WO2016021325A1 - Liquide de polissage pour polissage chimico-mécanique (cmp) et procédé de polissage l'utilisant - Google Patents

Liquide de polissage pour polissage chimico-mécanique (cmp) et procédé de polissage l'utilisant Download PDF

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WO2016021325A1
WO2016021325A1 PCT/JP2015/068377 JP2015068377W WO2016021325A1 WO 2016021325 A1 WO2016021325 A1 WO 2016021325A1 JP 2015068377 W JP2015068377 W JP 2015068377W WO 2016021325 A1 WO2016021325 A1 WO 2016021325A1
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Prior art keywords
polishing
cmp
additive
liquid
inorganic insulating
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PCT/JP2015/068377
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English (en)
Japanese (ja)
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吉川　茂
寿夫 瀧澤
宗宏 太田
奈央 山村
愛子 木野
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日立化成株式会社
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    • 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
    • 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 a CMP polishing liquid for use in chemical mechanical polishing (CMP), and a polishing method using the same.
  • CMP chemical mechanical polishing
  • the present invention relates to, for example, a CMP polishing liquid for polishing a semiconductor wafer material, and a polishing method using the same.
  • the present invention particularly relates to a polishing slurry for CMP for polishing silicon oxide provided on the surface of a semiconductor wafer, and a polishing method using the same.
  • the CMP technique is a technique for flattening the surface after forming a thin film on a substrate by chemical vapor deposition (CVD) or the like.
  • CVD chemical vapor deposition
  • processing by CMP is indispensable. If the surface of the substrate is uneven, inconveniences such as inability to focus in the exposure process and insufficient formation of a fine wiring structure occur.
  • the CMP technology is a process for forming an element isolation region by polishing a plasma oxide material (BPSG, HDP-SiO 2 , p-TEOS, etc.), a process for forming an interlayer insulating material, or a silicon oxide in a device manufacturing process.
  • the present invention is also applied to a step of flattening a plug (for example, an Al / Cu plug) after embedding a member (for example, a silicon oxide film) containing metal in a metal wiring.
  • CMP is usually performed using an apparatus capable of supplying a polishing liquid onto a polishing pad.
  • the substrate surface is polished by pressing the substrate against the polishing pad while supplying a polishing liquid between the substrate surface and the polishing pad.
  • a high-performance polishing liquid is one of elemental techniques, and various polishing liquids have been developed so far.
  • a groove is provided in advance on the substrate surface, and an inorganic insulating material (for example, silicon oxide) is formed by CVD or the like so as to fill the groove.
  • the element isolation region is formed by planarizing the surface of the inorganic insulating material by CMP.
  • STI shallow trench isolation
  • the polishing process of the inorganic insulating material is divided into two stages to improve the production efficiency.
  • the first step rough cutting step
  • the inorganic insulating material provided on the substrate is removed at high speed.
  • the second step finishing step
  • the inorganic insulating material is finished to an arbitrary thickness.
  • polishing liquids for CMP for removing inorganic insulating materials for example, silicon oxide
  • a polishing liquid containing a compound having a specific chemical structure is known as a polishing liquid that can be used in the first step (roughing step) (for example, see Patent Document 1 below).
  • the step removal property is given priority over the polishing rate in the first step.
  • the step removability indicates that the inorganic insulating material (convex portion surface) in the pattern wafer having the inorganic insulating material on the convex surface with respect to the polishing amount (polishing rate) of the inorganic insulating material in the blanket wafer having the inorganic insulating material on the surface.
  • Polishing amount (polishing speed) ratio polishing amount in pattern wafer / polishing amount in blanket wafer.
  • the step-removability may be low.
  • the decrease in the step removal property increases the removal time of the inorganic insulating material in the second step and causes a deterioration in throughput, and also decreases the flatness after polishing. If the flatness after polishing is lowered, the depth of focus of lithography cannot be ensured, and it becomes difficult to form a device.
  • the present invention is intended to solve the above-described problems, and an object of the present invention is to provide a polishing slurry for CMP that can achieve both a high polishing rate and step removal performance for an inorganic insulating material, and a polishing method using the same. .
  • the present inventors have made extensive studies on additives to be added to the CMP polishing liquid.
  • the present inventors prepared many polishing liquids for CMP using various organic compounds as additives. These CMP polishing liquids were used to polish the inorganic insulating material, and the polishing rate and the step removal performance were evaluated.
  • the use of 4-pyrone compounds having a specific chemical structure and compounds having acidic functional groups and basic functional groups as additives makes it possible to achieve both high polishing speed and step removal performance for inorganic insulating materials.
  • the present invention has been completed.
  • the CMP polishing liquid according to the present invention contains abrasive grains, a first additive, a second additive, and water, and the first additive is represented by the following general formula (1).
  • the second additive is a compound having an acidic functional group and a basic functional group. [Wherein, X 11 , X 12 and X 13 are each independently a hydrogen atom or a monovalent substituent. ]
  • the CMP polishing liquid according to the present invention can achieve both a high polishing rate and a step removal property for an inorganic insulating material.
  • the interaction between the polishing liquid for CMP and the inorganic insulating material can be achieved by using a 4-pyrone compound having a specific chemical structure as the first additive.
  • the polishing rate is increased.
  • the functional group of the second additive reacts with the inorganic insulating material.
  • strong load dependency occurs. Thereby, it is presumed that the step removability with a heavy load increases, and as a result, the step removability increases.
  • the CMP polishing liquid according to the present invention has a feature that it is possible to achieve both a high polishing rate and a high level difference removal property, and is therefore suitable for polishing an inorganic insulating material having irregularities.
  • the CMP polishing liquid according to the present invention has an advantage that both a high polishing rate and a high level of step removal can be achieved even when polishing a semiconductor material that is relatively difficult to remove steps with the conventional CMP polishing liquid. is there. For example, even when polishing an inorganic insulating material having a T-shaped or lattice-shaped concave or convex portion like a semiconductor substrate having a memory cell, both a high polishing rate and a high level difference can be achieved.
