WO2012071780A1 - 一种化学机械抛光浆料 - Google Patents
一种化学机械抛光浆料 Download PDFInfo
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- WO2012071780A1 WO2012071780A1 PCT/CN2011/001767 CN2011001767W WO2012071780A1 WO 2012071780 A1 WO2012071780 A1 WO 2012071780A1 CN 2011001767 W CN2011001767 W CN 2011001767W WO 2012071780 A1 WO2012071780 A1 WO 2012071780A1
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- Prior art keywords
- acid
- chemical mechanical
- mechanical polishing
- polishing slurry
- slurry according
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- 239000003899 bactericide agent Substances 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000012468 concentrated sample Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000004312 hexamethylene tetramine Substances 0.000 description 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 1
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 1
- 229960001340 histamine Drugs 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 150000003009 phosphonic acids Chemical class 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
- 238000001039 wet etching Methods 0.000 description 1
Classifications
-
- 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
- H01L21/3205—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]
Definitions
- the present invention relates to a chemical mechanical polishing slurry, and more particularly to a chemical mechanical polishing slurry for copper.
- the chemical mechanical polishing process of copper is generally divided into three steps.
- the first step is to remove a large amount of copper on the surface of the substrate with a high and low removal rate with a high downforce.
- the second step is to approach the barrier layer. When the downforce is reduced, the removal rate is reduced to polish the remaining metal copper and stopped at the barrier layer.
- step 3 the barrier layer and the partial dielectric layer and the metal copper are removed by the barrier polishing solution to achieve planarization.
- Chemical mechanical polishing fluids are used in both steps 1 and 2.
- copper polishing should remove excess copper on the barrier layer as soon as possible.
- the butterfly depression of the polished copper wire should be minimized.
- the copper wire is partially recessed before the copper is polished.
- polishing the copper on the dielectric material is easily removed (higher) under the body pressure, and the copper in the depression is subjected to polishing pressure than the main The body pressure is low and the copper removal rate is small. Therefore, in the copper polishing liquid, how to control the polishing rate of the polishing liquid under high down pressure and low down pressure is very critical. As the polishing progresses, the height difference of the copper is gradually reduced, and if the rate difference between the high and low pressures is too small, the butterfly depression is likely to increase.
- US Patent No. 6616717B2 discloses a composition for metal CMP, including an aqueous medium, an oxidizing agent and an organic polymer, and may also include a dispersing agent. The composition is capable of adjusting the rate of removal of the oxide layer;
- US Pat. No. 6,821,897 B2 discloses a method of copper CMP using a polymer complexing agent comprising a negatively charged polymer or copolymer, by polarity Change to adjust the removal rate;
- Chinese patent CN1459480A discloses a copper chemical-mechanical polishing process polishing solution, including a film former, a film forming aid and an abrasive.
- the film forming agent is a buffer composed of a strong alkali and acetic acid, corrosive.
- Small, improved polishing effect Chinese patent CN1256765C discloses a slurry for chemical mechanical polishing of copper, including a chelating organic acid buffer system such as citric acid (potassium), or adding an oxidizing agent, an etchant, etc., which can increase the copper removal rate. Up to 3000 angstroms per minute;
- Chinese patent CN1195896C discloses a CMP slurry manufacturing for copper and for integration A method of manufacturing a road, the polishing slurry comprising an oxidant, carboxylates, and triazole or triazole derivative, the slurry having good oxide selectivity.
- the polishing slurry for copper in the above patented technology has many problems, such as: the polishing speed is not fast enough, and the surface of the substrate after use is defective, scratched, stained, and the depression of the copper after the copper is excessively large. Therefore, it is necessary to develop new chemistry for copper. Summary of invention
- the object of the present invention is to overcome the deficiencies in the prior art and to provide a high downforce There is a higher copper removal rate, and the copper removal rate is lower at low down pressure, and the chemical mechanical polishing slurry of the butterfly depression of the polished copper wire can be improved.
- the polishing slurry provided by the present invention contains at least
- the slurry further contains abrasive particles, a complexing agent, and an oxidizing agent.
- the use of the slurry of the present invention maintains a high copper removal rate and improves the polished dishing after polishing.
- the chemical mechanical polishing paddle of the present invention comprises abrasive particles, a complexing agent, an oxidizing agent, and further comprises 5-phenyltetrazolium.
