WO2023032714A1 - Composition de polissage - Google Patents

Composition de polissage Download PDF

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Publication number
WO2023032714A1
WO2023032714A1 PCT/JP2022/031389 JP2022031389W WO2023032714A1 WO 2023032714 A1 WO2023032714 A1 WO 2023032714A1 JP 2022031389 W JP2022031389 W JP 2022031389W WO 2023032714 A1 WO2023032714 A1 WO 2023032714A1
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WIPO (PCT)
Prior art keywords
polishing
polishing composition
less
abrasive grains
hlm
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PCT/JP2022/031389
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English (en)
Japanese (ja)
Inventor
誼之 田邉
真希 浅田
公亮 土屋
Original Assignee
株式会社フジミインコーポレーテッド
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Priority to JP2023545450A priority Critical patent/JPWO2023032714A1/ja
Publication of WO2023032714A1 publication Critical patent/WO2023032714A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting

Definitions

  • the present invention relates to polishing compositions.
  • This application claims priority based on Japanese Patent Application No. 2021-142155 filed on September 1, 2021, the entire contents of which are incorporated herein by reference.
  • the polishing process includes, for example, a preliminary polishing process (preliminary polishing process) and a final polishing process (final polishing process).
  • the preliminary polishing process includes, for example, a rough polishing process (primary polishing process) and an intermediate polishing process (secondary polishing process).
  • Technical documents relating to the polishing composition used in the polishing step include, for example, Patent Documents 1 to 3.
  • HLM hard laser marks
  • the HLM portion itself of the silicon wafer is not used in the final product, if the degraded layer is not properly polished in the polishing step after applying the HLM, it may become raised and the yield may decrease more than necessary. .
  • the altered layer is altered to polysilicon or the like by the energy of the laser beam, making it difficult to polish. Therefore, in recent years, there has been a particular demand for a silicon wafer polishing composition capable of flattening the bumps on the HLM periphery (hereinafter also simply referred to as "bumps").
  • the easily polished portion other than the periphery of the HLM is applicable.
  • a situation may occur in which the portion of the HLM peripheral portion that is difficult to polish is selectively polished, and as a result, it is difficult to improve the ability to eliminate the bumps.
  • polishing that requires a polishing rate equal to or higher than a predetermined value, it tends to be difficult to achieve both the polishing rate and the elimination of the protuberance of the peripheral edge of the HLM. It would be practically useful if a polishing composition was provided that satisfies a practical polishing rate and has an excellent ability to eliminate protuberances on the periphery of the HLM.
  • the present invention has been made in view of this point, and an object thereof is to provide a polishing composition capable of maintaining both the polishing rate and eliminating the protuberance of the HLM peripheral edge.
  • a polishing composition contains abrasive grains, a basic compound, a lithium salt, and water.
  • the elimination of the HLM peripheral ridges means the height from the reference plane (reference plane) around the HLM of the substrate to be polished (typically a semiconductor substrate, such as a silicon wafer) to the highest point of the ridges. to make smaller.
  • the height from the reference surface around the HLM of the substrate to the highest point of the protrusion can be measured, for example, by the method described in Examples below.
  • the lithium salt is normal salt.
  • the lithium salt is at least one selected from the group consisting of lithium chloride, lithium carbonate and lithium sulfate.
  • the swelling elimination effect can be exhibited more effectively.
  • quaternary ammonium compounds are included as the basic compound.
  • a combination of a quaternary ammonium compound as a basic compound and a lithium salt it is easy to achieve both a desired polishing rate and elimination of protuberances on the periphery of the HLM.
  • a polishing composition containing a quaternary ammonium compound as a basic compound is also preferable in terms of improving the polishing rate.
  • a polishing composition according to a preferred embodiment contains silica particles as the abrasive grains.
  • silica particles as abrasive grains.
  • the effect of removing bumps can be more effectively exhibited while maintaining the polishing rate required for such polishing.
  • the polishing composition disclosed here can be used for polishing various materials. For example, it can be suitably used in a polishing step of a polishing object having a silicon material.
  • a polishing composition for example, for polishing a polishing object having a silicon material and having a surface to which an HLM is attached, a practical polishing rate can be maintained and De-bulging of the HLM perimeter can be achieved. Further, according to the polishing composition, it is possible to achieve a high polishing rate in polishing an object having a silicon material.
  • a preliminary polishing step for example, a preliminary polishing step for a polishing object having a silicon material
  • a higher polishing rate is required
  • maintenance of the polishing rate and HLM peripheral edge reduction can be achieved. Coexistence with elimination of bumps can be exhibited more effectively.
  • the polishing composition disclosed herein contains abrasive grains.
  • the material and properties of the abrasive grains are not particularly limited, and can be appropriately selected according to the mode of use of the polishing composition.