  • the polishing slurry for CMP containing the first additive in addition to achieving a high polishing rate for the inorganic insulating material, aggregation of abrasive grains can be suppressed.
  • the 4-pyrone compound having the specific structure described above is an additive that can increase the interaction between the polishing slurry for CMP and the inorganic insulating material. Therefore, since there is no effect of weakening the repulsive force such as electrostatic repulsive force between the abrasive grains, it is presumed that the aggregation of the abrasive grains can be suppressed.
  • the first additive is a group consisting of 3-hydroxy-2-methyl-4-pyrone, 5-hydroxy-2- (hydroxymethyl) -4-pyrone, and 2-ethyl-3-hydroxy-4-pyrone It is preferably at least one selected from the group. Thereby, a higher polishing rate can be obtained.
  • the acidic functional group of the second additive is preferably a sulfonic acid group.
  • the basic functional group of the second additive is preferably an amino group. In these cases, high step-removability can be easily obtained.
  • the second additive is more preferably at least one selected from the group consisting of sulfamic acid and aminobenzenesulfonic acid.
  • the content of the first additive is preferably 0.001 to 5 parts by mass with respect to 100 parts by mass of the CMP polishing liquid. Thereby, the improvement effect of the polishing rate can be obtained more efficiently.
  • the content of the second additive is preferably 0.0001 to 1 part by mass with respect to 100 parts by mass of the CMP polishing liquid.
  • the abrasive preferably contains a cerium compound.
  • the cerium-based compound is preferably cerium oxide.
  • the CMP polishing liquid according to the present invention may be used for polishing an inorganic insulating material. That is, the present invention provides an application of the CMP polishing liquid to polishing a substrate having an inorganic insulating material on the surface.
  • the present invention provides a polishing method using the CMP polishing liquid. That is, the polishing method according to the present invention is a polishing method for polishing a substrate having an inorganic insulating material on the surface, and the CMP polishing liquid according to the present invention is supplied between the inorganic insulating material and the polishing pad. And a step of polishing the inorganic insulating material with a polishing pad. According to such a polishing method, it is possible to achieve both a high polishing rate and a step removal property for the inorganic insulating material. In addition, since a high polishing rate is achieved without largely depending on the surface shape of the substrate to be polished, the polishing method is suitable for roughing an inorganic insulating material and polishing a semiconductor substrate having memory cells.
  • the present invention it is possible to achieve both a high polishing rate and a step removal property for an inorganic insulating material (for example, silicon oxide).
  • an inorganic insulating material for example, silicon oxide
  • ADVANTAGE OF THE INVENTION According to this invention, the application to the grinding
  • polishing of a silicon oxide of the polishing liquid for CMP can be provided.
  • ADVANTAGE OF THE INVENTION the application to the grinding
  • ADVANTAGE OF THE INVENTION the application to the grinding
  • ADVANTAGE OF THE INVENTION the application to polishing of the semiconductor substrate which has a memory cell of CMP polishing liquid can be provided.
  • ADVANTAGE OF THE INVENTION the application to the grinding
  • each component in the composition means the total amount of the plurality of substances present in the composition unless there is a specific notice when there are a plurality of substances corresponding to each component in the composition. .
  • the polishing slurry for CMP contains abrasive grains (polishing particles), a first additive, a second additive, and water, and the first additive is 4-pyrone. And a second additive is a compound having an acidic functional group and a basic functional group.
  • abrasive grains polishing particles
  • a second additive is a compound having an acidic functional group and a basic functional group.
  • the abrasive grains can include, for example, a cerium compound, alumina, silica, titania, zirconia, magnesia, mullite, silicon nitride, ⁇ -sialon, aluminum nitride, titanium nitride, silicon carbide, boron carbide, and the like.
  • a constituent component of these abrasive grains one kind may be used alone, or two or more kinds may be used in combination. Among these, the addition effect of the first additive and the second additive can be satisfactorily exhibited, and the high polishing rate and the step removal property for the inorganic insulating material having unevenness (for example, silicon oxide) are more highly compatible. From the viewpoint, a cerium-based compound is preferable.
  • a polishing liquid for CMP using abrasive grains containing a cerium-based compound has a feature that there are relatively few polishing flaws on a polished surface (referred to as a surface after polishing; hereinafter the same).
  • a surface after polishing Conventionally, from the viewpoint of easily achieving a high polishing rate for an inorganic insulating material (for example, silicon oxide), CMP polishing liquids containing silica particles as abrasive grains have been widely used.
  • CMP polishing liquids using silica particles generally have a problem that polishing scratches are likely to occur on the polished surface. In a device having a fine pattern with a wiring width of 45 nm or later, even a fine scratch that has not been a problem may affect the reliability of the device.
  • a conventional CMP polishing liquid using abrasive grains containing a cerium compound tends to have a slightly lower polishing rate for inorganic insulating materials (eg, silicon oxide) than a CMP polishing liquid using silica particles. It was.
  • a high polishing rate and a step difference with respect to an inorganic insulating material can be obtained by using an abrasive containing a cerium compound, the first additive, and the second additive in combination. Removability is compatible. This suggests that the combination of the cerium compound, the first additive, and the second additive is particularly effective for polishing.
  • cerium compound examples include cerium oxide, cerium hydroxide, ammonium cerium nitrate, cerium acetate, cerium sulfate hydrate, cerium bromate, cerium bromide, cerium chloride, cerium oxalate, cerium nitrate, and cerium carbonate. .
  • cerium oxide is preferable. By using cerium oxide, an excellent polished surface with few polishing flaws can be obtained while achieving both a high polishing rate and a high level difference removability.
  • the abrasive grains preferably include polycrystalline cerium oxide having a crystal grain boundary (for example, polycrystalline cerium oxide having a plurality of crystallites surrounded by the crystal grain boundary).