- the content of the 5-phenyltetrazole is preferably 0.001 wt% to 1 wt%, and further preferably 0.005 wt% to 0.1 wt%. Where wt% is the mass percentage.
- the abrasive particles described in the present invention may be a mixture of one or more of silica, alumina, doped aluminum or aluminum-coated silica, ceria, titania, polymer abrasive particles, and preferably It is silica.
- the mass percentage of the abrasive particles is preferably from 0.1 wt% to 20 w%; more preferably from 0.1 wt% to 10 wt%.
- the abrasive particles preferably have a particle diameter of 20 to 150 nm.
- the complexing agent described in the present invention may be an aminocarboxy complex and a salt thereof, an organic carboxylic acid and a salt thereof, an organic phosphonic acid, and a salt thereof.
- the aminocarboxy complex is glycine, alanine, valine, leucine, cephaline, phenylalanine, tyrosine, tryptophan, lysine, arginine, histamine Acid, serine, threonine, aspartic acid, glutamic acid, asparagine, glutamine, ammonia triacetic acid, ethylenediaminetetraacetic acid, cyclohexanetetraacetic acid, ethylenediamine disuccinic acid, diethylene three One or more of amine pentaacetic acid and triethylenetetramine hexaacetic acid;
- the organic carboxylic acid is acetic acid, oxalic acid, citric acid, tartaric acid, malonic acid, succinic acid, malic acid
- the mass percentage of the complexing agent is preferably 0.01 wt% to 10 wt%.
- the oxidizing agent described in the present invention may be hydrogen peroxide, urea peroxide, peroxyformic acid, peracetic acid, persulfate, percarbonate, periodic acid, perchloric acid, perboric acid, potassium permanganate, and One or more of ferric nitrate.
- the mass percentage of the oxidizing agent is preferably from 0.1 wt% to 10 wt%.
- the pH of the polishing liquid is preferably from 3 to 11, more preferably from 4 to 8.
- the polishing liquid of the present invention may further contain other conventional additives such as pH adjusters, viscosity modifiers, antifoaming agents, and bactericides in the art.
- the polishing liquid of the present invention can prepare a concentrated sample which is diluted with deionized water and added with an oxidizing agent before use.
- the positive progress of the present invention is that the polishing liquid of the present invention has a high removal rate under high down pressure, and the removal rate is low at low pressure, and the butterfly depression is small after polishing.
- the chemical mechanical polishing slurry of the present invention comprises abrasive particles, an oxidizing agent, a complexing agent and 5-phenyltetrazolium.
- the pH of the slurry is preferably from 3 to 11; and the content of 5-phenyltetrazole is preferably from 0.001 to 1% by weight.
- the abrasive particles may be selected from the group consisting of silica, alumina, doped aluminum, aluminum-coated silica, ceria, titania, polymer abrasive particles, or a mixture of several.
- the average diameter thereof is preferably from 20 to 150 nm, and the amount is in the range of from 0.1 wt% to 20 wt%.
- the complexing agent may be selected from the group consisting of aminocarboxylates and salts thereof, organic carboxylic acids and salts thereof, organic phosphonic acids and salts thereof, in amounts ranging from 0.01 wt% to 10 wt%.
- aminocarboxy complexes such as: glycine, alanine, valine, leucine, valine, phenylalanine, tyrosine, tryptophan, lysine, arginine, group Amino acid, serine, threonine, aspartic acid, glutamic acid, asparagine, glutamine, ammonia triacetic acid, ethylenediaminetetraacetic acid, cyclohexyltetraacetic acid, ethylenediamine disuccinic acid, One or more of ethylene triamine pentaacetic acid and triethylene tetraamine hexaacetic acid; the organic carboxylic acid such as: acetic acid, oxalic acid, citric acid, tartaric acid, malonic acid, succinic acid, malic acid, lactic acid, One or more of gallic acid and sulfosalicylic acid; the organic phosphonic acid such as: 2-phosphonium bromide-1, 2, 4-tricar
- the oxidizing agent may be selected from the group consisting of hydrogen peroxide, urea peroxide, peroxyformic acid, peracetic acid, persulfate, percarbonate, periodic acid, perchloric acid, perboric acid, potassium permanganate and ferric nitrate. One or more. The amount is in the range of 0.1 wt% to 10 wt%.
- Table 1 gives a comparison of the comparative polishing slurry 1 to 2 and the polishing composition of the present invention, the components 1 to 3 and the copper removal rate.