  • Examples of abrasive grains include inorganic particles, organic particles, and organic-inorganic composite particles.
  • inorganic particles include oxide particles such as silica particles, alumina particles, cerium oxide particles, chromium oxide particles, titanium dioxide particles, zirconium oxide particles, magnesium oxide particles, manganese dioxide particles, zinc oxide particles, and red iron oxide particles; nitride particles such as silicon nitride particles and boron nitride particles; carbide particles such as silicon carbide particles and boron carbide particles; diamond particles; and carbonates such as calcium carbonate and barium carbonate.
  • organic particles include polymethyl methacrylate (PMMA) particles, poly(meth)acrylic acid particles, polyacrylonitrile particles, and the like.
  • PMMA polymethyl methacrylate
  • (meth)acrylic acid is a generic term for acrylic acid and methacrylic acid.
  • Abrasive grains can be used singly or in combination of two or more.
  • abrasive grains inorganic particles are preferable, and particles made of oxides of metals or semi-metals are particularly preferable.
  • Suitable examples of abrasive grains that can be used in the technology disclosed herein include silica particles.
  • the technology disclosed herein can be preferably implemented, for example, in a mode in which the abrasive grains are substantially composed of silica particles.
  • substantially means that 95% by weight or more (preferably 98% by weight or more, more preferably 99% by weight or more, and may be 100% by weight) of the particles constituting the abrasive grains It refers to silica particles.
  • silica particles is not particularly limited and can be selected as appropriate.
  • a silica particle may be used individually by 1 type, and may be used in combination of 2 or more type.
  • Examples of silica particles include colloidal silica, fumed silica, precipitated silica, and the like. Colloidal silica is particularly preferred because it is less likely to cause scratches on the surface of the object to be polished and can exhibit good polishing performance (such as performance to reduce surface roughness).
  • the type of colloidal silica is not particularly limited and can be selected as appropriate. Colloidal silica may be used individually by 1 type, and may be used in combination of 2 or more type.
  • colloidal silica produced using water glass (sodium silicate) as a raw material by an ion exchange method or alkoxide colloidal silica can be preferably employed.
  • the alkoxide colloidal silica is colloidal silica produced by a hydrolytic condensation reaction of alkoxysilane.
  • the abrasive grains contained in the polishing composition may be in the form of primary particles or may be in the form of secondary particles in which a plurality of primary particles are associated. Further, the abrasive grains in the form of primary particles and the abrasive grains in the form of secondary particles may be mixed. In a preferred embodiment, at least part of the abrasive grains are contained in the polishing composition in the form of secondary particles.
  • the average primary particle size of the abrasive grains is not particularly limited, but is preferably 5 nm or more, more preferably 10 nm or more, and particularly preferably 10 nm or more, from the viewpoint of maintaining the polishing rate and improving the ability to eliminate bumps. is 20 nm or more. From the viewpoint of obtaining a higher polishing effect, the average primary particle size is preferably 25 nm or more, more preferably 30 nm or more. Abrasive grains having an average primary particle size of 40 nm or more may be used. In some embodiments, the average primary particle size can be, for example, greater than 40 nm, greater than 45 nm, greater than 50 nm.
  • the average primary particle size of the abrasive grains is preferably 200 nm or less, more preferably 150 nm or less, still more preferably 120 nm or less, and particularly preferably 100 nm or less. In some embodiments, the average primary particle size may be 75 nm or less, or 60 nm or less.
  • the specific surface area can be measured using, for example, a surface area measuring device manufactured by Micromeritex, trade name "Flow Sorb II 2300".
  • the average secondary particle size of the abrasive grains is not particularly limited, and can be appropriately selected from a range of, for example, about 15 nm to 300 nm. From the viewpoint of improving the ability to eliminate bumps, the average secondary particle size is preferably 30 nm or more, more preferably 35 nm or more. In some embodiments, the average secondary particle size may be, for example, 40 nm or greater, 45 nm or greater, preferably 50 nm or greater, even 60 nm or greater, or 65 nm or greater (eg, 70 nm or greater). Also, from the viewpoint of preventing scratches, the average secondary particle size is generally advantageously 250 nm or less, preferably 200 nm or less, and more preferably 150 nm or less. In some embodiments, the average secondary particle size may be 120 nm or less, or 110 nm or less.
  • the average secondary particle size of abrasive grains refers to the particle size measured by the dynamic light scattering method.
  • it can be measured using model "FPAR-1000" manufactured by Otsuka Electronics Co., Ltd. or its equivalent.
  • the shape (outer shape) of the abrasive grains may be spherical or non-spherical.
  • specific examples of non-spherical particles include peanut-shaped (that is, peanut shell-shaped), cocoon-shaped, confetti-shaped, and rugby ball-shaped particles.
  • the average aspect ratio of abrasive grains is not particularly limited.
