,抛光组合物可以含有较大量的BTA抑制剂,以便降低互连的除去速率。当BTA浓度大于0.05重量%时,不需要添加其它的腐蚀抑制剂。BTA的优选浓度是0.0025-2重量%。
除了腐蚀抑制剂外,溶液还可以包含0-20重量%非铁金属的络合剂。存在络合剂时,能防止溶解非铁金属互连而形成的金属离子的沉淀。最好,溶液含有0-10重量%非铁互连金属的络合剂。络合剂的例子有:乙酸、柠檬酸、乙酰乙酸乙酯、乙醇酸、乳酸、苹果酸、草酸、水杨酸、二硫代氨基甲酸二乙酯钠、琥珀酸、酒石酸、硫基乙醇酸、氨基乙酸、丙氨酸、天冬氨酸、乙二胺、三甲基二胺、丙二酸、戊二酸、3-羟基丁酸、丙酸、邻苯二甲酸、间苯二甲酸、3-羟基水杨酸、3,5-二羟基水杨酸、五棓子酸、葡糖酸、邻苯二酚、焦棓酚、丹宁酸,以及它们的盐和它们的混合物。较好的是,络合剂选自乙酸、柠檬酸、乙酰乙酸乙酯、乙醇酸、乳酸、苹果酸、草酸以及它们的混合物中的至少一种。最好是柠檬酸。
虽然含氮抛光剂能提供有效的不含磨料的抛光液体,但在某些应用中需要在抛光流体中加入磨料。抛光组合物可以任选含有至多50重量%(较好,0-40重量%)的磨料,用以促进阻挡物除去或组合的阻挡物和二氧化硅的除去,取决于集成形式,抛光组合物可以用来:i)除去在阻挡层下面的掩模层或膜;或ii)先除去阻挡层,然后除去含氧化硅的层。抛光组合物任选包含用来“机械”除去阻挡层的磨料。磨料优选是胶态磨料。磨料的例子包括:无机氧化物、金属硼化物、金属碳化物、金属氮化物、聚合物以及含有前述的至少一种的混合物的颗粒。合适的无机氧化物包括,例如二氧化硅(SiO2)、三氧化二铝(Al2O3)、二氧化锆(ZrO2)、二氧化铈(CeO2)、二氧化锰(MnO2)或含有前述至少一种氧化物的混合物。如果需要还可以使用这些无机氧化物的改性形式,如涂敷聚合物的无机氧化物颗粒和涂敷无机物的颗粒。合适的金属碳化物、硼化物和氮化物包括例如碳化硅、氮化硅、碳氮化硅(SiCN)、碳化硼、碳化钨、碳化锆、硼化铝、碳化钽、碳化钛或包含至少一种前述金属碳化物、硼化物和氮化物的组合。如果需要,也可以使用金刚石作为磨料。其它磨料有聚合物颗粒和涂敷聚合物的颗粒。优选的磨料是二氧化硅。
较好的是,磨料的含量是0.05-15重量%。在此范围之内,要求磨料含量大于或等于0.1重量%,较好大于或等于0.5重量%。还要求在此范围之内,小于或等于10重量%,较好小于或等于5重量%。
为防止过度的金属凹陷现象和介电体磨蚀,磨料的平均粒度小于或等于150纳米(nm)。为本说明书目的,粒度指磨料的平均粒度。要求使用平均粒度小于或等于100nm,较好小于或等于50nm的胶态磨料。使用平均粒度小于或等于40nm的胶态二氧化硅时,发生的介电体磨蚀和金属凹陷很轻微。胶态磨料的粒度减小至小于或等于40nm会提高抛光组合物的选择性;但是也会降低阻挡物的除去速率。此外,优选的胶态磨料可以包含添加剂,如分散剂、表面活性剂和缓冲剂,用以提高胶态磨料在酸性pH范围的稳定性。这样的一种胶态磨料是来自ClariantS.A.,of Puteaux,France的胶态磨料。化学机械抛光平面化组合物还可以包含光亮剂如氯化铵,pH缓冲剂、抗微生物剂和消泡剂。
如果抛光组合物不含磨料,则抛光垫的选择和调节对化学机械平面化(CMP)过程变得更为重要。例如,对某些不含磨料的组合物,使用固定的抛光垫能提高抛光性能。
使用微孔聚氨酯抛光垫,在测得小于13.8kPa垂直于晶片的压力条件下,测出浆料可以提供至少2至1的TaN/CDO选择比。对测定选择比特别有用的抛光垫是微孔聚氨酯抛光垫,如IC1000TM抛光垫(Rohm and Haas Electronic MaterialsCMP Technology销售)。较好的是,在测得小于13.8kPa垂直于晶片的压力下,用微孔聚氨酯抛光垫测定,浆料可以提供至少3至1的TaN/CDO选择比;最好为至少5至1的TaN/CDO选择比。调节表面活性剂浓度、浆料pH、氧化剂浓度和钽除去剂浓度,可以调节选择比。选择抑制剂、氧化剂、络合剂可以调节互连金属的除去速率。
实施例
所有试验采用200mm晶片,在室温进行。试验采用下面的晶片;TEOS SiO2、电镀铜、CDO(碳掺杂的低k-晶片,由SemiTech制造)、氮化钽、钽、SiCN和SiN。
