US20220049125A1 - Chemical mechanical polishing of substrates containing copper and ruthenium - Google Patents

Chemical mechanical polishing of substrates containing copper and ruthenium Download PDF

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US20220049125A1
US20220049125A1 US17/312,797 US201917312797A US2022049125A1 US 20220049125 A1 US20220049125 A1 US 20220049125A1 US 201917312797 A US201917312797 A US 201917312797A US 2022049125 A1 US2022049125 A1 US 2022049125A1
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chemical
mechanical polishing
cmp
presently
acid
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Haci Osman GUEVENC
Michael Lauter
Te Yu Wei
Wei Lan CHIU
Reza M. Golzarian
Julian Proelss
Leonardus Leunissen
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BASF SE
BASF Corp
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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
    • 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
    • C09K3/1409—Abrasive particles per se
    • 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
    • H01L21/302—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
    • H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
    • H01L21/30625—With simultaneous mechanical treatment, e.g. mechanico-chemical polishing
    • 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 presently claimed invention relates to a chemical-mechanical polishing (CMP) composition and chemical-mechanical polishing (CMP) methods.
  • CMP chemical-mechanical polishing
  • CMP chemical-mechanical polishing
  • the presently claimed invention particularly relates to a composition and process for chemical-mechanical polishing of substrates containing copper and ruthenium, specifically, semiconductor substrates containing copper and ruthenium.
  • CMP chemical mechanical polishing
  • CMP is employed to planarize surfaces.
  • CMP utilizes the interplay of chemical and mechanical action to achieve the planarity of the to-be-polished surfaces.
  • Chemical action is provided by a chemical composition, also referred to as CMP composition or CMP slurry.
  • Mechanical action is usually carried out by a polishing pad which is typically pressed onto the to-be-polished surface and mounted on a moving platen. The movement of the platen is usually linear, rotational or orbital.
  • a rotating wafer holder brings the to-be-polished wafer in contact with a polishing pad.
  • the CMP composition is usually applied between the to-be-polished wafer and the polishing pad.
  • Tantalum (Ta) and Tantalum nitride (TaN) are conventionally used as barrier layer material to prevent device contamination caused by copper diffusing through the dielectric layer.
  • Ruthenium (Ru) has been recently identified as a promising barrier layer material to replace the current tantalum barrier layer and the copper (Cu) seed layer.
  • the insolubility of copper in ruthenium makes ruthenium attractive as barrier layer material, and copper can also be directly deposited onto the ruthenium layer due to the lower resistivity of ruthenium.
  • CMP processes in the presence of a CMP composition comprising a surfactant and an aromatic compound for chemical-mechanical polishing of substrates comprising copper and ruthenium are known and described, for instance, in the following references.
  • compositions for chemical-mechanical polishing using low contact pressures to remove ruthenium from substrates comprising a dispersing medium, abrasive particles and having pH in the range of 8 to 12.
  • U.S. Pat. No. 7,265,055 B2 describes a method for chemical-mechanical polishing a substrate comprising copper, ruthenium, tantalum, and dielectric layers. The method uses a polishing pad and a CMP composition or agent comprising alpha-alumina abrasive particles treated with negatively charged polymers or copolymers
  • US 2008/0105652 A1 discloses a chemical mechanical polishing composition
  • a chemical mechanical polishing composition comprising an abrasive, an oxidizing agent, an amphiphilic non-ionic surfactant, calcium or magnesium ion, a corrosion inhibitor for copper and water, having pH in the range of about 6 to about 12.
  • US 2013/0005149 A1 discloses a chemical mechanical polishing composition
  • a chemical mechanical polishing composition comprising (a) at least one type of abrasive particles, (b) at least two oxidizing agents, (c) at least one pH adjusting agent, and (d) deionized water, (e) optionally comprising at least one antioxidant, and a method for the chemical-mechanical planarization of a substrate containing at least one copper layer, at least one ruthenium layer, and at least one tantalum layer.
  • U.S. Pat. No. 6,852,009 B2 discloses a polishing composition
  • a polishing composition comprising silicon dioxide, at least one basic substance selected from the group consisting of an inorganic salt of an alkali metal, an ammonium salt, piperazine and ethylenediamine, at least one chelating agent and water.
  • the basic substance is used for wafer polish to suppress metal contamination and diffusion into the wafers.
  • a further object of the presently claimed invention is to remove pad staining and particles from the wafer surface and polishing pad which are formed because of chemical-mechanical polishing of substrates used in the semiconductor industry.
  • the CMP compositions of the presently claimed invention as described hereinbelow provide a high material removal rate (MRR) of the substrate to be preferably polished and a clean pad polishing surface free of metal debris.
  • MRR material removal rate
  • CMP chemical-mechanical polishing
  • the presently claimed invention is directed to a method for the manufacture of semiconductor devices comprising the chemical-mechanical polishing of a substrate in the presence of the chemical-mechanical polishing (CMP) composition described hereinabove or hereinbelow.
  • CMP chemical-mechanical polishing
  • the presently claimed invention is directed to a use of the chemical-mechanical polishing composition (CMP) for chemical-mechanical polishing of a substrate used in the semiconductor industry.
  • CMP chemical-mechanical polishing composition
  • the CMP composition of the presently claimed invention provides a stable formulation or dispersion, wherein no phase separation occurs.
  • steps of a method or use or assay there is no time or time interval coherence between the steps, that is, the steps may be carried out simultaneously or there may be time intervals of seconds, minutes, hours, days, weeks, months or even years between such steps, unless otherwise indicated in the application as set forth herein above or below.
  • ‘% by weight’ or ‘wt. %’ as used in the presently claimed invention is with respect to the total weight of the coating composition. Further, sum of wt. % of all the compounds, as described hereinbelow, in the respective component adds up to 100 wt.-%.
  • a corrosion inhibitor is defined as a chemical compound forming a protective molecular layer on the surface of a metal.
  • a chelating agent is defined as a chemical compound that forms soluble, complex molecules with certain metal ions, inactivating the ions so that they cannot normally react with other elements or ions to produce precipitates or scale.
  • a low-k material is a material having a k value (dielectric constant) of less than 3.5, preferably less than 3.0, more preferably less than 2.7.
  • An ultra-low-k material Is a material having a k value (dielectric constant) of less than 2.4.
  • colloidal inorganic particles are inorganic particles which are produced by a wet precipitation process; and fumed inorganic particles are particles produced by high temperature flame hydrolysis of for example metal chloride precursor with hydrogen in the presence of oxygen, for example using the Aerosil® process.
  • colloidal silica refers to silicon dioxide that has been prepared by condensation polymerization of Si(OH) 4 .
  • the precursor Si(OH) 4 can be obtained, for example, by hydrolysis of high purity alkoxysilanes, or by acidification of aqueous silicate solutions.
  • colloidal silica can be prepared in accordance with U.S. Pat. No. 5,230,833 or can be obtained as any of various commercially available products, such as the Fuso® PL-1, PL-2, and PL-3 products, and the Nalco 1050, 2327 and 2329 products, as well as other similar products avail-able from DuPont, Bayer, Applied Research, Nissan Chemical, Nyacol and Clariant.
  • the mean particle size is defined as the d 50 value of the particle size distribution of the inorganic abrasive particles (A) in the aqueous medium (H).
  • the mean particle size is measured for example using dynamic light scattering (DLS) or static light scattering (SLS) methods.
  • DLS dynamic light scattering
  • SLS static light scattering
  • DLS dynamic light scattering
  • a Horiba LB-550 V DLS, dynamic light scattering measurement
  • the decay constants are proportional to the diffusion coefficient, D t , of the inorganic abrasive particle and are used to calculate particle size according to the Stokes-Einstein equation:
  • the suspended particles are assumed to (1) have a spherical morphology and (2) be uniformly dispersed (i.e. not agglomerated) throughout the aqueous medium.