  • the average aspect ratio of the abrasive grains is theoretically 1.0 or more, can be 1.05 or more, 1.10 or more, and may be 1.15 or more. An increase in the average aspect ratio tends to improve the polishing rate.
  • the average aspect ratio of the abrasive grains is greater than 1.2 (specifically greater than 1.20), such as 1.22 or greater. Abrasive grains having an average aspect ratio of greater than 1.2 are typical examples of the non-spherical abrasive grains described above.
  • the average aspect ratio of the abrasive grains is preferably 3.0 or less, more preferably 2.0 or less, from the viewpoint of reducing scratches and improving the stability of polishing.
  • the average aspect ratio of the abrasive grains can be, for example, 1.5 or less, 1.4 or less, or 1.3 or less.
  • the shape (outer shape) and average aspect ratio of the abrasive grains can be grasped, for example, by electron microscope observation.
  • a specific procedure for grasping the average aspect ratio for example, using a scanning electron microscope (SEM), for a predetermined number (for example, 200) of abrasive particles that can recognize the shape of independent particles, each particle Draw the smallest rectangle that bounds the image. Then, regarding the rectangle drawn for each particle image, the value obtained by dividing the length of the long side (the value of the major axis) by the length of the short side (the value of the minor axis) is the ratio of the major axis to the minor axis (aspect ratio ).
  • the average aspect ratio can be obtained by arithmetically averaging the aspect ratios of the predetermined number of particles.
  • the content of abrasive grains is not particularly limited, and can be set as appropriate according to the purpose.
  • the content of abrasive grains relative to the total weight of the polishing composition may be, for example, 0.01% by weight or more, 0.05% by weight or more, or 0.1% by weight or more.
  • the abrasive content may be 0.2 wt% or more, 0.5 wt% or more, or 0.6 wt% or more.
  • the content of abrasive grains may be, for example, 10% by weight or less, 5% by weight or less, or 3% by weight or less. Well, it may be 2% by weight or less, 1.5% by weight or less, 1.2% by weight or less, or 1.0% by weight or less. These contents can be preferably applied to the contents in the polishing liquid (working slurry) supplied to the object to be polished, for example.
  • the content of abrasive grains is usually 50% by weight or less from the viewpoint of storage stability and filterability. appropriate, and more preferably 40% by weight or less. Also, from the viewpoint of making the most of the advantage of using a concentrated liquid, the content of abrasive grains is preferably 1% by weight or more, more preferably 5% by weight or more.
  • the polishing composition disclosed herein contains a basic compound.
  • the basic compound refers to a compound that has the function of increasing the pH of the polishing composition when added to the composition.
  • the basic compound functions to chemically polish the surface to be polished, and can contribute to improving the polishing rate.
  • the basic compounds disclosed herein do not include lithium salts.
  • the basic compound may be an organic basic compound or an inorganic basic compound.
  • a basic compound can be used individually by 1 type or in combination of 2 or more types.
  • organic basic compounds include quaternary ammonium salts such as tetraalkylammonium salts.
  • Anions in the above ammonium salts can be, for example, OH ⁇ , F ⁇ , Cl ⁇ , Br ⁇ , I ⁇ , ClO 4 ⁇ , BH 4 ⁇ , HCO 3 ⁇ and the like.
  • quaternary ammonium salts such as choline, tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrapropylammonium hydroxide, tetrabutylammonium hydroxide, and tetramethylammonium hydrogen carbonate can be preferably used.
  • tetramethylammonium hydroxide is preferred.
  • organic basic compounds include quaternary phosphonium salts such as tetraalkylphosphonium salts.
  • Anions in the above phosphonium salts can be, for example, OH ⁇ , F ⁇ , Cl ⁇ , Br ⁇ , I ⁇ , ClO 4 ⁇ , BH 4 ⁇ , HCO 3 ⁇ and the like.
  • halides and hydroxides of tetramethylphosphonium, tetraethylphosphonium, tetrapropylphosphonium, tetrabutylphosphonium and the like can be preferably used.
  • organic basic compounds include methylamine, dimethylamine, trimethylamine, ethylamine, diethylamine, triethylamine, ethylenediamine, monoethanolamine, N-( ⁇ -aminoethyl)ethanolamine, hexamethylenediamine, diethylenetriamine, triethylene.
  • amines such as tetramine
  • piperazines such as 1-(2-aminoethyl)piperazine and N-methylpiperazine
  • azoles such as imidazole and triazole
  • guanidine
  • inorganic basic compounds include ammonia; ammonia, alkali metal or alkaline earth metal hydroxides; ammonia, alkali metal or alkaline earth metal carbonates; ammonia, alkali metal or alkaline earth metal hydrogen carbonates. salt and the like; and the like.
  • specific examples of the hydroxide include potassium hydroxide and sodium hydroxide.