使用IC1000或Politex抛光垫(Rohm and Haas Electronic Materials CMPTechnology制造),在Strasbaugh 6EC上进行抛光。除非特别指出,向下的抛光力为2psi(13.8kPa)。Kinik金刚石调节磨盘(“1508070”150微米金刚石粒度,80微米的突起高度和70微米间距)保持抛光垫的表面粗糙度。面板和载体的速度分别为120和114rpm。浆料流量为200ml/min。由抛光前后的膜厚度差除以抛光时间计算出除去速率。用Wave Optiprobe 2600,并使用绘制49个位置点来测定TEOS、CDO、SiCN和SiN的厚度。在CDE上,并采用绘制91个位置点来测定氮化钽、钽和铜的厚度。列出的所有除去速率单位都是/min。抛光时间为60秒,但对除去速率小的抛光制剂,时间延长到120秒,用以提高精确性。
在本说明书中,字母代表比较例,数字代表本发明。表1包含0.00005-0.01重量%聚乙二醇醚硫酸盐的除去阻挡的浆料配方。
表1
浆料 | BTA(重量%) | 柠檬酸(重量%) | 二氧化硅(重量%) | 硫酸氢胍(重量%) | 抗微生物剂(重量%) | pH | 聚乙二醇醚硫酸盐(重量%) |
A | 0.1 | 0.5 | 12 | 1 | 0.01 | 9 | 0 |
1 | 0.1 | 0.5 | 12 | 1 | 0.01 | 9 | 0.00005 |
2 | 0.1 | 0.5 | 12 | 1 | 0.01 | 9 | 0.0001 |
3 | 0.1 | 0.5 | 12 | 1 | 0.01 | 9 | 0.0003 |
4 | 0.1 | 0.5 | 12 | 1 | 0.01 | 9 | 0.0007 |
5 | 0.1 | 0.5 | 12 | 1 | 0.01 | 9 | 0.001 |
6 | 0.1 | 0.5 | 12 | 1 | 0.01 | 9 | 0.003 |
7 | 0.1 | 0.5 | 12 | 1 | 0.01 | 9 | 0.006 |
8 | 0.1 | 0.5 | 12 | 1 | 0.01 | 9 | 0.01 |
BTA=苯并三唑;二氧化硅是Klebosol II,平均粒度50nm,AZ Electroic Materials制造;聚乙二醇醚硫酸盐=Disponil FES 77IS,由Cognis/Chemicals Group制造,具有R(EO)33SO3Na的名义组成,其中R是脂肪醇,EO是环氧乙烷;抗微生物剂是NEOLONETM,由Rohm and Haas Company制造,具有50.0-52.0%甲基-4-异噻唑啉-3-酮、45.0-47.0%丙二醇和<3%相关反应产物。
表2列出使用表1抛光溶液时的抛光除去速率(/min)。
表2
1 psi(6.9kPa) | 2 ps(13.8kPa) | |||||||||
浆料 | CDO | TaN | TEOS | Cu | SiCN | CDO | TaN | TEOS | Cu | SiCN |
A | 1248 | 930 | 490 | 31 | 806 | 2673 | 1484 | 960 | 61 | 1566 |
1 | 763 | 950 | 471 | 46 | 749 | 2329 | 1575 | 1008 | 59 | 1513 |
2 | 704 | 944 | 480 | 37 | 822 | 2173 | 1593 | 1001 | 69 | 1616 |
3 | 231 | 961 | 459 | 34 | 833 | 720 | 1551 | 1019 | 58 | 1577 |
4 | 76 | 928 | 466 | 35 | 561 | 144 | 1586 | 1015 | 56 | 1444 |
5 | 80 | 1494 | 839 | 42 | ||||||
6 | 36 | 1524 | 697 | 44 | ||||||
7 | 20 | 1392 | 657 | 21 | ||||||
8 | 15 | 1365 | 591 | 41 |