- the components other than the oxidizing agent are uniformly mixed. percentage up with water to 100% by mass, adjusted to a desired pH with KOH or HN0 3. Add oxidizing agent before use and mix well.
- the copper (Cu) is polished by using the comparative polishing liquid 1 to 2 and the polishing liquid ⁇ 3 of the present invention.
- the polishing rate is shown in Table 1. Polishing conditions: Copper wafer, 3 psi/psi psi, polishing disc and polishing head speed 70/80 rpm, polishing pad PPG MX710, polishing fluid flow rate 100 ml/min, polishing machine for Logitech PM5 Polisher.
- Table 2 gives a comparison of the components of the comparative polishing liquid 3 and the polishing liquid of the present invention, examples 4 to 5, and the removal rate of copper.
- the components other than the oxidizing agent are uniformly mixed, and water is used. the percentage complement to 100% by mass, adjusted to a desired pH with KOH or HN0 3. Add oxidizing agent before use and mix well.
- the copper (Cu) is polished by using the comparative polishing liquid 3 and the polishing liquid 4 to 5 of the present invention.
- the polishing rate is shown in Table 3. Polishing conditions: copper wafer, downforce 3Psi/1psi, t-disc and polishing head speed 93/87rpm, polishing pad IC1010, polishing solution flow rate 200ml/min, polishing machine 8" Mirra.
- Table 3 gives a comparison of the contrast of the polishing liquid 4 and the polishing liquid of Example 6 of the present invention and the butterfly depression at the polished copper wire.
- the components other than the oxidizing agent are uniformly mixed. percentage up with water to 100% by mass, adjusted to a desired pH with KOH or HN0 3. Add oxidizing agent before use and mix well.
- the patterned copper (Cu) wafer was polished using a comparative polishing liquid 4 and the polishing liquid 6 of the present invention.
- the butterfly depression at 100 X 100 ⁇ m copper wire after polishing is shown in Table 3.
