WO2012075687A1 - 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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- WO2012075687A1 WO2012075687A1 PCT/CN2011/002056 CN2011002056W WO2012075687A1 WO 2012075687 A1 WO2012075687 A1 WO 2012075687A1 CN 2011002056 W CN2011002056 W CN 2011002056W WO 2012075687 A1 WO2012075687 A1 WO 2012075687A1
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- WIPO (PCT)
- Prior art keywords
- acid
- polishing slurry
- copper
- slurry according
- polishing
- Prior art date
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- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- DBTDEFJAFBUGPP-UHFFFAOYSA-N Methanethial Chemical compound S=C DBTDEFJAFBUGPP-UHFFFAOYSA-N 0.000 description 1
- VCOYRKXQRUGBKS-UHFFFAOYSA-N N.[Cl] Chemical compound N.[Cl] VCOYRKXQRUGBKS-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- DQRWXBITHVMAPE-UHFFFAOYSA-N [O].[O].[O].[O].C(CN)N Chemical compound [O].[O].[O].[O].C(CN)N DQRWXBITHVMAPE-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000012468 concentrated sample Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency 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
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000001033 ether group Chemical group 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- ZDGGJQMSELMHLK-UHFFFAOYSA-N m-Trifluoromethylhippuric acid Chemical compound OC(=O)CNC(=O)C1=CC=CC(C(F)(F)F)=C1 ZDGGJQMSELMHLK-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 230000011987 methylation Effects 0.000 description 1
- 238000007069 methylation reaction Methods 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- YACKEPLHDIMKIO-UHFFFAOYSA-N methylphosphonic acid Chemical compound CP(O)(O)=O YACKEPLHDIMKIO-UHFFFAOYSA-N 0.000 description 1
- 238000006772 olefination reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- KHIWWQKSHDUIBK-UHFFFAOYSA-N periodic acid Chemical compound OI(=O)(=O)=O KHIWWQKSHDUIBK-UHFFFAOYSA-N 0.000 description 1
- 125000000864 peroxy group Chemical group O(O*)* 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- CJNKWHOPRMQSBW-UHFFFAOYSA-N trioxidanylethene Chemical group OOOC=C CJNKWHOPRMQSBW-UHFFFAOYSA-N 0.000 description 1
- 238000006886 vinylation 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
-
- 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 paddle 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 block.
- the layer lowers the downforce, lowers the removal rate, polishes the remaining metal copper and stops at the barrier layer.
- the barrier layer polishing solution is used to remove the barrier layer and part of the dielectric layer and the metal copper to achieve planarization. Copper 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-shaped depression of the polished copper wire should be minimized.
- the copper wire is partially recessed before the copper is polished. When polished, the copper on the dielectric material is easily removed (higher) under the bulk pressure, while the copper in the recess is subjected to a lower polishing pressure than the bulk pressure, and the copper removal rate is small. As the polishing progresses, the height difference of the copper will gradually decrease, and the recognition will be confirmed. flattened.
- the passivation film of copper is easily removed even at a lower pressure (such as a copper line depression), resulting in planarization efficiency. Reduced, the polished butterfly depression increases.
- the polishing slurry for copper described above has a polishing speed that is not fast enough, and there are defects, scratches, stains, and residual copper on the surface of the substrate after use, or the depression of the copper block after polishing is too large, or exists during polishing. Local or overall corrosion and high static corrosion rates of copper at normal temperatures and polishing temperatures (eg, 50 ° C). Therefore, it is necessary to develop a new chemical mechanical polishing paddle for copper. Summary of invention
- the polishing slurry contains at least one phosphate surfactant, and the slurry further contains abrasive particles, a complexing agent, and an oxidizing agent.
- the use of the slurry of the present invention can reduce the static corrosion rate of copper, suppress the removal rate of copper at low pressure, and reduce the dishing of the polished copper block.