CDO=Novellus的CORAL碳掺杂氧化物
正方形例子表示未测试
表2表明,少量聚乙二醇硫酸盐对碳掺杂氧化物的除去速率有较大作用,而对其它材料层的除去速率没有明显的作用。阴离子部分有排斥带负电的二氧化硅表面的作用,能进一步提高选择性和限制表面活性剂和磨料之间的相互作用。此外,胍提高了TaN和SiCN的除去速率。
表3提供一组试验用的不含胍浆料。
表3
浆料 | BTA(重量%) | 抗微生物剂(重量%) | 二氧化硅(重量%) | pH | 聚乙二醇醚硫酸盐(重量%) |
9 | 0.10 | 0.01 | 12.0 | 9 | 0.06 |
10 | 0.10 | 0.01 | 12.5 | 9 | 0.06 |
11 | 0.10 | 0.01 | 13.0 | 9 | 0.06 |
12 | 0.10 | 0.01 | 11.5 | 9 | 0.06 |
13 | 0.10 | 0.01 | 11.0 | 9 | 0.06 |
14 | 0.10 | 0.01 | 12.0 | 9 | 0.03 |
15 | 0.10 | 0.01 | 12.0 | 9 | 0.05 |
16 | 0.10 | 0.01 | 12.0 | 9 | 0.07 |
BTA=苯并三唑;抗微生物剂=Kordek MLXTM,由Rohm and Haas Company制造,9.5-9.9%甲基-4-异噻唑啉-3-酮,89.1-89.5%水和≤1.0的相关反应产物;二氧化硅是Klebosol II,平均粒度50nm,AZ Electroic Materials制造;聚乙二醇醚硫酸盐=Disponil FES 77IS,由Cognis/Chemicals Group制造,具有R(EO)33SO3Na的名义组成,其中R是脂肪醇,EO是环氧乙烷。
表4列出试验表1抛光溶液时的抛光除去速率(/min)。
表4
浆料 | TaN | TEOS | CDO | SiCN | Cu | SiN | Ta |
9 | 1799 | 478 | -12 | 57 | 37 | 278 | 573 |
10 | 1795 | 570 | -19 | 66 | 38 | 328 | 582 |
11 | 1586 | 720 | -13 | 85 | 167 | 435 | 571 |
12 | 1776 | 614 | -9 | 69 | 145 | 349 | 563 |
13 | 1773 | 586 | -17 | 73 | 23 | 327 | 556 |
14 | 1704 | 710 | -9 | 129 | 14 | 385 | 520 |
15 | 1571 | 768 | -9 | 98 | 84 | 416 | 527 |
16 | 1616 | 708 | -49 | 84 | 13 | 399 | 510 |
CDO=Novellus的CORAL碳掺杂氧化物
表4表明,少量聚乙二醇醚硫酸盐能有效地防止对碳掺杂氧化物层上的抛光除去作用,对CDO的除去速率为负数并不表明CDO层的生长,而是表明CDO的除去速率小于设备能检测极限。此外,这些数据证实,胍是对溶液除去其它层如阻挡层能力的任选组分。
表5列出使用各种二氧化硅磨料并用硝酸调小pH的溶液的抛光除去速率(/min)。
表5
浆料 | BTA(重量%) | 柠檬酸(重量%) | pH | PEGS(重量%) | TaN | TEOS | CDO | SiCN | Cu | SiN | Ta |
17 | 0.1 | 12 | 9 | 0.06 | 1779 | 467 | 9 | 55 | 97 | 258 | 567 |
18 | 0.1 | 12 | 7 | 0.06 | 1584 | 400 | 19 | 207 | 29 | 283 | 486 |
19 | 0.1 | 12 | 5 | 0.06 | 1116 | 308 | 47 | 809 | 88 | 401 | 261 |
20 | 0.1 | 12 | 3 | 0.06 | 1008 | 402 | 100 | 1225 | 96 | 546 | 643 |