  • the particle size distribution of the fumed or colloidal inorganic particle dispersion is usually measured in a plastic cuvette at 0.1 to 1.0% solid concentration and dilution, if necessary, is carried out with the dispersion medium or ultra-pure water.
  • the BET surface of the inorganic abrasive particles is determined according to DIN ISO 9277:2010-09.
  • a surfactant is defined as a surface-active compound which decreases the surface tension of a liquid, the interfacial tension between two liquids, or that between a liquid and a solid.
  • water-soluble means that the relevant component or ingredient of the composition can be dissolved in the aqueous phase on the molecular level.
  • water-dispersible means that the relevant component or ingredient of the composition can be dispersed in the aqueous phase and forms a stable emulsion or suspension.
  • an oxidizing agent is defined as a chemical compound which can oxidize the to-be-polished substrate or one of its layers.
  • a pH adjusting agent is defined as a compound which is added to have its pH value adjusted to the required value.
  • CMP Chemical Mechanical Polishing
  • CMP chemical-mechanical polishing
  • the CMP composition (Q) comprises the components (A), (B), (C), (D), (E), (F), (G), (H) and optionally further components as described below.
  • the at least one inorganic abrasive particle (A) is selected from the group consisting of a metal oxide, a metal nitride, a metal carbide, a silicide, a boride, a ceramic, a diamond, an organic/inorganic hybrid particle and silica.
  • the chemical nature of at least one inorganic abrasive particle (A) is not particularly limited.
  • (A) may be of the same chemical nature or a mixture of particles of different chemical nature.
  • particles (A) of the same chemical nature are preferred.
  • the inorganic abrasive particles (A) are selected from the group consisting of a metal oxide, a metal nitride, a metal carbide, including a metalloid, a metalloid oxide or carbide, a silicide, a boride, a ceramic, a diamond, an organic/inorganic hybrid particle, silica, and any mixture of inorganic particles.
  • the at least one inorganic abrasive particle (A) can be any inorganic abrasive particle (A).
  • the at least one inorganic particle (A) is selected from the group consisting of colloidal or fumed inorganic particle or a mixture thereof. Among them, oxides and carbides of metals or metalloids are preferred.
  • the at least one inorganic particle (A) is preferably selected from the group consisting of alumina, ceria, copper oxide, iron oxide, nickel oxide, manganese oxide, silica, silicon nitride, silicon carbide, tin oxide, titania, titanium carbide, tungsten oxide, yttrium oxide, zirconia, or mixtures or composites thereof.
  • the at least one inorganic particle (A) is more preferably selected from the group consisting of alumina, ceria, silica, titania, zirconia, or mixtures or composites thereof.
  • (A) are silica particles.
  • the at least one inorganic particle (A) is most preferably colloidal silica particle.
  • the concentration of the at least one inorganic abrasive particle (A) is in the range of from ⁇ 0.01 wt. % to ⁇ 10 wt. % based on the total weight of the chemical-mechanical polishing composition.
  • the concentration of the at least one inorganic abrasive particle (A) is not more than 10 wt. %, preferably not more than 5 wt. %, particularly not more than 3 wt. %, for example not more than 2 wt. %, most preferably not more than 1.8 wt. %, particularly not more than 1.5 wt. %, based on the total weight of the composition (Q).
  • the concentration of the at least one inorganic abrasive particle (A) is preferably at least 0.01 wt. %, more preferably at least 0.1 wt. %, most preferably at least 0.2 wt.
  • the concentration of the at least one inorganic abrasive particle (A) is more preferably is in the range of from ⁇ 0.4 wt. % to ⁇ 1.2 wt. % based on the total weight of the CMP composition (Q).
  • the at least one inorganic abrasive particle (A) can be contained in the CMP composition (Q) in various particle size distributions.
  • the particle size distribution of the at least one inorganic abrasive particle (A) can be monomodal or multimodal. In case of multimodal particle size distribution, bimodal is often preferred.
  • a monomodal particle size distribution is preferred for the inorganic abrasive particles (A).
  • the particle size distribution of the inorganic abrasive particles (A) is not particularly limited.
  • the average particle diameter of the at least one inorganic abrasive particle (A) is in the range of ⁇ 1 nm to ⁇ 1000 nm determined according to dynamic light scattering technique.
  • the mean or average particle size of the at least one inorganic abrasive particle (A) can vary within a wide range.
  • the mean particle size of the at least one inorganic abrasive particle (A) is in the range of from ⁇ 1 nm to ⁇ 1000 nm, preferably in the range of from ⁇ 10 nm to ⁇ 400 nm, more preferably in the range of from ⁇ 20 nm to ⁇ 200 nm, more preferably in the range of from ⁇ 25 nm to ⁇ 180 nm, most preferably in the range of from ⁇ 30 nm to ⁇ 170 nm, particularly preferably in the range of from ⁇ 40 nm to ⁇ 160 nm, particularly most preferably in the range of from ⁇ 45 nm to ⁇ 150 nm, in each case measured with dynamic light scattering techniques using instruments for example a High Performance Particle Sizer (HPPS) from Malvern Instruments, Ltd. or Horiba
  • HPPS High Performance Particle
  • the BET surface of the at least one inorganic abrasive particle (A) can vary within a wide range.
  • the BET surface of the at least one inorganic abrasive particle (A) is in the range of from ⁇ 1 m 2 /g to ⁇ 500 m 2 /g, more preferably in the range of from ⁇ 5 m 2 /g to ⁇ 250 m2/g, most preferably in the range of from ⁇ 10 m 2 /g to ⁇ 100 m 2 /g, particularly preferably in the range of from ⁇ 20 m 2 /g to ⁇ 95 m 2 /g, particularly most preferably in the range of from ⁇ 25 m 2 /g to ⁇ 92 m 2 /g, in each case determined according to DIN ISO 9277:2010-09.
  • the at least one inorganic abrasive particle (A) can be of various shapes.
  • the particles (A) may be of one or essentially only one type of shape.
  • the particles (A) have different shapes.
  • two types of differently shaped particles (A) may be present.
  • (A) can have the shape of agglomerates, cubes, cubes with bevelled edges, octahedrons, icosahedrons, cocoons, nodules or spheres with or without protrusions or indentations.
  • the inorganic abrasive particles (A) are preferably essentially spherical, whereby typically these have protrusions or indentations.
  • the at least one inorganic abrasive particle (A) are preferably cocoon-shaped.
  • the cocoons may be with or without protrusions or indentations.
  • Cocoon-shaped particles are particles with a minor axis of from ⁇ 10 nm to ⁇ 200 nm, a ratio of major/minor axis of from ⁇ 1.4 to ⁇ 2.2, more preferably of from ⁇ 1.6 to ⁇ 2.0.
  • they have an averaged shape factor of from ⁇ 0.7 to ⁇ 0.97, more preferably of from ⁇ 0.77 to ⁇ 0.92, preferably an averaged sphericity of from ⁇ 0.4 to ⁇ 0.9, more preferably of from ⁇ 0.5 to ⁇ 0.7 and preferably an averaged equivalent circle diameter of from ⁇ 41 nm to ⁇ 66 nm, more preferably of from ⁇ 48 nm to ⁇ 60 nm, in each case determined by transmission electron microscopy and scanning electron microscopy.
  • the shape factor gives information on the shape and the indentations of an individual particle and can be calculated according to the following formula:
  • the shape factor of a spherical particle without indentations is 1.
  • the value of shape factor decreases when the number of indentations increases.
  • the sphericity gives information on the elongation of an individual particle using the moment about the mean and can be calculated according to the following formula wherein M are the centres of gravity of the respective particle:
  • Mxy ⁇ [( x ⁇ x mean)*( y ⁇ y mean)]/ N
  • the sphericity of a spherical particle is 1.
  • the value of the sphericity decreases when particles are elongated.
  • the equivalent circle diameter (also abbreviated as ECD in the following) of an individual non-circular particle gives information on the diameter of a circle which has the same area as the respective non-circular particle.
  • the averaged shape factor, averaged sphericity and averaged ECD are the arithmetic averages of the respective property related to the analysed number of particles.