  • Specific examples of the carbonate or hydrogencarbonate include ammonium hydrogencarbonate, ammonium carbonate, potassium hydrogencarbonate, potassium carbonate, sodium hydrogencarbonate and sodium carbonate.
  • Preferred basic compounds include ammonia, potassium hydroxide, sodium hydroxide, tetramethylammonium hydroxide, tetraethylammonium hydroxide, ammonium hydrogen carbonate, ammonium carbonate, potassium hydrogen carbonate, potassium carbonate, sodium hydrogen carbonate and sodium carbonate. . Preferred among them are ammonia, potassium hydroxide, sodium hydroxide, tetramethylammonium hydroxide and potassium carbonate.
  • Preferred basic compounds from the standpoint of improving swelling dissolving properties include quaternary ammoniums (quaternary ammonium salts). The quaternary ammoniums may be used singly or in combination of two or more. Tetramethylammonium hydroxide is particularly preferably used. From the viewpoint of improving the polishing rate, it is preferable to use a carbonate such as potassium carbonate.
  • the content of the basic compound with respect to the total amount of the polishing composition is preferably 0.01% by weight or more, more preferably 0.05% by weight or more, and still more preferably 0.1% by weight, from the viewpoint of polishing rate and swelling elimination property. % or more. Stability can also be improved by increasing the content of basic compounds.
  • the upper limit of the content of the basic compound is suitably 5% by weight or less, preferably 2% by weight or less, more preferably 1% by weight or less, still more preferably 1% by weight or less from the viewpoint of surface quality and the like. It is 0.5% by weight or less.
  • the said content points out the total content of 2 or more types of basic compounds.
  • the content of the basic compound is usually 10% by weight or less from the viewpoint of storage stability and filterability. suitable, and more preferably 5% by weight or less.
  • the content of the basic compound is preferably 0.1% by weight or more, more preferably 0.5% by weight or more, and still more preferably 0.9% by weight or more. is.
  • the weight ratio ( CB / CA ) of the basic compound content CB to the abrasive grain content CA in the polishing composition is not particularly limited as long as the effect of the technology disclosed herein is exhibited. .
  • the ratio (C B /C A ) is, for example, about 0.01 or more, preferably 0.05 or more, more preferably 0.05 or more, more preferably It is 0.1 or more, and may be 0.2 or more, for example. From the viewpoint of mechanical polishing with abrasive grains and dispersion stability of the composition, the above ratio (C B /C A ) is, for example, about 1 or less, preferably 0.8 or less. , more preferably 0.6 or less, and may be, for example, 0.5 or less.
  • the polishing composition disclosed herein contains a lithium salt.
  • a polishing composition containing a lithium salt can effectively eliminate the swelling of the HLM peripheral edge while maintaining the polishing rate.
  • Lithium ions, which constitute the lithium salt have a high affinity for the HLM periphery, and are therefore thought to be able to act effectively on the HLM periphery.
  • the polishing composition contains abrasive grains, a basic compound, and a lithium salt, the effect of mechanical polishing by the abrasive grains, promoting polishing (chemical polishing) by the basic compound, and improving workability of the HLM periphery by the lithium salt. It is thought that the The mechanism described above is the inventor's consideration based on experimental results, and the technology disclosed herein should not be construed as being limited to the mechanism described above.
  • lithium salt examples include lithium chloride, lithium bromide, lithium fluoride, lithium nitrate, lithium sulfate, lithium carbonate, lithium hydrogen carbonate, lithium acetate, and lithium hydroxide.
  • One of the lithium salts may be used alone, or two or more may be used in combination.
  • the lithium salt may be a normal salt generated by the reaction of acid-derived hydrogen ions (H + ) and base-derived hydroxide ions (OH ⁇ ) in just proportion.
  • a lithium salt that is a normal salt in this way, there is a tendency that the swelling elimination effect is exhibited more effectively.
  • lithium salts include lithium chloride, lithium bromide, lithium fluoride, lithium nitrate, lithium sulfate, lithium carbonate, and lithium acetate.
  • lithium chloride, lithium sulfate, and lithium carbonate are preferable, and lithium sulfate and lithium carbonate are more preferable from the viewpoint of the swelling elimination effect.
  • Lithium chloride and lithium sulfate are preferred from the viewpoint of maintaining and improving the polishing rate.
  • the molar concentration of the lithium salt in the polishing composition (the total molar concentration thereof when containing a plurality of types of lithium salts) is not particularly limited. From the viewpoint of achieving higher processability at the periphery, the concentration is preferably 3 mmol/L or more, more preferably 5 mmol/L or more, and still more preferably 10 mmol/L or more. From the viewpoint of dispersion stability and the like, the molar concentration of the lithium salt is, for example, about 1000 mmol/L or less, preferably 100 mmol/L or less, more preferably 50 mmol/L or less, and 30 mmol/L. /L or less.