- a specific method of the present invention is to add a phosphate surfactant to the polishing slurry, and the phosphate surfactant has the following structure: RO, RO-(CH 2 CH 2 0) n , RCOO-(CH 2 CH 2 0) n ) or a polyol phosphate containing two or more structural formulas 1.
- the content of the phosphate surfactant in the present invention is 0.0005 to 2% by weight, preferably 0.001 to 1% by weight.
- the abrasive particles described in the present invention include silica, alumina, doped aluminum or aluminum-coated silica, ceria, titania and/or polymeric abrasive particles.
- the weight percentage of the abrasive particles is preferably from 0.1 to 20%; more preferably from 0.1 to 10%.
- the abrasive particles have a particle diameter of 20 to 150 nm.
- the complexing agent is an aminocarboxylate compound and a salt thereof, an organic carboxylic acid and a salt thereof, an organic phosphonic acid and a salt thereof, and an organic amine.
- the aminocarboxylate compound is specifically glycine, alanine, valine, leucine, valine, phenylalanine, tyrosine, tryptophan, lysine, arginine, histidine , serine, aspartic acid, glutamic acid, asparagine, glutamine, ammonia triacetic acid, ethylenediaminetetraacetic acid, cyclohexyltetraacetic acid, ethylenediamine disuccinic acid, diethylenetriaminepentaacetic acid and One or more of triethylenetetraamine hexaacetic acid;
- the organic carboxylic acid is acetic acid, oxalic acid, citric acid, tartaric acid, malonic acid, succinic acid, malic acid, lactic acid,
- the salts are potassium, sodium and/or ammonium.
- the content of the complexing agent is 0.01 to 10% by mass.
- the oxidizing agent is 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 content of the oxidizing agent is 0.05 to 10% by mass.
- the polishing liquid of the present invention has a pH of from 3 to 11, preferably from 4 to 8.
- the polishing liquid of the present invention may further contain other conventional additives in the art such as a corrosion inhibitor, a pH adjuster, a viscosity modifier, an antifoaming agent, and a bactericide to achieve a polishing effect.
- the polishing liquid of the present invention can prepare a concentrated sample, which is diluted with deionized water to the concentration range of the present invention and added with an oxidizing agent before use.
- the positive progress of the present invention is that the polishing slurry of the present invention can significantly reduce the static etching rate of copper, suppress the removal rate of copper at low pressure, and reduce the dishing of the copper block after polishing of the pattern wafer.
- Table 1 shows Examples 1 to 47 of the chemical mechanical polishing liquid of the present invention. According to the formulation given in the table, the components other than the oxidizing agent were uniformly mixed, and the mass percentage was made up to 100% with water. Adjust to the desired pH with KOH or 1 ⁇ 0 3 . Add oxidizing agent before use and mix well. Table 1 Examples 1 ⁇ 47
- Methyl cellulose (0.01%) alkane defoaming boron
- Table 2 gives a comparison of the static corrosion rates of the comparative polishing slurries 1 to 5 and the polishing paddle examples 48 to 58 of the present invention and copper.
- the components other than the oxidizing agent are mixed. uniform, the percentage made 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 blank copper (Cu) was placed in the comparative polishing slurry 1 to 5 and the polishing slurry of the present invention in Examples 48 to 58 for soaking for 30 minutes, and the difference in thickness of the copper before and after the immersion was measured to obtain the static corrosion rate.
- Table 2 Comparative copper polishing rate 1 ⁇ 5 and copper static corrosion rate of the polishing liquid examples 48 to 58 of the present invention
- the static corrosion rate of copper can be preferably suppressed after adding at least one phosphate ester surfactant to Examples 48 to 58 as compared with Comparative Examples 1 to 5 to which no phosphate ester surfactant is added. It helps to reduce the removal rate of copper at low pressure and contributes to the improvement of planarization efficiency.