  • the procedure for particle shape characterization is as follows.
  • An aqueous cocoon-shaped silica particle dispersion with 20 wt. % solid content is dispersed on a carbon foil and is dried.
  • the dried dispersion is analyzed by using Energy Filtered-Transmission Electron Microscopy (EF-TEM) (120 kilo volts) and Scanning Electron Microscopy secondary electron image (SEM-SE) (5 kilo volts).
  • EF-TEM Energy Filtered-Transmission Electron Microscopy
  • SEM-SE Scanning Electron Microscopy secondary electron image
  • the EF-TEM image having a resolution of 2 k, 16 Bit, 0.6851 nm/pixel is used for the analysis.
  • the images are binary coded using the threshold after noise suppression. Afterwards the particles are manually separated. Overlying and edge particles are discriminated and not used for the analysis.
  • ECD, shape factor and sphericity as defined before are calculated and statistically classified.
  • cocoon-shaped particles include but is not limited to FUSO® PL-3 manufactured by Fuso Chemical Corporation having an average primary particle size (d1) of 35 nm and an average secondary particle size (d2) of 70 nm.
  • the at least one inorganic abrasive particle (A) is silica particle having an average primary particle size (d1) of 35 nm and an average secondary particle size (d2) of 70 nm.
  • the at least one inorganic abrasive particle (A) is colloidal silica particle having an average primary particle size (d1) of 35 nm and an average secondary particle size (d2) of 70 nm.
  • the at least one inorganic abrasive particle (A) is cocoon-shaped silica particle having an average primary particle size (d1) of 35 nm and an average secondary particle size (d2) of 70 nm.
  • the CMP composition (Q) further comprises at least one chelating agent (B).
  • the chelating agent (B) is different from the components (A), (C), (D), (E), (F) and (G).
  • the at least one chelating agent (B) is a carboxylic acid, more preferably, the at least one chelating agent (B) is a compound comprising at least two carboxylic acid ( ⁇ COOH) or carboxylate (—COO—) groups.
  • the at least one chelating agent (B) is selected from the group consisting of dicarboxylic acids and tricarboxylic acids.
  • the at least one chelating agent (B) is selected from the group consisting of malonic acid, tartaric acid, succinic acid, citric acid, acetic acid, adipic acid, malic acid, maleic acid, butyric acid, glutaric acid, glycolic acid, formic acid, lactic acid, lauric acid, malic acid, maleic acid, myristic acid, fumaric acid, palmitic acid, propionic acid, pyruvic acid, stearic acid, valeric acid, 2-methylburyric acid, n-hexanoic acid, 3,3-dimethylbutyric acid, 2-ethylbutyric acid, 4-methylpentanoic acid, n-heptanoic acid, 2-methylhexanoic acid, n-octanoic acid, 2-ethylhexanoic acid, propane-1,2,3-tricarboxylic acid, butane-1,2,3,4-tetracarboxylic
  • the at least one chelating agent (B) is selected from the group consisting of malonic acid, tartaric acid, succinic acid, adipic acid, malic acid, maleic acid, oxalic acid and fumaric acid.
  • the at least one chelating agent (B) is citric acid.
  • the at least one chelating agent (B) is particularly preferably selected from the group consisting of malonic acid, citric acid, adipic acid, propane-1,2,3-tricarboxylic acid, butane-1,2,3,4-tetracarboxylic acid, and pentane-1,2,3,4,5-pentacarboxylic acid, and an aromatic compound comprising an acid group (Y).
  • the at least one chelating agent (B) is particularly preferably is a compound comprising at least three carboxylic acid (—COOH) or carboxylate (—COO—) groups.
  • the at least one chelating agent (B) is particularly preferably selected from the group consisting of malonic acid, citric acid, and an aromatic compound comprising an acid group (Y).
  • (B) is an aromatic compound comprising an acid group (Y).
  • the aromatic compound comprising an acid group (Y) is referred to as (B11) in the following.
  • Representative examples include but are not limited to benzenecarboxylic acid comprising at least two carboxylic acid (—COOH) groups, or a salt thereof.
  • the at least one chelating agent (B) is particularly preferably a benzenedicarboxylic acid.
  • the acid group (Y) is defined as being (Y) and its deprotonated form.
  • the acid group (Y) comprised in the aromatic compound (B11) is preferably any acid group so that the pKa value (logarithmic measure of the acid dissociation constant) of
  • the acid group (Y) is preferably directly covalently bound to the aromatic ring system of the aromatic compound (B11).
  • the aromatic compound (B11) comprises per aromatic ring at least two acid groups (Y).
  • the aromatic compound (B11) comprises at least one, preferably at least two, most preferably 2 to 6, particularly preferably 2 to 4, for example 2 acid groups (Y).
  • the aromatic compound (B11) preferably comprises—per aromatic ring—at least one, more preferably at least two, most preferably 2 to 4, for example 2 acid groups (Y).
  • the aromatic compound (B11) comprises at least one benzene ring, and (B11) preferably comprises—per benzene ring—at least one, more preferably at least two, most preferably 2 to 4, for example 2 acid groups (Y).
  • the aromatic compound (B11) comprises at least one benzene ring, and (B11) preferably comprises—per benzene ring—at least one, more preferably at least two, most preferably 2 to 4, for example 2 carboxylic acid (—COOH) groups or their deprotonated form.
  • the aromatic compound (B11) is a benzenecarboxylic acid comprising at least one, more preferably at least two, most preferably 2 to 4, for example 2 carboxylic acid (—COOH) groups, or a salt thereof.
  • the aromatic compound (B11) is a benzenecarboxylic acid comprising at least one, more preferably at least two, most preferably 2 to 4, for example 2 carboxylic acid (—COOH) groups which are directly covalently bound to the benzene ring, or a salt thereof.
  • the aromatic compound (B11) is most preferably phthalic acid, terephthalic acid, isophthalic acid, 5-hydroxy-isophthalic acid, benzene-1,2,3-tricarboxylic acid, benzene-1,2,3,4-tetracarboxylic acid, or a derivative thereof, or a salt thereof, particularly terephthalic acid, isophthalic acid, 5-hydroxy-isophthalic acid, benzene-1,2,3,4-tetracarboxylic acid, or a derivative thereof, or a salt thereof, for example terephthalic acid, isophthalic acid, or 5-hydroxy-isophthalic acid.
  • the at least one chelating agent (B) is present in an amount in the range of from ⁇ 0.001 wt. % to ⁇ 2.5 wt. % based on the total weight of the chemical-mechanical polishing composition (Q).
  • the chelating agent (B) is preferably not more than 2.5 wt. %, preferably not more than 1 wt. %, based on the total weight of the CMP composition (Q).
  • the amount of (B) is preferably at least 0.001 wt. %, more preferably at least 0.01 wt. %, most preferably at least 0.07 wt. %, based on the total weight of the CMP composition (Q).
  • the CMP composition (Q) further comprises at least one corrosion inhibitor (C).
  • the corrosion inhibitor (C) is different from the components (A), (B), (D), (E), (F) and (G).
  • the at least one corrosion inhibitors (C) is a triazole.
  • the at least one corrosion-inhibitor (C) triazole is selected from the group consisting of unsubstituted benzotriazole, substituted benzotriazoles, unsubstituted 1,2,3-triazole, substituted 1,2,3-triazoles, unsubstituted 1,2,4-triazole and substituted 1,2,4-triazoles.
  • the at least one corrosion-inhibitor (C) is a substituted benzotriazole which is selected from the group consisting of 4-methyl benzotriazole, 5-methyl benzotriazole, 5,6-dimethyl-benzotriazole, 5-chloro-benzotriazole, 1-octanyl benzotriazole, carboxy-benzotriazole, butyl-benzotriazole, 6-ethyl-1H-1,2,4 benzotriazole, (1-pyrrolidinyl methyl) benzotriazole, 1-n-butyl-benzotriazole, benzotriazole-5-carboxylic acid, 4,5,6,7-tetrahydro-1H-benzotriazole, tolyltriazole, 5-bromo-1H-benzotriazole, 5-tert-butyl-1H-benzotriazole, 5-(benzoyl)-1H-benzotriazole, 5,6-dibromo
  • the corrosion-inhibitor (C) is present in an amount in the range of ⁇ 0.001 wt. % to ⁇ 1 wt. % based on the total weight of the chemical-mechanical polishing composition.