  • the weight ratio (C L /C B ) of the content C L of the lithium salt to the content C B of the basic compound in the polishing composition is not particularly limited.
  • the weight ratio (C L /C B ) can be appropriately set so as to maintain or improve the polishing rate and the ability to eliminate bumps in a well-balanced manner.
  • the ratio (C L /C B ) is, for example, about 0.01 or more, preferably 0.1 or more, more preferably 0.2 or more. .3 or more, or 0.5 or more.
  • the ratio (C L /C B ) is, for example, about 10 or less, preferably 3 or less, more preferably 1 or less, and 0.7 or less. may be less than or equal to 0.4.
  • the polishing composition disclosed herein contains water.
  • water ion-exchanged water (deionized water), pure water, ultrapure water, distilled water, or the like can be preferably used.
  • the water used preferably has a total transition metal ion content of, for example, 100 ppb or less, in order to avoid as much as possible inhibition of the functions of other components contained in the polishing composition.
  • the purity of water can be increased by removing impurity ions using an ion exchange resin, removing foreign substances using a filter, and performing operations such as distillation.
  • the polishing composition disclosed herein may, if necessary, further contain an organic solvent (lower alcohol, lower ketone, etc.) that can be uniformly mixed with water.
  • water is preferably 90% by volume or more, more preferably 95% by volume or more (for example, 99 to 100% by volume) of the solvent contained in the polishing composition.
  • the polishing composition disclosed herein contains a sulfur-containing anion salt (an S-containing anion salt), a water-soluble polymer, a surfactant, a chelating agent, an antiseptic, as long as the effects of the present invention are not significantly hindered.
  • Known additives that can be used in polishing compositions for example, polishing compositions used in the polishing step of silicon wafers, such as agents and antifungal agents, may be further contained as necessary.
  • the salt of the S-containing anion may be an organic salt or an inorganic salt.
  • the salt of the S-containing anion can be used singly or in combination of two or more. It should be noted that the salts of S-containing anions disclosed herein do not include lithium salts.
  • Preferred examples of the salt of the S-containing anion include inorganic salts. Examples of the above inorganic salts include sulfates, sulfites, hydrogensulfites, thiosulfates, and the like. Cations constituting these salts are not particularly limited, and examples thereof include alkali metals (sodium, potassium, etc.), alkaline earth metals (calcium, strontium, barium, etc.), magnesium, ammonium and the like.
  • the above inorganic salts can be used singly or in combination of two or more.
  • Specific examples of the above sulfates include sodium sulfate, potassium sulfate, and ammonium sulfate.
  • Specific examples of the sulfite include sodium sulfite, potassium sulfite, ammonium sulfite, and the like.
  • Examples of the hydrogen sulfite include sodium hydrogen sulfite, potassium hydrogen sulfite, and ammonium hydrogen sulfite.
  • Examples of the thiosulfate include sodium thiosulfate and potassium thiosulfate.
  • the above S-containing anion salts include sulfonic acids such as methanesulfonic acid, ethanesulfonic acid, propanesulfonic acid, 1-butanesulfonic acid; 1,2-ethanedisulfonic acid, 1,3-propanedisulfonic acid, 1,4- disulfonic acids such as butanedisulfonic acid; hydroxyalkylsulfonic acids such as hydroxymethanesulfonic acid and 2-hydroxyethanesulfonic acid; alkylsulfuric acids such as methylsulfuric acid and ethylsulfuric acid; sulfamic acid; good.
  • the cation constituting the organic salt is not particularly limited, and examples thereof include alkali metals (sodium, potassium, etc.), alkaline earth metals (calcium, strontium, barium, etc.), magnesium, ammonium and the like.
  • the water-soluble polymer may be used singly or in combination of two or more.
  • examples of the water-soluble polymer include cellulose derivatives, starch derivatives, polymers containing oxyalkylene units, polymers containing nitrogen atoms, vinyl alcohol-based polymers, and polymers containing carboxylic acids (including anhydrides).
  • Specific examples include hydroxyethyl cellulose, pullulan, random copolymers and block copolymers of ethylene oxide and propylene oxide, polyvinyl alcohol, polyglycerin, polyisoprene sulfonic acid, polyvinyl sulfonic acid, polyallylsulfonic acid, polyisoamine Rensulfonic Acid, Polystyrene Sulfonate, Polyacrylate, Polyvinyl Acetate, Polyethylene Glycol, Polyvinylimidazole, Polyvinylcarbazole, Polyvinylpyrrolidone, Polyacryloylmorpholine, Polyvinylcaprolactam, Polyvinylpiperidine, Olefin-(Anhydrous) Maleic Acid Copolymer , styrene-(anhydride) maleic acid copolymer and the like.