  • the polycrystalline cerium oxide particles having such a structure are different from simple aggregates in which single crystal particles are aggregated, and become fine due to stress during polishing, and at the same time, have an active surface (a surface not exposed to the outside before becoming fine). Since it appears one after another, it is considered that a high polishing rate for an inorganic insulating material (for example, silicon oxide) can be maintained at a high level.
  • Such polycrystalline cerium oxide particles are described in detail in, for example, International Publication No. WO99 / 31195.
  • the method for producing abrasive grains containing cerium oxide is not particularly limited, and examples include a liquid phase synthesis; a method of oxidizing by baking or hydrogen peroxide.
  • a method of firing a cerium source such as cerium carbonate is preferred.
  • the firing temperature is preferably 350 to 900 ° C.
  • the produced cerium oxide particles are aggregated, it is preferably mechanically pulverized.
  • the pulverization method is not particularly limited, but for example, dry pulverization using a jet mill or the like; wet pulverization using a planetary bead mill or the like is preferable.
  • the jet mill is described in, for example, “Chemical Engineering Papers”, Vol. 6, No. (1980), pp. 527-532.
  • the average particle size of the abrasive grains is preferably 50 nm or more, more preferably 70 nm or more, and still more preferably 80 nm or more.
  • the polishing rate for the inorganic insulating material for example, silicon oxide
  • the average particle size of the abrasive grains is preferably 500 nm or less, more preferably 300 nm or less, still more preferably 280 nm or less, particularly preferably 250 nm or less, and extremely preferably 200 nm or less.
  • the average particle size is 500 nm or less, polishing scratches can be suppressed as compared with the case where the average particle size exceeds 500 nm.
  • a conventionally known method can be used.
  • control of the firing temperature, firing time, pulverization conditions, etc .; application of filtration, classification, etc. may be mentioned.
  • the average particle diameter of the abrasive grains means the median value of the volume distribution obtained by measuring the slurry sample in which the abrasive grains are dispersed with a dynamic light scattering particle size distribution meter. Specifically, it is a value measured using LB-500 (trade name) manufactured by HORIBA, Ltd. Adjust the content of abrasive grains in the slurry sample so that the abrasive grain content is 0.5% by mass based on the total mass of the slurry sample, and set this in the LB-500 to measure the median volume distribution I do. The degree of agglomeration of abrasive grains can also be evaluated by measuring the median diameter (cumulative median value) with LB-500.
  • the content of the abrasive grains is 0.5 mass% based on the total mass of the slurry sample by concentrating or diluting the CMP polishing liquid with water. After adjusting the content of the abrasive grains of the slurry sample so as to become, it can be measured by the same method.
  • the content of the abrasive grains is preferably 0.10 parts by mass or more, more preferably 0.15 parts by mass or more, and further 0.20 parts by mass or more with respect to 100 parts by mass of the polishing slurry for CMP. preferable.
  • the content of the abrasive is preferably 10 parts by mass or less, more preferably 5.0 parts by mass or less, still more preferably 3.0 parts by mass or less, and 2.0 parts by mass with respect to 100 parts by mass of the polishing slurry for CMP.
  • the following is particularly preferable, and 1.0 mass part or less is extremely preferable.
  • the content of the abrasive grains is 10 parts by mass or less, the aggregation of the abrasive grains tends to be suppressed as compared with the case where the content exceeds 10 parts by mass, and a high polishing rate tends to be achieved.
  • the first additive is a 4-pyrone compound represented by the following general formula (1).
  • the polishing slurry for CMP according to the present embodiment by using the 4-pyrone compound represented by the general formula (1) as the first additive, compared to the conventional polishing slurry for CMP, A high polishing rate for inorganic insulating materials can be achieved.
  • X 11 , X 12 and X 13 are each independently a hydrogen atom or a monovalent substituent.
  • the monovalent substituent include an aldehyde group, a hydroxy group (hydroxyl group), a carboxyl group, a sulfonic acid group, a phosphoric acid group, a bromine atom, a chlorine atom, an iodine atom, a fluorine atom, a nitro group, a hydrazine group, and a carbon number of 1 to 8 alkyl groups (which may be substituted with OH, COOH, Br, Cl, I, or NO 2 ), aryl groups having 6 to 12 carbon atoms, alkenyl groups having 1 to 8 carbon atoms, and the like.
  • a methyl group, an ethyl group, or a hydroxymethyl group is preferable.
  • the monovalent substituent is bonded to a carbon atom adjacent to the oxy group from the viewpoint of easy synthesis. It is preferable. That is, it is preferable that at least one of X 11 and X 12 is a monovalent substituent. Furthermore, easy in view of improvement is obtained of the abrasive grains of the polishing ability, it is preferable that at least two are hydrogen atom of X 11, X 12 and X 13, among the X 11, X 12 and X 13 2 More preferably, one is a hydrogen atom.
  • the 4-pyrone compound has a structure in which a hydroxy group is bonded to at least a carbon atom adjacent to the carbon atom of the carbonyl group.
  • the “4-pyrone compound” has a 6-membered ring ( ⁇ -pyrone ring) structure in which an oxy group and a carbonyl group are included and the carbonyl group is located at the 4-position with respect to the oxy group. It is a heterocyclic compound.
  • a hydroxy group is bonded to a carbon atom adjacent to the carbonyl group in the ⁇ -pyrone ring, and a substituent other than a hydrogen atom is attached to the other carbon atom. May be substituted.
  • 3-hydroxy-2-methyl-4-pyrone also known as 3-hydroxy-2-methyl-4H-pyran-4-one, Maltol
  • 5-hydroxy-2- (hydroxymethyl) -4-pyrone also known as 5-hydroxy-2- (hydroxymethyl) -4H-pyran-4-one, kojic acid
  • 2-ethyl-3 At least one compound selected from the group consisting of -hydroxy-4-pyrone (alias: 2-ethyl-3-hydroxy-4H-pyran-4-one) is preferred.
  • the first additive one kind may be used alone, or two or more kinds may be used in combination.
  • a high polishing rate can also be obtained by using a combination of two or more of the first additives.