  • the at least one corrosion inhibitor (C) is preferably present in an amount of not more than 10 wt. %, more preferably not more than 2 wt. %, most preferably not more than 1 wt. %, most preferably not more than 0.5 wt. %, particularly not more than 0.15 wt. %, for example not more than 0.08 wt. %, based on the total weight of the CMP composition (Q).
  • the amount of (C) is preferably at least 0.0001 wt. %, more preferably at least 0.001 wt. %, most preferably at least 0.005 wt. %, particularly at least 0.02 wt. %, for example at least 0.04 wt. %, based on the total weight of the CMP composition (Q).
  • the CMP composition (Q) further comprises at least one non-ionic surfactant (D).
  • the non-ionic surfactant (D) is different from the components (A), (B), (C), (E), (F) and (G).
  • the at least one non-ionic surfactant (D) is preferably water-soluble and/or water-dispersible, more preferably water-soluble.
  • the at least one non-ionic surfactant (D) comprises a polyoxyalkylene group.
  • the at least one non-ionic surfactant (D) is preferably an amphiphilic non-ionic surfactant, i.e. a surfactant which comprises at least one hydrophobic group (b1) and at least one hydrophilic group (b2).
  • the non-ionic surfactant (D) can comprise more than one hydrophobic group (b1), e.g., 2, 3 or more groups (b1), which are separated from each other by at least one hydrophilic group (b2) as described hereinbelow.
  • the non-ionic surfactant (D) can comprise more than one hydrophilic group (b2), e.g., 2, 3 or more groups (b2) which are separated from each other by hydrophobic groups (b1) as described hereinbelow.
  • the at least one non-ionic surfactant (D) can have different block like general structures.
  • Representative examples of block like structures include but are not limited to the following:
  • the hydrophobic group (b1) is preferably an alkyl group, more preferably an alkyl group having 4 to 40, most preferably 5 to 20, particularly preferably 7 to 18, in particular 10 to 16, for example 11 to 14 carbon atoms.
  • the hydrophilic group (b2) is preferably a polyoxyalkylene group.
  • the polyoxyalkylene group can be oligomeric or polymeric. More preferably, the hydrophilic group (b2) is selected polyoxyalkylene groups comprising
  • the monomer units (b21) is not identical to monomer units (b22), and the polyoxyalkylene group of (b2) containing the monomer units (b21) and (b22) in random, alternating, gradient and/or block-like distribution.
  • hydrophilic group (b2) is selected from polyoxyalkylene groups comprising
  • the oxyalkylene monomer units other than oxyethylene monomer units (b22) preferably are substituted oxyalkylene monomer units wherein the substituents are selected from the group consisting of alkyl, cycloalkyl, aryl, alkyl-cycloalkyl, alkyl-aryl, cycloalkyl-aryl and alkyl-cycloalkyl-aryl groups.
  • the oxyalkylene monomer units other than oxyethylene monomer units (b22) are
  • the substituents of the substituted oxiranes (X) themselves can also carry inert substituents, i.e., the substituents which do not adversely affect the copolymerization of the oxiranes (X) and the surface activity of the non-ionic surfactants (D).
  • inert substituents include but are not limited to fluorine and chlorine atoms, nitro groups and nitrile groups.
  • the inert substituents if present, are present in amounts that they do not adversely affect the hydrophilic-hydrophobic balance of the non-ionic surfactant (D).
  • the substituents of the substituted oxiranes (X) preferably do not carry inert substituents.
  • the substituents of the substituted oxiranes (X) are preferably selected from the group consisting of alkyl groups having 1 to 10 carbon atoms, cycloalkyl groups having 5 to 10 carbon atoms in spirocyclic, exocyclic and/or annealed configuration, aryl groups having 6 to 10 carbon atoms, alkyl-cycloalkyl groups having 6 to 20 carbon atoms, alkyl-aryl groups having 7 to 20 carbon atoms, cycloalkyl-aryl group 11 to 20 carbon atoms, and alkyl-cycloalkyl-aryl groups having 12 to 30 carbon atoms.
  • the substituents of the substituted oxiranes (X) are more preferably selected from the group consisting of alkyl groups having 1 to 10 carbon atoms, the substituents of the substituted oxiranes (X) are particularly preferably selected from the group consisting of alkyl groups having 1 to 6 carbon atoms.
  • oxiranes include but are not limited to methyl oxirane (propyleneoxide) and/or ethyl oxirane (butylene oxide), particularly methyl oxirane.
  • the hydrophilic group (b2) preferably consists of the monomer units (b21) and (b22).
  • the hydrophilic group (b2) is preferably a polyoxyethylene, polyoxypropylene or polyoxybutylene group, more preferably a polyoxyethylene group.
  • the polyoxyalkylene group acting as hydrophilic group (b2) consists the monomer units (b21) and (b22) in random, alternating, gradient and/or block like distribution.
  • hydrophilic group (b2) can have only one type of distribution:
  • the hydrophilic group (b2) consists of at least two types of distributions, e.g., an oligomeric or polymeric segment having a random distribution and an oligomeric or polymeric segment having alternating distribution.
  • the hydrophilic group (b2) has only one type of distribution, and most preferably, the distribution is random or block like.
  • the molar ratio of (b21) to (b22) can vary broadly and, therefore, can be adjusted most advantageously to the particular requirements of the composition, the process and the use of the presently claimed invention.
  • the molar ratio (b21):(b22) is preferably from 100:1 to 1:1, more preferably, from 60:1 to 1.5:1 and, most preferably, from 50:1 to 1.5:1, and particularly preferably, from 25:1 to 1.5:1, and particularly, from 15:1 to 2:1, and for example, from 9:1 to 2:1.
  • the degree of polymerization of the oligomeric and polymeric polyoxyalkylene groups acting as hydrophilic groups (b2) can vary broadly and, therefore, can be adjusted most advantageously to the particular requirements of the composition, the process and the use of the presently claimed invention.
  • the degree of polymerization is preferably in the range of from 5 to 100, preferably 5 to 90, and most preferably, 5 to 80.
  • the at least one non-ionic surfactant (D) is particularly preferably an amphiphilic non-ionic polyoxyethylene-polyoxypropylene alkyl ether surfactant which is a mixture of molecules containing, on the average, an alkyl group having 10 to 16 carbon atoms and 5 to 20 oxyethylene monomer units (b21) and 2 to 8 oxypropylene monomer units in random distribution.
  • the at least one non-ionic surfactant (D) is an amphiphilic non-ionic polyoxyethylene-polyoxypropylene alkyl ether surfactant which is a mixture of molecules containing, on the average, an alkyl group having 11 to 14 carbon atoms and 12 to 20 oxyethylene monomer units and 3 to 5 oxypropylene monomer units in random distribution.
  • the at least one non-ionic surfactant (D) is present in an amount in the range of ⁇ 0.01 wt. % to ⁇ 10 wt. % based on the total weight of the CMP composition (Q).
  • the amount of the at least one non-ionic surfactant (D) is not more than 10 wt. %, more preferably not more than 3 wt. %, most preferably not more than 1 wt. %, particularly preferably not more than 0.5 wt. %, particularly not more than 0.1 wt. %, for example not more than 0.05 wt. %, based on the total weight of the CMP composition (Q).
  • the amount of the at least one non-ionic surfactant (D) is at least 0.00001 wt. %, more preferably at least 0.0001 wt. %, most preferably at least 0.0008 wt. %, particularly preferably at least 0.002 wt. %, particularly at least 0.005 wt. %, for example at least 0.008 wt. %, based on the total weight of the CMP composition (Q).