- Effect Example 2 A blank copper (Cu) wafer and a patterned copper wafer were polished using a comparative polishing liquid 1 and a polishing liquid 50, 51 of the present invention. The polishing rate of the obtained copper is shown in Fig. 1. The polishing conditions of the pattern wafer and the dishing value of the copper block are shown in Table 3.
- phosphate ester surfactants are added to Examples 50 and 51 as compared with Example 1 in which no phosphate ester surfactant is added, and the surfactant can inhibit copper under low pressure.
- the removal rate is beneficial to reduce the dishing on the patterned copper wafer, while maintaining a high copper removal rate under high pressure and increasing the throughput.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Materials Engineering (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)
Description
一种化学机械抛光浆料 技术领域
本发明涉及一种用于铜的化学机械抛光桨料。 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 A1向 Cu转化。 与 A1相比, Cu布线具有电阻率低, 抗电迁移能 率高, RC延迟时间短, Cu布线的优势已使其替代 A1成为半导体制作中的 互联金属。但是目前还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公知技术, 因此铜的化学机械抛光方法被认 为是最有效的工艺方法。 - 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步中均使用到铜化学机械抛光液。
.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。 随着抛光的进行, 铜的高度差会逐渐减小, 达到 确'认 本
平坦化。 但是在抛光过程中, 如果铜抛光液的化学作用太强, 静态腐蚀速率 太高, 则铜的钝化膜即使在较低压力下 (如铜线凹陷处) 也易于被去除, 导 致平坦化效率降低, 抛光后的蝶形凹陷增大。
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: 专利 号为 US 6,616,717公开了一种用于金属 CMP的组合物和方法;专利号为 US 5,527,423 公开了一种用于金属层的化学机械抛光浆料; 专利号为 US 6,821 ,897 公开了一种使用聚合体络合剂的铜 CMP 的方法; 专利号为 CN 02114147.9 公开了一种铜化学一机械抛光工艺用抛光液; 专利号为 CN 01818940.7公开了铜的化学机械抛光所用的浆料; 专利号为 CN 98120987.4 公幵了一种用于铜的 CMP浆液制造以及用于集成电路的制造方法。 但是上 述用于铜的抛光浆料存在抛光速度不够快,使用后衬底表面存在缺陷、划伤、 粘污和铜的残留, 或者是抛光后铜块的凹陷过大, 或者是抛光过程中存在着 局部或整体腐蚀以及铜在常温和抛光温度 (如 50°C ) 下的静态腐蚀速率较 高等问题。 因此有必要开发出新的用于铜的化学机械抛光桨料。 发明概要