  • the first additive is preferably water-soluble.
  • a desired amount of the first additive can be dissolved well in the polishing slurry for CMP, and an effect of improving the polishing rate and agglomeration of abrasive grains can be achieved.
  • the suppression effect can be achieved to a higher level.
  • the solubility of the first additive in 100 g of water at room temperature (25 ° C.) is preferably 0.001 g or more, more preferably 0.005 g or more, still more preferably 0.01 g or more, and particularly preferably 0.05 g or more.
  • the upper limit of solubility is not particularly limited.
  • the content of the first additive is preferably 0.001 parts by mass or more, more preferably 0.005 parts by mass or more, still more preferably 0.01 parts by mass or more, with respect to 100 parts by mass of the polishing slurry for CMP. 0.02 parts by mass or more is particularly preferable, and 0.03 parts by mass or more is very preferable.
  • the content of the first additive is 0.001 part by mass or more, there is a tendency that a stable polishing rate is easily achieved as compared to the case of less than 0.001 part by mass.
  • the content of the first additive is preferably 5 parts by mass or less, more preferably 3 parts by mass or less, still more preferably 1 part by mass or less, and 0.5 parts by mass or less with respect to 100 parts by mass of the polishing slurry for CMP. Is particularly preferable, and 0.3 parts by mass or less is extremely preferable.
  • the content of the first additive is 5 parts by mass or less, aggregation of abrasive grains tends to be suppressed as compared with the case where the content exceeds 5 parts by mass, and a high polishing rate tends to be easily achieved.
  • the CMP polishing liquid according to the present embodiment contains a compound having an acidic functional group and a basic functional group (excluding a compound corresponding to the first additive) as the second additive. Thereby, in addition to a high polishing rate, high step removal performance can be obtained.
  • An acidic functional group is a functional group that exhibits acidity in an aqueous solution.
  • Examples of the acidic functional group include a sulfonic acid group, a sulfonic acid group, a carboxyl group, a carboxylic acid group, a phosphoric acid group, and a phosphoric acid group, and a sulfonic acid group is preferable.
  • the basic functional group is a functional group that exhibits basicity in an aqueous solution. Examples of basic functional groups include amino groups.
  • the acid dissociation constant pKa of the second additive at room temperature (25 ° C.) (the negative common logarithm of the equilibrium constant Ka (logarithm of the reciprocal), and when there are two or more pKa, the lowest first step pKa1) is Less than 4 is preferable, 3.5 or less is more preferable, and 3.3 or less is more preferable.
  • the lower limit of the acid dissociation constant pKa is not particularly limited and is, for example, ⁇ 10 or more.
  • an amino group-containing sulfonic acid compound is preferable.
  • the “amino group-containing sulfonic acid compound” means at least one selected from the group consisting of a sulfonic acid group (sulfo group, —SO 3 H) and a sulfonic acid group (—SO 3 M: M is a metal atom), an amino group (—NH 2 ) in one molecule.
  • the metal atom M of the sulfonate group include alkali metals such as Na and K, and alkaline earth metals such as Mg and Ca.
  • amino group-containing sulfonic acid compounds include sulfamic acid (also known as amidosulfuric acid), aminomethanesulfonic acid, aminoethanesulfonic acid (1-aminoethanesulfonic acid, 2-aminoethanesulfonic acid, etc.), aminopropanesulfonic acid, amino Benzenesulfonic acid (ortanylic acid (also known as 2-aminobenzenesulfonic acid), methanylic acid (also known as 3-aminobenzenesulfonic acid), sulfanilic acid (also known as 4-aminobenzenesulfonic acid), aminonaphthalenesulfonic acid, These salts (for example, salts containing the metal atom M) and the like can be mentioned.
  • sulfamic acid also known as amidosulfuric acid
  • aminomethanesulfonic acid aminoethanesulfonic acid (1-aminoethanesulfonic acid
  • the second additive is preferably at least one selected from the group consisting of sulfamic acid and aminobenzene sulfonic acid from the viewpoint of easily obtaining high step removal, and at least selected from the group consisting of sulfamic acid and sulfanilic acid.
  • One type is more preferable.
  • the second additive one kind may be used alone, or two or more kinds may be used in combination.
  • the molecular weight of the second additive is preferably 500 or less, more preferably 300 or less, still more preferably 250 or less, and even more preferably 200 or less, from the viewpoint that the functional group of the second additive easily reacts with the inorganic insulating material. Particularly preferred.
  • the lower limit of the molecular weight is, for example, 50 or more.
  • the content of the second additive is preferably 0.0001 parts by mass or more, more preferably 0.0005 parts by mass or more, and still more preferably 0.001 parts by mass or more with respect to 100 parts by mass of the polishing slurry for CMP.
  • the content of the second additive is preferably 1 part by mass or less, more preferably 0.5 part by mass or less, still more preferably 0.2 part by mass or less, relative to 100 parts by mass of the polishing slurry for CMP.
  • 1 part by mass or less is particularly preferable, 0.05 part by mass or less is extremely preferable, 0.01 part by mass or less is very preferable, and 0.007 part by mass or less is even more preferable.
  • the content of the second additive is 1 part by mass or less, it tends to suppress the aggregation of abrasive grains compared to the case where the content exceeds 1 part by mass, and tends to achieve both a high polishing rate and high step removal performance. is there.
  • the content of the second additive can be adjusted according to the type of the first additive.
  • the water contained in the CMP polishing liquid according to the present embodiment is not particularly limited, but deionized water, ion-exchanged water, and ultrapure water are preferable. In addition, you may use polar solvents, such as ethanol and acetone, together with water as needed.
  • the CMP polishing liquid according to this embodiment may contain a surfactant from the viewpoint of improving the dispersion stability of the abrasive grains and / or the flatness of the polished surface.
  • a surfactant examples include ionic surfactants and nonionic surfactants, and nonionic surfactants are preferred.
  • the surfactant one kind may be used alone, or two or more kinds may be used in combination.