  • the at least one non-ionic surfactant (D) has number average molecular weight in the range of ⁇ 1500 g/mol to ⁇ 400 g/mol, preferably in the range of ⁇ 1000 g/mol to ⁇ 500 g/mol, most preferably in the range of ⁇ 900 g/mol to ⁇ 600 g/mol, in each case determined by gel permeation chromatography (abbreviated as “GPC” in the following).
  • the CMP composition (Q) further comprises at least one pad-cleaning agent (E).
  • the pad-cleaning agent (E) is different from the components (A), (B), (C), (D), (F) and (G).
  • At least one pad-cleaning agent (E) is selected from polymers and co-polymers of acrylic acid, metacrylic acid and maleic acid.
  • the polymers and co-polymers of acrylic acid, metacrylic acid and maleic acid have a number average molecular weight in the range of ⁇ 500 g/mol to ⁇ 10000 g/mol determined according to gel permeation chromatography at 40° C.
  • the polymers and co-polymers of acrylic acid, metacrylic acid and maleic acid have a number average molecular weight in the range of ⁇ 1000 g/mol to ⁇ 7500 g/mol determined according to gel permeation chromatography at 40° C.
  • At least one pad-cleaning agent (E) is selected from copolymer of acrylic, copolymer of metacrylic acid and copolymer of maleic acid.
  • At least one pad-cleaning agent (E) is selected from copolymer of poly acrylic acid, poly metacrylic acid, acrylic acid and metacrylic acid.
  • At least one pad-cleaning agent (E) is selected from polymers of acrylic acid, metacrylic acid and maleic acid.
  • At least one pad-cleaning agent (E) is selected from poly (acrylic acid-co-maleic acid) copolymers.
  • the concentration of the at least one pad-cleaning agent (E) is in the range of ⁇ 0.001 wt. % to ⁇ 1 wt. % based on the total weight of the CMP composition (Q).
  • the concentration of the at least one pad-cleaning agent is preferably not more than 5 wt. %, more preferably not more than 1 wt. %, more preferably not more than 0.5 wt. %, most preferably not more than 0.1 wt. %, based on the total weight of the CMP composition (Q).
  • the concentration of the at least one pad-cleaning agent is preferably at least at least 0.0001 wt. %, more preferably at least 0.001 wt. %, most preferably at least 0.005 wt. %, in particularly preferably at least 0.05 wt. %, more particularly preferably at least 0.01 wt. % based on the total weight of the CMP composition (Q).
  • the CMP composition (Q) further comprises at least one carbonate or hydrogen carbonate (F).
  • the carbonate comprises at least one CO 3 2 ⁇ anion
  • a hydrogen carbonate comprises at least one HCO 3 ⁇ anion.
  • the carbonate or hydrogen carbonate salt (F) preferably do not comprise any anions other than CO 3 2 ⁇ or HCO 3 ⁇ anion.
  • the CMP composition (Q) further comprises at least one carbonate. The at least one carbonate preferably do not comprise any anions other than the CO 3 2 ⁇ anion.
  • the at least one carbonate or hydrogen carbonate (F) comprises at least one cation selected from the group consisting of NH 4 + cation, organic ammonium cations, N-heterocyclic cations, alkali metal, and earth alkali metal cation. More preferably, (F) comprises at least one NH 4 + , alkali metal or earth alkali metal cation. Most preferably, (F) comprises at least one alkali metal cation. Particularly preferably, (F) is an alkali carbonate or an alkali hydrogen carbonate. Particularly more preferably, (F) comprises at least one sodium or potassium cation. Particularly most preferably, (F) comprises at least one potassium cation. Particularly, (F) is potassium carbonate or potassium hydrogen carbonate. For example, (F) is potassium carbonate.
  • An organic ammonium cation is any cation of the formula [NR 11 R 12 R 13 R 14 ]+, wherein R 11 , R 12 , R 13 is—independently from each other—H, alkyl, aryl, alkylaryl, or arylalkyl, and R 14 is alkyl, aryl, alkylaryl, or arylalkyl.
  • the concentration of the at least one carbonate or hydrogen carbonate is in the range of from ⁇ 0.001 wt. % to ⁇ 1 wt. %.
  • the concentration of the at least one carbonate or hydrogen carbonate is not more than 10 wt. %, more preferably not more than 5 wt. %, most preferably not more than 3 wt. %, particularly preferably not more than 2 wt. %, particularly not more than 1 wt. %, for example not more than 0.7 wt. %, based on the total weight of the CMP composition (Q).
  • the concentration of the at least one carbonate or hydrogen carbonate is at least 0.001 wt. %, more preferably at least 0.01 wt. %, most preferably at least 0.05 wt. %, particularly preferably at least 0.1 wt. %, particularly at least 0.2 wt. %, based on the total weight of the CMP composition (Q).
  • the CMP composition (Q) of the presently claimed invention further comprises at least one oxidizing agent (G).
  • the at least one oxidizing agent (G) is different from the components (A), (B), (C), (D), (E) and (F).
  • the at least one oxidizing agent (G) is selected from the group consisting of organic peroxides, inorganic peroxides, persulfates, iodates, periodic acids, periodates, permanganates, perchloric acids, perchlorates, bromic acids and bromates.
  • the at least one oxidizing agent (G) is peroxide.
  • (G) is hydrogen peroxide.
  • the concentration of the at least one oxidizing agent (G) is not more than 10 wt. %, more preferably not more than 5 wt. %, more preferably not more than 3.5 wt. %, most preferably not more than 2 wt. %, in each case based on the total weight of the CMP composition (Q).
  • the concentration of the at least one oxidizing agent (G) is at least 0.01 wt. %, more preferably at least 0.05 wt. %, most preferably at least 0.5 wt. %, in each case based on the total weight of the CMP (Q).
  • the concentration of hydrogen peroxide as oxidizing agent is preferably ⁇ 1 wt. % to ⁇ 5 wt. %, more preferably ⁇ 2 wt. % to ⁇ 3.5 wt. %, for instance 2.5 wt. %, most preferably ⁇ 1 wt. % to ⁇ 2 wt. %, in each case based on the total weight of the CMP composition (Q).
  • the CMP composition (Q) of the presently claimed invention further comprises an aqueous medium (H).
  • the aqueous medium (H) can be of one type or a mixture of different types of aqueous media.
  • the aqueous medium (H) can be any medium which contains water.
  • the aqueous medium (H) is a mixture of water and an organic solvent miscible with water.
  • organic solvent include but are not limited to C 1 to C 3 alcohol, an alkylene glycol and alkylene glycol derivatives. More preferably, the aqueous medium (H) is water. Most preferably, aqueous medium (H) is de-ionized water.
  • the amounts of the components other than (H) are in total y % by weight of the CMP composition (Q), then the amount of (H) is (100 ⁇ y) % by weight of the CMP composition.
  • the amount of the aqueous medium (H) in the CMP composition (Q) is not more than 99.9 wt. %, more preferably not more than 99.6 wt. %, most preferably not more than 99 wt. %, particularly preferably not more than 98 wt. %, particularly not more than 97 wt. %, for example not more than 95 wt. %, based on the total weight of the CMP composition (Q).
  • the amount of the aqueous medium (H) in the CMP composition (Q) is at least 60 wt. %, more preferably at least 70 wt.
  • the properties of the CMP composition (Q), such as stability and polishing performance, may depend on the pH of the corresponding composition.
  • the pH value of the CMP composition (Q) is preferably not more than 14, more preferably not more than 13, most preferably not more than 12, particularly preferably not more than 11.5, particularly most preferably not more than 11, particularly not more than 10.7, for example not more than 10.5.
  • the pH value of the CMP composition (Q) is preferably at least 6, more preferably at least 7, most preferably at least 8, particularly preferably at least 8.5, particularly most preferably at least 9, particularly at least 9.5, for example at least 9.7.