  • the technology disclosed herein can also be preferably carried out in an aspect in which the polishing composition does not substantially contain a water-soluble polymer,
  • the molecular weight of the water-soluble polymer is not particularly limited in the technology disclosed herein.
  • the weight average molecular weight (Mw) of the water-soluble polymer can be about 200 ⁇ 10 4 or less, and 150 ⁇ 10 4 or less is suitable.
  • the above Mw may be about 100 ⁇ 10 4 or less, or about 50 ⁇ 10 4 or less.
  • the above Mw is usually about 0.2 ⁇ 10 4 or more, and preferably about 0.5 ⁇ 10 4 or more. and may be about 0.8 ⁇ 10 4 or more.
  • Mw of the water-soluble polymer a value based on aqueous gel permeation chromatography (GPC) (water-based, converted to polyethylene oxide) can be adopted.
  • GPC gel permeation chromatography
  • One type of surfactant may be used alone, or two or more types may be used in combination.
  • the surfactant are not particularly limited, and include anionic surfactants, nonionic surfactants, cationic surfactants, and amphoteric surfactants.
  • Use of a surfactant eg, a water-soluble organic compound having a molecular weight of less than 0.2 ⁇ 10 4 ) can improve the dispersion stability of the polishing composition.
  • Mw of the surfactant a value determined by GPC (aqueous system, converted to polyethylene glycol) or a value calculated from a chemical formula can be employed.
  • the polishing composition has a composition in which the amount of water-soluble polymer and surfactant used is limited.
  • the total amount of water-soluble polymer and surfactant in the polishing composition (e.g., polishing liquid) may be less than 0.3 wt%, may be less than 0.2 wt%, or may be less than 0.1 wt% less than, less than 0.03 wt% or less than 0.01 wt%.
  • the technique disclosed herein is an aspect in which the polishing composition does not substantially contain a water-soluble polymer and/or a surfactant, that is, at least intentionally contains a water-soluble polymer and/or a surfactant. It can also be preferably implemented in a mode that does not allow
  • the above chelating agents may be used singly or in combination of two or more.
  • chelating agents include aminocarboxylic acid chelating agents and organic phosphonic acid chelating agents.
  • aminocarboxylic acid-based chelating agents include ethylenediaminetetraacetic acid, sodium ethylenediaminetetraacetate, nitrilotriacetic acid, sodium nitrilotriacetate, ammonium nitrilotriacetate, hydroxyethylethylenediaminetriacetic acid, sodium hydroxyethylethylenediaminetriacetate, diethylenetriaminepentaacetic acid.
  • organic phosphonic acid chelating agents include 2-aminoethylphosphonic acid, 1-hydroxyethylidene-1,1-diphosphonic acid, aminotri(methylenephosphonic acid), ethylenediaminetetrakis(methylenephosphonic acid), diethylenetriaminepenta(methylenephosphonic acid), ethane-1,1-diphosphonic acid, ethane-1,1,2-triphosphonic acid, ethane-1-hydroxy-1,1-diphosphonic acid, ethane-1-hydroxy-1,1,2-triphosphonic acid , ethane-1,2-dicarboxy-1,2-diphosphonic acid, methanehydroxyphosphonic acid, 2-phosphonobutane-1,2-dicarboxylic acid, 1-phosphonobutane-2,3,4-tricarboxylic acid and ⁇ -methylphosphonic acid.
  • organic phosphonic acid-based chelating agents are more preferred. Preferred among these are ethylenediaminetetrakis(methylenephosphonic acid), diethylenetriaminepenta(methylenephosphonic acid) and diethylenetriaminepentaacetic acid. Particularly preferred chelating agents include ethylenediaminetetrakis(methylenephosphonic acid) and diethylenetriaminepenta(methylenephosphonic acid).
  • antiseptics and antifungal agents examples include isothiazoline compounds, paraoxybenzoic acid esters, phenoxyethanol, and the like.
  • the polishing composition disclosed herein preferably does not substantially contain an oxidizing agent. If the polishing composition contains an oxidizing agent, the supply of the composition oxidizes the surface of the substrate (for example, the surface of a silicon wafer) to form an oxide film, which lowers the polishing rate. Because it is possible.
  • the phrase "the polishing composition substantially does not contain an oxidizing agent" means that the polishing composition does not contain an oxidizing agent at least intentionally. is acceptable.
  • the above-mentioned trace amount means that the molar concentration of the oxidizing agent in the polishing composition is 0.0005 mol/L or less (preferably 0.0001 mol/L or less, more preferably 0.00001 mol/L or less, particularly preferably 0.0001 mol/L or less).
  • a preferred embodiment of the polishing composition does not contain an oxidizing agent.
  • the polishing composition disclosed herein can be preferably carried out in a mode containing none of hydrogen peroxide, sodium persulfate, ammonium persulfate and sodium dichloroisocyanurate, for example.