21 | 0.1 | 8 | 9 | 0.06 | 1766 | 202 | 23 | 25 | 55 | 128 | 135 |
22 | 0.1 | 8 | 7 | 0.06 | 1559 | 183 | 32 | 68 | -18 | 135 | 320 |
23 | 0.1 | 8 | 5 | 0.06 | 1168 | 140 | 21 | 374 | 9 | 230 | 3 |
24 | 0.1 | 8 | 3 | 0.06 | 872 | 178 | 30 | 764 | 116 | 457 | 557 |
25 | 0.1 | 4 | 5 | 0.06 | 48 | 59 | -3 | 47 | 85 | 126 | 2 |
26 | 0.1 | 4 | 3 | 0.06 | 773 | 111 | -14 | 260 | 65 | 513 | 605 |
所有溶液含有0.01重量%Kordek MLXTM抗微生物剂,由Rohm and Haas Company制造,9.5-9.9%甲基-4-异噻唑啉-3-酮,89.1-89.5%水和≤1.0的相关反应产物;BTA=苯并三唑;二氧化硅是Klebosol II,平均粒度50nm,AZ Electroic Materials制造;PEGS(聚乙二醇醚硫酸盐)=Disponil FES 77IS,由Cognis/Chemicals Group制造,具有R(EO)33SO3Na的名义组成,其中R是脂肪醇,EO是环氧乙烷;CDO=Novellus的CORAL碳掺杂氧化物。
表5表明,虽然聚乙二醇醚硫酸盐随pH值减小而失去部分有效性,但是该溶液在碱性和酸性时溶液都能减小对碳掺杂氧化物的除去速率。此外,聚乙二醇醚硫酸盐对低浓度和高浓度二氧化硅磨料情况下都有效。
此外,所述溶液和方法对除去钽阻挡材料如钽、氮化钽和氧化钽以及遮盖层如氮化硅和氧化硅都能提供优良的选择性,同时不会除去碳掺杂氧化物层。此外,所述溶液能选择性地除去阻挡层、遮盖层、介电层、逆反射层以及硬掩模,以降低或消除介电质磨蚀。
Claims (10)
1.一种用来在低-k介电体存在情况下进行选择性除去的水溶液,该溶液包含0-25重量%氧化剂;0.00002-5重量%多组分表面活性剂,该多组分表面活性剂具有疏水性尾部、非离子亲水性部分和阴离子亲水性部分,疏水性尾部具有6-30个碳原子,非离子亲水性部分具有10-300个碳原子;0-15重量%对非铁金属的抑制剂;0-50重量%磨料;0-20重量%非铁金属的络合剂;以及水。
2.如权利要求1所述的溶液,其特征在于,非离子亲水性部分含有聚环氧乙烷。
3.如权利要求1所述的溶液,其特征在于,阴离子部分含有羧酸、磺酸、硫酸、膦酸、及其盐和它们的混合物中的至少一种。
4.一种用来在低-k介电体存在情况下进行选择性除去的水溶液,该溶液包含0-20重量%氧化剂;0.00005-2重量%多组分表面活性剂,该多组分表面活性剂具有疏水性尾部、非离子亲水性部分和阴离子亲水性部分,疏水性尾部具有8-20个碳原子,非离子亲水性部分具有20-200个碳原子;0.001-15重量%对非铁金属的抑制剂;0-40重量%磨料;0-10重量%非铁金属的络合剂;以及水。
5.如权利要求4所述的溶液,其特征在于,非离子亲水性部分含有聚环氧乙烷。
6.如权利要求4所述的溶液,其特征在于,阴离子部分含有羧酸、磺酸、硫酸、膦酸、及其盐和它们的混合物中的至少一种。
7.如权利要求4所述的溶液,其特征在于,所述溶液包含0.1-10重量%阻挡物除去剂,所述阻挡物除去剂选自亚胺衍生物化合物、肼衍生物化合物以及它们的混合物。
8.如权利要求4所述的溶液,其特征在于,所述疏水性部分含有12-16个碳原子,非离子部分含有25-150个碳原子。
9.一种从半导体基板上除去一层的至少一部分的方法,该方法包括用一种抛光溶液抛光半导体基板的步骤,所述抛光溶液包含:0-25重量%氧化剂;0.00002-5重量%多组分表面活性剂,该多组分表面活性剂具有疏水性尾部、非离子亲水性部分和阴离子亲水性部分,疏水性尾部具有6-30个碳原子,非离子亲水性部分具有10-300个碳原子;0-15重量%对非铁金属的抑制剂;0-50重量%磨料;0-20重量%非铁金属的络合剂;以及水。