  • the pH value of the CMP composition (Q) is preferably in the range of from ⁇ 6 to ⁇ 14, preferably from ⁇ 7 to ⁇ 13, more preferably from A8 to ⁇ 12, most preferably from A8 to ⁇ 11, particularly preferably from 9 to ⁇ 10.5, particularly more preferably from 9 to ⁇ 10.3, particularly most preferably in the range of from ⁇ 9.25 to ⁇ 10.
  • the pH of the CMP composition is in the range of from A8 to ⁇ 11.
  • the pH of the CMP composition is in the range of from ⁇ 9.25 to ⁇ 11.
  • the CMP composition (Q) of the presently claimed invention can further optionally contain at least one pH adjusting agent (1).
  • the at least one pH adjusting agent (1) is different from the components (A), (B), (C), (D), (E), (F) and (G).
  • the at least one pH adjusting agent (1) is selected from the group consisting of inorganic acids, carboxylic acids, amine bases, alkali hydroxides, ammonium hydroxides, including tetraalkylammonium hydroxides.
  • the at least one pH adjusting agent (1) is selected from the group consisting of nitric acid, sulfuric acid, ammonia, sodium hydroxide and potassium hydroxide.
  • the pH adjusting agent (1) is potassium hydroxide.
  • the amount of the at least one pH adjusting agent (1) is preferably not more than 10 wt. %, more preferably not more than 2 wt. %, most preferably not more than 0.5 wt. %, particularly not more than 0.1 wt. %, for example not more than 0.05 wt. %, based on the total weight of the CMP composition (Q).
  • the amount of the at least one pH adjusting agent (1) is preferably at least 0.0005 wt. %, more preferably at least 0.005 wt. %, most preferably at least 0.025 wt. %, particularly at least 0.1 wt. %, for example at least 0.4 wt. %, based on the total weight of the CMP composition (Q).
  • the CMP composition (Q) can optionally contain additives.
  • additives include but are not limited to stabilizers.
  • the additives commonly employed in CMP compositions are for example used to stabilize the dispersion, or improve the polishing performance, or the selectivity between different layers.
  • the concentration of the additives is not more than 10 wt. %, more preferably not more than 1 wt. %, most preferably not more than 0.1 wt. %, for example not more than 0.01 wt. %, based on the total weight of the CMP composition (Q).
  • the concentration of the additives is at least 0.0001 wt. %, more preferably at least 0.001 wt. %, most preferably at least 0.01 wt. %, for example at least 0.1 wt. %, based on the total weight of the CMP composition (Q).
  • CMP chemical-mechanical polishing
  • CMP chemical-mechanical polishing
  • CMP chemical-mechanical polishing
  • CMP chemical-mechanical polishing
  • C a corrosion-inhibitor (C) selected from the group consisting of unsubstituted benzotriazole, substituted benzotriazoles, unsubstituted 1,2,3-triazole, substituted 1,2,3-triazoles, unsubstituted 1,2,4-triazole and substituted 1,2,4-triazoles;
  • G an oxidizing agent selected from the group consisting of organic or inorganic peroxide, a persulfate, an iodate, periodic acid, a periodate, a permanganate, perchloric acid, a perchlorate, bromic acid and a bromate; and
  • CMP chemical-mechanical polishing
  • dicarboxylic acid selected from the group consisting of malonic acid, tartaric acid, succinic acid, adipic acid, malic acid, maleic acid, oxalic acid and fumaric acid;
  • C a corrosion-inhibitor (C) selected from the group consisting of unsubstituted benzotriazole, substituted benzotriazoles, unsubstituted 1,2,3-triazole, substituted 1,2,3-triazoles, unsubstituted 1,2,4-triazole and substituted 1,2,4-triazoles;
  • G an oxidizing agent selected from the group consisting of organic or inorganic peroxide, a persulfate, an iodate, periodic acid, a periodate, a permanganate, perchloric acid, a perchlorate, bromic acid and a bromate; and
  • CMP chemical-mechanical polishing
  • dicarboxylic acid selected from the group consisting of malonic acid, tartaric acid, succinic acid, adipic acid, malic acid, maleic acid, oxalic acid and fumaric acid;
  • C a corrosion-inhibitor (C) selected from the group consisting of unsubstituted benzotriazole and substituted benzotriazoles;
  • a pad-cleaning agent selected from poly (acrylic acid-co-maleic acid) copolymers with a number average molecular weight in the range of ⁇ 500 g/mol to ⁇ 10000 g/mol determined according to gel permeation chromatography at 40° C.;
  • CMP chemical-mechanical polishing
  • C a corrosion-inhibitor (C) selected from the group consisting of unsubstituted benzotriazole and substituted benzotriazoles;
  • a pad-cleaning agent selected from poly (acrylic acid-co-maleic acid) copolymers with a number average molecular weight in the range of ⁇ 500 g/mol to ⁇ 10000 g/mol determined according to gel permeation chromatography at 40° C.;
  • CMP chemical-mechanical polishing
  • pH of the chemical-mechanical polishing (CMP) composition is in the range of 8 to ⁇ 11.
  • CMP chemical-mechanical polishing
  • (B) ⁇ 0.001 wt. % to ⁇ 2.5 wt. % of at least one chelating agent selected from carboxylic acids;
  • weight percentages are in each case is based on the total weight of the chemical-mechanical polishing composition (CMP).
  • CMP chemical-mechanical polishing
  • (B) ⁇ 0.001 wt. % to ⁇ 2.5 wt. % of at least one chelating agent selected from carboxylic acids;
  • weight percentages are in each case is based on the total weight of the chemical-mechanical polishing composition (CMP); and wherein the pH of the chemical-mechanical polishing (CMP) composition is in the range of
  • CMP chemical-mechanical polishing
  • weight percentages are in each case is based total weight of the chemical-mechanical polishing composition (CMP).
  • CMP chemical-mechanical polishing
  • weight percentages are in each case is based total weight of the chemical-mechanical polishing composition (CMP).
  • pH of the chemical-mechanical polishing (CMP) composition is in the range of ⁇ 9.25 to ⁇ 11.
  • CMP chemical-mechanical polishing
  • weight percentages are in each case is based total weight of the chemical-mechanical polishing composition (CMP).
  • CMP chemical-mechanical polishing
  • weight percentages are in each case is based total weight of the chemical-mechanical polishing composition (CMP); and wherein the pH of the chemical-mechanical polishing (CMP) composition is in the range of ⁇ 9.25 to ⁇ 11.
  • the processes for preparation of CMP compositions are generally known. These processes may be applied to the preparation of the CMP composition of the presently claimed invention. This can be carried out by dispersing or dissolving the components described hereinabove (A), (B), (C), (D), (E), (F), (G) and other optional components in the aqueous medium (H), preferably water, and optionally by adjusting the pH value through adding an acid, a base, a buffer or a pH adjusting agent.
  • the customary and standard mixing processes and mixing apparatuses such as agitated vessels, high shear impellers, ultrasonic mixers, homogenizer nozzles or counter flow mixers, can be used.
  • the polishing process is generally known and can be carried out with the processes and the equipment under the conditions customarily used for the CMP in the fabrication of wafers with integrated circuits. There is no restriction on the equipment with which the polishing process can be carried out.
  • the typical equipment for the CMP process consists of a rotating platen which is covered with a polishing pad. Also, orbital polishers can be used.
  • the wafer is mounted on a carrier or chuck. The side of the wafer being processed is facing the polishing pad (single side polishing process). A retaining ring secures the wafer in the horizontal position.
  • the larger diameter platen is also generally horizontally positioned and presents a surface parallel to that of the wafer to be polished.
  • the polishing pad on the platen contacts the wafer surface during the planarization process.
  • the wafer is pressed onto the polishing pad.
  • Both the carrier and the platen are usually caused to rotate around their respective shafts extending perpendicular from the carrier and the platen.
  • the rotating carrier shaft may remain fixed in position relative to the rotating platen or may oscillate horizontally relative to the platen.