本发明的目的是克服现有技术中存在的缺陷, 提供一种用于铜的化学 机械抛光浆料。这种抛光浆料至少含有一种磷酸酯类表面活性剂, 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降低铜的静态腐 蚀速率, 抑制铜在低压力下得去除速率, 降低抛光后铜块的碟型凹陷。
具体的说, 本发明的具体方法是向抛光浆液中加入一种磷酸酯类表面活 性剂, 所述的磷酸酯类表面活性剂具有如下结构:
RO, RO-(CH2CH20)n , RCOO-(CH2CH20)n) 或含有两个以上结构式 1的多元醇磷酸酯。
其中 R为 C8〜C22的垸基或垸基苯、甘油基(C3H5Or)等; n=3〜30, M=H,
K, NH4, (CH2CH20)卜 3ΝΗ3 和 /或 Na。
本发明中所述的磷酸酯类表面活性剂的含量为重量百分比 0.0005〜2%, 较佳为 0.001~1%
本发明中所述的研磨颗粒包括二氧化硅、 氧化铝、 掺杂铝或覆盖铝的二 氧化硅、二氧化铈、二氧化钛和 /或高分子研磨颗粒。所述的研磨颗粒的重量 百分比浓度较佳为 0.1〜20 %; 更佳为 0.1〜10%。 所述的研磨颗粒的粒径为 20〜150nm。
所述的络合剂为氨羧化合物及其盐、有机羧酸及其盐、有机膦酸及其盐、 有机胺。 所述的氨羧化合物具体为甘氨酸、 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、 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 ·, 所述的有机胺为乙二胺、 二乙烯 三胺、 五甲基二乙烯三胺、 多乙烯多胺、 三乙烯四胺、 四乙烯五胺等。 所述
的盐为钾盐、钠盐和 /或铵盐。所述的络合剂的含量为质量百分比 0.01〜10%。 所述的氧化剂为过氧化氢、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。
所述的氧化剂的含量为质量百分比 0.05〜10 %。
本发明的抛光液的 pH为 3〜11, 较佳的为 4〜8。
本发明的抛光液中,还可以含有本领域其他常规添加剂,如腐蚀抑制剂、 pH调节剂、 粘度调节剂、 消泡剂和杀菌剂等来达到抛光效果。
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到本发明的 浓度范围并加入氧化剂。
本发明的积极进步效果在于: 本发明的抛光浆液可以显著降低铜的静态 腐蚀速率, 抑制铜在低压力下的去除速率, 降低图形晶片抛光后的铜块的碟 型凹陷。 发明内容
下面用实施例来进一步说明本发明, 但本发明并不受其限制。
实施例 1~47
表 1给出了本发明的化学机械抛光液的实施例 1〜47, 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 1^03调节到所需要的 pH值。 使用前加氧化剂, 混合均匀即可。
表 1 实施例 1~47
实施例 研磨颗粒 磷酸酯 络合剂 氧化剂 PH 含 含 含 具 里 里 体
\vt 具体物. 含量 wt 具体 wt 物
% 质 wt% 具体物质 % 物质 % 质 过 氧
Si02 化
1 3 (20nm) 0.001 C8H17〇P03H2 0.01 草酸 2 氢 3 过 氧
Si02 丁二 化
2 1 (20nm) 0.002 C12H25OPO3H2 5 酸 1 氢 3 锰
Si02 丙二 酸
3 20 (40nm) 0.005 C16H33OPO3H2 0.1 酸 3 钾 3 硝
SiO, 苹果 酸
4 1 (40nm) 0.001 C18H37OPO3H2 2 酸 0.5 铁 4 过 氧
Si02 化
5 1 (50nm) 0.005 C22H45OPO3H2 0.5 乳酸 5 氢 4 过 氧
Si02 没食 化
6 10 (60nm) 0.003 (Ci2H250)2P02H 0.5 子酸 8 氢 4 过 磺基 氧
Si02 水杨 化
7 1 (70nm) 0.005 (C14H290)2P02H 1 酸 10 氢 4 过 氧