  • Nonionic surfactants include polyoxypropylene polyoxyethylene alkyl ether, polyoxyethylene alkyl ether, polyoxyethylene alkyl allyl ether, polyoxyethylene polyoxypropylene ether derivatives, polyoxypropylene glyceryl ether, polyethylene glycol oxyethylene Ether type surfactants such as adducts, oxyethylene adducts of methoxypolyethylene glycol, oxyethylene adducts of acetylenic diols; ester type surfactants such as sorbitan fatty acid esters and glycerol borate fatty acid esters; polyoxyethylene alkylamines Amino ether type surfactants such as polyoxyethylene sorbitan fatty acid ester, polyoxyethylene glycerol borate fatty acid ester Ether ester type surfactants such as tellurium and polyoxyethylene alkyl ester; alkanolamide type surfactants such as fatty acid alkanolamide and polyoxyethylene fatty acid
  • the CMP polishing liquid according to the present embodiment may contain other components in addition to the surfactant in accordance with desired characteristics.
  • examples of such components include pH adjusters as described later, pH buffering agents for suppressing fluctuations in pH, aminocarboxylic acids, and cyclic monocarboxylic acids. It is desirable that the content of these components be in a range that does not excessively reduce the effect of the polishing liquid.
  • the pH of the polishing slurry for CMP according to this embodiment is preferably 8.0 or less, more preferably less than 8.0, still more preferably 7.0 or less, particularly preferably 6.0 or less, and extremely preferably 5.0 or less. Preferably, 4.5 or less is very preferable, and 4.0 or less is even more preferable.
  • the polishing slurry for CMP according to this embodiment preferably has a pH of 1.5 or more, more preferably 2.0 or more, still more preferably 2.5 or more, and particularly preferably 3.0 or more.
  • the absolute value of the zeta potential of the inorganic insulating material (for example, silicon oxide) can be increased as compared with the case of less than 1.5, and a higher polishing rate is achieved.
  • the pH is defined as the pH at a liquid temperature of 25 ° C.
  • the pH of the CMP polishing liquid according to the present embodiment can be measured with a pH meter (for example, model number PHL-40 manufactured by Electrochemical Instrument Co., Ltd.).
  • a pH meter for example, model number PHL-40 manufactured by Electrochemical Instrument Co., Ltd.
  • two pH meters are calibrated using phthalate pH buffer solution (pH 4.01) and neutral phosphate pH buffer solution (pH 6.86) as standard buffers, and then the electrodes of the pH meter are polished. Put in the solution and measure the value after 2 minutes or more has stabilized. At this time, both the standard buffer solution and the polishing solution are set to 25 ° C.
  • the pH of the CMP polishing liquid within the range of 1.5 to 8.0.
  • Proton or hydroxy anion acts on the compound blended as an additive to change the chemical form of the compound, and against the inorganic insulating material (for example, silicon oxide) and / or stopper material (for example, silicon nitride) on the substrate surface. Improves wettability and affinity.
  • the abrasive grains contain cerium oxide, the contact efficiency between the abrasive grains and the inorganic insulating material (for example, silicon oxide) is improved, and a higher polishing rate is achieved. This is because the sign of the zeta potential of cerium oxide is positive while the sign of the zeta potential of an inorganic insulating material (for example, silicon oxide) is negative, and electrostatic attraction acts between the two.
  • the pH of the polishing slurry for CMP varies depending on the type of compound used as an additive.
  • the CMP polishing liquid may contain a pH adjusting agent in order to adjust the pH to the above range.
  • the pH adjuster is not particularly limited, and examples thereof include acids such as nitric acid, sulfuric acid, hydrochloric acid, phosphoric acid, boric acid and acetic acid; bases such as sodium hydroxide, ammonia, potassium hydroxide and calcium hydroxide. From the viewpoint of improving productivity, a CMP polishing liquid may be prepared without using a pH adjuster, and such a CMP polishing liquid may be applied to CMP as it is.
  • the polishing liquid for CMP can be classified into (A) normal type, (B) concentrated type, and (C) two-liquid type, and the preparation method and usage differ depending on the type.
  • the normal type is a polishing liquid that can be used as it is without pretreatment such as dilution during polishing.
  • the concentrated type is a polishing liquid in which the contents are concentrated in comparison with the (A) normal type in consideration of convenience of storage or transportation.
  • the two-liquid type is divided into a liquid A containing a certain component and a liquid B containing other components at the time of storage or transportation, and the liquid A and the liquid B are mixed and used at the time of use. A polishing liquid.
  • the normal type can be obtained by dissolving or dispersing the abrasive grains, the first additive, the second additive, and, if necessary, other components in water, which is the main dispersion medium. it can.
  • 100 parts by weight of polishing slurry for CMP having 0.5 parts by weight of abrasive grains, 0.1 parts by weight of first additive, and 0.001 parts by weight of second additive.
  • the CMP polishing liquid 1000 g may be adjusted to contain 5 g of abrasive grains, 1 g of the first additive, and 0.01 g of the second additive.
  • the polishing liquid for CMP can be prepared using, for example, a stirrer, a homogenizer, an ultrasonic disperser, a wet ball mill, or the like.
  • the fine graining treatment of the abrasive grains can be carried out by a sedimentation classification method or a method using a high pressure homogenizer.
  • the sedimentation classification method is a method having a step of forcibly sedimenting coarse particles of slurry containing abrasive grains with a centrifuge and a step of taking out only the supernatant.
  • a method using a high-pressure homogenizer is a method in which abrasive grains in a dispersion medium collide with each other at a high pressure.
  • the concentrated type is diluted with water so that the content of the contained components becomes a desired content immediately before use.
  • (A) Liquid characteristics (pH, grain size of abrasive grains, etc.) and polishing characteristics (polishing rate for inorganic insulating material (for example, silicon oxide), inorganic insulation for stopper material (for example, silicon nitride) similar to normal type Stirring or abrasive dispersion may be performed for an arbitrary time until a material (for example, silicon oxide polishing selectivity) can be reproduced.