  • the polishing composition disclosed herein is supplied to an object to be polished, for example, in the form of a polishing liquid (working slurry) containing the polishing composition, and used for polishing the object to be polished.
  • the polishing composition disclosed herein may be diluted (for example, diluted with water) and used as a polishing liquid, or may be used as a polishing liquid as it is. That is, the concept of the polishing composition in the technology disclosed herein includes both a working slurry supplied to an object to be polished and used for polishing the object, and a concentrated solution (undiluted solution) of the working slurry. is included.
  • the concentration ratio of the concentrated solution may be, for example, about 2 to 140 times by volume, and usually about 5 to 80 times is appropriate.
  • the pH of the polishing composition is, for example, 8.0 or higher, preferably 8.5 or higher, more preferably 9.0 or higher, still more preferably 9.5 or higher, and 10.0 or higher (e.g., 10.5 above). As the pH increases, the polishing rate tends to improve. On the other hand, from the viewpoint of preventing dissolution of abrasive grains (for example, silica particles) and suppressing deterioration of the mechanical polishing action due to the abrasive grains, the pH of the polishing liquid is usually 12.0 or less. , is preferably 11.8 or less, more preferably 11.5 or less. These pH values can be preferably applied to both the pH of the polishing liquid (working slurry) supplied to the object to be polished and the pH of its concentrated liquid.
  • the pH of the polishing composition is measured using a pH meter (for example, a glass electrode type hydrogen ion concentration indicator (model number F-23) manufactured by Horiba, Ltd.) and a standard buffer solution (phthalate pH buffer solution pH: 4.01 (25°C), neutral phosphate pH buffer pH: 6.86 (25°C), carbonate pH buffer pH: 10.01 (25°C)) after three-point calibration can be grasped by placing the glass electrode in the polishing composition and measuring the value after 2 minutes or more have passed and the value has stabilized.
  • a pH meter for example, a glass electrode type hydrogen ion concentration indicator (model number F-23) manufactured by Horiba, Ltd.
  • a standard buffer solution phthalate pH buffer solution pH: 4.01 (25°C), neutral phosphate pH buffer pH: 6.86 (25°C), carbonate pH buffer pH: 10.01 (25°C)
  • the polishing composition disclosed herein may be a one-component type or a multi-component type including a two-component type.
  • the part A containing at least abrasive grains and the part B containing the rest of the components may be mixed and diluted at an appropriate timing as necessary to prepare the polishing liquid.
  • each component contained in the polishing composition may be mixed using a well-known mixing device such as a blade stirrer, an ultrasonic disperser, or a homomixer.
  • a well-known mixing device such as a blade stirrer, an ultrasonic disperser, or a homomixer.
  • the manner in which these components are mixed is not particularly limited. For example, all the components may be mixed at once, or they may be mixed in an appropriately set order.
  • the polishing composition disclosed herein can be used for polishing an object to be polished, for example, in a mode including the following operations. That is, a working slurry containing any one of the polishing compositions disclosed herein is prepared. Then, the polishing composition is supplied to the object to be polished, and the object is polished by a conventional method.
  • an object to be polished is set in a general polishing apparatus, and the polishing composition is supplied to the surface of the object to be polished (surface to be polished) through the polishing pad of the polishing apparatus.
  • the polishing pad is pressed against the surface of the object to be polished, and the two are relatively moved (for example, rotationally moved). Polishing of the object to be polished is completed through such a polishing process.
  • the polishing pad used in the polishing process is not particularly limited.
  • any of polyurethane foam type, non-woven fabric type, suede type, containing abrasive grains, and containing no abrasive grains may be used.
  • As the polishing apparatus a double-side polishing apparatus that polishes both surfaces of the object to be polished may be used, or a single-side polishing apparatus that polishes only one side of the object may be used.
  • the above-mentioned polishing composition may be used in a manner that it is disposed of after being used for polishing (so-called "flowing over"), or may be circulated and used repeatedly.
  • the method of recycling the polishing composition there is a method of recovering the used polishing composition discharged from the polishing apparatus in a tank and supplying the recovered polishing composition to the polishing apparatus again. .
  • the polishing composition disclosed herein can be applied to polishing objects having various materials and shapes.
  • the material of the object to be polished includes, for example, silicon materials, metals or semimetals such as aluminum, nickel, tungsten, copper, tantalum, titanium, and stainless steel, or alloys thereof; quartz glass, aluminosilicate glass, vitreous carbon, and the like. glass-like substances; ceramic materials such as alumina, silica, sapphire, silicon nitride, tantalum nitride and titanium carbide; compound semiconductor substrate materials such as silicon carbide, gallium nitride and gallium arsenide; resin materials such as polyimide resin; .
  • the object to be polished may be made of a plurality of these materials.
  • the polishing composition disclosed here is suitable for polishing an object having a silicon material.