A1203 化
8 3 (30nm) 0.01 (C16H330)2P02H 3 醋酸 1 脲 4 过 氧
Ce02 檬 乙
9 2 (50nm) 0.01 C3H5O3(CH2CH2O)20(PO3H2)3 8 酸铵 5 酸 4 过 硫
Ti02 酒石 酸
10 1 ( 120nm) 0.01 C3H5O3(CH2CH2〇)30(PO3H2)3 2 酸钾 0.5 钾 4
2-膦
酸丁
'院基 过
- 1 ,2,4- 氧
Si02 三羧 乙
1 1 3 ( 150nm) 0.02 C3H5〇3(CH2CH2O)10(P〇3H2)3 2 酸 3 酸 4
乙二
胺四 过 亚甲 硫
SiO: 基膦 酸
2 (80nm) 0.005 C3H503(CH2CH20)15(P03K2)3 2 酸 4 钾 5 二乙
烯三 过 胺五 硫
Si02 甲叉 酸
8 ( l OOnm) 0.005 C3H5O3(CH2CH2O)30(PO3Na2)3 Ί 膦酸 2.5 铵 5 羟基 过 亚乙 氧
Si02 基二 化
0.5 (70nm) 0.0】 C3H503(CH2CH20)2Q(P03H2)3 2 膦酸 3.5 氢 4
氨基 过 三亚 氧
Si02 甲基 化
0.5 (80nm) 0.01 C8H170(CH2CH20)3P03H2 2 膦酸 4.5 脲 4
2-羟 过 基膦 氧
Si02 酸基 乙
0.5 ( l OOnm) 0.01 Ci2H250(CH2CH20)9P03H2 乙酸 0.8 酸 4
多氨
基多
醚基 过 亚甲 硫
SiO, 基膦 酸
0.5 (100nm) 0.02 C8H17O(CH2CH2O)20PO3K2 2 酸 0.8 钾 5 乙二 过 胺四 氧
Si02 甲叉 化
12 (l OOnm) 0.003 C18H370(CH2CH20)3P03H2 3 膦酸 0.1 氢 5 乙二 过 胺四 氧
SiO, 乙酸 乙
0.5 (l OOnm) 0.01 C18H370(CH2CH20)1()P03K2 1 二钠 3 . 酸 5 乙二 过 胺二 氧
SiO, 琥珀 化
5 (70nm) 0.02 [C12H250(CH2CH2〇)7]2P03K 1 酸 1 氢 5 过 环己 硫
SiO, 垸四 酸
0.5 (l OOnm) 0.01 [C18H370(CH2CH20)9】2P03NH4 1 乙酸 1 钾 5 二乙
烯三 过 胺五 硫
Si02 乙酸 酸
0.5 ( l OOnm) 0.01 [C14H290(CH2CH20)3】2P03K 1 1 铵 5
过 氧
Si02 C9H19C6H40(CH2CH20)12P03 氨三 化
0.5 ( l OOnm) 0.005 H2 3 乙酸 5 氢 5
2-膦
酸丁
院基 过
-1 ,2,4- 氧
Si02 C9H19C6H40(CH2CH20)7P03H 三羧 化
2 (70nm) 0.005 2 1 酸 2 氢 4
过 硫 的 S i02 C8H17C6H40(CH2CH20)1 C)P03【 苏氨 酸
] (70nm) 0.001 NH(CH2CH2OH)】2 10 酸 2 铵 5 过 掺杂铝 氧 的 Si。2 C9H19C6H4O(CH2CH2O)10PO3( 丙氨 化
0.5 (20nm) 0.005 NH4)2 5 酸 2 氢 4 聚甲基 过 丙烯酸 氧 甲酯 [C8H17C6H4O(CH2CH2O)10]2PO 缬氨 化
5 ( 150ηιτι) 0.003 2K 5 酸 2 脲 5 过 聚苯乙 氧 烯 [C9H19C6H4O(CH2CH2O)10]2P 亮氨 化
4 ( 120nm) 0.002 02K 6 酸 5 氢 5 过 氧
Si02 苯丙 化
0.1 (70nm) 0.001 C8H17C6H4OPO3K2 6 氨酸 3 氢 5 过 氧
Si02 苏氨 化
15 (70nm) 0.01 CgHigCshUOPOgKz 8 酸 2 氢 5 过 氧
Si02 天冬 化
0.2 (70nm) 0.0】 (C9H19C6H40)2P02NH4 8 酰胺 2 氢 6
Si02 [C17H35COO(CH2CH20)3]2P02 丝氨 氯