  • the concentration type the volume is reduced according to the degree of concentration, so that the cost for storage and transportation can be reduced.
  • the concentration ratio is preferably 1.5 times or more, more preferably 2 times or more, further preferably 3 times or more, and particularly preferably 5 times or more. When the concentration ratio is 1.5 times or more, it is possible to obtain merit related to storage and transportation as compared to the case of less than 1.5 times.
  • the concentration factor is preferably 40 times or less, more preferably 20 times or less, and still more preferably 15 times or less. When the concentration ratio is 40 times or less, it is easy to suppress the aggregation of abrasive grains as compared to the case where the concentration ratio exceeds 40 times.
  • (B) The point to be noted when using the concentrated type is that the pH changes before and after dilution with water.
  • the pH of the concentrated type polishing liquid should be set low in advance, taking into account the increase in pH due to mixing with water. That's fine. For example, when water (pH: about 5.6) in which carbon dioxide is dissolved is used and (B) concentrated type polishing liquid having pH 4.0 is diluted 10 times, the pH of the diluted polishing liquid is 4. It rises to about 3.
  • the pH of the concentrated type is preferably 1.5 to 7.0 from the viewpoint of obtaining a polishing liquid having a suitable pH after dilution with water.
  • the lower limit of the pH is preferably 1.5 or more, more preferably 2.0 or more, and further preferably 2.5 or more.
  • the upper limit of the pH is preferably 7.0 or less, more preferably 6.7 or less, still more preferably 6.0 or less, and particularly preferably 5.5 or less from the viewpoint of suppressing the aggregation of abrasive grains.
  • the two-liquid type has an advantage that it can avoid agglomeration of abrasive grains and the like as compared with the (B) concentrated type.
  • the component which each of the liquid A and the liquid B contains is arbitrary.
  • a slurry containing abrasive grains and surfactants blended as necessary is prepared as liquid A, and a solution containing additives and other ingredients blended as needed is liquid B.
  • liquid A a slurry containing abrasive grains and surfactants blended as necessary
  • liquid B a solution containing additives and other ingredients blended as needed.
  • any acid or alkali may be added to the liquid A to adjust the pH.
  • the two-liquid type polishing liquid is useful when the polishing characteristics are deteriorated in a relatively short time due to aggregation of abrasive grains or the like in a state where the respective components are mixed.
  • at least one of the liquid A and the liquid B may be a concentrated type.
  • the liquid A, the liquid B, and water may be mixed when using the polishing liquid.
  • the concentration ratio and pH of the liquid A or the liquid B are arbitrary, and the liquid characteristics and polishing characteristics of the final mixture may be the same as those of the (A) normal type polishing liquid.
  • the polishing method according to the present embodiment includes a polishing step of polishing an inorganic insulating material (for example, silicon oxide) using the CMP polishing liquid according to the present embodiment.
  • an inorganic insulating material for example, silicon oxide
  • the substrate having an inorganic insulating material for example, silicon oxide
  • the polishing step the substrate having an inorganic insulating material (for example, silicon oxide) on the surface is polished and planarized by the CMP technique using the CMP polishing liquid according to the present embodiment.
  • the CMP polishing liquid according to this embodiment includes an inorganic insulating material on a substrate having an inorganic insulating material (for example, silicon oxide) on the surface, and a predetermined polishing member (for example, A step of polishing the inorganic insulating material by the polishing member while being supplied to the polishing pad.
  • the inorganic insulating material is polished to remove at least a part of the inorganic insulating material.
  • the inorganic insulating material to be polished may be in the form of a film (inorganic insulating film such as a silicon oxide film).
  • the content and pH of each component of the CMP polishing liquid are appropriately adjusted.
  • the polishing method according to the present embodiment is suitable for polishing a substrate having an inorganic insulating material (for example, silicon oxide) on the surface in the following device manufacturing process.
  • Devices include diodes, transistors, compound semiconductors, thermistors, varistors, thyristors and other individual semiconductors; DRAM (dynamic random access memory), SRAM (static random access memory), EPROM (erasable programmable read) ⁇ Only memory (memory), mask ROM (mask read only memory), EEPROM (electrically erasable programmable read only memory), storage devices such as flash memory; theoretical circuit such as microprocessor, DSP, ASIC, etc. Element; Integrated circuit element such as compound semiconductor represented by MMIC (monolithic microwave integrated circuit); Hybrid integrated circuit (hybrid IC); Light-emitting diode; Such as photoelectric conversion elements, such as elements and the like.
  • the CMP polishing liquid according to the present embodiment can achieve both a high polishing rate and a high level difference removal property. Therefore, the polishing method using the CMP polishing liquid can be applied to a substrate for which it has been difficult to achieve a high polishing rate by the conventional method using the CMP polishing liquid.
  • the polishing method according to the present embodiment is particularly suitable for flattening a surface to be polished having a step (unevenness) on the surface.
  • An example of a substrate having such a surface to be polished is a logic semiconductor substrate.
  • the surface of the substrate may have a T-shaped or lattice-shaped concave or convex portion, and the polishing method according to the present embodiment is viewed from above (in the direction facing the surface of the substrate). It is suitable for polishing a substrate having on its surface a portion in which concave portions or convex portions are provided in a T shape or a lattice shape.
  • an inorganic insulating material for example, silicon oxide
  • a semiconductor substrate having memory cells for example, a substrate of a device such as a DRAM or flash memory
  • the CMP polishing liquid according to the present embodiment has a high polishing speed and a high step removal property. It shows that they can be compatible.
  • the substrate to which the polishing method according to this embodiment can be applied is not limited to a substrate in which the entire surface of the substrate is formed of a silicon oxide film, but a silicon nitride film, a polycrystalline silicon film, or the like in addition to the silicon oxide film is formed on the substrate surface. Further, it may be a substrate.