  • the silicon material preferably contains at least one material selected from the group consisting of silicon single crystal, amorphous silicon and polysilicon.
  • the above polishing composition is particularly suitable for polishing substrates having silicon single crystals (for example, silicon wafers).
  • the polishing composition is excellent in the ability to eliminate bumps around the HLM (bump elimination property), and thus can be preferably applied to polishing a surface to be polished including the surface to which the HLM is attached.
  • the polishing composition disclosed herein can be used in a preliminary polishing step, more specifically, a rough polishing step (primary polishing step), which is the first polishing step in the polishing step, and an intermediate polishing step (secondary polishing step) that follows.
  • polishing composition disclosed herein in the preliminary polishing step to achieve both maintenance of the polishing rate and elimination of the protuberance at the periphery of the HLM. especially meaningful.
  • the silicon wafer Prior to the polishing step using the polishing composition disclosed herein, the silicon wafer is subjected to general treatments that can be applied to silicon wafers, such as lapping, etching, and application of the HLM described above. good too.
  • the silicon wafer has a surface made of silicon, for example.
  • Such a silicon wafer is preferably a silicon single crystal wafer, for example, a silicon single crystal wafer obtained by slicing a silicon single crystal ingot.
  • the polishing composition disclosed herein is suitable for use in polishing HLM-attached silicon single crystal wafers.
  • the polishing composition disclosed herein can also be suitably used for polishing an object having no HLM.
  • ⁇ Preparation of polishing composition> Colloidal silica (average primary particle size: 55 nm) as abrasive grains, tetramethylammonium hydroxide (TMAH) as a basic compound, lithium salts shown in Table 1, and ion-exchanged water were mixed to perform polishing.
  • a composition concentrate for was prepared. By diluting the obtained polishing composition concentrate with ion-exchanged water to a volume ratio of 10 times, colloidal silica was added at 1% by weight, TMAH at 0.2% by weight, and lithium salt at concentrations shown in Table 1.
  • a polishing composition was obtained. wt % in the table is weight %, and "-" indicates non-use.
  • Polishing device Single-sided polishing device manufactured by Nihon Engis Co., Ltd., model "EJ-380IN” Polishing pressure: 12kPa Surface plate rotation speed: +50 rpm (Counterclockwise rotation is positive (+). Same below.) Head rotation speed: +50 rpm Polishing pad: manufactured by Nitta Dupont, trade name "SUBA800” Polishing liquid supply rate: 50 mL/min (using continuous flow) Holding temperature of polishing environment: 25°C Polishing allowance: 4 ⁇ m
  • HLM flatness For the silicon wafer after polishing, the surface profile of the HLM periphery was measured using a stylus surface roughness profiler (SURFCOM 1500DX, manufactured by Tokyo Seimitsu Co., Ltd.). Specifically, the needle of the measuring machine was brought into contact with the surface of the substrate and moved along the HLM peripheral edge to measure the height of the raised portion and the height of the raised portion (reference plane). Then, the height [ ⁇ m] from the reference plane to the highest point of the protrusion was taken as the HLM flatness. The obtained HLM flatness was converted into a relative value (relative HLM flatness [%]) with the flatness of Comparative Example 1 as 100%. The results obtained are shown in Table 1 in the column "Relative HLM Flatness". If the relative HLM flatness is 70% or less, it is evaluated as being excellent in swelling elimination property, and if it is less than 60%, it is evaluated as being superior in swelling elimination performance.
  • polishing rate R [cm/min] in each example and comparative example was calculated by the following formulas (1) to (3).
  • the obtained polishing rate R was converted into a relative value (relative polishing rate [%]) with the polishing rate of Comparative Example 1 as 100%.
  • the obtained results are shown in the column of "relative polishing rate” in Table 1. If the relative polishing rate is 100% or more, it is evaluated that the polishing rate is maintained.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
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  • Power Engineering (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)

Abstract

L'invention concerne une composition de polissage permettant à la fois de maintenir un taux de polissage et à la fois d'éliminer un bombement de la périphérie d'une marque laser dure (HLM), la composition de polissage comprenant des grains abrasifs, un composé basique, un sel de lithium et de l'eau.
PCT/JP2022/031389 2021-09-01 2022-08-19 Composition de polissage WO2023032714A1 (fr)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002226836A (ja) * 2001-02-02 2002-08-14 Fujimi Inc 研磨用組成物およびそれを用いた研磨方法
WO2005090511A1 (fr) * 2004-03-19 2005-09-29 Tytemn Corporation Composition de polissage et procédé de polissage

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002226836A (ja) * 2001-02-02 2002-08-14 Fujimi Inc 研磨用組成物およびそれを用いた研磨方法
WO2005090511A1 (fr) * 2004-03-19 2005-09-29 Tytemn Corporation Composition de polissage et procédé de polissage

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