0.2 (70nm) 0.02 K 5 酸 2 酸 6 过 氧 化
Si02 C1 1 H23COO(CH2CH20)15P03( 脯氨 氢
0.3 (70 0.02 NH4)2 1 酸 3 6 过
0.5 [C12H25〇(CH2CH20)3】2P02K 氧
SiO, 色氨 化
] (70nm) 0.0005 C12H250(CH2CH20)3P03K2 3 酸 1 氢 6
1
0.5 [C8H170(CH2CH20)3]2P〇2K 过 氧
Si02 C9H19C6H40(CH2CH20)7P03K 蛋氨 化
2 (70nm) 0.0005 2 3 酸 1 氢 6 过 氧
Si02 天冬 化
3 (80nm) 0.001 C16H33OP03(NH4)2 3 氨酸 2 氢 7 i
Si02 谷氨 碘
3 (80nm) 0.002 (C14H290)2P02NH4 3 酸 2 酸 7 过 氧
Si02 C16H33OP03[NH2(CH2CH2OH) 精氨 化
1 (80nm) 0.003 2]2 1 酸 1 氢 8 过 氧
Si02 赖氨 化
1 (80nm) 0.05 C8H17OP03[NH(CH2CH2OH)3]2 1 .5 酸 ] 氢 9 过 氧
Si02 组氨 化
1 (80— 0.1 (C16H330)2P〇2Na 1 .5 酸 3 氢 9 五甲 过 基二 氧
Si02 乙烯 化
0.5 (80nm) 0.2 C14H29OPO3K2 2 三胺 3 氢 10 过 多乙 氧
Si02 C8H17O(CH2CH2O)20PO3(NH4) 烯多 化
0.5 (80nm) 0.5 2 1 胺 3 氢 1 1 过 三乙 氧
Si02 C16H33〇P03H2[NH(CH2CH20 烯四 化
0.5 (80nm) 1 H)2]2 1 胺 3 氢 1 1 过 四乙 氧
Si02 C8H17OP03H2[N(CH2CH2OH)3j 稀五 化
0.5 (80nm) 2 2 1 胺 2 氢 1 1
0.0005 C12H25OPO3K2 过 氧 甲
Si02 谷氨 酸
0.5 (80nm) 0.5 (C12H250)2P〇2K 0.05 酰胺 2 10
三乙 过 烯四 碳
Si02 胺六 酸
6 (80nm) ] C18H37OPO3K2 0.05 乙酸 2 钠 10
二乙
Si02 C16H330(CH2CH20)9P〇3[NH3( 烯三
0.5 (80nm) 0.5 CH2CH2OH)】2 0.05 胺
甲基纤维素 (0.01%) 烷消泡 硼
47 添加剂 (wt%) ).01%) 2 酸 10
效果实施例
表 2给出了对比抛光浆料 1〜5和本发明的抛光桨料实施例 48〜58组分 及铜的静态腐蚀速率对比, 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。
将空片铜 (Cu)放入对比抛光浆料 1〜5和本发明的抛光浆料实施例 48〜 58中浸泡, 浸泡时间 30分钟, 测量浸泡前后铜的厚度差得到其静态腐蚀速 率见表 2。 表 2 对比抛光液 1〜5和本发明抛光液实施例 48〜58的铜静态腐蚀速率
铜静 态腐 蚀速 率 实 施 ( /mi 例 f磨颗粒 磷酸酯 络合剂 氧化剂 H n) 含 含
含 量 里
量 含量 wt 具体 wt 具体物
wt% 具体物质 wt% 具体物质 % 物质 % 质
Si02 过氧化
对比 1 1 (lOOnm) 无 1
无 甘氨酸 1 氢 6 680
Si02 CeHi7C6H 0(CH2 过氧化
48 1 (lOOnm) 0.0005 CH2O)10PO3K2 甘氨酸 1 氢 6 605
Si02 C8Hi7CeH4〇(CH2 过氧化
49 1 (lOOnm) 1
0.001 CH2O)10PO3K2 甘氨酸 1 氢 6 332
Si02 CsHi7C6H40(CH2 过氧化
50 1 (lOOnm) 1
0 005 CH2O)10PO3K2 甘氨酸 1 氢 6 20
Si02 C8H17C6H4〇P〇3K 过氧化
51 1 ( l OOnm) 1
0.1 2 甘氨酸 2 氢 6 0
Si02 [CsH17C6H40(CH2 过氧化