- Polishing conditions patterned copper wafer, 3Psi in the first step, 1 psi in the second step, 93/87 rpm polishing disc and polishing head, polishing pad IC1010, polishing fluid flow rate 200ml/min, polishing machine
- the station is 8" Mirra.
- Table 4 shows the formulation of each component of Examples 7 to 53 of the chemical mechanical polishing slurry of the present invention. According to the formulation given in the table, the components other than the oxidizing agent are uniformly mixed, and the mass percentage is made up to 100% with water. . Adjust to the desired pH with KOH or HNO 3 . Add oxidizing agent before use and mix well. The composition of the components given in Table 4 was also effective in suppressing the removal rate under low pressure and maintaining the removal rate under high pressure.
- the chemical mechanical polishing slurry of the present invention may further comprise additives such as methyl cellulose, polysilicon antifoaming agent, etc., such as the composition of the slurry as follows:
- 5-phenyltetrazole 0.5 wt%; diethylene trife: 0.05 wt% ; perboric acid: 2 wt%; methylcellulose: 0.01 wt% ; polysilicon antifoaming agent: 0.01 wt%;
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- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
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- Mechanical Treatment Of Semiconductor (AREA)
Description
一种化学机械抛光浆料 技术领域
本发明涉及一种化学机械抛光浆料,尤其涉及一种用于铜的化学机械抛 光浆料。
技术背景
随着微电子技术的发展,甚大规模集成电路芯片集成度已达几十亿个元 器件, 特征尺寸己经进入纳米级, 这就要求微电子工艺中的几百道工序, 尤 其是多层布线、 衬底、 介质必须要经过化学机械平坦化。甚大规模集成布线 正由传统的 AI向 Cu转化, 与 AI相比, Cu布线具有电阻率低、抗电迁移能 率高、 RC延迟时间短等优势,已使其替代 AI成为半导体制作中的互联金属。 但是目前却没有对铜材进行有效地等离子蚀刻或湿法蚀刻、以使铜互连在集 成电路中充分形成的技术, 铜的化学机械抛光方法是目前最有效的工艺方 法 · :■■■: · · : ■
铜的化学机械抛光过程一般分为 3个步骤,第 1步是先用较高的下压力, 以快且高效的去除速率除去衬底表面上大量的铜,第 2步是在快要接近阻挡 层时降低下压力, 降低去除速率抛光剩余的金属铜并停在阻挡层, 第 3步再 用阻挡层抛光液去除阻挡层及部分介电层和金属铜, 实现平坦化。 其中第 1 步和第 2步中均使用到化学机械抛光液。
铜抛光一方面要尽快去除阻挡层上多余的铜,另一方面要尽量减小抛光 后铜线的蝶形凹陷。 在铜抛光前, 铜线带有部分凹陷。 抛光时, 介质材料上 的铜在主体压力下(较高)易于被去除, 而凹陷处的铜所受的抛光压力比主