  • the direction of rotation of the carrier is typically, though not necessarily, the same as that of the platen.
  • the speeds of rotation for the carrier and the platen are generally, though not necessarily, set at different values.
  • the CMP composition of the presently claimed invention is usually applied onto the polishing pad as a continuous stream or in dropwise fashion. Customarily, the temperature of the platen is set at temperatures of from 10 to 70° C.
  • the load on the wafer can be applied by a flat plate made of steel for example, covered with a soft pad that is often called backing film. If more advanced equipment is being used a flexible membrane that is loaded with air or nitrogen pressure presses the wafer onto the pad. Such a membrane carrier is preferred for low down force processes when a hard-polishing pad is used, because the down pressure distribution on the wafer is more uniform compared to that of a carrier with a hard platen design. Carriers with the option to control the pressure distribution on the wafer may also be used according to the presently claimed invention. They are usually designed with several different chambers that can be loaded to a certain degree independently from each other.
  • the down pressure or down force is a downward pressure or a downward force which is applied by the carrier to the wafer pressing it against the pad during CMP.
  • This down pressure or down force can for example be measured in pound per square inch (abbreviated as psi)
  • the down pressure is 2 psi or lower.
  • the down pressure is in the range of from 0.1 psi to 1.9 psi, more preferably in the range of from 0.3 psi to 1.8 psi, most preferably in the range of from 0.4 psi to 1.7 psi, particularly preferable in the range of from 0.8 psi to 1.6 psi, for example 1.5 psi.
  • An aspect of the presently claimed invention is directed to a method for the manufacture of semiconductor devices comprising the chemical-mechanical polishing of a substrate in the presence of the chemical-mechanical polishing composition (Q) described hereinabove and hereinbelow.
  • the method for the manufacture of semiconductor devices comprises the CMP of a substrate comprising a surface region containing or consisting of at least one copper layer and/or at least one ruthenium layer or alloys thereof.
  • the substrate comprises at least one copper layer and/or at least one ruthenium layer or alloys thereof.
  • the semiconductor device which can be manufactured by the process according to the presently claimed invention is not particularly limited.
  • the semiconductor devices can be electronic components comprising semiconducting materials, as for example silicon, germanium, and Ill-V materials.
  • Semiconductor devices can be those which are manufactured as single discrete devices or those which are manufactured as integrated circuits (ICs) consisting of several devices manufactured and interconnected on a wafer.
  • Semiconductor devices can be two terminal devices for example a diode, three terminal devices for example a bipolar transistor, four terminal devices for example a Hall effect sensor or multi-terminal devices.
  • the semiconductor device is a multi-terminal device.
  • Multi-terminal devices can be logic devices as integrated circuits and microprocessors or memory devices as random-access memory (RAM), read only memory (ROM) and phase change random access memory (PCRAM).
  • RAM random-access memory
  • ROM read only memory
  • PCRAM phase change random access memory
  • the semiconductor device is a multi-terminal logic device.
  • the semiconductor device is an integrated circuit or microprocessor.
  • ruthenium is used as adhesion or barrier layer for copper interconnects.
  • ruthenium In its nano-crystalline form ruthenium is contained for example in memory devices and as metal gate in MOSFET. Ruthenium can also be used as a seed to enable plating of copper by electro-deposition. Ruthenium and ruthenium alloy can also be used as wiring instead of copper for one or more layers.
  • a capacitor CAP can be formed by successive layers of metal, insulator, metal (MIM) and a thin film resistor at the same level. Circuit designers can now wire to the TaN thin film resistor at the lowest metal level, which reduces parasitics and allows more efficient usage of the existing wiring levels.
  • the excess copper and/or ruthenium and the adhesion/barrier layer comprising ruthenium in form of, for example metal nitrides or metal carbon nitrides, such as Ru/TaN, Ru/TiN, Ru/TaCN, Ru/TiCN, or for example as a single ruthenium alloy layer, such as RuMo, RuTa, RuTi and RuW above the dielectrics, can be removed by the chemical mechanical polishing process according to the presently claimed invention.
  • this ruthenium and/or ruthenium alloy can be produced or obtained in different ways.
  • Ruthenium and ruthenium alloy can be produced by ALD, PVD or CVD processes. It is possible that ruthenium or ruthenium alloy is deposited onto a barrier material. Proper materials for barrier application are well known in the arts.
  • the barrier prevents metal atoms or ions like ruthenium or copper from diffusing into the dielectric layer and improves the adhesion properties of the conductive layer.
  • Ta/TaN, Ti/TiN can be used.
  • this ruthenium and/or ruthenium alloy can be of any type, form, or shape.
  • This ruthenium and/or ruthenium alloy preferably has the shape of a layer and/or overgrowth. If this ruthenium and/or ruthenium alloy has the shape of a layer and/or overgrowth, the ruthenium and/or ruthenium alloy content is preferably more than 90%, more preferably more than 95%, most preferably more than 98%, particularly more than 99%, for example more than 99.9% by weight of the corresponding layer and/or overgrowth.
  • This ruthenium and/or ruthenium alloy has been preferably filled or grown in trenches or plugs between other substrates, more preferably filled or grown in trenches or plugs in dielectric materials like for example SiO2, silicon, low-k (BD1, BD2) or ultra-low-k materials, or other isolating and semiconducting material used in the semiconductor industry.
  • dielectric materials like for example SiO2, silicon, low-k (BD1, BD2) or ultra-low-k materials, or other isolating and semiconducting material used in the semiconductor industry.
  • TSV Through Silicon Vias
  • insulated materials such as polymers
  • photoresist and/or polyimide can be used as insulating material between the subsequent processing steps of wet etch and CMP for insulating/isolating properties after revealing the TSV from the backside of the wafer.
  • barrier materials to prevent metal ions from diffusing into the dielectric material can for example be Ti/TiN, Ta/TaN or Ru or Ru-alloys, Co or Co-alloys.
  • the CMP composition of the presently claimed invention preferably removes the barrier layers and maintain the integrity of the low-k and ultra-low-k materials, i.e., provides a particularly high selectivity of barrier layer over low-k or ultra-low-k materials regarding the material removal rates (MRRs).
  • MRRs material removal rates
  • the CMP composition of the presently claimed invention provides at least one of the following properties: (a) high MRR of barrier layer, (b) low MRR of copper layer, (c) low MRR of low-k or ultra-low-k materials, (d) high selectivity of barrier layer over copper layer with regard to MRR, (e) high selectivity of barrier layer over low-k and ultra-low-k materials with regard to MRR.
  • the CMP composition of the presently claimed invention provides at least one of the following properties: (a′) high MRR of tantalum or tantalum nitride, (b′) low MRR of copper layer, (c′) low MRR of low-k or ultra-low-k materials, (d′) high selectivity of ruthenium, tantalum or tantalum nitride over copper with regard to MRR, and (e′) high selectivity of tantalum nitride or ruthenium over low-k or ultra-low-k materials with regard to MRR. Furthermore, the CMP composition of the presently claimed invention provides a long shelf life, while high MRR of barrier layer is maintained.
  • the selectivity of ruthenium to copper with regard to the material removal rate is preferably higher than 0.05, more preferably higher than 0.2, most preferably higher than 1, particularly higher than 2.5, especially higher than 20, for example higher than 40.
  • the selectivity may be advantageously adjusted by the combination of high material removal rate (MRR) of ruthenium and low MRR of copper or the other way around.
  • the CMP composition of the presently claimed invention can be used in the CMP process as ready-to-use slurry, they have a long shelf-life and show a stable particle size distribution over long time. Thus, they are easy to handle and to store. They show an excellent polishing performance, particularly with regard to (a′) high MRR of tantalum nitride, (b′) high MRR of ruthenium (c′) low MRR of copper layer, (d′) low MRR of low-k or ultra-low-k materials, (e′) high selectivity of tantalum nitride or ruthenium over copper with regard to MRR, and (e′) high selectivity of tantalum nitride or ruthenium over low-k or ultra-low-k materials with regard to MRR.