  • the polishing method according to the present embodiment includes an inorganic insulating film such as a silicon oxide film, a glass film, and silicon nitride on a wiring board having predetermined wiring; polysilicon, Al, Cu, Ti, TiN, W, Ta It can also be applied to a substrate on which a film mainly containing TaN or the like is formed.
  • Examples of a method for forming a silicon oxide film on the substrate surface include a low pressure CVD method and a plasma CVD method.
  • a low pressure CVD method for example, monosilane (SiH 4 ) is used as the Si source, and oxygen (O 2 ) is used as the oxygen source.
  • SiH 4 monosilane
  • oxygen O 2
  • a silicon oxide film is formed.
  • heat treatment is performed at a temperature of 1000 ° C. or lower after CVD.
  • the plasma CVD method has an advantage that a chemical reaction requiring a high temperature can be performed at a low temperature under normal thermal equilibrium.
  • As the reaction gas for example, SiH 4, SiH 4 -N 2 O -containing gas using N 2 O as oxygen source, and, TEOS-O 2 system using tetraethoxysilane (TEOS) to Si source as Si source Gas (TEOS-plasma CVD method) can be mentioned.
  • the substrate temperature is preferably 250 to 400 ° C.
  • the reaction pressure is preferably 67 to 400 Pa.
  • the silicon oxide film to be polished may be doped with an element such as phosphorus or boron.
  • the silicon nitride film can be formed by a low pressure CVD method, a plasma CVD method, or the like.
  • the low pressure CVD method for example, dichlorosilane (SiH 2 Cl 2 ) is used as the Si source, and ammonia (NH 3 ) is used as the nitrogen source.
  • NH 3 ammonia
  • SiH 2 Cl 2 —NH 3 oxidation reaction at a high temperature of 900 ° C.
  • a silicon nitride film is formed.
  • SiH 4 —NH 3 based gas using SiH 4 as a Si source and NH 3 as a nitrogen source is used as a reactive gas.
  • the substrate temperature is preferably 300 to 400 ° C.
  • the first step (roughing step) of polishing the silicon oxide film 3 at a high polishing rate and high step removal property, and the remaining silicon oxide film 3 have an arbitrary film thickness.
  • a second step (finishing step) for polishing at a high polishing rate is a process for forming an STI structure on a substrate (wafer) by CMP in the polishing method according to the present embodiment.
  • FIG. 1A is a cross-sectional view showing a substrate before polishing.
  • FIG. 1B is a cross-sectional view showing the substrate after the first step.
  • FIG.1 (c) is sectional drawing which shows the board
  • CMP CMP
  • a substrate (wafer) is disposed on the polishing pad so that the surface of the silicon oxide film 3 and the polishing pad come into contact with each other, and the surface of the silicon oxide film 3 is polished by the polishing pad. . More specifically, the surface to be polished of the silicon oxide film 3 is pressed against the polishing pad of the polishing surface plate, and the two are relative to each other in a state where the polishing liquid for CMP is supplied between the surface to be polished and the polishing pad. The silicon oxide film 3 is polished by moving to.
  • the CMP polishing liquid according to the present embodiment can be applied to both the first step and the second step, but can be used in the first step because it can achieve both a high polishing rate and a high level difference removal property. It is particularly preferred. Although the case where the polishing process is performed in two stages is illustrated here, the polishing process can be performed in one stage from the state shown in FIG. 1A to the state shown in FIG.
  • polishing apparatus for example, an apparatus including a holder for holding a substrate, a polishing surface plate to which the polishing pad is attached, and means for supplying a polishing liquid onto the polishing pad is suitable.
  • the polishing apparatus include polishing apparatuses manufactured by Ebara Manufacturing Co., Ltd. (model numbers: EPO-111, EPO-222, FREX200, and FREX300), APPLIED MATERIALS polishing apparatuses (trade name: Mirara 3400, Reflexion polishing machine), and the like.
  • a polishing pad For example, a general nonwoven fabric, a polyurethane foam, a porous fluororesin, etc. can be used. Further, the polishing pad is preferably subjected to groove processing so that the polishing liquid is accumulated.
  • the polishing conditions are not particularly limited, but from the viewpoint of suppressing the substrate from popping out, the rotation speed of the polishing platen is preferably 200 min ⁇ 1 or less, and the pressure (working load) applied to the substrate causes scratches on the polishing surface. From the viewpoint of suppression, 100 kPa or less is preferable.
  • the substrate is thoroughly washed in running water, and further, water droplets adhering to the substrate are removed by a spin dryer or the like and then dried.
  • polishing in this way, surface irregularities can be eliminated and a smooth surface can be obtained over the entire surface of the substrate.
  • a substrate having a desired number of layers can be manufactured by repeating the formation of the film and the step of polishing the film a predetermined number of times.
  • the substrate thus obtained can be used as various electronic parts and mechanical parts.
  • semiconductor elements include: semiconductor elements; optical glasses such as photomasks, lenses, and prisms; inorganic conductive films such as ITO; optical integrated circuits / optical switching elements / optical waveguides composed of glass and crystalline materials; Examples include optical single crystals such as scintillators; solid laser single crystals; sapphire substrates for blue laser LEDs; semiconductor single crystals such as SiC, GaP and GaAs; glass substrates for magnetic disks; magnetic heads and the like.
  • the average particle size of the abrasive grains was measured using a dynamic light scattering particle size distribution meter (trade name: LB-500, manufactured by Horiba, Ltd.). As a result, the average particle size was 150 nm.
  • the liquid phase after the above centrifugation was diluted with deionized water to adjust the abrasive content to 5.0% by mass. Further, immediately before polishing, each compound shown in Table 1 or Table 2 is added to the liquid phase in which the content of abrasive grains is adjusted to 5.0% by mass so as to have the content described in each table. The pH was adjusted to 3.4 using organic acid or ammonia. Thereafter, stirring was performed for 10 minutes to obtain a polishing slurry for CMP. The content of abrasive grains in the CMP polishing liquid was as shown in the table.