体压力低, 铜去除速率小。 因此, 在铜抛光液中, 如何控制抛光液在高下压 力和低下压力下的抛光速率是非常关键的。 随着抛光的进行, 铜的高度差会 逐渐减小, 如果在高、 低压下的速率差太小, 则容易导致蝶形凹陷增大。
目前, 出现了一系列的适合于抛光 Cu的化学机械抛光浆料, 如: 美国 专利 US6616717B2公开了一种用于金属 CMP的组合物, 包括水介质、 氧 化剂和有机高分子, 还可以包括分散剂, 该组合物能够调节氧化层的去处速 率; 美国专利 US6821897B2公开了一种使用聚合体络合剂的铜 CMP的方 法, 所用浆料包括带负有电荷的聚合物或共聚物, 通过极性的改变来调节去 除速率; 中国专利 CN1459480A公开了一种铜化学一机械抛光工艺用抛光 液, 包括成膜剂、 成膜助剂和磨料, 成膜剂为强碱与醋酸组成的缓冲液, 腐 蚀性小, 改善了抛光效果; 中国专利 CN1256765C公开的铜的化学机械抛 光所用的浆料, 包括柠檬酸 (钾)等螯合有机酸缓冲体系, 或加入氧化剂、 腐 蚀剂等, 能够将铜移除速率提高到大于 3000 埃每分钟; 中国专利 CN1195896C公开了一种用于铜的 CMP浆液制造以及用于集成电路的制造 方法, 所用抛光浆料包括氧化剂、 羧酸盐以及***或***衍生物, 该浆料具 有良好的氧化物选择性。但是上述专利技术中用于铜的抛光浆料存在诸多问 题, 如: 抛光速度不够快, 使用后衬底表面存在缺陷、 划伤、 粘污和铜的残 后铜块的凹陷过大等。 因此有必要开发出新的用于铜的化学
发明概要
本发明的目的是克服现有技术中存在的缺陷,提供一种在高下压力下具
有较高的铜的去除速率, 而在低下压力下铜的去除速率较低, 且可以改善抛 光后铜线的蝶形凹陷的化学机械抛光浆料。本发明提供的抛光浆料至少含有
5-苯基四氮唑, 该浆料还含有研磨颗粒、 络合剂、 氧化剂。 使用本发明的浆 料的可以保持较高的铜的去除速率, 改善抛光后的蝶形凹陷。
本发明化学机械抛光桨料包括研磨颗粒、 络合剂、 氧化剂, 还包括 5- 苯基四氮唑。
其中,所述的 5-苯基四氮唑的含量优选为 0.001 wt%~1 wt%, 并进一步 优选为 0.005 wt%~0.1 wt%。 其中, wt%为质量百分含量。
本发明中所述的研磨颗粒可以是二氧化硅、氧化铝、掺杂铝或覆盖铝的 二氧化硅、 二氧化铈、 二氧化钛、 高分子研磨颗粒中的一种或几种的混合, 并优选为二氧化硅。
其中, 所述的研磨颗粒的质量百分含量优选为 0.1 wt%-20w %; 更佳 为 0.1 wt%~10 wt%。 所述的研磨颗粒的粒径优选为 20~150nm。
本发明中所述的络合剂可以是氨羧络合物及其盐、有机羧酸及其盐、有 机膦酸及其盐。 所述的氨羧络合物为甘氨酸、 丙氨酸、缬氨酸、 亮氨酸、脑 氨酸、 苯丙氨酸、 酪氨酸、 色氨酸、 赖氨酸、 精氨酸、 组氨酸、 丝氨酸、 苏 氨酸、天冬氨酸、谷氨酸、天冬酰胺、谷氨酰胺、氨三乙酸、 乙二胺四乙酸、 环己 四乙酸、 乙二胺二琥珀酸、二乙烯三胺五乙酸和三乙烯四胺六乙酸中 的一种或多种; 所述的有机羧酸为醋酸、 草酸、 柠檬酸、 酒石酸、 丙二酸、 丁二酸、 苹果酸、 乳酸、 没食子酸和磺基水杨酸中的一种或多种; 所述的有 机膦酸为 2-膦酸丁垸 -1, 2, 4-三羧酸、 氨基三甲叉膦酸、 羟基乙叉二膦酸、 乙二胺四甲叉膦酸、 二乙烯三胺五甲叉膦酸、 2-羟基膦酸基乙酸、 乙二胺四
甲叉膦酸和多氨基多醚基甲叉膦酸中的一种或多种; 所述的盐可以是铵盐、 钾盐和钠盐。
其中, 所述的络合剂的质量百分含量优选为 0.01 wt%〜10wt%。
本发明中所述的氧化剂可以是过氧化氢、过氧化脲、 过氧甲酸、 过氧乙 酸、 过硫酸盐、 过碳酸盐、 高碘酸、 高氯酸、 高硼酸、 高锰酸钾和硝酸铁中 的一种或多种。
其中, 所述的氧化剂的质量百分含量优选为 0.1 wt%~10 wt%。
其中, 所述的抛光液的 pH优选为 3〜11, 进一步优选为为 4~8。
本发明的抛光液中,还可以含有本领域其他常规 ¾加剂,如 pH调节剂、 粘度调节剂、 消泡剂和杀菌剂等。
本发明的抛光液可制备浓缩样品,在使用前用去离子水稀释并加入氧化 剂。
本发明的积极进步效果在于:本发明的抛光液在高下压力下具有较高的 去除速率, 而在低压力下去除速率较低, 抛光后蝶形凹陷小。 发明内容
本发明化学机械抛光浆料, 包括了研磨颗粒、氧化剂、络合剂和 5-苯基 四氮唑。 其中, 所述浆料 PH值优选为 3〜11; 5-苯基四氮唑的含量优选为 0.001〜1 wt%。
所述研磨颗粒可以选自二氧化硅、氧化铝、掺杂铝、覆盖铝的二氧化硅、 二氧化铈、 二氧化钛、 高分子研磨颗粒中的一种或几种的混合。 其平均直径 优选为 20~150nm, 用量在 0.1 wt%~20wt%范围内。