  • the CMP composition of the presently claimed invention shows a longer shelf life, agglomeration within the CMP composition of the presently claimed invention can be avoided, while high MRR of barrier layer was maintained. Since the amounts of its components are held down to a minimum, the CMP composition (Q) and the CMP process according to the presently claimed invention can be used or applied in a cost-effective way.
  • An aspect of the presently claimed invention is directed to a use of the chemical-mechanical polishing composition of the presently claimed invention for chemical-mechanical polishing of a substrate used in the semiconductor industry.
  • the use of the chemical-mechanical polishing composition of the presently claimed invention for chemical-mechanical polishing of a substrate the substrate comprises
  • the use of the chemical-mechanical polishing composition of the presently claimed invention for chemical-mechanical polishing of a substrate the substrate comprises
  • Silica based slurries were used to polish copper and/or ruthenium coated wafers.
  • the slurry composition comprises:
  • the oxidizing agent (G) (1% H 2 O 2 ) was added right before (1 to 15 min) the slurry had been used for chemical mechanical polishing (CMP).
  • aqueous stock solution of each compound (B), (C), (D), (E), (F) and (G) are prepared by dissolving the desired amount of the respective compound in ultra-pure water (UPW).
  • KOH is preferably used to support dissolution.
  • the pH of the stock solution is adjusted to ⁇ pH 9 by KOH.
  • the stock solutions of (B) have a concentration of the respective additive of 10 wt. %, that of (C), (D) and (E) of 1.0 wt. %.
  • a dispersion is used as provided by the supplier, typically about 20%-30% abrasive concentration by weight.
  • the oxidizing agent (G) is used as 30 wt. % stock solutions.
  • aqueous cocoon-shaped silica particle dispersion with 20 wt. % solid content was dispersed on a carbon foil and was dried.
  • the dried dispersion was analyzed by using Energy Filtered-Transmission Electron Microscopy (EF-TEM) (120 kilo volts) and Scanning Electron Microscopy secondary electron image (SEM-SE) (5 kilo volts).
  • EF-TEM Energy Filtered-Transmission Electron Microscopy
  • SEM-SE Scanning Electron Microscopy secondary electron image
  • the EF-TEM image with a resolution of 2 k, 16 Bit, 0.6851 nm/pixel was used for the analysis.
  • the images were binary coded using the threshold after noise suppression. Afterwards the particles were manually separated. Overlying and edge particles were discriminated and not used for the analysis. ECD, shape factor and sphericity as defined before were calculated and statistically classified.
  • A2 are agglomerated particles with a specific surface area of around 90 m 2 /g having an average primary particle size (d1) of 35 nm and an average secondary particle size (d2) of 75 nm (as determined using dynamic light scattering techniques via a Horiba instrument) (for example Fuso® PL-3H) were used.
  • Apparatus Mirra-mesa (Applied Materials) down pressure: 1.5 psi for all substrates, Ru 2 psi; polishing table/carrier speed: 93/87 rpm; slurry flow rate: 200 ml/min; polishing time: Ru 60 s, Cu 60 s, TEOS 60 s, TaN 60 s, BD2 60 s polishing pad: Fujibo H800 NW; conditioning tool: 3M A189L diamond abrasive disk for AMAT CMP machines, in-situ conditioning with 5 lbf down force.
  • Apparatus GnP (G&P Technology) down pressure: 2 psi for coupon wafer polishing table/carrier speed: 93/87 rpm slurry flow rate: 200 ml/min polishing time: Ru 60 s, Cu 60 s, TEOS 60 s, TaN 60 s, BD2 60 s for main polishing.
  • polishing pad Fujibo H800 NW conditioning tool: A189L conditioning type: In-situ. Oscillation. 65 rpm, downforce 5 lbf for main polishing 60s
  • the slurry is stirred in a local supply station.
  • Cu and Ru film Resistage RG-120/RT-80, 4 point probe instrument (NAPSON Corporation)
  • TEOS Opti-Probe 2600 (Therma Wave, KLA-Tencor)
  • TaN Resistage RG-120/RT-80
  • 4 point probe instrument NAPSON Corporation
  • BD1 Opti-Probe 2600 (Therma Wave, KLA-Tencor)
  • Film thickness is measured pre and post CMP with a 49-point scan (5 mm edge exclusion). The thickness loss is averaged and divided by the polishing time to give the material removal rate (MRR).
  • MRR material removal rate
  • Ru coated wafers Resistage RG-120/RT-80, 4-point probe instrument (NAPSON Corporation) Cu coated wafers: Resistage RG-120/RT-80, 4-point probe instrument (NAPSON Corporation) TaN: Resistage RG-120/RT-80, 4-point probe instrument (NAPSON Corporation)
  • TEOS Opti-Probe 2600 (Therma Wave, KLA-Tencor)
  • BD2 Opti-Probe 2600 (Therma Wave, KLA-Tencor)
  • BD1 Opti-Probe 2600 (Therma Wave, KLA-Tencor)
  • the pH—value is measured with a pH combination electrode (Schott, blue line 22 pH electrode).
  • CMP Chemical mechanical polishing
  • Pad staining experiment with copper (Cu) ions Pad staining experiments with copper ions were conducted by adding 50 ppm CuSO4.5H2O to the slurry prior polishing on a Fujibo H804 pad and the mixture was then applied on the pad while polishing a ruthenium (Ru) wafer until the coated ruthenium film is totally removed from the wafer surface. Then the pad was removed from the polisher to let it dry completely.
  • Cu copper
  • Pad picture was taken, and picture analysis was done by using an imaging software. This experiment resembles accumulation of ruthenium and copper debris on pad. Fujibo H804 pad was used in these experiments for easier analysis of the stains (species accumulation) on the pad since it is a white pad.
  • Pad staining experiments with Cu ions were conducted by adding 50 ppm CuSO 4 .5H 2 O to the slurry prior polishing on a Fujibo H804 pad and the mixture was then applied on the pad while polishing a ruthenium (Ru) coupon size of 30 mm ⁇ 30 mm until the coated ruthenium film is totally removed from the coupon surface. (Ru coupon is diced out of a 200 mm Ru wafer).
  • Pad staining experiments were quantified for comparison of the different slurry compositions. After pad staining experiments were performed, the polishing pad used was taken out from the polisher and then dried at room temperature. The picture of the pad was taken by using a digital camera under defined lightening conditions (the same for all pads) and a defined area of the picture (500 ⁇ 500 pixels) was cropped using a software for gray scale analysis. The software generates a value in between 0 (dark) and 255 (white). For quantitative analysis of pad pictures, mean value for the analyzed pixel area was taken.
  • FIG. 1 shows the correlation results of GnP ruthenium coupon polishing and 200 mm Mirra Mesa wafer polishing with and without Cu ions. As it is displayed in FIG. 1 , there is a reasonable correlation between GnP ruthenium coupon polishing and 200 mm wafer polishing. It can be concluded that the generated pad staining results are independent of the size of the ruthenium wafer/coupon.
  • Tables 1 and 2 shows the material removal rate (MRR) for different substrates and the pad staining with and without copper ions.
  • MRR material removal rate
  • Addition of Planapur® CP 12 SEG prevented adsorption of ruthenium, copper and ruthenium debris compared to the slurry without these additives at pH of 9.25.
  • Tables 1 and 2 shows the impact of pad-cleaning agent Planapur® CP 12 SEG along with BTA that generates the cleanest pad surface.
  • Table 2 shows the most significant impact of pH in material removal rates.
  • the CMP compositions of the examples according to the presently claimed invention show improved performance, in terms of ruthenium to copper selectivity, high material removal rates of ruthenium at low abrasive (A) concentration, low material removal rates of the low k material, a low etching behavior and a high dispersion stability.
  • the pad cleaning agent Planapur® CP 12 SEG adsorb to the Cu/Ru debris and make the debris more hydrophilic, which makes the removal of the debris from the polishing environment easier.

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