52 1 (lOOnm) 0.1 CH2O)10]2PO2K 1 甘氨酸 2 氢 6 0
由表 2可见, 与未添加磷酸酯表面活性剂的对比例 1〜5相比, 实施例 48〜58 中添加了至少一种磷酸酯表面活性剂后,能较好的抑制铜的静态腐蚀 速率, 有助于降低铜在低压下的去除速率, 有助于平坦化效率的提高。 效果实施例 2 采用对比抛光液 1和本发明的抛光液 50, 51, 对空片铜 (Cu) 晶片及 有图案的铜晶片进行抛光。 所得的铜的抛光速率见图 1, 图形晶片的抛光条 件及铜块的碟型凹陷值见表 3
空片抛光条件:铜晶片:下压力 l〜3psi;抛光盘及抛光头转速 93/87rpm,
抛光垫 IC 1010, 抛光液流速 150ml/min, 抛光机台为 8" Mirra。 有图案的铜晶片抛光工艺条件: 抛光盘及抛光头转速 93/87rpm, 抛光垫 IC1010, 抛光液流速 150ml/min, 抛光机台为 8" Mirra。 在抛光盘 1上用相 应的下压力抛光有图案的铜晶片至残留铜约 3000A, 然后再在抛光盘 2上用 相应的下压力将残留的铜清除并过抛 20秒。用 XE-300P原子力显微镜测量 有图案的铜晶片上 80um*80um 的铜块的碟型凹陷值。
表 3 有图案的铜晶片的抛光条件及抛光后铜晶片 80iim*80Um铜块处 的凹陷值
由图 1及表 3可见, 与未添加磷酸酯表面活性剂实施例 1相比, 实施例 50和 51中添加了磷酸酯表面活性剂, 该表面活性剂能较多的抑制铜在低下 压力下的去除速率, 有利于降低在有图案的铜晶片上的碟型凹陷, 而在高压 力下能保持较高的铜去除速率, 提高了产能。
Claims
1、 一种化学机械抛光浆液, 其包括: 一种磷酸酯类表面活性剂、 研磨 颗粒、 络合剂和氧化剂。
RCOO-(CH2CH20)n) 或含有两个以上结构式 1的多元醇磷酸酯,
其中 R为 C8〜C22的烷基或烷基苯、甘油基(C3H5Or)等; n=3〜30, M=H,
K, NI-I4, (CHsCHsC wNHn禾口 /或 Na。
3、 如权利要求 1或 2所述的抛光浆液, 其特征在于, 所述的磷酸酯类 表面活性剂的含量为重量百分比 0.0005〜2%。
4、 如权利要求 3所述的抛光浆液, 其特征在于, 所述的磷酸酯类表面 活性剂的含量为重量百分比 0.001〜1%。
5、 如权利要求 1 所述的抛光浆液, 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、 二氧化钛和 /或高 分子研磨颗粒。
6、 如权利要求 1 所述的抛光浆液, 其特征在于, 所述的研磨颗粒的重 量百分比浓度为 0.1〜20 %。
7、 如权利要求 1 或 5所述的抛光浆液, 其特征在于, 所述的研磨颗粒 的粒径为 20〜】50nm。
8、 如权利要求 1 所述的抛光浆液, 其特征在于, 所述的络合剂为氨羧 化合物及其盐、 有机羧酸及其盐、 有机膦酸及其盐和 /或有机胺。
9、 如权利要求 8所述的抛光浆液, 其特征在于, 所述的氨羧化合物选 自甘氨酸、 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、 天冬氨酸、 苏氨酸、 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 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; 所述的有机胺为乙二胺、 二乙烯三胺、 五甲基二乙烯三胺、 多 乙烯多胺、 三乙烯四胺、 四乙烯五胺; 所述的盐为钾盐、 钠盐和 /或铵盐。
10、 如权利要求 1所述的抛光浆液, 其特征在于, 所述的络合剂的含量 为质量百分比 0.01〜10%。
1 1、 如权利要求 1所述的抛光浆液, 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、 如权利要求 1所述的抛光浆液, 其特征在于, 所述的氧化剂的含量 为质量百分比 0.05〜10 %。
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