  • the pH of the CMP polishing liquid was determined under the following conditions. Measurement temperature: 25 ⁇ 5 ° C Measuring instrument: manufactured by Electrochemical Instrument Co., Ltd. Model number: PHL-40
  • the CMP polishing liquids according to Examples 1 to 7 obtained in this way were diluted with pure water so that the abrasive content was 0.5% by mass based on the total mass of the sample.
  • a sample for diameter measurement was obtained.
  • the average particle size of the abrasive grains was measured by a dynamic light scattering type particle size distribution analyzer (trade name: LB-500, manufactured by Horiba, Ltd.), and all were 150 ⁇ 5 nm.
  • the polishing slurry for CMP according to Examples 1 to 7 is a polishing solution prepared using the first additive and the second additive.
  • the CMP polishing liquid according to Comparative Examples 1 to 3 is a polishing liquid prepared without using the second additive.
  • the CMP polishing liquid according to Comparative Example 4 is a polishing liquid prepared without using the first additive and the second additive.
  • the CMP polishing liquid according to Comparative Example 5 and Comparative Example 6 is a polishing liquid prepared without using the first additive.
  • “A” is 5-hydroxy-2-hydroxymethyl-4-pyrone (also known as kojic acid)
  • “B” is 3-hydroxy-2 -Methyl-4-pyrone (also known as maltol).
  • a blanket wafer having a silicon oxide film on the surface as a film to be polished was prepared.
  • a blanket wafer is a wafer having a silicon oxide film having a thickness of 1000 nm disposed on a silicon substrate having a diameter of 300 mm.
  • a pattern wafer (trade name: SEMATECH764, manufactured by ADVANTECH) having an uneven silicon oxide film as a film to be polished was prepared.
  • a silicon nitride film (film thickness: 1500 nm) is formed as a stopper film on a part of a silicon substrate having a diameter of 300 mm, and then a recess is formed by etching the silicon substrate without the silicon nitride film by 350 nm.
  • the blanket wafer and the pattern wafer were polished using a polishing apparatus (manufactured by APPLIED MATERIALS, trade name: Reflexion LK).
  • the wafer was set in a holder having a suction pad for attaching the wafer.
  • a polishing pad made of porous urethane resin k-groove groove, manufactured by Rodel, model number: IC-1010 was attached to a polishing surface plate having a diameter of 800 mm.
  • the holder was placed on the polishing pad with the silicon oxide film forming surface of the wafer facing down.
  • the wafer pressing pressure was set to 28 kPa.
  • each of the CMP polishing liquids prepared by the above method was dropped onto the polishing pad attached to the polishing platen at a flow rate of 250 mL / min, and the polishing platen and the wafer were rotated at a rotational speed of 93 min ⁇ 1 and 87 min, respectively.
  • the silicon oxide film was polished by rotating at -1 . Thereafter, the polished wafer was thoroughly washed with pure water using a PVA brush (polyvinyl alcohol brush) and then dried.
  • the time X required for polishing the silicon oxide film by 300 nm was calculated as the time for polishing the pattern wafer for each polishing liquid for CMP.
  • the pattern wafer was polished for the time X by using each polishing liquid for CMP.
  • the amount of film thickness change before and after polishing of the silicon oxide film on the convex part of the pattern wafer was measured using an optical interference type film thickness measuring device (trade name: RE-3000, manufactured by Dainippon Screen Mfg. Co., Ltd.).
  • the film thickness change amount at this time was determined as a pattern wafer polishing amount (PTW).
  • divided the pattern wafer polishing amount by 300 nm was computed as level
  • Examples 1 to 7 using the first additive and the second additive had higher step removal performance than Comparative Examples 1 to 6. Further, in Examples 1 to 7, it was shown that the silicon oxide film can be polished while achieving both a high polishing rate and a high level difference removing property.
  • the average particle diameter of the abrasive grains was measured after one day from the preparation of the polishing liquid by mixing the respective components of the polishing liquid.
  • the particle size was 150 nm, which was the same as the particle size at the time of preparing abrasive grains. Thereby, it was confirmed that aggregation of a particle size is suppressed.
  • a polishing slurry for CMP that can achieve both a high polishing rate and a step removal property for a silicon oxide film.
  • the present invention also provides a polishing method using the CMP polishing liquid.

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

Abstract

L'invention porte sur un liquide de polissage pour le polissage chimico-mécanique (CMP), contenant des grains abrasifs, un premier additif, un second additif et de l'eau. Le premier additif est un composé de 4-pyrone représenté par la formule générale (1) et le second additif est un composé ayant un groupe fonctionnel acide et un groupe fonctionnel basique. (Dans la formule, chacun de X11, X12 et X13 représente indépendamment un atome d'hydrogène ou un substituant monovalent.)
PCT/JP2015/068377 2014-08-07 2015-06-25 Liquide de polissage pour polissage chimico-mécanique (cmp) et procédé de polissage l'utilisant WO2016021325A1 (fr)

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WO2011081109A1 (fr) * 2009-12-28 2011-07-07 日立化成工業株式会社 Liquide de polissage pour planarisation chimico-mécanique et procédé de polissage utilisant celui-ci
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WO2007038077A2 (fr) * 2005-09-26 2007-04-05 Cabot Microelectronics Corporation Compositions et procedes de polissage chimico-mecanique du tantale (cmp)
JP2008053371A (ja) * 2006-08-23 2008-03-06 Fujifilm Corp 半導体デバイスの研磨方法
WO2010067844A1 (fr) * 2008-12-11 2010-06-17 日立化成工業株式会社 Solution de polissage mécanochimique et procédé de polissage associé
WO2011081109A1 (fr) * 2009-12-28 2011-07-07 日立化成工業株式会社 Liquide de polissage pour planarisation chimico-mécanique et procédé de polissage utilisant celui-ci
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JP2013038211A (ja) * 2011-08-08 2013-02-21 Hitachi Chem Co Ltd Ｃｍｐ用研磨液及びこれを用いた研磨方法

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