所述络合剂可以选自氨羧络合物及其盐、 有机羧酸及其盐、 有机膦酸及 其盐, 其用量在 0.01 wt%~10wt%范围内。 所述的氨羧络合物如: 甘氨酸、 丙氨酸、 缬氨酸、 亮氨酸、 脯氨酸、 苯丙氨酸、 酪氨酸、 色氨酸、 赖氨酸、 精氨酸、 组氨酸、 丝氨酸、 苏氨酸、 天冬氨酸、 谷氨酸、 天冬酰胺、 谷氨酰 胺、 氨三乙酸、 乙二胺四乙酸、 环己垸四乙酸、 乙二胺二琥珀酸、 二乙烯三 胺五乙酸和三乙烯四胺六乙酸中的一种或多种; 所述的有机羧酸如: 醋酸、 草酸、 柠檬酸、 酒石酸、 丙二酸、 丁二酸、 苹果酸、 乳酸、 没食子酸和磺基 水杨酸中的一种或多种; 所述的有机膦酸如: 2-膦酸丁垸 -1, 2, 4-三羧酸、 氨基三甲叉膦酸、 羟基乙叉二膦酸、 乙二胺四甲叉膦酸、 二乙烯三胺五甲叉 膦酸、 2-羟基膦酸基乙酸、 乙二胺四甲叉膦酸和多氨基多醚基甲叉膦酸中的 一种或多种; 所述的盐可以是铵盐、 钾盐和钠盐。
所述氧化剂可以选自过氧化氢、 过氧化脲、 过氧甲酸、 过氧乙酸、 过硫 酸盐、 过碳酸盐、 高碘酸、 高氯酸、 高硼酸、 高锰酸钾和硝酸铁中的一种或 多种。 其用量在 0.1 wt%~10wt %范围内。
下面用实施例来进一步说明本发明, ¾本发明保护范围弁不受其限制。 效果对比 1
表 1给出了对比抛光浆料 1〜2和本发明的抛光浆料实施例 1~3组分及 铜去除速率对比, 按表中所给配方, 将除氧化剂以外的其他组分混合均匀, 用水补足质量百分比至 100%, 用 KOH 或 HN03调节到所需要的 pH值。 使用前加氧化剂, 混合均匀即可。
采用对比抛光液 1~2和本发明的抛光液〜 3, 对空片铜(Cu)进行抛光。 抛光速率见表 1。
抛光条件: 铜晶片, 下压力 3psi/1 psi, 抛光盘及抛光头转速 70/80rpm, 抛光垫 PPG MX710, 抛光液流速 100ml/min, 抛光机台为 Logitech PM5 Polisher。
由表 1可见, 与未添加腐蚀抑制剂的对比例 1相比, 实施例 1~3中添 加了 5-苯基四氮唑为腐蚀抑制剂后,能较好的抑制铜在低下压力下的去除速 率, 有利于降低在有图案的铜晶片上的凹陷, 而在高压力下能保持较高的铜 去除速率, 能保持较高的产能。而添加腐蚀抑制剂苯并三氮唑的对比例 2虽 然在低压下具有较低的去除速率, 但高压力下的去除速率也很低, 生产能力 大大降低。 ' 对比抛光液 1~2和本发明抛光液实施例 1~3的铜去除速率
效果对比 2 表 2给出了对比抛光液 3和本发明的抛光液实施例 4~5组分和铜去除 速率对比, 按表中所给配方, 将除氧化剂以外的其他组分混合均匀, 用水补 足质量百分比至 100%, 用 KOH 或 HN03调节到所需要的 pH值。 使用前 加氧化剂, 混合均匀即可。
对比抛光液 3和本发明抛光液实施例 4~5的铜去除速率
采用对比抛光液 3和本发明的抛光液 4~5, 对空片铜 (Cu)进行抛光。 抛光速率见表 3。抛光条件: 铜晶片, 下压力 3Psi/1psi, t光盘及抛光头转 速 93/87rpm,抛光垫 IC1010,抛光液流速 200ml/min,抛光机台为 8" Mirra。
由表 3可见, 与添加腐蚀抑制剂 1, 2, 4-三氮唑的对比例 3相比, 实 施例 4〜5中添加了 5-苯基四氮唑后, 能较好的抑制铜在低下压力下的去除 速率, 有利于降低在有图案的铜晶片上的凹陷, 而在高压力下能保持很高的 铜去除速率, 有利于快速去除大量的铜。
效果对比 3
表 3给出了对比抛光液 4和本发明的抛光液实施例 6组分和抛光后铜线 处的蝶形凹陷对比,按表中所给配方,将除氧化剂以外的其他组分混合均匀, 用水补足质量百分比至 100%, 用 KOH 或 HN03调节到所需要的 pH值。 使用前加氧化剂, 混合均匀即可。
采用对比抛光液 4和本发明的抛光液 6, 对有图形的铜(Cu)晶片进行 抛光。 抛光后在 100 X 100微米的铜线处的蝶形凹陷见表 3。 抛光条件: 有 图形的铜晶片, 第一个步下压力为 3Psi,第二步下压力为 1 psi,抛光盘及抛 光头转速 93/87rpm, 抛光垫 IC1010, 抛光液流速 200ml/min, 抛光机台为 8" Mirra。
表 3 使用对比抛光液 4和本发明抛光液实施例 6的铜蝶形凹陷对比
表 4给出了本发明的化学机械抛光浆料的实施例 7〜53的各组分配方, 按表中所给配方, 将除氧化剂以外的其他组分混合均匀, 用水补足质量百分 比至 100%。 用 KOH 或 HN03调节到所需要的 pH值。 使用前加入氧化剂, 混合均匀即可。按照表 4给出的组分配方同样能够有效抑制低压力压下的去 除速率、 而保持高压力下的去除速率。