10.如权利要求9所述的方法,其特征在于,所述抛光停止在碳掺杂氧化物层。
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2004
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-
2005
- 2005-12-06 DE DE102005058271A patent/DE102005058271A1/de not_active Ceased
- 2005-12-08 TW TW094143315A patent/TWI374172B/zh active
- 2005-12-15 KR KR1020050123712A patent/KR101107638B1/ko active IP Right Grant
- 2005-12-22 JP JP2005369099A patent/JP2006196887A/ja active Pending
- 2005-12-22 FR FR0513118A patent/FR2879618B1/fr not_active Expired - Fee Related
- 2005-12-22 CN CNB2005101361633A patent/CN100378188C/zh active Active
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CN101372089B (zh) * | 2006-12-21 | 2011-07-06 | 杜邦纳米材料气体产品有限公司 | 在化学机械抛光期间调节低k对铜除去速率的方法和浆料 |
CN101225282B (zh) * | 2007-01-19 | 2013-05-01 | 安集微电子(上海)有限公司 | 一种低介电材料抛光液 |
CN101358109B (zh) * | 2007-08-03 | 2012-01-11 | 罗门哈斯电子材料Cmp控股股份有限公司 | 用来除去聚合物阻挡层的抛光浆液 |
CN101358108B (zh) * | 2007-08-03 | 2012-02-01 | 罗门哈斯电子材料Cmp控股股份有限公司 | 选择性阻挡层抛光浆液 |
CN102061132A (zh) * | 2009-11-12 | 2011-05-18 | 罗门哈斯电子材料Cmp控股股份有限公司 | 化学机械抛光组合物及其相关方法 |
CN105264117A (zh) * | 2013-03-15 | 2016-01-20 | 嘉柏微电子材料股份公司 | 用于铜后化学机械平坦化的含水清洗组合物 |
TWI701323B (zh) * | 2018-10-31 | 2020-08-11 | 南韓商榮昌化工股份有限公司 | 用於研磨銅阻障層的漿料組成物 |
Also Published As
Publication number | Publication date |
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US20060131275A1 (en) | 2006-06-22 |
US7790618B2 (en) | 2010-09-07 |
KR20060071875A (ko) | 2006-06-27 |
TWI374172B (en) | 2012-10-11 |
FR2879618B1 (fr) | 2010-06-25 |
JP2006196887A (ja) | 2006-07-27 |
TW200626690A (en) | 2006-08-01 |
KR101107638B1 (ko) | 2012-01-25 |
CN100378188C (zh) | 2008-04-02 |
DE102005058271A1 (de) | 2006-07-13 |
FR2879618A1 (fr) | 2006-06-23 |
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