表 4 实施例 7~52
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Si02 多乙
(80nm 过氧
49 ) 0.5 1 烯多 3 11
化氢
0.5 胺
Si02 三乙
(80nm 过氧
50 ) 0.02 1 烯四 3 11
化氢
0.5 胺
Si02 四乙
nm 过氧
51 (80 ) 0.01 1 烯五 2 11
化氢
0.5 胺
Si02
52 (80nm) 谷氨 过氧
0.1 0.05 2 10
酰胺 甲酸
0.5
Si02 三乙
(80nm) 烯四 过碳
53 1 0.05 2 10
胺六 酸钠
0.5
乙酸
实施例 54
本发明化学机械抛光浆料, 还可以包括如甲基纤维素、 聚硅垸消泡剂等 添加剂, 如所述浆料组成成分如下:
Si02 (粒径 80nm): 0.5wt%;
5-苯基四氮唑: 0.5wt%; 二乙烯三 fe: 0.05wt%; 高硼酸: 2wt%; 甲基纤维素: 0.01 wt%; 聚硅垸消泡剂: 0.01wt%;
PH: 10。 以上对本发明的具体实施例进行了详细描述,其中未提及的操作方法应 当理解为本技术领域常规操作方法。 上述实施例只是作为范例, 本发明并不 限制于以上描述的具体实施例。 对于本领域技术人员而言, 任何对本发明进
行的等同修改和替代也都在本发明的范畴之中。 因此, 在不脱离本发明的精 神和范围下所作的均等变换和修改, 都应涵盖在本发明的范围内。
Claims
1 . 一种化学机械抛光浆料, 其特征在于, 至少含有 5-苯基四氮唑、 研 磨颗粒、 络合剂和氧化剂。
2. 根据权利要求 1所述的化学机械抛光浆料, 其特征在于, 所述的 5- 苯基四氮唑的质量百分含量为 0.001~1 wt%
3. 根据权利要求 2所述的化学机械抛光浆料, 其特征在于, 所述的 5- 苯基四氮唑的质量百分含量为 0.005~0.1 wt%。
4. 根据权利要求 1所述的化学机械抛光浆料, 其特征在于, 所述的研 磨颗粒为二氧化硅、 氧化铝、 掺杂铝或覆盖铝的二氧化硅、 二氧化铈、 二氧 化钛、 高分子研磨颗粒中的一种或几种的混合。
5. 根据权利要求 4所述的化学机械抛光浆料, 其特征在于, 所述的研 磨颗粒的质量百分含量为 0.1〜20 %。
6. 根据权利要求 5所述的化学机械抛光浆料, 其特征在于, 所述的研 磨颗粒的质量百分含量为 0.1〜10%。
. 根据权利要求 4所述的化学机械抛光浆料, 其 征在于, 所述的研 磨颗粒的平均粒径为 20〜: I50nm。
8. 根据权利要求 1所述的化学 械拋光浆枓, 其特征在于, 所述的络 合剂为氨羧络合物、 有机羧酸、 有机膦酸、 及上述化合物的盐中的一种或几 种的混合。
9. 根据权利要求 8所述的化学机械抛光浆料, 其特征在于, 所述的氨 羧络合物选自甘氨酸、 丙氨酸、 缬氨酸、 亮氨酸、 脯氨酸、 苯丙 酸、 酪氨 酸、 色氨酸、 赖氨酸、 精氨酸、 组氨酸、 丝氨酸、 苏氨酸、天冬氨酸、 谷氨 酸、 天冬酰胺、 谷氨酰胺、 氨三乙酸、 乙二胺四乙酸、 环己垸四乙酸、 乙二 胺二琥珀酸、 二乙烯三胺五乙酸和三乙烯四胺六乙酸中的一种或多种; 所述 的有机羧酸选自醋酸、 草酸、 柠檬酸、 酒石酸、 丙二酸、 丁二酸、 苹果酸、 乳酸、没食子酸和磺基水杨酸中的一种或多种; 所述的有机膦酸选自 2-膦酸 丁垸 -1, 2, 4-三羧酸、 氨基三甲叉膦酸、 羟基乙叉二膦酸、 乙二胺四甲叉膦 酸、 二乙烯三胺五甲叉膦酸、 2-羟基膦酸基乙酸、 乙二胺四甲叉膦酸和多氨 基多醚基甲叉膦酸中的一种或多种。 所述的盐为铵盐、 钾盐及钠盐。
10. 根据权利要求 8或 9所述的化学机械抛光浆料, 其特征在于, 所述 的络合剂的质量百分含量为 0.01〜10%。
11 . 根据权利要求 1所述的化学机械抛光浆料, 其特征在于, 所述的氧 化剂选自过氧化氢、过氧化脲、过氧甲酸、过氧乙酸、过硫酸盐、过碳酸盐、 高碘酸、 高氯酸、 高硼酸、 高锰酸钾和硝酸铁中的一种或多种。
12. 根据权利要求 11 所述的化学机械抛光浆料, 其特征在于, 所述的 氧化剂的质量百分含量为 0.1~10%。
13. 根据权利要求 1所述的化学机械抛光浆料, 其特征在于, ^ff述浆料 PH值为 3〜11。
14. 根据权利要求 13所述的化学机械抛光浆料, 其特征在于, 所述浆 料 PH值为 4〜8。
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